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UDK 669+621.7+51/54(05)=163.42=111=112.2
1962.
god./year
1966. -
1978.
god./years
ISSN 0543-5846
METABK 45 (4) 269-352 (2006)
metalurgija
metallurgy
4
Osnivač časopisa - Društvo inženjera i tehničara Željezare Sisak
Founder of the Journal - Society of Engineers and Technitians of Steel Works Sisak
Suizdavači časopisa - Tehnološki Fakultet Sveučilišta u Zagrebu
/ Odjeli u Sisku
- Institut za metalurgiju Sisak
Co-Publishers of the Journal - Technological Faculty University of Zagreb
/ Departments in Sisak
- Institute for Metallurgy Sisak
45
METALURGIJA, vol. 45, br. 4, str. 269-352 Zagreb, listopad / prosinac (October / December) 2006.
th
year

UDK 669+621.7+51/54(05)=163.42=111=112.2
METALURGIJA
METALLURGY
Izdavač / Publisher: Hrvatsko metalurško društvo (HMD) - Croatian Metallurgical Society (CMS)
Adresa / Address: Berislavićeva 6, 10 000 Zagreb, Hrvatska / Croatia
Phone/Fax: + 385 1 619 86 89 (service), Phone: + 385 98 317 173
Internet / On line: http://pubwww.srce.hr/metalurg
(On line) ISSN 1334-2576, (CD-ROM) ISSN 1334-2584
Urednički odbor / Editorial Board:
ISSN 0543-5846
METABK 45 (4) 269-352 (2006)
METALURGIJA, vol. 45, br. 4, str. 269-352 Zagreb, listopad / prosinac (October / December) 2006.
I. ALFIREVIĆ, Zagreb - Croatia, I. BUDIĆ, Slavonski Brod - Croatia, R. DEŽELIĆ, Split - Croatia,
S. DOBATKIN, Moscow - Russia, H. HIEBLER, Leoben - Austria, M. HOLTZER, Krakow - Poland,
M. JENKO, Ljubljana - Slovenia, M. JURKOVIĆ, Rijeka - Croatia, R. KAWALLA, Freiberg - Germany,
I. MAMUZIĆ, Sisak - Croatia, L. MIHOK, Košice - Slovakia, V. ROUBIČEK, Ostrava - Czech,
A. VELIČKO, Dnipropetrovsk - Ukraine, F. VODOPIVEC, Ljubljana - Slovenia
Glavni i odgovorni urednik / Editor-in-chief: ILIJA MAMUZIĆ, ilija.mamuzic@public.carnet.hr
Lektori / Linguistic Advisers: B. RÖMER, hrvatski jezik/Croatian language, M. MIRILOVIĆ † , engleski i
njemački jezik / English and the German language
Tehnički urednici / Technical Editors: M. GOLJA, golja@siscia.simet.hr, J. BUTORAC
Internet / On line and CD-ROM: J. LOPATIČ, delta-computers@pu.t-com.hr, UDK / UDC: LJ. VUKOVIĆ
METALURGIJA izlazi u četiri broja godišnje. Godišnja pretplata 53 EUR (protuvrijednost u kunama).
Pretplatu prima Hrvatsko metalurško društvo.
METALLURGy is published quarterly. Subscription rates per year 53 EUR. Subscription should be paid to:
Croatian Metallurgical Society.
Komp. obrada / Comp. design: DELTA COMPUTERS d.o.o., Tisak / Print: LKDL-Print d.o.o.
Naklada / Print: 600 primjeraka / pieces. Rukopise ne vraćamo. / Manuscript are not returned.
Članci objavljeni u časopisu “Metalurgija” referiraju se u međunarodnim sekundarnim publikacijama i bazama podataka.
Articles published in the journal “METALLURGy” are indexed in the international secundary periodicals and databases:
- Science Citation Index (ISI-SCÍ)
- Research Alert (ISI)
- Metals Abstracts
- EI Compendex Plus
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- Chemical Abstracts
- Mechanical Engineering Abstracts
- Aluminium Industry Abstracts
- Dialog Sourceone (SM) Engineering
- Energy Science Technology
- Engineered Materials Abstracts
- Analytical Abstracts Online
- Chemical Engineering and Biotechnology Abstracts
- Referativny Zhurnal
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Fotopreslici članka mogu se dobiti u The Genuine Article service, Institute for Scientific Information 3501 Market Street
Philadelhia PA 19104 USA, i Copyright Clearance Center, ASM International; Materials Park, Ohio 44073-0002, USA.
Photocopies of the articles are available through The Genuine Article service, Institute for Scientific Information 3501
Market Street Philadelhia PA 19104 USA, and Copyright Clearance Center, ASM International; Materials Park, Ohio
44073-0002, USA.
Časopisu “Metalurgija” daje novčanu potporu: Ministarstvo znanosti, obrazovanja i športa Republike Hrvatske.
Journal “Metallurgy” is financially supported by: Ministry of Science, Education and Sports Republic of Croatia.

Content - Sadržaj
I. Mamuzić
Survey of 7 th International Symposium of Croatian Metallurgical Society
Pregled Sedmog međunarodnog Simpozija Hrvatskog metalurškog društva
I. Mamuzić
Minutes of the Meeting of the Editorial Board of Journal Metalurgija
Zapisnik sa sastanka Uredničkog odbora časopisa Metalurgija
Editorial Board of the Journal Metalurgija
Urednički odbor časopisa Metalurgija
Rule Book of the Journal Metalurgija
Pravilnik časopisa Metalurgija
Original Scientific Papers - Izvorni znanstveni radovi
M. Bizjak, L. Kosec, B. Kosec, I. Anžel
The Characterization of Phase Transformations in Rapidly
Solidified Al-Fe and Cu-Fe Alloys through Measurements of the Electrical Resistance and DSC
Karakterizacija faznih transformacija brzo skrutnutih Al-Fe
i Cu-Fe slitina pomoću mjerenja električne otpornosti i diferencijalno skenirajuće kalorimetrije
S. Bockus
A Study of the Microstructure and Mechanical Properties of Continuously Cast Iron Products
Studij mikrostrukture i mehaničkih svojstava kontinuirano lijevanih željeznih proizvoda
Preliminary Notes - Prethodna priopćenja
K. Jelšovská, B. Pandula
Nuclear Magnetic Resonance Spectral Function and Moments
for Proton Pairs in Powdered Paramagnetic Substances MnSO 4 ·H 2 O and NiSO 4 ·H 2 O
Funkcija spektra magnetne rezonancije
jezgre i momenata za parove u praškastim paramagnetnim tvarima MnSO 4 ·H 2 O i NiSO 4 ·H 2 O
D. Kudelas, R. Rybár, G. Fischer
Concept
of Accumulation System Configuration Enabling the Usage of Low-Potential Wind Energy
Koncept
konfiguracije akumulacijskog sustava koji omogućava uporabu nisko potencijalne energije vjetra
K. Kostúr
Regulation of the Heating Furnace in Tube Rolling Mill
Regulacija zagrijevne peći u valjaonici cijevi
M. Jurković, Z. Jurković, M. Mahmić
An Analysis and Modelling of Spinning Process without Wall-Thickness Reduction
Analiza i modeliranje procesa rotacijskog tiskanja bez stanjenja debljine stjenke
271
277
279
281
287
291
299
303
307

Review Papers - Pregledni radovi
S. V. Dobatkin, J. Zrník, I. Mamuzić
Nanostructures by Severe Plastic Deformation of Steels: Advantages and Problems
Nanostrukture dobivene intenzivnom plastičnom deformacijom: postignuća i poteškoće
J. Zrník, I. Mamuzić, S. V. Dobatkin
Recent Progress in High Strength Low Carbon Steels
Najnoviji napredak kod visokočvrstih niskougljičnih čelika
J. Dańko, M. Holtzer
The State of Art and Foresight of World’s Casting Production
Stanje i predmnijevanje svjetske proizvodnje odljevaka
Z. Keran, M. Skunca, M. Math
Finite Element Approach to Analysis of Axisymmetric Reverse Drawing Process
Pristup metodom
konačnih elemenata analizi procesa osnosimetričnog protusmjernog dubokog vučenja
P. Virdzek, K. Teplická
Progressive Methods in Design and their Application in Engineering Industry
Napredne metode u dizajnu i njihova primjena u strojarstvu
Review - Prikaz
I. Mamuzić
Popis recenzenata članaka objavljenih u časopisu Metalurgija u 2006. godini
List of Reviewers of the Articles Published in Journal Metallurgy in the Year 2006
313
323
333
341
347
352

I. MAMUZIĆ: SURVEY OF 7th I. MAMUZIĆ, President of Croatian INTERNATIONAL Metallurgycal Society
SYMPOSIUM OF CROATIAN METALLURgICAL SOCIETY
“Materials and Metallurgy”
http://pubwww.srce.hr/metalurg
7th International Symposium of Croatian Metallurgical Society “Materials and Metallurgy”
was held as a part of:
- 55th anniversary of the foundation of Croatian Metallurgical Society (from Society of Engineers and
Technician Steel Works Sisak 1952 y.);
- 45th anniversary of the foundation and publication of the Journal Metallurgy.
At the 7 th International Symposium of Croatian Metallurgical Society “Materials and Metallurgy”
the following countries had participated:
1. Austria
2. Belgium
3. Beloruss
4. Bosnia and Herzegovina
5. Brasil
6. Bulgaria
7. China
8. Croatia
9. Czech Republic
10. England
11. Egypt
12. France
Survey of 7 th International Symposium
of Croatian Metallurgical Society
S H M D
’2006.
Šibenik 2006, June 18 - 22
Solaris Holiday Resort, Croatia
13. germany
14. Hungary
15. India
16. Iran
17. Italy
18. Japan
19. Korea
20. Lithuania
21. Netherlands
22. Poland
23. Portugal
prof. Franc
Vodopivec
Opening Ceremony of Symposium
24. Romania
25. Russia
26. Serbia and Montenegro
27. Slovakia
28. Slovenia
29. South Africa
30. Spain
31. Sweden
32. Turkey
33. Ukraine
34. USA
The aim of this Symposium is to point out
all the possibilities of the materials and achievements in metallurgy.
prof. Ilija
Mamuzić
METALURGIJA 45 (2006) 4, 271-275 271

I. MAMUZIĆ: SURVEY OF 7 th INTERNATIONAL SYMPOSIUM OF CROATIAN METALLURgICAL SOCIETY
ORGANIZER
CROATIAN METALLURgICAL SOCIETY (CMS)
PATRONS
- European Steel Federation
- International Iron and Steel Institute
- Ministry of Science, Education and Sport Republic of
Croatia,
- Croatian Chamber of Economy
CO-ORGANIZERS
- Academy of Engineering Science of Ukraine
- University of Mining and Metallurgy, Faculty of Foundry
Enginering, Krakow
- University of Ljubljana, Faculty of Natural Science
and Engineering
- Baikov Institute of Metallurgy and Materials Science,
Russian Academy of Sciences, Moscow, Russia
- University of Sarajevo, Faculty for Metallurgy and
Materials Science, Zenica
- National Metallurgical Academy of Ukraine
- Technical University of Košice, Faculty of Metallurgy
- Technical University of Košice, Faculty of Mechanical
Engineering
- Technical University of Košice, Berg Faculty
- University of Zagreb, Faculty of Mechanical Engineering
and Naval Architecture
- University of Osijek, Faculty of Mechanical Engineering,
Slavonski Brod
- University of Rijeka, Technical Faculty
- VŠB Technical University of Ostrava
- University of Split, Faculty of Eleectrical Engineering,
Mechanical Engineering and Naval Architecture
- Institute of Metals and Technology, Ljubljana
- Institute of Materials Research of the Slovak Academy
of Sciences in Košice
- Steel Works Split
- Moscow State Steel and Alloys Institute
- Physico-Technical Institute National Academie of Science
Minsk
- Politehnica University of Bucharest
- Institute of Metallurgy “Kemal Kapetanović”, Zenica
- Pisarenko Institute of Problems of Strength NASU,
Kiev
- Dnepropetrovsk National University
- Iron Metallurgy, Prague
- Slovak University of Technology in Bratislava, Faculty
of Materials Science and Technology
CO-OPERATION WITH ORGANIZATIONS
- german Iron and Steel Institute (VDEh)
- ATS - Association Technique de la Siderurgie Francaise
- CENIM - Centro National de Investigaciones Metalurgicas
Spain
272
- ChSM - The Chinese Society for Metals China
- CRM - Centre de Recherches Metallurgiques Belgium
- Eisenhütte Österreich - The Austrian Society for Metallurgy
- Iron and Steel Society, USA
- ISIJ - The Iron and Steel Institute of Japan
- JERN - Jernkontoret, Sweden
- SRM Romanian Society for Metallurgy
- SITPH - Association of Polish Metallurgical Engineers
- HOOgOVENS The Netherlands
- SHS - Slovak Metallurgical Society
- Sociedade Portuguesa de Materiais
- MVAE - Association of Hungarian Steel Industry
- Steel Federation of the Czech Republic
- Union of Bulgarian Metallurgists
- IBS - Instituto Brasileiro de Siderurgia
- AIM - Associazione Italiana di Metallurgia
- The Japan Institute of Metals
SCIENTIFIC COMMITTEE
J. Alfirević Croatia H. Hiebler Austria
M. Jurković Croatia R. Kawalla Germany
L. Kosec Slovenia L. Mihok Slovakia
I. Mamuzić Croatia-President S. Nikulin Russia
P. Rybar Slovakia V. Trošćenko Ukraine
F. Vodopivec Slovenia-Vice Pres. A. Veličko Ukraine
HONOUR BOARD
A. Avramov Bulgaria P. Ayed France
M. Badida Slovakia I. Budić Croatia
J. Butterfild England J. Christmas Belgium
Z. Crnečki Croatia T. Ćurko Croatia
Ž. Domazet Croatia N. Domljanović Croatia
P. Fajfar Slovenia E. Ch. Frank S. Africa
J. Frenay Belgium P. Grgač Slovakia
H. Jäger Austria M. Jenko Slovenia
A. Karić B. and H. A. Kochubey Ukraine
I. Koštan Croatia C. Madaschi Italia
T. Mikac Craotia A. Normantyn England
M. Oruč B. and H. L. Parilak Slovakia
G. Parvu Romania I. Pučko Croatia
V. Roubiček Czech R. J. Sinay Slovakia
S. Sundberg Sweden P. Tardy Hungaria
R. Turk Slovenia F. A. Zaghla Egypt
Z. Zengyong China
ORGANIZING COMMITTEE
V. Živković Croatia-President
M. Buršak Slovakia-Vice President
D.Constantinescu Rom. S. Dobatkin Russia
A.I. GordienkoBeloruss V. Harčenko Ukraine
M. Holtzer Poland J. Kliber Czech R.
W. Lehnert Germany D. Novak Croatia
V. Šatoha Ukraine I. Vitez Croatia
METALURGIJA 45 (2006) 4, 271-275

I. MAMUZIĆ: SURVEY OF 7 th INTERNATIONAL SYMPOSIUM OF CROATIAN METALLURgICAL SOCIETY
TOPICS OF THE SYMPOSIUM WERE:
Materials
- New Materials
- Refractory Materials
- The Development
- Applications
- Physical Metallurgy
Metallurgy
- Process Metallurgy and Foundry
- Plastic Processing of Metals and Alloys
- Technologies
- Energetics
- Ecology in Metallurgy
- Quality Assurance and Quality Management
There were 475 reports, 799 authors and coauthors
registered for the seventh International Symposium of the
Croatian Metallurgical Society.
250 participants were present at the symposium. Symposium
activity took place through plenary lectures and
four sections (poster):
Plenary lectures................................................................... 12
Materials - Section “A”.................................................... 188
Process Metallurgy - Section “B”................................. 113
Plastic Processing - Section “C”................................... 69
Metallurgy and Related Topics - Section “D”.......... 93
For the plenary lectures research topics were selected
relating partly to the new materials and partly to the increase
of efficiency of metallurgical procedures, decrease of
required energy as well as improving of products quality
(Aluminium and High Strength Steels).
PLENARY LECTURES WERE:
Ľ. Mihok, P. Demeter, D. Baricová, K. Seilerová;
Faculty of Metallurgy Technical University of Košice,
Košice, Slovakia
Utilization of Ironmaking and Steelmaking Slags
W. Lehnert, R. Kawalla, D. Hübgen; Institut für Metallformung,
TU Bergakademie Freiberg, Germany
Herstellung von Hochwertigen
Bädern und Blechen aus Aluminiumwerkstoffen
M. Holtzer, J. Dańko; Faculty of Foundry Engineering
University of Mining and Metallurgy, Cracow, Poland
The State of
Art and Foresight of World’s Casting Production
S. Dobatkin, J. Zrnik*, I. Mamuzić**; Baikov Institute
of Metallurgy and Materials Science, Russian Academy of
Sciences, Moscow, Russia, *COMTES FHT, Plzen, Czech
Republic, **Faculty of Metallurgy University of Zagreb,
Sisak, Croatia
Nanostructures by Severe Plastic
Deformation of Steels: Advantages and Problems
J. Zrník, I. Mamuzić*, S. V. Dobatkin**; Comtes FHT,
Ltd., Plzen, Czech Republic, *Faculty of Metallurgy
University of Zagreb, Sisak, Croatia, **Moscow Institute
of Metallurgy and Materials Science, Russian Academy
of Sciences, Moscow, Russia
Recent Progress in High Strength Low Carbon Steels
F. Vodopivec, M. Jenko, J. Vojvodič - Tuma; Institute of
Metals and Technology, Ljubljana, Slovenia
Stability of
MC Carbide Particles Size in Creep Resisting Steels
O. Golovko, I. Mamuzić*, O. Grydin; National Metallurgical
Academy of Ukraine, Dnepropetrovsk, Ukraine,
*Faculty of Metallurgy University of Zagreb, Sisak,
Croatia
Method for Pocket Die Design on the Base of Numerical
Investigations of Aluminium Extrusion Process
Ya. V. Frolov, I. Mamuzić*, V. N. Danchenko; National
Metallurgical Academy of Ukraine, Dnepropetrovsk,
Ukraine, *Faculty of Metallurgy University of Zagreb,
Sisak, Croatia
The Heat Conditions of the Cold Pilger Rolling
Comprehensive outline of plenary reports (the 5 reports)
were published in the journal Metalurgija 45 (2006)
3, 147-184 as the article, other 3 plenary report will be
published in Metalurgija 45 (2006) 4. The summaries
of all lectures of 7th Symposium were published also in
Metalurgija 45 (2006) 3, 185-268.
Review of the lectures of Poster section were also published
in the Journal Metalurgija 45 (2006) 3:
- Review of the lectures of materials - section “A”, Metalurgija
45 (2006) 3, 191-194;
- Review of the lectures in process metallurgy - section
“B”, Metalurgija 45 (2006) 3, 221-224;
- Review of the lectures of plastic processing - section
“C”, Metalurgija 45 (2006) 3, 239-241;
- Review of the lectures of metallurgy and related topics
- section “D”, Metalurgija 45 (2006) 3, 253-255.
For this symposium the reports were prepared by the
authors and coauthors from various world universities,
institutes, academies and companies. It is to be emphasised
that the scientists from three Croatian universities (Zagreb,
Rijeka, Osijek) participated in the symposium.
In the time of 7 th Symposium was also held:
- meeting of International Editorial Board of the Journal
Metalurgija.
METALURGIJA 45 (2006) 4, 271-275 273

I. MAMUZIĆ: SURVEY OF 7 th INTERNATIONAL SYMPOSIUM OF CROATIAN METALLURgICAL SOCIETY
Based of the recommendation of Menaning Board
of Croatian Metallurgical Society, Editorial Board has
adopted:
- Rule Book on the Journal Metalurgija, the articles 5. and
10.;
- for the Editor - in - chief is reelected Acad. Prof. D. Sc.
I. Mamuzić instead of the period 2004-2008 y. for the
period 2006-2010 y.
More than 150 participants were included in a round
table session on the achievements, conclusions and closing
of the 7 th International symposium “Materials and
Metallurgy”.
In the discussions it was confirmed that the symposiums
organized by Croatian Metallurgical Society have
become traditional assembly of experts and scientists
of various profiles: metallurgists, geologists, physicists,
chemists, mechanical engineers etc.
With a demonstration of their best achievements they
all assist the metallurgy in Croatia to call the same attention
as it does otherwise in the world.
Subsequently we give some of the discussions on the
7 th Symposium following sections:
F. Vodopivec: Materials - Section “A”
188 summaries were selected for this section of the
symposium. It is, thus, understandable that in the range
of time given, it was not possible to prepare a real survey,
but only a short recording of main topics investigated and
of the purposes aimed. To obtain a better overview on the
content of this section of the symposium, the summaries
were classified in 16 groups on the base of the content, as
it could be understood from the summary. In most of the
summaries the accent is given to the goal and the method of
investigation and little information is given on the achieved
results. It is, thus, possible that a number of summaries
were not placed in the suited group.
A wide range of topics is presented: the formation of
microstructure by solidification, hot working, and heat
treatment, equilibrium and kinetics of phase formation,
tensile properties from crio over ambient to very high
temperature, fatigue strength by stressing and combined
stressing and fretting, creep rate at elevated and very high
temperature, calculation of phase equilibira and kinetics,
new and improved methods for the characterization,
improvement of technology, development of new alloys,
modelling of properties and processes, and calculation of
stresses by operation and of lifetime of parts of machines
and structures. In a number of summaries remarkable
achievements, theoretical and for application, are presented.
In this aspect, the average quality and relevance
for application of the achievements reported, although
274
only in summaries, are improved in comparison to the
previous symposium.
In the majority of summaries the alloy investigated are
different steels. In a number of summaries also results on
investigations on aluminium, titanium, magnesium, nickel,
zirconium, niobium, molybdenum, copper and heavy metals
alloys are reported. In most of the groups, the exception is
only the group “Aluminium and magnesium” alloys, investigations
on alloys with different base metal are included.
In comparison to the previous symposium, the number
of summaries reporting on investigations on amorphous
and nano grain size alloys and summaries with theoretical
calculations of equilibria and properties as well as modelling
are increased. Of equal importance is the considerable
number of summaries on calculation of the stressing of
parts in use and of degradation of properties due to surface
oxydation or microstructural processes at the temperature
of operation f.i. steels in parts of thermal power works.
The summaries were submitted mainly scientists from
universities and institutes. Authors from industrial companies
are found in 22 summaries, mostly in those submitted
from Slovenian scientists.
The number of authors of summaries is in the range
one to seven, mostly two or three.
The countries of origins of authors are: Croatia,
Ucraine, Russia, Bela Rus, Litva, Polonia, Slovakia, Czech
Republik, Slovenia, Romania, Turkey, Spain and Bosnia-
Herzegovina. Authors from different countries are found
in a small number of summaries, also.
These groups are:
- processing of ferrous and non ferrous alloys;
- powder metallurgy;
- physical metallurgy;
- mechanical properties;
- wet and dry corrosion, corrosion resistance;
- surface technology;
- computer calculation and modelling;
- composites;
- methodology of investigation;
- aluminium and magnesium alloys;
- non ferrous alloys;
- welding, microstructure and properties of welds;
- nano and amorphous alloys;
- application and degradation in service;
- miscellaneous;
- non metallic’s.
Ľ. Mihok: Process Metallurgy - Section “B”
The section contained 113 papers. According to their
scope they were subdivided into fourteen groups:
- coke production;
- sintering of fine materials;
- pig iron production;
METALURGIJA 45 (2006) 4, 271-275

I. MAMUZIĆ: SURVEY OF 7 th INTERNATIONAL SYMPOSIUM OF CROATIAN METALLURgICAL SOCIETY
- steel production;
- non - ferrous metals;
- foundry metallurgy;
- refractories;
- production of ferroalloys;
- thermal energetics;
- environment aspects;
- smelting reduction;
- welding;
- inorganic materials;
- miscellaneous.
In same cases it was difficult to include the contribution
into specific group as it contained information related
to more fields.
The Symposium presented many new information both
to scientists and factory staff members and we hope that
this high level will be kept in the future. Our thanks are
directed to organizers.
P. Fajfar: Plastic processing - Section “C”
69 contributions have been received for Section C on
Plastic processing of materials. According to their scope
they were subdivided into 9 groups:
- plastic deformation;
- plate and shape rolling;
- extrusion;
- wire drawing;
- tubes production;
- sheet metal forming;
- reheating process;
- modernization;
- miscellaneous.
The most numerous are the contributions of the scientists
from Croatia, Poland, Slovenia, Russia, Slovakia, Bosnia
and Herzegovina, Czech Republic, germany, Turkey and
Romania. Survey of the authors shows that nearly one fifth
of the contributions are the result of co-operation between
research institutes from different countries. The most evident
is co-operation of Croatian scientists with colleagues from
Ukraine, Slovenia, Slovakia and Bosnia and Herzegovina.
Most contributions have been sent by research institutions
(59), 12 of them are result of co-operation between research
institutions and industry and only 4 of them have been written
by authors who work only in industry.
The variety topics and different ways of the solutions
of problems treated in papers presented is a confirmation of
vitality of metallurgical science in Europe and in Croatia.
From this point of view the organizer of 7 th International
Symposium of Croatian Metallurgical Society may be
satisfied.
P. Fajfar: Metallurgy and Related Topics - Section “D”
93 contributions have been received for Section D
on Metallurgy and related topics. The most numerous are
the contributions of the scientists from Slovakia, Ukraine,
Croatia, Poland, Russia and s. o. With the exception of four
contributions presented from enterprises, the rest of them
are results of scientific work in research and educational
institutes.
Topics of section D are:
- marketing and management in metallurgical and mining
enterprises;
- mineral engineering;
- energy sources;
- environment pollution;
- heat transfer;
- science on materials;
- computer science;
- other applications.
Although the papers presented in the section “Metallurgy
and related topics” are very heterogeneous according
to scientific discipline, quality and subject matter of most
of the papers justify their including into the program of the
symposium. Their usefulness for the branch of metall-urgy
can be seen in the possibility of comparison in meth-ods
and techniques used in applied research and resolving
certain professional problems. First, this refers to mineral
dressing and other disciplines that it leans on. Secondly,
this refers to computer application for resolving technological
problems. Thus, it can be concluded that including
papers from other disciplines adjacent to metallurgy and
wider into the program of the symposium is useful and
stimulating in interdisciplinary terms for future.
Based on the analysis and evaluation of the subject matter
of the symposium, the symposium has been appraised
positively and it has been acknowledged that it has its place
in the international exchange of knowledge.
It is reasonable to conclude that the demonstrated results
of scientific and professional investigation accompanied
by the complete and quality manifestations, especially
discussions at the round table prove that the organizing of
the 7 th International symposium of Croatian Metallurgical
Society “Materials and Metallurgy” in Šibenik 2006, June
18 - 22 was justified. Especially has to be emphasized that
the participants will keep wonderful memories of Šibenik
and Solaris Hotels.
Based on the agreement of Meeting of World Metallurgical
Societys, Düsseldorf, November 2005 y. and the
conclusion of the round table the next 8 th International
Symposium of Croatian Metallurgical Society “Materials
and Metallurgy” will be held 2008 - June 21 - 25.
METALURGIJA 45 (2006) 4, 271-275 275

8 th INTERNATIONAL SYMPOSIUM
OF
CROATIAN METALLURGICAL SOCIETY
All the informations please see:
http://pubwww.srce.hr/metalurg
S H M D ’2008.
MATERIALS AND METALLURGY
CALL FOR PARTICIPATION
The 8 th Symposium is also in the “Calendar of International Conferences for 2008”
(Meeting of World Metallurgical Societys, Düsseldorf, November 2005).
CROATIA, June, 21 - 25, 2008

I. I. mamuzIć, mamuzIć: Editor-in-chief mINuTES of Journal ThE mEETINg Metalurgija of ThE EdITorIal I. mamuzIć, Board glavni of i JourNal odgovorni urednik Metalurgija časopisa Metalurgija
M I N U T E S
of the meeting of the Editorial Board of Journal
Metalurgija, held on 19 June 2006 in the hotel Ivan
- Solaris with the beginning at 7 Pm.
Present: I. alfirević, l. mihok, f. Vodopivec, S. dobatkin,
I. mamuzić, m. holtzer, V. roubiček, I. Vitez
(deputy for I. Budić), d. hübgen (deputy for r.
Kawalla), d. Živković (deputy for r. deželić).
absent: m. Jurković, m. Jenko, h. hiebler, a. Veličko
(excused).
The Editor-in-chief, I. mamuzić opened the meeting
and proposed the following
AGENDA
1. recommendations of managing Board of Croatian
metallurgical Society (CmS)-Please ENCl.
2. opinion on the Journal Metalurgija and recommendations
for the future work.
3. other business.
The agenda was unanimously accepted.
Re. 1. The members of the Editorial Board have received
earlier the material for this point of agenda, i.e.:
at its 12 th session of 6 april 2006 held on the occasion
of the 45th anniversary of the appearance of metallurgy
Journal, after a conducted discussion the managing Board
of the Croatian metallurgical Society (CmS) made for the
Editorial Board of metallurgy Journal the following
rECommENdaTIoNS
a. CmS President and Editor-in Chief of metallurgy Journal
are to be elected for a 4-year term. Earlier these elections
were held at 2-year intervals. In view of this, the
managing Board recommends to the Editorial Board to
re-elect the incumbent Editor-in Chief mr. I. mamuzić
(2004-2008) for the term 2006-2010.
B. The ministry of Science, Education and Sports has
passed the ordinance on the Publication of Journals
whereby criteria for subsidising the publication of journals
are tightened. This particularly applies to reviewing
and the composition of editorial boards.
- In this regard, the rules of Procedure of metallurgy
Journal shall be amended in article 5 by adding: “with
at least one reelection”.
- The following text shall be added to article 10: “In case
of their absence, the members of the Editorial Board
can send their approvals or disapprovals of particular
items on the agenda or else designate a proxy. a member
may not be absent from more than 4 meetings in
succession”.
Z A P I S N I K
sa sastanka uredničkog odbora časopisa
Metalurgija, održanog 19.06.2006. u hotelu Ivan -
Solaris sa početkom u 19 00 .
Nazočni: I. alfirević, l. mihok, f. Vodopivec, S. dobatkin,
I. mamuzić, m. holtzer, V. roubiček, I. Vitez
(zamjena za I. Budić), d. hübgen (zamjena za r.
Kawalla), d. Živković (zamjena za r. deželić).
Izočni: m. Jurković, m. Jenko, h. hiebler, a. Veličko
(opravdano).
Sastanak je otvorio glavni i odgovorni urednik I.
mamuzić te predložio slijedeći
DNEVNI RED
1. Preporuke upravnog odbora hrvatskog metalurškog
društva.
2. mišljenje o časopisu Metalurgija i preporuke za budući
rad.
3. razno.
dnevni red je jednoglasno prihvaćen.
Ad. 1. Članovi uredničkog odbora pohvalno su ranije
dobili materijal za ovu točku dnevnog reda, tj.:
Povodom 45. obljetnice tiskanja časopisa metalurgija,
nakon provedene rasprave, upravni odbor hrvatskog
metalurškog društva (hmd) na svojoj 12. sjednici
održanoj dana 06.04.2006. goidne donio je uredničkom
odboru časopisa Metalurgija sljedeće
PrEPoruKE
a) Izbor predsjednika hmd-a te glavnog i odgovornog
urednika časopisa metalurgija je na 4 godine. ovi izbori
su se dosad odvijali u razlici 2 godine. glede toga
upravni odbor predlaže upravnom odboru na sljedećoj
sjednici u 2006. godini reizabrati glavnog i odgovornog
urednika I. mamuzić (2004.-2008.) na mandatno razdoblje
2006.-2010. godine.
B) ministarstvo znanosti, obrazovanja i športa donijelo je
Pravilnik o izdavanju časopisa, kojim su pooštreni uvjeti
dodjele novčane potpore ministarstva za tisak časopisa.
Posebice se to odnosi na recenzije i sastav uredničkog
odbora.
- glede toga u Pravilnik o načinu rada časopisa Metalurgija,
u točki 5. je dopuna: “barem s jednim reizborom“.
- u točki 10. dodaje se tekst: “u slučaju izočnosti,
članovi uredničkog odbora mogu pismeno dostaviti
svoje pozitivne ili negativne odluke na točke dnevnog
reda ili odrediti zamjenika. maksimalna dozvoljena
izočnost uzastopno je na 4 sastanka“.
METALURGIJA 45 (2006) 4, 277-278 277

I. mamuzIć: mINuTES of ThE mEETINg of ThE EdITorIal Board of JourNal Metalurgija
a. Based on the past results of the Jornal Metalurgija, longterm
successful voluntary work of the Editor-in-chief,
Prof. I. mamuzić, on the proposal of Prof. I. alfirevića
was unanimously taken the following
278
DECESION
for the Editor-in-chief is elected Prof. I. mamuzić in
the period 2006-2010.
The decesion comes to force immediately.
B. after of the discussion, the Editorial Board of the Journal
Metalurgija unanimously accepted the amendments
fot the atricles 5. and 10.
Re. 2. The members of the Editorial Board appraised past
activity of the Journal:
- being included in tertiary and secondary publications
and databases,
- regularity in publishing (each issue is printed several
months before dead-line),
- journal equipments, consistency of pictures, etc.
- Editorial Board member form Croatia reported some
mistakes in translations (English - Croatian and the
other way round). however, we will try to minimise
these-kind mistakes in future work,
Journal Metalurgija covers technical as well as other
areas, consequently such a broad range of different texts
is difficult to revise, i.e. translate (English - german -
Croatian languages).
Re. 3. The next meeting of the International Editorial
Board (in accordance with the article 10. of the rule
Book) is proposed to be held during the 8 th Symposium
of Croatian metallurgical Society (21 - 25 June 2008).
The meting ended at 9 Pm.
The members of
Editorial Board on the
meeting 11 June 2006,
from the left, stend: d.
Živković (deputy for r.
deželić), m. holtzer, I.
mamuzić, l. mihok, V.
roubiček, S. dobatkin;
sit: I. Vitez (deputy for
I. Budić), I. alfirević,
d. hübgen (deputy for
r. Kawalla), f. Vodopivec
a) Na temelju dosadašnjih rezultata časopisa Metalurgija,
dugogodišnjeg uspješnog dragovoljačkog rada
glavnog i odgovornog urednika Prof. I. mamuzića, na
prijedlog Prof. I. alfirevića jednoglasno je donesena,
sukladno članku 2. Pravilnika,
ODLUKA
za glavnog i odgovornog urednika izabire se Prof. I.
mamuzić u razdoblju 2006. - 2010. godine.
odluka stupa na snagu odmah.
B) Nakon provedene rasprave jednoglasno su prihvaćene
izmjene - dopune u točkama 5. i 10., koje će biti
ugrađene u Pravilnik o radu časopisa Metalurgija.
Ad. 2. Članovi uredničkog odbora pohvalno su se izrazili
o dosadašnjoj djelatnosti časopisa:
- uključenost u tercijarne i sekundarne publikacije i
baze podataka;
- redovitost tiskanja (svaki broj se tiska nekoliko mjeseci
pred termin važenja);
- opremljenost časopisa, ujednačenost izrade svih slika,
itd.
- hrvatski članovi uredništva su naveli manje greške u
prijevodima (engleski - hrvatski i obrnuto), što će se
nastojati poboljšati.
Časopis Metalurgija pokriva tehnička i ostala područja
pa je tako različite tekstove teško lektorirati, odnosno
prevoditi (engleski, njemačji, hrvatski jezik).
Ad. 3. Idući sastanak međunarodnog uredničkog odbora
(sukladno članku 10. Pravilnika) predložen je tijekom
8. simpozija hrvatskog metalurškog društva (21. -
25.06.2008. godine).
Sastanak je završio u 21 00 .
Članovi uredničkog
odbora na sastanku
11.06.2006., slijeva,
stoje: d. Živković (zamjena
za r. deželić),
m. holtzer, I. mamuzić,
l. mihok, V. roubiček,
S. dobatkin; sjede: I.
Vitez (zamjena za I.
Budić), I. alfirević, d.
d. hübgen (zamjena za
r. Kawalla), f. Vodopivec
METALURGIJA 45 (2006) 4, 277-278

Editorial EdIToRIAL Board BoARd of the of Journal ThE JoURnAL MetalurgijaMetalurgija:
RULE Urednički Book odbor of ThE časopisa JoURnAL Metalurgija Metalurgija
RulE Book of thE
JouRnal Metalurgija
amendments to the Rule Book of the
Journal Metalurgija
Based on the Rule Book of Croatian Metallurgical Society,
Article 21., Paragraph 2., 3., Editorial Board of the Journal Metalurgija
on its session held on 19 June 2006 has adopted
RulE Book
on the Journal Metalurgija
1. Starting point for this “Rule Book” is the Rule Book on the
Journal Metalurgija that was adopted by Publishing Council of
the journal Metalurgija on 7 May 1991. Little modifications
were necessary because the Act on Publishing Activities in
the Republic of Croatia anticipated no publishing councils
for single Journals. Consequently, the Publishing Council of
Journal Metalurgija suspended its activities in 1993 (List of
members of the Publishing Council was no longer published
in Metalurgija (1993) 3). The competences and obligations
of Publishing Council are transferred to Editorial Board or
Publisher (i.e. co-publisher) or founder of the Journal.
2. The term of office of the Editor-in-chief is four years. Editorin-chief
can be re-elected by Editorial Board. The number of
terms is not limited.
3. Editor-in-chief is authorized to choose, appoint and discharge
the members of Editorial Board, deputy Editor-in-chief,
Technical Editors, Linguistic Advisers (Croatian, English and
German language) and other assistants.
4. Editor-in-chief, with the purpose to raise the level of the
Journal Metalurgija to the worldwide level, select as well
the members of Editorial Board in Croatia as abroad. The
International Editorial Board may count 15 members at most
(including Editor-in-chief).
5. The members of the Editorial Board need to be well-known
scientists with their works published in recognized world
periodicals, by their vocation at least senior research fellow
(full professor) with at least one re-election and must be able to
speak two world languages (one of them must be English).
6. The members of Editorial Board cover special scientific
(professional) fields in metallurgy as follows:
- physical metallurgy and materials,
- processing metallurgy (non-ferrous and ferrous metallurgy),
- mechanical metallurgy (manufacturing, energy supply, ecology
etc.),
- related (adjoing) professions:
mechanical engineering, chemistry, physics etc.
7. The members of Editorial Board are not representatives of
legal persons of their firms but they are physical persons as
prominent scientists from inland and foreign countries.
8. In the International Editorial Board - for the reason of reducing
editorial costs - each member of Editorial Board will in his
scientific (professional) field independently give suggestions
for a reviewer (or personally make such reviews but not more
than 5 per year).
Pravilnik časoPisa Metalurgija
izmjene i dopune Pravilnika časopisa Metalurgija
na temelju Statuta hrvatskog metalurškog društva (hMd)
članak 21., Stavak 2., 3., Urednički odbor časopisa Metalurgija
na sjednici održanoj dana 19.06.2006. godine potvrđuje
PRaVIlnIk
Časopisa Metalurgija
1. Izvorište za ovaj “Pravilnik” je Pravilnik časopisa Metalurgija
donešen na Izdavačkom savjetu časopisa Metalurgija dana
07.05.1991. godine. Manje izmjene su bile potrebite jer Zakon
o izdavačkoj djelatnosti Republike Hrvatske nije više predmnijevao
Izdavačke savjete pojedinih časopisa, to je i Izdavački
Savjet časopisa Metalurgija prestao djelovati u 1993. godini
(Lista Izdavačkog Savjeta nije više objavljena u Metalurgiji
(1993.) 3.). Ovlasti i zaduženja Izdavačkog Savjeta se prenose
ili na Urednički odbor, ili izdavača (odnosno suizdavača) ili
osnivača časopisa.
2. Zvanični mandat glavnog i odgovornog urednika je četiri
godine. Glavni i odgovorni urednik može biti iznovice biran
po Uredničkom odboru. Broj mandata nije ograničen.
3. Glavni i odgovorni urednik je ovlašten za izbor, imenovanje i
razrješavanje članova Uredničkog odbora, zamjenika glavnog
i odgovornog urednika, tehničkih urednika, lektora (hrvatski,
engleski i njemački jezik) i ostalih pomoćnika.
4. Glavni i odgovorni urednik u svrhu podizanja časopisa Metalurgija
na svjetsku razinu, odabire i članove Uredničkog
odbora iz inozemstva i tuzemstva. Međunarodni Urednički
odbor može imati najviše 15 članova (računajući i glavnog
- odgovornog urednika).
5. Članovi Uredničkog odbora trebaju biti priznati znanstvenici s
objavljenim radovima u prestižnim časopisima u svijetu, najmanje
u zvanju znanstvenog savjetnika (redovitoga profesora)
barem s jednim reizborom uz poznavanje dva svjetska jezika
(jedan obvezatan engleski).
6. Članovi Uredničkog odbora pokrivaju određena znanstvena
(stručna) područja iz metalurgije i to:
- fizičke metalurgije i materijala,
- procesne metalurgije (obojena i crna metalurgija),
- mehaničke metalurgije (preradba, energetika, ekologija itd.),
- srodne (dodirne) struke: strojarstvo, kemija, fizika, itd.
7. Članovi Uredničkog odbora nisu zastupnici pravnih osoba gdje
su zaposlenici nego su fizičke osobe, kao istaknuti znanstvenici
iz tuzemstva i inozemstva.
8. Uspostavom međunarodnog Uredničkog odbora, a zbog smanjenja
troškova uređivanja, svaki član Uredničkog odbora će
sa svog znanstvenog (stručnog) područja davati samostalno
prijedlog recenzenta (ili osobno napraviti recenziju, ali ne više
od pet u godini).
9. Ovlašćuje se uži dio Uredničkog odbora (glavni i odgovorni
urednik, te tehnički suradnici) zaprimiti članke, te ih proslijediti
članovima Uredničkog odbora za izbor recenzenta (iz
članka 8.). Sa sastanka užeg dijela Uredničkog odbora vodi se
zapisnik, a sastanci se održavaju najmanje 4 puta godišnje.
METALURGIJA 45 (2006) 4, 279-280 279

EdIToRIAL BoARd of ThE JoURnAL Metalurgija: RULE Book of ThE JoURnAL Metalurgija
9. The narrow part of the Editorial Board (Editor-in-chief and
Technical Editors) is empowered to overtake the articles and
deliver them to the members of Editorial Board to choose
reviewer (according to the Article 8). At the session of the
narrow part of the Editorial Board a minutes is taken down
and the sessions are held 4 times a year at least.
10. Each member of the International Editorial Board must receive
every issue of the Journal Metalurgija so that he may send his
written remarks if wished and necessary. In this way, in view
to reducing financial costs, the session of the International
Editorial Board may be held at least once in two years. In
case of their absence, the members of the Editorial Board can
sand their approvals or disapprovals of particular items on the
agenda or else designate a proxy. A member may not be absent
from more than 4 meeting in succession. on these sessions
minutes are taken. At the same time, the members of Editorial
Board in inland and in foreigin countries are completely
equalized in their rights and obligations.
11. The term of office of all the members of Editorial Board,
Technical Editors and others is not limited. It depends only
upon the results and assistance in the publishing of the journal
Metalurgija, which is appraised by the Editor-in-chief (s.
Article no. 3. of this Rule Book). Every appointed member
may submit his resignation if he wishes. The Editor-in-chief is
recomended to invite such a member to talks and explanation
(if the members in resignation responds to the written invitation
of the Editor-in-chief).
12. The circle of foreign authors must be expanded. In order to
increase the level of the Journal to the worldwide level, the
papers from abroad are desirable to be written predominantly
in English.
13. Publishers (i. e. co-publishers or founders) provide the necessary
financial assets for the publishing of the journal Metalurgija.
The Editor-in-chief is charged with financial operations
of the Journal Metalurgija. Specially, he provides - if possible
- additional financial assets (he submits written requirements
to many competitions, look for donors, organizes various
conferences). By his own choice he appoints a phototypesetter,
printing etc.
14. Membership in Editorial Board is voluntery. The authors are
not paid equally. The assets have to be provided for other
staff members (Editor-in-chief, Technical Editors, Linguistic
advisers and other ancillary staff). The value of these works
and tasks is determined on the level of previous Rule Book
for the related Journal “Strojarstvo” which, being within
everybody’s reach, is not written herewith (eg. the salary
of the Editor-in-chief is leveled with the salary of assistant
professor, the salary of Technical Editor is 30 % level of the
salary of assistant professor and so on).
15. finances of the Journal Metalurgija are managed on the bank
account of the publisher or founder with a separate sub-account.
The cosignatory of financial documentation for the
Journal Metalurgija must be the Editor-in-chief. The Editorin-chief
is entitled to choose the drawing account on which
the finances of the Journal Metalurgija (publisher or founder)
are conducted.
16. The Rule Book may be modificated in the same way as it was
adopted. This Rule Book comes into force immediately.
280
10. Svaki član međunarodnog Uredničkog odbora obvezatno dobija
svaki tiskani broj časopisa Metalurgija, te po želji i potrebi
dostavlja možebitno svoje primjedbe i to u pismenom obliku.
Na ovaj način, a u nakani smanjenja financijskih troškova,
sastanci međunarodnog Uredničkog odbora mogu se održavati
najmanje jedanput u dvije godine. U slučaju izočnosi, članovi
Uredničkog odbora mogu pismeno dostaviti svoje pozitivne ili
negativne odluke na točke Dnevnog reda ili odrediti zamjenika.
Maksimalna dozvoljena izočnosto je uzastopno na 4 sastanka.
Sa sastanka se vodi zapisnik. Istodobno su po pravima i obvezama
u cjelosti izjednačeni članovi Uredničkog odbora iz
inozemstva i tuzemstva.
11. Mandat svih članova Uredničkog odbora, tehničkih urednika
i ostalih nije ograničen, a ovisno o rezultatima i pomoći u
izdavanju časopisa Metalurgija, što procjenjuje glavni i
odgovorni urednik (vidjeti članak 3. ovog Pravilnika). Svi
imenovani članovi mogu po želji i dati ostavke na svoje
članstvo. Preporuča se glavnom i odgovornom uredniku
pozvati tog člana na dogovor i pojašnjenja (ukoliko se član
u ostavci odazove pismenom pozivu glavnog i odgovornog
urednika).
12. obvezatno je proširiti krug autora iz inozemstva. Zbog
podizanja razine časopisa u svijetu poželjno je članke iz
inozemstva pisati pretežito na engleskom jeziku.
13. Izdavači (odnosno suizdavači ili osnivači) osiguravaju potrebita
financijska sredstva za cjelovito izdavanje časopisa Metalurgija.
Glavni i odgovorni urednik je zadužen za financijsko
poslovanje časopisa Metalurgija. Posebice po mogućnosti
osigurava dodatna novčana sredstva (dostavlja pismene
zahtjeve na razne Natječaje, traži donatore, orgnizira različite
konferencije). Odabire po vlastitom izboru izvođača fotosloga,
tisak itd.
14. Članstvo u Uredničkom odboru je dragovoljačko. Autori se
jednako ne plaćaju. Sredstva treba osigurati za ostale djelatnike
(glavnog i odgovornog urednika, tehničke urednike, lektore i
ostale pomoćne poslove). Vrijednost ovih poslova i zadataka
se utvrđuje na razini već ranije donešenog Pravilnika za srodni
časopis “Strojarstvo”, a koji je dostupan javnosti i ovdje se ne
prepisuje (na pr. plaća glavnog odgovornog urednika na razini
plaće sveučilišnog docenta, tehničkog urednika na razini 30
% plaće docenta itd).
15. Financijsko poslovanje časopisa Metalurgija vodi se na žiro
računu izdavača ili osnivača i to na posebnom podračunu.
Supotpisnik financijske dokumentacije za časopis Metalurgija
je obvezatno glavni i odgovorni urednik. Glavni i odgovorni
urednik ima pravo izbora žiro računa gdje će se voditi financijsko
poslovanje časopisa Metalurgija (ili kod izdavača ili
osnivača).
16. Pravilnik se može mijenjati jednakim postupkom kako je i
donešen. ovaj pravilnik stupa na snagu odmah.
METALURGIJA 45 (2006) 4, 279-280

M. M. BizjAk, BIzJAk L. et kosec, al.: ThE B. ChARACTERIzATIon kosec, i. AnžeL of PhAsE TRAnsfoRMATIons In RAPIdLy soLIdIfIEd Issn 0543-5846 ...
METABk 45 (4) 281-286 (2006)
UdC - Udk 669.15:621.317.4:536.6=111
The CharaCTerizaTion of Phase
TransformaTions in raPidly solidified al-fe and Cu-fe alloys
Through measuremenTs of The eleCTriCal resisTanCe and dsC
M. Bizjak, L. kosec, B. kosec, faculty of natural sciences and Engineering
University of Ljubljana, slovenia, i. Anžel, Faculty of Mechanical
Engineering University of Maribor, slovenia
Received - Primljeno: 2005-10-21
Accepted - Prihvaćeno: 2006-02-20
Original Scientific Paper - Izvorni znanstveni rad
For the characterization of the phase transformations in the alloys during the heat treatment the various methods
of the thermal analyses are available. Thermogravimetry, differential thermal analysis (DTA) and the differential
scanning calorimetry (DSC) are the most frequently used methods. The phase transformations proceed in two
stages, i.e. nucleation and the growth of the new phase. Both processes are closely linked with the movement of
the atoms. Rapidly solidified alloys often contain the elements with the low diffusivity. During the transition from
the unstable to the stable state the energy changes are small, therefore the characterization of the changes by
DTA, DSC is very difficult and could not be measured. During the heat treatment the phase transformations of
the rapidly solidified alloys of Al-Fe and Cu-Fe were successfully detected by the simultaneous measurements of
the electrical resistance, and were compared by the DSC method. By determination of the temperature regions
of the phase transitions or temperatures, where the dynamics of the changes is maximal, the samples were
heat treated and analysed by the scanning and transmission electron microscopy respectively.
Key words: rapidly solidified Al-Fe and Cu-Fe alloys, transformations, electrical resistance, differential scanning
calorimetry
Karakterizacija faznih transformacija brzo skrutnutih Al-Fe i Cu-Fe slitina pomoću mjerenja električne
otpornosti i diferencijalno skenirajuće kalorimetrije. Za karakterizaciju faznih transformacija slitina tijekom
toplinske obrade koriste se različite metode toplinske analize (DTA). Najčešće korištene metode su termogravimetrija,
diferencijalno toplinska analiza i diferencijalna skenirajuća kalorimetrija (DSK). Fazne se transformacije
odvijaju u dva stadija, tj. nukleacija i rast nove faze. Oba su procesa usko povezana s gibanjem atoma.
Brzo skrutnute slitine često sadrže elemente niske difuznosti. Tijekom prijelaza iz nestabilnog u stabilno stanje
energetske su promjene male i zato je karakterizacija promjena pomoću DTA i DSK veoma teška i ne mjerljiva.
Za vrijeme toplinske obrade mikrostrukturne transformacije brzo skrutnutih Al-Fe i Cu-Fe slitina uspješno su
detektirane istodobnim mjerenjem električnog otpora. Određivanjem temperaturnih područja faznih prijelaza ili
temperatura, gdje su dinamičke promjene maksimalne, uzorci su toplinski obrađeni i analizirani pomoću skener
i transmisijske elektronske mikroskopije.
Ključne riječi: brzo skrutnute Al-Fe i Cu-Fe slitine, transformacije, električna otpornost, diferencijalna skenirajuća
kalorimetrija
inTroduCTion
Many methods exist for the analysis and for the characterization
of the phase transformations of the rapidly
solidified alloys, which are also described in the literature
[1 - 3]. frequently used methods are the scanning electron
microscopy (sEM), transmission electron microscopy
(TEM), and the diffraction of the X - rays (XRd). All the
results should be in mutual agreement. for determination
of the phase transformations of the samples during the heat
treatment the different methods of the thermal analysis are
available, by which the physical properties of the substances
and the reaction products are examined as the function of
the temperature. Among those the thermography (TM), dTA
and dsC are the most frequently used methods. At the most
analytical procedures the phase transformations at the constant
temperature are examined, and less frequently after the
given involved program. The results of the measurements of
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the heat excited processes are the heating and cooling curves
as the function of the temperature. The kinetics parameters
established by the measurements are detailed in the book
of Chena and kirsha [4].
The phase transformations are possible only, if the free
energy change of the system is lowered. While the possible
phase transformations are established by thermodynamics,
their progress to form the microstructure depends by
the kinetics. The phase transformations proceed in two
stages, i.e. nucleation and the growth of the new phase.
Both processes are closely linked with the movement of
the atoms. The parallel development of the powder metallurgy
and the procedures of the rapidly solidification enable
the manufacture of the new alloys [5]. Rapidly solidified
alloys often contain the elements, which have the small
diffusivity, so that the changes of the reaction energies for
the transition from unstable into the stable state are low.
These phenomena intensify difficulties to investigate the
alloys by dsC and dTA.
eXPerimenTal WorK
Making of the rapidly solidified ribbons
Alloys of Al-fe (4,7 mas. % fe) and Cu-fe (4,4 mas.
% Fe) were remelted in the vacuum induction furnace, and
then cast into the metal mould of the diameter of 45 mm.
Thus made alloys were inserted into the graphite crucible.
The component parts of the graphite crucible are shown
in Figure 1.a. The rapidly solidified ribbons were made in
the pilot plant shown in Figure 1.b [6, 7].
Both alloys were inductively remelted in argon at the
pressure of 350 mbar. Under the argon overpressure in the
graphite crucible the molten alloy was sprayed through the
nozzle on the rotating disc of the copper alloy. The heel was
formed at the contact of the melt with the roll as the origin of
282
the formation of the continuously rapidly solidified ribbons.
The chemical compositions and the dimensions of ribbons
are presented in Table 1.
differential scanning calorimetry
Microstructural transformations of the rapidly solidified
alloys were examined by Dsc at the constant heating rate
of 5 °C/min. The differences of the thermoelectric voltages
between the investigated and the reference samples were
measured. The results of measurements were presented
on the heating curve, which introduce the dependence
between the consumed and the liberated energy regarding
to the temperature. The tests were performed on the
sTA 449 device of the netsch firm, which enable precise
investigation of the physical and chemical processes. The
results of the Dsc were compared with the results obtained
by measurements of the electrical resistance of ribbons of
the rapidly solidified alloy.
measurement of
the electrical resistance
for the simultaneous measurement
of the electrical resistance
the four-probe d.C.
method was used [8 - 10]. it was
applied on ribbons of 200 to 250
mm length, which was coiled up
on the 50 mm long ceramic tube.
Reliability and repeatability of
measurements were assured by
the special girder construction
for the samples with the tungsten
and platinum lines (figure 2.).
during the heat treatment of the
samples the electrical resistance
was measured in the tube furnace
and the temperature by the thermocouple of Pt - Pt 10 %
Rh, which was attached to the sample respectively. The
temperature heating program of the furnace was controlled
by the eurotherm control system. The thermocouple with the
reverse loop and thyristor were regulating that system.
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The voltage drop on the sample, which was heated by
the constant rate, was measured at the constant electric
current by the amplifier with the closed loop (Figure 3.).
The computer collected the temperature data through
the rectifier and the voltage drops through the GPiB
intermediate every 5 seconds. The electrical resistance
was simultaneously calculated at known electric current
through the sample and measured voltage drop. After the
completed measurement of the electrical resistance at the
heating rate of 5 °c the samples were quenched to preserve
the microstructure. By establishing the temperature regions
of the phase transformations the samples were suitable heat
treated and analysed by sEM and TEM.
resulTs and disCussion
microstructure of
rapidly solidified Al-Fe 4,7 mas. % alloy
Rapidly solidified ribbons of the aluminium alloys with
various iron content have different microstructure through
the thickness. Two zones named zone A and B after H. jones
are characteristic for the microstructure [11, 12]. zone A
with the nano-cell is in contact to the disc, and the zone B
is extending to the upper free surface (figure 4.a).
Primary α Al phase of the observed region is forming
the interior of the cells, and the excess iron quantity is
precipitating on their walls. in zone B the precipitates of
the high-temperature phase are seen, which are located in
the middle of the oblong cells (figure 4.b and 4.c).
microstructure of
rapidly solidified Cu-Fe 4,4 mas. % alloy
In the lateral section the microstructure of rapidly
solidified ribbons of cu-Fe alloy is constituted of more
zones (figure 5.a). At the contact disc surface the zone of
fine globular grains appeared, which proceed to the zone
of columnar - crystal in the middle of the ribbon. The
zone of the coarse globular grains is in the upper part of
the ribbon and is enriched with the iron. in Figure 5.b the
zone of fine globular grains is shown.
As is seen in figure 5.b, the microstructure is homogeneous
and the precipitated particles are not observed on the
grain boundary or within the grains respectively. By TeM
investigation the zone with columnar crystals was observed
in the middle of the ribbon. The spot on the crystal boundary
with the numerous dislocations and fine precipitates of the
size of some nanometres is shown in Figure 5.c.
Phase transformations and
the results of the thermal analysis
Phase transformations of the rapidly solidified ribbons
of Al-fe in Cu-fe alloys in dependence of the temperature
with the heating rate of 5 °c were followed by Dsc and
measurements of the electrical resistance. in Figure 6. two
Dsc thermograms without endothermic and exothermic
peaks are seen. Therefore there is no sign of the precipitation
from the supersaturated solid solution or the transitions
of the intermetallic compounds from the unstable
into the stable state respectively.
The electrical resistance changes depending on the
temperature are shown in Figure 7. Due to the phase
transformations the temperature dependence of the elec-
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trical resistance is changing too. Linear parts of the curve
represent the resistance change regarding to the increasing
temperature. At fixed temperature the deviations of the linearity
are observed. With higher temperature the electrical
resistance is temporarily decreasing and then it is increasing
again. The deviations of the linearity are well visible.
The temperatures, at which those deviations of linearity
were appeared, are more visible on the curves of the
first differential of the electrical resistance with respect
to the temperature (Figure 7.a). on these curves two
temperature intervals of changes are seen. The first one
is between 315 and 480 °c with the minimum of 428 °C,
284
and the second one is between 515 and 570 °C. In figure
7.b the result of the simultaneous measurement of the
electrical resistance of the rapidly solidified cu-Fe alloy
is presented. The electrical resistance change is lower
before the iron precipitation from the supersaturated
solid solution of copper than after that. Therefore the
temperature coefficient of the electrical resistance is lower
for the supersaturated solid solution of copper than for
the precipitated iron. from the temperature depending
diagram of the electrical resistance both temperatures of
the interval changes were directly read and are between
318 °C and 660 °C.
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Phase transformations of the Al-fe alloy, that correspond
to the first temperature interval of the electrical
resistance changes, are the decompositions of the cell microstructure
linked with the transformation of the unstable
intermetallic phases formed during the rapid solidification
into the stable ones and the iron precipitation from the
supersaturated solid solution of α Al . After the decompo-
sition of the cell microstructure the globular, oblong and
acicular particles are present in the matrix (figure 8.a).
The changes formed after the second temperature interval
are linked with the transformation of the needles into the
oblong or globular particles and of the metastable phases
into the stable ones respectively (figure 8.b). The most
significant reaction of the first interval of the electrical
resistance changes is the iron precipitation from the supersaturated
solid solution. But the transition of the unstable
into the final stable state is indicated by both temperature
intervals of changes. The results of the analysis of the
phase transformations are shown in Table 2.
The characteristic of the phase transformations of
rapidly solidified cu-Fe alloy is the decomposition of the
α Cu solid solution. The microstructure of the ribbon which
was in contact with the cooling disc after the heating over
the temperature interval of the phase transformations is
presented in Figure 9.a. That difference is shown before
and after the heat treatment.
during the heating over the temperature interval of the
phase transformations the iron-enriched particles start to
precipitate. it was established by TeM (Figure 9.b), where
essentially greater magnifications are possible as by seM,
that within the matrix the large number of the precipitated
particles of the size of 5 to 20 nm are mainly presented.
Particles of the size of 50 to 100 nm are observed also on
the grain boundaries (figure 9.a).
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ConClusions
Phase transformations in the ribbons of rapidly solidified
alloys of Al-Fe and cu-Fe during the heating were
286
successfully investigated by measurements of the electrical
resistance.
it was established that the electrical resistance is effective
sensitive method for sensing of the phase transformations
by elements of the low diffusivity in the alloys, where
the changes on Dsc were not perceived.
The most significant reactions during the heating of the
ribbons over the first interval change is the iron precipitation
from the supersaturated solid solution of α and α Al Cu
. The transformation process of unstable phases into the
stable ones was simultaneously taking place beside the iron
precipitation. At transition over the changes of the second
interval the transformation of the metastable phases of
aluminium with iron into the stable phase of Al fe and
13 4
acicular structure into the globular one were taking place
respectively.
referenCes
[1] C. d. Lien, M. A. nicolet, Journal Vacuum science Technology B
2 (1984), 783.
[2] k. n. Tu, G. ottaviani, U. Goesele, h. foel, Journal of Applied
Physics 54 (1983) 4, 758.
[3] X. W. Wendlandt:Thermal analysis, 3 rd , j. Wiley&sons, new York,
1986.
[4] X. R. Chen, y. kirsh: Analysis of Thermally stimulated Processes,
Pergamon Press, oxford, (1981).
[5] i. Mamuzić, Metalurgija 43 (2004) 1, 3 - 12.
[6] B. kosec, Euroteh 3 (2004) 5, 32 - 33.
[7] G. Lojen, i. Anžel, A. c. kneissl, A. križman, e. Unterweger, B.
kosec, M. Bizjak, Journal of Materials Processing Technology 162
- 163 (2005), 220 - 229.
[8] M. ohring: The Materials science of Thin films, Academic Press,
san diego, (1992).
[9] L. B. Valdes, Proceedings of the IRE 42, (1954).
[10] G. Riontino, C. Antonione, L. Battezzati, A. zanada, Material
science Engineering A 123 (1991), 1166 - 1169.
[11] h. Jones, Materials science and Engineering 5 (1969/70) 1, 1 - 18.
[12] M. H. jacobs, A. G. Doggett, M. j. stowell, journal of Materials
science 9 (1974), 1631 - 1643.
METALURGIJA 45 (2006) 4, 281-286

S. S. BockUS BockUS: A STUdy of ThE MIcRoSTRUcTURE And MEchAnIcAL pRopERTIES of ... ISSn 0543-5846
METABk 45 (4) 287-290 (2006)
Udc - Udk 621.74.047=111
A study of the microstructure And
mechAnicAl properties of continuously cAst iron products
S. Bockus, kaunas University of Technology, kaunas, Lithuania
Received - primljeno: 2005-07-10
Accepted - Prihvaćeno: 2006-02-15
Original Scientific Paper - Izvorni znanstveni rad
The horizontal continuous casting has a lot of advantages in comparison with traditional casting methods.
But it has a few disadvantages and unsolved problems. The objective of this research was the experimental
investigation of the effect of chemical composition of cast iron and the casting conditions on the microstructure
and properties of continuously cast ingots. As a result, tensile strength, Brinell hardness, and pearlite content
increased with increasing Cr, Cu, and Sb additions and decreasing carbon equivalent. As for microstructure of
graphite, higher silicon to carbon ratio and lower solidification rate decreased a zone of interdendritic graphite.
Nomograph of continuously cast iron structure was made.
Key words: continuous casting, cast iron, mechanical properties, microstructure
Studij mikrostrukture i mehaničkih svojstava kontinuirano lijevanih željeznih proizvoda. Horizontalno
kontinuirano lijevanje ima brojne prednosti u usporedbi s tradicionalnim načinima lijevanja. Ali ono ima i nekoliko
nedostataka i neriješenih problema. Cilj ovog istraživanja je bio ekspereminentalno utvrđivanje ujecaja
kemijskog sastava lijevanog željeza i uvjeta lijevanja na mikrostrukturu i svojstva kontinuirano lijevanih ingota.
Kao rezultat istraživanja utvrđeno je da vlačna čvrstoća, tvrdoća (HB) i sadržaj perlita rastu s porastom dodatka
Cr, Cu i Sb, te smanjenjem ekvivalenta ugljika. S obzirom na mikrostrukturu grafita, viši odnos silicija i ugljika,
te niža brzina skrućivanja smanjuju zonu interdendritnog grafita. Izrađenje i strukturni nomogram kontinuirano
lijevanog željeza.
Ključne riječi: kontinuirano lijevanje, lijevano željezo, mehanička svojstva, mikrostruktura
introduction
The rapid progress of technology requires improve the
mechanical and operational properties of the main casting
alloy - cast iron. In this respect continuous casting iron is in
exceptional position by its properties [1]. continuous casting
has its peculiarities, which, first of all predetermine grey
cast iron microstructure and properties [2]. It is well known
that the quality and properties of cast products are strongly
related to the microstructure developed during solidification.
This especially can be seen in the cross-sections of the cast
iron ingots, where anomalous, intermediate and normal
structural zones can be obtained. This is the result of specific
ingot cooling and solidification conditions [3, 4]. Therefore,
it is important to investigate the effect of the cooling rate
on the microstructure of metal in order to regulate properties
of ingots. Investigations of the continuously cast iron
microstructure are important, because, by change of casting
parameters it is possible to obtain necessary ingots properties
in these parts of cross-section, where damaging effect of
operational factors is most strong. It is well known that the
quality and properties of cast products are strongly related
to the chemical composition of cast iron too. however,
only limited information is available in the literature about
the effect of chemical composition on continuously cast
iron ingots properties. consequently, the aim of the present
paper was to investigate the effects of the solidification rate
and various chemical elements on the microstructure and
mechanical properties of continuously cast products.
experimentAl procedures
cast iron was melted in the standard line frequency
induction furnace of capacity the 10 t. The iron charge contained
steel scrap, cast iron returns, ferrosilicon (feSi75),
ferromanganese (feMn75), ferrochrome (fecr65), pure
copper and antimony. The average chemical composition
of cast irons aimed at 3,4 - 3,6 % c, 2,0 - 2,1 % Si, 0,4
- 0,5 % Mn, 0,15 - 0,6 % cr, 0,03 - 0,04 % S and 0,08 -
0,09 % p. The industrial continuous casting machine was
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S. BockUS: A STUdy of ThE MIcRoSTRUcTURE And MEchAnIcAL pRopERTIES of ...
used. The capacity of the not heated metal receiver of
the machine was 2 tons. The cylindrical and rectangular
specimens were cast by continuous casting.
Effect of chemical composition on continuous casting
ingots initial microstructure was investigated on various
composition cast iron (eutectic Se = 0,8 - 1,0, ratio of
silicon to carbon Si/c = 0,5 - 0,9).
A microstructural analysis was made by optical microscopy.
The graphite flake type, form, and size were defined
by procedure described in the European Standard “cast
iron - designation of microstructure of graphite” (En ISo
945-1994). The procedure of quantitative metalography was
carried out in accordance with Russian Standard “Iron castings
with different form of graphite. Evaluation of structure“
(GoST 3443-87). The microstructures observed were identified
from the corresponding reference diagrams included
in this standard. The tensile test was been determined on
the machined test pieces prepared from samples cut from
the continuously cast ingots in accordance with En 1561.
The test piece diameter was 16 mm. The hardness was been
determined as Brinell hardness from the samples cut from
a casting, according to standard En 10003-1.
results And discussion
Investigation of the microstructure of the continuously
cast 100 × 50 mm cross-section ingots showed that there
was point graphite in surface of the ingots edges. It was
situated in between dendrites. At about 10 mm distance
from the surface the point graphite became substantially
bigger but it was located among dendrites yet. Additionally,
dendrites arms were substantially bigger than they
were in the ingots surface. In 20 mm thickness layer from
the surface almost all graphite was flaky. In the more
deeply located layers the flakes fattened.
There was only 6 percent of a pearlite in the ingots surface
layer. Such little amount of pearlite results from cooling
rate. high cooling rate raises the number of nucleation sites
and reduces the coagulative and coalescentive processes.
As a result, it reduces the carbon diffusion path during the
eutectoid transformation and increases the amount of ferrite
in the structure. on the other hand, there is not time enough
for the growing of the nucleuses to take place, and finally
there are many point graphite in the cast iron structure.
The effect of these two factors on continuously cast
ingots was investigated on various composition cast iron
(eutectic Se = 0,8 - 1,0; ratio of silicon to carbon Si/c =
0,5 - 0,9). Results of the tests are generalized in the structural
nomograph shown in the figure 1. The difference of
presented nomograph from analogical nomographs is that
zone with interdendritic graphite is included and the critical
values of solidification rates are fixed; when approaching
to these values, graphite formation way becomes different.
Investigation of the effect of ratio Si/c on cast iron micro-
288
structure showed that, when Si/c = 0,5 - 0,6 one form of the
graphite transforms to another in the narrow solidification
rate interval. In the cast irons with ratio Si/c = 0,7 - 0,9 interdendritic
graphite forms up at higher solidification rates.
Thus, for continuous casting the cast iron with higher silicon
to carbon ratio should be used for two reasons: to decrease
occurrence of hard spots in a cast iron and to decrease
zone of interdendritic graphite. Besides, grey cast iron with
higher silicon to carbon ratio and lower degree of eutectic
is stronger and resistant to cracking.
The effect of carbon equivalent (cE) on the tensile
strength in the 50 × 50 mm cross-section billet is given
in figure 2. As this figure shows, the tensile strength
decrease significantly with an increase in CE, as a result
of increase in ferrite content.
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S. BockUS: A STUdy of ThE MIcRoSTRUcTURE And MEchAnIcAL pRopERTIES of ...
Well known pearlitization improving elements such
like chrome, tin, manganese, and copper not only help to
form up pearlitic structure, but also make it fine. Figure 3.
shows the influence of manganese on the pearlite content
in the continuously cast billet.
Inoculation with manganese increases the hardness of
billets, too. The hardness increases up to 180 - 207 hB in
the central section of a casting (figure 4.). The increase
of hardness is explained by a sudden decrease of ferrite
content in the structure. When Mn > 1,0 percent, the in-
crease of hardness relates to pearlite, becoming more and
more fine, and to the increase of tied carbon content. This
is proved by the decrease of graphite content in the entire
cross-section. White structure, appearing due to greater
manganese content in castings, is avoided successfully
by a graphitizing inoculation.
Investigating the effect of inoculation with chromium
on the microstructure in the central section of 50 × 50 mm
cross-section billet, it was found that inoculation with chromium
decreases ferrite content a little. When chromium content
in a metal increases from 0,15 to 0,25 percent, pearlite
content in the central section of a billet increases from 87
to 96 percent, and in some specimens even to 100 percent.
pearlite content in the surface layer of billets increased almost
twice - from 22 to 40 percent (figure 5.). chromium
had no effect on the size of graphite insertions.
After addition of copper to cast iron, the size of graphite
inclusions increases, pearlite dispersion increases, and
ferrite content in all zones of a casting decreases. cast iron
with 0,7 % cu has 10 percent of ferrite in the surface layer,
and not more than 3 percent in the central section. When the
concentration of copper in cast iron is greater than 1 percent,
ferrite disappears in the central section completely, and it
does not exceed 3 percent in the surface layer. The hardness
increases quickly (about 30 units) when cu content is
about 1 percent. Tensile strength changes correspondingly.
The increase of the values of mechanical properties can be
explained by the increase of pearlite content, as well by the
appearing surplus phase, rich in cu.
The effect of chromium content on the mechanical
properties of continuously cast billets is given in figures
6. and 7.
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Antimony helps to form pearlite in cast iron [5]. It is not
expensive, and it is well absorbed by cast iron. Antimony
stops the growth of graphite and austenite crystals, that’s
why crystallizing phases become more dispersed, and
properties of a solidified casting become more even in the
cross-section of the casting. Inoculation with antimony increases
the hardness from 160 - 170 to 180 - 190 hB in the
surface layer of a casting, and from 175 - 185 to 210 - 230
hB in the central section. When antimony content grows in
cast iron, the hardness of a casting increases, more pearlite
appear in cast iron but tensile strength increases only to a
certain limit, which depends on chemical composition of
cast iron and which equals approximately to 0,1 percent,
and then it starts to decrease. When inoculation is made
only with antimony, graphitization of cast iron decreases
a little, therefore, it is better to apply a combined inoculation,
i.e. antimony with a graphitizing one.
290
conclusions
on the basis of presented experimental results and their
discussion, the following conclusions can be drawn:
1. The zone of interdendritic graphite can be decreased
with increasing silicon to carbon ratio and decreasing
solidification rate.
2. Tensile strength and Brinell hardness of continuously
cast ingots increased with increasing Mn, cr, cu, and Sb
additions and decreasing carbon equivalent. however,
Sb increased tensile strength only to a certain limit,
which equals approximately to 0,1 percent, and then
Sb started to decrease it.
3. The microstructural analyses showed that Mn, cr, cu,
and Sb additions increased pearlite content. All these
elements had stronger effect in the surface layers than
in central sections. Antimony helped to unify the microstructure
in the cross-section of the castings. on the
other hand, pearlite content in the structure decreased
with increasing carbon equivalent.
references
[1] L. haenny, G.Zambelli, Engineering fracture Mechanics 19 (1988)
1, 113 - 121.
[2] c. cicutti, R. Boeri, Scripta Materialia 45 (2001), 1455 - 1460.
[3] S. k. das, Bull. Mater. Sci. 24 (2001) 4, 373 - 378.
[4] A. M. Bodiako, E. I. Marukovich, E. B. Ten, choi kiyoung, proceedings,
65th World foundry congress. Gyeongju, korea, 2002,
p. 157 - 166.
[5] S. V. kartoškin, Ju. p. kremnev, L. Ja. kozlov, proceedings, 5th
congress of the Russian founders. Radunica publishers, Moscow,
2001, p. 242-244.
METALURGIJA 45 (2006) 4, 287-290

K. K. JELŠOVSKÁ, JELŠOVSKÁ B. et PANDULA al.: NUCLEAR MAGNETIC RESONANCE SPECTRAL FUNCTION AND MOMENTS ISSN 0543-5846 FOR ...
METABK 45 (4) 291-297 (2006)
UDC - UDK 537.6:548.562:620.179.14=111
NUCLEAR MAGNETIC RESONANCE
SPECTRAL FUNCTION AND MOMENTS FOR PROTON
PAIRS IN POWDERED PARAMAGNETIC SUBSTANCES MnSO 4 ·H 2 O AND NiSO 4 ·H 2 O
K. Jelšovská, Faculty of Electrical Engineering and Informatics Technical
University of Košice, Košice, Slovakia, B. Pandula, BERG Faculty
Technical University of Košice, Košice, Slovakia
Received - Primljeno: 2005-01-25
Accepted - Prihvaćeno: 2006-03-25
Preliminary Note - Prethodno priopćenje
The NMR spectrum is determined by interaction of resonating nuclei between the particles of the substance.
These interactions depend on the spatial arrangement of the particles and their motion. Parameters characterizing
interactions between the paramagnetic ions Me 2+ (Me = Mn and Ni) and the protons of crystalline water
in powdered MnSO 4 ·1H 2 O and NiSO 4 ·1H 2 O were derived from the temperature dependences on the second
moment of the NMR spectra. The parameters characterizing the local magnetic field acting on the proton pairs
were calculated and compared with those obtaind from the analysis of the shape of the NMR spectrum.
Key words: nuclear magnetic resonance (NMR), magnetic substances, hydrates
Funkcija spektra magnetne rezonancije jezgre i momenata za parove u praškastim paramagnetnim
tvarima MnSO 4 ·1H 2 O i NiSO 4 ·1H 2 O. MRJ spektar je određen interakcijom rezonantnih jezgri između čestica
materije. Te interakcije ovise o prostornom rasporedu čestica i njihovog kretanja. Parametri koji karakteriziraju
interakcije između paramagnetnih iona Me 2+ (Me = Mn i Ni) i protona kristalne vode u praškastim MnSO 4 ·1H 2 O
i NiSO 4 ·1H 2 O su izvedene iz ovisnosti tempreture o drugom momentu MRJ spektra. Parametri koji obilježavaju
lokalno magnetno polje koje djeluje na parove protona su izračunati i uspoređeni s onima koji su dobiveni iz
analize oblika MRJ spektra.
Ključne riječi: magnetna rezonancija jezgre (MRJ), magnetne tvari, hidrati
INTRODUCTION
The influence of paramagnetic ions on the shape and
the second moment of the proton NMR line and some
problems associated with the NMR study line shape and
with the local magnetic field calculations in paramagnetic
substances were studied in papers [1 - 6].
In this paper we analyse the dependences of the NMR
second moment M 2 on temperature. Beside the second moment
M 20 which corresponds to the nuclear dipole-dipole
interactions, the Curie-Weiss constant θ and the magnetic
moment µ i of paramagnetic ions may be determined from
the temperature dependences. The two parameters θ and
M 20 may be determined directly from experimental data.
However, some knowledge on crystralline structures
for studied substances required for calculation of the
magnetic moment µ i . The parameters characterizing the
local magnetic field acting on the resonating nuclei may
be calculated on the basis of the structural data. We have
calculated these parameters according to a simplified
structural model in which only two paramagnetic ions Me 2+
(Me = Mn, Ni) are allowed to interact with the proton pair
of crystalline water. The spectral function was calculated
for MnSO 4 ·1H 2 O and NiSO 4 ·1H 2 O and the parameters
characterizing the local magnetic field were evaluated
from experimental spectrum.
THEORETICAL PART
In examining the NMR phenomenon the 1 H - 1 H nuclei
are in a magnetic field with induction [1 - 4, 9]:
( i) ( n)
r d d
B = B + B + B
where:
METALURGIJA 45 (2006) 4, 291-297 291
(1)
B r - the induction of the external magnetic field, B r =
2π·f r /γ, f r = 14,1 MHz or 30,0 Mz (in this case) is
the resonance frequency, and γ is the gyromagnetic
constant of the 1 H nuclei;

K. JELŠOVSKÁ et al.: NUCLEAR MAGNETIC RESONANCE SPECTRAL FUNCTION AND MOMENTS FOR ...
( i)
d
B - the induction of the magnetic field formed by the
paramagnetic ions Me2+ (Me = Mn, Ni), including
demagnetising effects which operate in these substances;
( n)
B d - the induction of the magnetic field in the area of a
single nuclei formed by another nucleus of the quasiisolated
pair H-H.
The inductions B d and B d can be expressed according
to papers [1, 3] in the form:
292
( i)
( n)
( )
( ) (
2
i µ 0 ⋅µ
i Br
2 2
Bd = A1 cos ϑ + A2
sin ϑcos2 ϕ
4π ⋅3k T −θ
and
B
( n) 0 p
d
3
2 4π
rp
where:
+ B sin ϑsin 2ϕ + B sin 2ϑsin ϕ
3
2
1 2
+ B3 sin 2ϑ cosϕ
+ C
2 ⎟⎠
(2)
3 µ µ
= ± −
2 ( 3cos ϑ 1 ) ,
⎞
⎟
(3)
µ 0 - the permeability of vacuum,
µ i - the magnetic moment of paramagnetic ions,
k - Boltzmann’s constant,
T - the temperature,
θ - Curie-Weiss constant,
µ p - the proton’s magnetic moment,
r p - the proton - proton distance in the crystalline water.
The angles ϕ and ϑ characterize the orientation of
external magnetic field r B in the reference frame used.
The parameters A , A , B , B , B and C depend on the
1 2 1 2 3
configuration of paramagnetic ions and resonating nuclei
and are expressed as [1, 3]:
A = 3∑ r P cos β ,
1
−3
l 2 l
l
1
A = ∑ r P cos β cos2 α ,
−3
2
2
2 l
l 2 l l
1
B = ∑ r P cos β sin 2 α ,
−3
2
1
2 l
l 2 l l
1
B = ∑ r P cos β sin α ,
−3
l
2
2 l
l 2 l l
1
B = ∑ r P cos β cos α ,
−3
l
3
2 l
l 2 l l
1
C = − A1,
3
(4)
where:
rl
- the vector joining the reference nucleus with the l
- th paramagnetic ion,
α , β - the angles characterizing the orientation of r l l l and
m
P are Legendre polynomials.
2
According to equations (2) and (3) the local magne-
( i) ( n)
tic field Bloc = Bd + Bd
may be thought as a quadratic
form relative to the components of the unit vector
er ( sin ϑcos ϕ,sin ϑsin ϕ,cos ϑ)
parallel to Br. This quadratic
form may be diagonalized and the roots of the secular
equation determine the invariant parameters of the local
magnetic field (denoted as B x ,
+ B y ,
+ B z ,
+ Bx ,
− By ,
− z
B− ), through
which the spatial function may be expressed [1].
According to [1, 3] the second moment of NMR spectrum
may be expressed in the form:
M
2
ABr
=
( T − θ)
2 2 ,
where
2 4
0 ⎟ i
⎟ 2
(5)
⎛ µ ⎞ µ 4 2 2 2 2 2
A = ⎜
⎡A1 3 ( A2 B1 B2 B3
) ⎤
⎜ ⋅ ⋅ + + + + .
⎜⎝ 4π ⎟⎠
9k 45 ⎢⎣ ⎥⎦
(6)
The equation (5) expresses the temperature and the
field dependence of the second moment in paramagnetic.
For isolated proton pairs the second moment M 20 may be
expressed in the form [1, 4]:
M
0 p
20 3
5 4πrp
2
9 ⎛µ µ ⎞
⎟
=
⎜ ⎟
⎜ ⎟ .
⎜⎝ ⎠ ⎟
(7)
For the spectral function f 0 (x) of the isolated pairs of
the nuclei, we used the following form [1, 3, 7]:
+ −
F0 ( x) = f0 ( x) + f0 ( x) , x = B− Br
(8)
for (ε) = + or –
ε ε
⎧⎪ 0,
Bz < x <
Bx
⎪ K( k)
( ε) ( ε)
⎪
, Bx < x < By
,
⎪ ( ε) ( ε) ( ε)
⎪ ( B ) ( )
( )
z − x By − B
ε
x
f0 ( x)
= ⎪
⎨ (9)
⎪ ⎛1 ⎞
⎪ K ⎜ ⎟
⎪ ⎜ ⎟
⎪ ⎜⎝ k ⎟
( ε) ( ε
⎪
⎠
)
⎪
, By < x < Bz
,
⎪ ( ε) ( ε) ( ε)
⎪ ( x− Bx ) ( Bz − By
)
⎪⎩
where:
( ) ( ) ,
METALURGIJA 45 (2006) 4, 291-297

K. JELŠOVSKÁ et al.: NUCLEAR MAGNETIC RESONANCE SPECTRAL FUNCTION AND MOMENTS FOR ...
k =
and
( ε) ( ε) ( ε)
( x− Bx ) ( Bz − By
)
( ε) ( ε) ( ε)
( Bz − x) ( By − Bx
)
K( k)
=
∫
dα
.
2
1−k sin α
(10)
In the above equations B x ,
+ B y ,
+ B z ,
+ Bx ,
− By ,
− z
B− are
the components of the local field fulfilling the relationship
[1 - 6]:
∑
k
( ) 2
k k
ε
B e = 0.
The magnetic interaction between different pairs of the
nuclei was taken into account by means of convolution of
the spectral function for isolated pairs with the normalized
Gaussian function. Taking into account the fact that the
experimental NMR spectra was recorded in the form of
derivation of the absorption spectra, the modelling function
of the spectrum for crystalline water was selected in the
derivation form [1 - 6]:
F′ ( x) = F0 ( x) S′ ∫ ( ξ − x) d ξ,
x ∈ .
(11)
S′ ( ξ − x)
is the derivation form of the Gaussian function:
( ) 2
ξ−x
−
1
2
2βG
S( ξ − x)
= ⋅e
.
2πβ
G
(12)
The spectral function F′ ( x)
may be calculated numerically
[7]. The moments M of the spectral function
n
F′ ( x)
by equation (11) may be expressed analytically in
the form [3]:
( 0) ( 0) 2
( 0)
1 = 1 2 = 2 + βG
3 = 3
M M , M M , M M ,
( 0) ( 0) 2 4
4 = 4 + 2 G + G
M M 6M β 3 β .
where:
( 0)
n
M - the corresponding moments for isolated pairs,
- the parameter of the Gaussian function.
β G
EXPERIMENTAL PART
(13)
Broad - line NMR measurements were performed on
powdered samples of MnSO 4 ·1H 2 O and NiSO 4 ·1H 2 O press-
ed to a cylindrical form in diameter 8 mm and about 20 mm
in height. The temperature dependences were measured at
two frequencies: f r = 14,1 MHz (0,331 T) and f 30,0
1
r =
2
MHz (0,705 T) in the temperature range from 123 K to 313
K. Measurements at frequency 30,0 MHz were done at the
Institute of Physics, A. Mickiewicz University in Poznan.
The experimental conditions and the method of calculation
of moments of the NMR spectra were the same as those
described in our previous papers [1 - 6].
RESULTS AND DISCUSSION
The proton NMR spectra of substances MnSO 4 ·1H 2 O
and NiSO 4 ·1H 2 O have an asymmetric form caused by the
anisotropy of he local magnetic field acting on resonating
nuclei. The central part of the spectra is somewhat distorted
by a narrow signal which corresponds to the free water
present in the sample as moisture. The spectra measured at
room temperature and at different frequencies are similar to
each other, but they differ in their widths. The higher is the
frequency, the greater is the width of the spectrum.
The temperature dependences of the second moment
M 2 are shown in Figure 1. Besides the individual
dependences M (T) measured at f 2 r or f
1 r is convenient
2
to analyse the temperature depenence of the difference
∆ M = M B − M B The dependence of ∆M on
2
( r ) ( r )
2 2 2 2 .
1
METALURGIJA 45 (2006) 4, 291-297 293

K. JELŠOVSKÁ et al.: NUCLEAR MAGNETIC RESONANCE SPECTRAL FUNCTION AND MOMENTS FOR ...
T may be linearized and the parameters A and θ can be
easily determined. According to equation (5) the following
relation holds:
[ ∆ M ] 2 =
294
1
− T −
2
θ
2 2 ( r − r )
A B B
2 1
.
(14)
The dependence of [ ] 1
M 2
2
−
∆ on temperature is also
shown in Figure 1.
As expected, this dependence is linear and the straight
line drawn through the experimental points is expressed
by equation (14) with the following values of Curie-Weiss
parameters θ and A for NiSO ·1H O: θ = –13 K and A =
4 2
2,026×10 –2K2 . For MnSO ·1H O parameters determined
4 2
by the least squares are: parameter θ = –9,9 K and A =
10,54×10 –2K2 . As the parameters θ and A are known, the
second moment M may be evaluated by means of equation
20
(5). It was done by extraction of the term ( ) 2
2
A⋅ Br T − θ from
the experimental values of M at each measured temperature.
2
By means of this procedure we have obtained the value
of M = (19,50 ± 0,95)×10 20 –8T2 for NiSO ·1H O and for
4 2
MnSO ·1H O is M = (21,30 ± 1,2)×10 4 2 20 –8T 2 .
A negative value of the temperature parameter θ shows
that NiSO ·1H O and MnSO ·1H O should be antiferro-
4 2 4 2
magnetic at the temperatures T < θ [9]. Measurements
of the temperature dependences of the molar magnetic
susceptibility in the temperature range from 5 K up to 300
K (Charles University Prague, Dept. of Metal Physics)
confirmed this conclusion.
By means of NMR measurements
(according to equation
(6)) it is possible to determine
the magnitude of the
magnetic moment µ of para-
i
magnetic ions in a given substance,
however, the structural
parameters A and B have to
i i
be known. We have calculated
them in the approximation
in which the nearest enviroment
of the crystalline water
molecule is formed by two
Me2+ (Me = Mn, Ni) ions. This
configuration is shovn in Figure 2. and Figure 3.
The individual hydrates from MeSO ·1H O group were
4 2
studied by X-ray method [7, 8]. All the hydrates of this group
are isomorphous with the monoclinic unit cell. According
to [7, 8] the Me2+ ions have octahedral surrounding formed
by two atoms O and by four atoms of O which belong
w S
− 2
to the different ionic complexes SO 4 . Each molecule of
crystal water has tetrahedral surrounding formed by two
Me 2+ ions and by two oxygen atoms O . Separation of the
S
individual particles and bond angles taken from papers [7,
8] are: r Ow Ni = 0,206 nm, r OwMn = 0,225 nm, r OwH = 0,1 nm;
ξ is the angle between Me – O – Me = 123° and η is the
w
angle H – O – H = 109,5° for our hydrates.
1 w 2
The local coordinate system O was chosen in such a
xyz
way that the origin O lies in the centre of joining the atoms
H and H , the x axis runs through the point where the
1 2
oxygen atom O is placed and it lies in the plabe formed
w
by O , Me and Me ions. The structural parameters A , B w 1 2 i i
and C were calculated from relation (4) using the structural
data stated above. The final form of these parameters for
MnSO ·1H O, are:
4 2
A 1 = – 2,17624·r –3 , A 2 = – 0,48730·r –3 ,
B 1 = B 2 = 0, B 3 = – 1,10865·r –3
and, for NiSO 4 ·1H 2 O, are:
A 1 = – 2.05780·r –3 , A 2 = – 0,9601·r –3 ,
B 1 = B 2 = 0, B 3 = – 1,19930·r –3 , (15)
where r is the distance between the Me-ions and H-atoms
(expressed in the units of 10 –10 m). All distances Me 1 – H 1,
Me 1 – H 2 , Me 2 – H 1 and Me 2 – H 2 are the same, r = 0,265
nm for Me = Mn and r = 0,253 nm for Me = Ni.
The structural parameters given by relation (15) are
expressed for hydrogen nucleus H 1 . The respective parameters
for hydrogen nucleus H 2 are the same as those
for H 1 but they differ from each other in the sign of the
parameter B , i.e. B (H1 ) = –B (H2 ). However, the quantity
3 3
3
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K. JELŠOVSKÁ et al.: NUCLEAR MAGNETIC RESONANCE SPECTRAL FUNCTION AND MOMENTS FOR ...
( )
2 2 2 2 2
A1 + 3 A2 + B1 + B2 + B3
standing in equation (6) has the
same value for both protons H and H . Using the experi-
1 2
mental value for parameter A in equation (6) we have found
that the magnetic moment µ of paramagnetic ion Mn i 2+ in
MnSO ·1H O is 5,74 µ and Ni 4 2 B 2+ in NiSO ·1H O is 3,49 µ ,
4 2 B
where µ = 0,9273×10 B –23 J·K –1 is the Bohr’s magneton.
Measurements of magnetic molar susceptibily for our
hydrates in the temperature range 5 ≈ 300 K have shown
that the NMR method gives valuable information about
the magnetic properties of paramagnetic subsancies. From
measurements of susceptibility we have found: magnetic
moment µ of paramagnetic ion Mn i 2+ in MnSO ·1H O is
4 2
5,72 µ and in NiSO ·1H O is 3,31 µ , Curie-Weiss param-
B 4 2 B
eter θ: for MnSO ·1H O is θ = –21 K and for NiSO ·1H O
4 2 4 2
is θ = –18,5 K.
According to equations (1-3) it is now possible to calculate
the magnitude B of the local magnetic field acting
loc
on proton pair. B means in our case the component of the
loc
local magnetic field parallel to the external magnetic field
B . By means of equation (2, 4) and (15) the magnitude of
r
B may be expressed as a quadratic form:
loc
( ) ( )
( ) 2
( ε)
2 2
loc = ′ 2 + ′ ε x + ′ ′ ε − 2 x
B A C e C A e
where:
+ A′ + C′ e + 2B′
e e
1ε ε x 3 x z
2 2
µ 0 µ i Br µ 0 µ i Br
A′ 1ε = A1 + ε3 δn,
A′ 2 =
A2
,
4π k( T −θ) 4π
k( T −θ)
2 2
0 0
3 3
( ) ( )
,
µ µ i Br µ µ i Br
B′ = B C′ ε = C −εδ
4π k T −θ 4π
k T −θ
and
3 µ µ 0 δn
= .
2 4π
r
p
3
p
( n)
,
n
(16)
(17)
The symbol ε stands for the two signs (±) in B d which
results from the quantum mechanical solution [1, 3, 4].
From the data stated above it is now possible to construct
the theoretical maps of the local field B (ϑ, ϕ), for
loc
given temperature T and the magnitude of the external
magnetic field B . Another way for determining the local
r
field is based on the analysis of the NMR line shape. The
spectral function for isolated proton pairs in paramagnetics
was derived in the works [3, 5]. To obtain this function
the quadratic form (15) has to be transformed into the
canonical form:
( ) ( ) ( )
( ) 2
( )
ε ε 2 ε ε 2
loc = ′ x x + ′ ′
y y + z z
( ) ( )
B B e B e B e
,
(18)
where e′ x, e′ y, e′
z are the components of the unit vector e′ ,
characterizing the direction of the vector r B in the new coor-
( ε) ( ε) ( ε )
dinate system, and the principal components Bx , By , Bz
are the roots of the secular equation:
C′ + A′ −λ
0
B′
2 3
0 C′ − A′
− λ 0 = 0.
METALURGIJA 45 (2006) 4, 291-297 295
ε
ε
2
B′ 0 C′ + A′
−λ
3 ε 1ε
(19)
The spectral function F (x) = f (x) + f (x) where x
0 + –
= B – B , is completely determined by the sets of val-
r
( ε) ( ε) ( ε )
ues Bx , By , Bz
[3, 5]. Using the structural data on
MeSO ·1H O stated previously, the equation (19) gives the
4 2
following values for B ε for NiSO ·1H O:
4 2
( ) ,
i
+ + +
B = − 7,62, B = 2,94, B = 4,68,
x y z
− − −
B = 6,70, B = − 5,57, B = 12,27,
x y z
and, for MnSO 4 ·1H 2 O:
+ + +
B = − 5,94, B = 0,25, B = 5,69,
x y z
− − −
B = − 9,36, B = − 6,52, B = 15,92,
x y z
(20)
(21)
calculated for T = 293 K and B = 0,331·T. All values of
r
B ε are expressed in the units of 10 –4 T.
( )
i
The spectral function F (x) calculated for these values
0
for NiSO ·1H O together with the experimental spectrum
4 2
recorded in the derivate form are shown in Figure 4.
As we can see, the theoretical spectrum reflects quite
( )
well the features of the experimental one. The points Bie ε
in the experimental spectrum (in Figure 4.) correspond to
( )
the respective values Bi ε of the calculated spectral function.
( )
The position of the points Bie ε on the x axis relative to the
origin O are as follows:
+ + +
B = − 8,4, B = 4,0, B = 5,8,
xe ye ze
− − −
B = − 6,0, B = − 4,0, B = 11,4.
xe ye ze
( )
They are different from the corresponding Bi ε stated
above in (19). It can be shown that the sum of principal
components of local field is always zero, i.e.:
∑
k,
ε
( )
k
B 0,
ε
=
(22)
if the components are related to the resonance field of
the free protons, for which x = B – B r = 0. The origin O′
on the x - axis for the theoretical spectrum was chosen in
such a way.

K. JELŠOVSKÁ et al.: NUCLEAR MAGNETIC RESONANCE SPECTRAL FUNCTION AND MOMENTS FOR ...
The origin O on the x axis for the experimental spectrum
may be chosen quite arbitrary if we have no possibility to
measure external magnetic field during the experiment.
Hence, the abscissa values x both spectra may be shifted
relatively to each other as it is also in our case. To make these
two axes equivalent, the centre of gravity for experimental
spectra 0 ∗ has to be found.
The position of the new origin 0 ∗ relative to the old
one 0 is defined as:
1 ( )
x0 Bk .
6 k
ε
∗
= ∑ ε
(23)
296
The quantity of x0 ∗ is identical with the first moment
M of the experimental spectrum related to the origin 0. In
1
aur case x0 ∗ ( )
calculated from the quantities Bie ε stated above
0,467×10 –4 T and the new redefined quantities (
denoted again as B ε are:
( )
i
+ + +
B = − 8,86, B = 3,53, B = 5,33,
x y z
− − −
B = − 6,47, B = − 4,47, B = 10,94.
x y z
All values of
( )
Bie ε – 0
( )
Bi ε are expressed in the units of 10 –4 T.
x ∗ )
(24)
( )
We may consider the set of values Bi ε in (23) as the
experimental values of the principal components of local
magnetic field as they are derived from the experimnental
spectrum. The relative differences between the corresponding
theoretical and experimental values of B ε are in the
( )
i
range from 3 % (for x
B− ) up to 24 % (for y
B− ). The differ-
ences between the theoretical and experimental values of
( )
Bi ε are not so significant as they seem to be at first sight
if we take into account the used approximation.
In the [6] it was shown that the proportion of the free
bonded water in monohydrate MnSO ·1H O was approxi-
4 2
mately 9 % (as regards the number of H O molecules). This
2
is less than in the NiSO ·1H O. Monohydrate MnSO ·1H O
4 2 4 2
is not so sensitive than NiSO ·1H O on the free water, that
4 2
was recorded on the experimental NMR spectra. After the
analysis of the components of the local magnetic field from
experimental spectra, when x0 ∗ = 0,221×10 –4T,
we have obtained
these values of the components of the local fields:
+ + +
B = − 5,71, B = 0,23, B = 5,70,
x y z
− − −
B = − 9,51, B = − 6,42, B = 15,69,
x y z
all in the units 10 –4 T. The relative differences between the
corresponding theoretical and experimental values of B ε
( )
i
are in the range from 1,1 % (for z
B− ) up to 15 % (for y
B+ ).
In our study we are calculated the components of the
local magnetic field also from the measurements of the
molar magnetic susceptibility. Using the structural data on
NiSO ·1H O stated previously, the equations (16 - 19) gives
4 2
the following values for B ε at temperature T = 293 K:
( )
i
+ + +
B = − 7,85, B = 3,2, B = 4,65,
x y z
− − −
B = − 6,40, B = − 5,44, B = 11,88,
x y z
and, for MnSO 4 ·1H 2 O:
+ + +
B = − 6,02, B = 0,46, B = 5,55,
x y z
− − −
B = − 9,36, B = − 6,51, B = 15,87.
x y z
All values of
( )
Bi ε are expressed in the units of 10 –4 T.
METALURGIJA 45 (2006) 4, 291-297

K. JELŠOVSKÁ et al.: NUCLEAR MAGNETIC RESONANCE SPECTRAL FUNCTION AND MOMENTS FOR ...
The final modelling spectrum (by the equations (11,12))
of the monohydrate NiSO 4 ·1H 2 O with the parameters obtained
from NMR measurements and from measurements of
the molar magnetic susceptibility is shown at the Figure 5.
The parameter β in the equation (11) was done by extrac-
G
( 0)
tion of the term M = M and M =
2exp 2 2teor 2 . M In our case:
β = 1,6×10 G –4 ·T.
The comparison of the experimental spectra with the
modelling spectra showed the shift of the central part of
experimental NMR spectra distorted by a narrow signal
corresponds to the free water present in the sample as
moisture.
Figure 6. shows the experimental and modelling theoretical
NMR spectrum for the substance MnSO 4 ·1H 2 O
which is obtained by optimalisation [6].
The best-fit parameter in equation (12) is β G =
1,81×10 –4 ·T.
CONCLUSION
The analysis of the field and temperature dependence on
the NMR second moment for proton of crystalline water in
paramagnetic MnSO 4 ·1H 2 O and NiSO 4 ·1H 2 O give results
which are in a good agreement with the theory. Several
physically important parameters characterizing the studied
paramagnetic substances may be derived from NMR spectra.
Quasi isolated pairs of resonating nuclei should prove
to be sensitive probes for detection of the local magnetic
fields acting on them.
The NMR calculated spectral function, although in the
scope of approximative model of the structure and interactions,
can serve as a key for identification of the local
field components in the experimental NMR spectra. More
accurate determination of the parameters of the spectrum
thus enables a more correct physical interpretation of the
processes in the substance.
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[2] J. Murín, Czech. J. Phys. B 36 (1986), 551 - 554.
[3] K. Jelšovská, J. Murín, Czech. J. Phys. B 39 (1989), 1161 - 1170.
[4] K. Jelšovská, J. Murín, B. Pandula: Data and Results Management
in Seismology and Engineering Geophysics, Regional conference
with international participation, Ostrava 1 (2000), 31 - 35.
[5] K. Jelšovská, E. Boldižárová, Acta Montanistica Slovaca Košice
3 (2000) 7, 301 - 305.
[6] V. Hronský, J. Murín, K. Jelšovská, Transactions of TU Košice 5
(1995) 2, 145 - 149.
[7] Y. Le Fuf, J. Coing - Boyat, G. Bassi, C. R. Acad. Sci. Paris C 262
(1966), 532 - 540.
[8] H. R. Oswald, Helv. Chim. Acta 48 (1965) 590 - 600 I, 600 - 615
II.
[9] Ch. Kittel: Introduction to Solid State Physics (in slovak),
Academia, Praha 1985, Chap.15 and 16.
METALURGIJA 45 (2006) 4, 291-297 297

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D. D. KUDELAs, KUDELAs R. et RYBáR, al.: CONCEPT G. FIsCHER OF ACCUMULATION sYsTEM CONFIGURATION ENABLING THE IssN UsAGE 0543-5846 ...
METABK 45 (4) 299-302 (2006)
UDC - UDK 621.5:62–68:621.31=111
CONCEPT OF ACCUMULATION SYSTEM
CONFIGURATION ENABLING THE USAGE OF LOW-POTENTIAL WIND ENERGY
D. Kudelas, R. Rybár, BERG Faculty Technical University of Košice,
Košice, slovakia, G. Fischer, Rektorat Technical University of Košice,
Košice, slovakia
Received - Primljeno: 2005-06-09
Accepted - Prihvaćeno: 2006-04-20
Preliminary Note - Prethodno priopćenje
The construction concept will allow gaining the maximum value of aerodynamic effectiveness in a wide range
of service conditions. In this way conceived wind aggregate will enable capturing the low-potential wind energy
and its transformation and accumulation into electric energy usable as peak energy by the means of energetic
converters with capacitance accumulation. Part of the solution is also a configuration concept of objective
wind energetic unit with non-electric accumulation with trend to the possibility of a wide usage in the energetic
network structures.
Key words: wind energy, renewable energy sources, accumulation of energy, wind aggregate
Koncept konfiguracije akumulacijskog sustava koji omogućava uporabu nisko potencijalne energije
vjetra. Predloženi konstrukcijski koncept omogućiti će postizanje maksimalne aerodinamične učinkovitosti u
širokom rasponu eksploatacijskih uvjeta. Pretpostavljen agregat na vjetar će omogućiti prikupljanje nisko potencijalne
energije vjetra te akumulaciju i transformaciju te energije u električnu energiju, iskoristivu kao vršna
energija, pomoću energetskih pretvarača i akumulatora. Dio predloženih rješenja je također konstrukcijski koncept
energetske jedinice na vjetar s neelektričnom akumulacijom koja bi trebala naći široku uporabu u energetskim
mrežnim strukturama.
Ključne riječi: energija vjetra, obnovljivi izvori energije, akumulacija energije, vjetrov uređaj
INTRODUCTION
In comparison with western-European countries, the
slovak Republic as an inland country disposes with considerably
lower wind-energetic potential determined by
weather conditions. The basic criterion for estimation of
potential is the average wind velocity. Generally, the type
of locality is considered according to the average wind
velocity and the annual energy production can be determined
referring to the air flow area unit which annually
flows through the propeller diameter.
From the technical power-plant usage of wind energy
the area of slovakia belongs to a region with relatively
low wind potential. This is caused by the fact, that the
technology of electric power production by propeller wind
power-stations is based on the usage of uniformly flowing
wind with quasi constant velocity and flow direction. These
capital expensive equipments reach nominal output in wind
velocities in interval approximately 10 - 15 m/s. Only few
high locations of the most exposed mountain ranges of
slovakia (2 % of the area) can satisfy these conditions.
The starting wind velocity for axial-flow wind powerstations
with regulation stahl is approximately 3,5 to 5 m/s
and for power-stations with regulation pitch, with generators
working in wide range of revolutions, 2,5 up to 3,5
m/s. Wind aggregates with vertical revolution axis existing
today, using the pressure principle are - in comparison
with propeller aggregates - characterised by low service
effectiveness and they are not used in electroenergetics.
SOLUTION CONCEPT
According to the above mentioned facts there arouse
the need to develop wind equipment, concept of which
will take into account more specifics, from the view of the
character of the flow in the area of Slovakia, as well as from
the view of the position in the electric network.
As the aim we have chosen to design a stable standpoint
with sufficient storage tank of wind energy, possibly with
storage tank of compressed air. Wind energy serves as the
primary resource, when it powers the compressor, which fills
the pneumatic accumulator (storage tank of compressed air).
METALURGIJA 45 (2006) 4, 299-302 299

D. KUDELAs et al.: CONCEPT OF ACCUMULATION sYsTEM CONFIGURATION ENABLING THE UsAGE ...
The compressed air is in the time of peak endurance
consumed from the pneumatic accumulators
for the work of pneumatic engine, which
powers the generator and the produced electric
energy is being supplied to the public network.
In the time of insufficient output of wind energy
the compressor is powered by classical energy
resource. Wind energy serves as complementary
resource for the compressor drive. At work we
consider a pressure container with volume V =
10 000 l. In the necessary compressor concept
we consider producing compressed air as well as
electric energy also in the time of windlessness
that is why we have to introduce the energetic and cubical
piston compressor concept.
DETERMINATION OF THE ENERGETIC
AND CUBICAL COMPRESSOR CONCEPT
Pressure tank should be filled with air from the compressor
powered by mechanical energy from the wind
equipment. We are considering a piston compressor for
this purpose. Volume change of compressed air is caused
by a direct reverse piston movement in the working area
of the compressor. The working area of compressor is
being formed of a working cylinder,
which is closed by the cylinder cover
from one side and from the other side
the area is sealed by the piston. In the
cover intake and forcing distribution
valves are stored. On the cover of the
cylinder also suction and delivery valves
are located. The air compressor includes
crank mechanism, connecting rod,
piston gudgeon pin and caulking rings.
The compressor piston is labelled as
single-acting (i = 1), because during the
air compression in the working area of
the compressor only one frontal piston
area is used.
Compressor efficiency [1, 2] is the
amount of gas flowing during a time unit through the
discharge branch of the compressor. Volume efficiency
v / (m3 /h) is being re-counted to relative status, i.e. to
pressure and temperature in suction branch. In technical
conditions the efficiency is related to technically normal
status (pressure p = 100 kPa and temperature t = 20 °C).
Mass efficiency of the compressor m k / (kg/h) is then recounted
volume efficiency of relative status.
Polytrophic exponent for older air compressors is n =
1,2, for newer air compressors it is n = 1,25 - 1,3 and for
large compressors it is being considered n = 1,4.
Volume concept of the compressor is being solved
by the construction concept of the main proportions of
300
the compressor for requested efficiency. The result of the
concept is a determination of the main proportions of the
compressor piston, which are completed by revolutions
of driven compressor shaft.
The energetic compressor concept is understood as the
determination of the necessary compressor work, input
and drive of the given compressor. In 10000 l pressure
tank approximately 2,7 m 3 of air will be used for the work
of pneumatic engine which we gained during pressure
modification from 8000000 Pa to 630000 Pa.
The necessary suction output (Table 1.) and volume
and energetic concept will be performed for an air storage
tank with volume 10000 l (Table 2.).
ENERGY ACCUMULATION
The problem of energy accumulation produced by the
usage of wind, the production of economic and effective
equipment is one of the basic tasks which need to be solved
in the range of the question of using wind power. selection
of the type and capacity of the accumulation equipment
coheres with the dependability of stored energy supply.
In accordance to the versatility of wind conditions, as to
difficult forecast of wind conditions, it is proper to provide
the wind station with accumulation equipment, eventually
to use a non-wind energy station.
METALURGIJA 45 (2006) 4, 299-302

D. KUDELAs et al.: CONCEPT OF ACCUMULATION sYsTEM CONFIGURATION ENABLING THE UsAGE ...
The accumulation equipment observes following tasks:
- stabilization of variable aggregate output in the conditions
of fluently changing wind velocities,
- harmonization of the production timetable graphics
and energy consumption with the aim of delivering the
energy to the consumer also in period in which the wind
aggregate does not work or when its output comes short
for connected loading,
- increase in total production of the wind equipment,
- increase in the effectiveness of wind energy usage,
- the possibility of gaining the peak output in short period
of time.
Air accumulators are storage tanks into which air is being
condensed by compressor powered by wind engine and
consequently it is being consumed for the work of air engine.
In the dependence of ordering the wind engine can be
overcast by the compressor completely or partially, when
it delivers part of the energy through the generator and the
rest to the air accumulator. In the fist case a capacitance
accumulator is considered which secures whole work of
the station, and in the second case a buffering accumulator
is considered which secures only the lacking energy of the
wind engine at decreasing the wind speed.
Wind equipment using the energy of wind flow is powering
the compressor, which compresses
the air into pneumatic accumulators. From
these storage tanks is the compressed air
being used for the work of pneumatic
engine of the working machine.
PNEUMATIC
ENGINE AIR CONSUMPTION
Pneumatic engines are mechanical
equipment intended for transformation
of pneumatic energy of compressed air
to mechanical energy [1, 2]. A big disadvantage
is low effectiveness of pneumatic
traction of approximately 15 %, as well
as the necessity of air modification (contaminant
and moisture removal). To the
benefits belongs also the possibility of usage in industry
in dusty and explosive environment, the ability of constant
transferring to the maximum supercharge up to the total
engine interception without drive protection and the start
of the engine in full charge.
Air compressed by compressor is being forced down
to storage tank, from where it is being used for work of
the pneumatic engine which powers the generator. Asynchronous
generator can be used as the generator. Asynchronous
generator is the most frequent current resource
at actual small wind power-stations. One of its advantages
is dependability, simplicity and minimum maintenance
requirements. As asynchronous generator it is possible to
use almost every asynchronous electro engine with closecut
anchor without modifications.
1. Electromotor in the function of asynchronous generator
can supply current only to public three phase electrodistribution
network.
2. Electromotor in the function of asynchronous generator
in common circumstances cannot be used in places
where is this network missing. so it cannot work as an
emergency resource during blackout or as the unique
resource in non-electric locality.
3. It is not necessary to faze the generator to the network
complicatedly.
4. The generator does not require any regulation of voltage
and frequency.
5. The engine powering this generator does not need a
revolution controller. The generator itself will slack
up the water-wheel or the turbine to corresponding
revolutions. suitable gearing relation will secure the
optimum mode of turbine work in that moment.
In calculations we get high air consumption v = 9,34
m 3 /h (Table 3.) from which results the fact that a storage
tank with volume 10 000 l and pressure 0,8 MPa should be
able to power such pneumatic engine for 17 minutes.
It is necessary to decrease the air consumption, and
for this reason we are considering an equipment of the
pneumatic winged engine with number of vanes 24.
Air consumption decreased to v = 5,48 m 3 /h (Table 4.)
This means that a storage tank with volume 10 000 l filled
to pressure of 0,8 MPa, could power the pneumatic engine
defined by us for 30 minutes.
WIND EqUIPMENT
The study comes from the philosophy of transformation
of the wind kinetic energy, which passes through flow
METALURGIJA 45 (2006) 4, 299-302 301

D. KUDELAs et al.: CONCEPT OF ACCUMULATION sYsTEM CONFIGURATION ENABLING THE UsAGE ...
area of wind engine into mechanical work necessary for
compressor power. Wind engine transforms part of the
energy into mechanical work, part of the energy stays
unused and part of the energy of steady flow transforms
into air whirling behind the rotor. This all comes from the
theoretically possible wind usage.
According to the fact that we need a large torsion
moment, we have to consider a multivane or savonious
rotor. In the blade rotor the air current flowing through
the propeller area has the same effect for all fans during
the propeller rotation. For the propeller drive are used
aerodynamic forces of buoyancy and resistance of the
aerodynamic profile. Output coefficient in correctly proposed
propeller comes near to the theoretical value of Betz
coefficient. It has relatively high revolutions suitable for
generator drive. With the increasing number of propeller
blades is the effectiveness decreasing, revolution by which
is gained the maximum propeller effectiveness decline, but
the torsion moment increases.
It is obvious in a multivane wheel which is during low
revolutions more suitable for drive of piston pumps, as
well as piston compressors, but not for the drive of generators
for electric energy production. Multivan propeller
is suitable for all places where it is necessary to lower
the number of propeller revolutions. slight lowering of
the effectiveness will be replaced by increasing the rotor
diameter.
In the case of savonious rotor is the kinetic energy
of air current transformed to pressure, which pushes the
curved vane of the rotor in front of itself. Recessive vane is
being driven by wind; progressive vane is being inhibited
by the wind, so that a half of the rotor is participated in
production of the torsion moment. Rotors of this type are
suitable for pumps and similar equipments, which require
large torsion moment but low revolutions. since only a
half of the rotor participates during the rotation in the
production of torsion moment, the effectiveness is lower
than the effectiveness of previous types.
302
According to technically usable
wind velocity which is v = 3 m/s i.e.
minimum wind velocity at which the
wind equipment begins to work and
the average wind velocity in Košice
v = 3,6 m/s considered compressors
connected to wind equipments are
dimensioned to wind velocity v = 4
m/s using savonious rotor (rotor area
S = 57 m 2 ) or six-vane wind rotor (rotor
area S = 26 m 2 ). The value of v = 4
m/s gains the wind in Košice and its
outskirts mainly in afternoon hours.
CONCLUSION
submitted work solves in an original way the usage
of wind energy in outskirts of Košice, which is typical
locality with average wind velocity 3,6 m/s with dominant
northern current. According to the fact, that literature (and
practice) considers cost-effective use of wind energy from
the level of 5 m/s, we were searching for a solution, for
which are the mentioned velocities sufficient. There has
been introduced a solution, which should work as a top
power-station, although in this case with a very low output.
Here it is necessary to realize, that a new system solution
is concerned and sequential modifications and improvements
can emphasize the effect.
In the proposed solution are still not achieved results
by which it would be possible to cover whole time of
energetic peak, but there is a possibility of getting near
to this point using pressure tank with higher pressure. In
the proposed concept were used data about pressure tanks
which are commonly available in slovakia.
In comparison with such renewable resource of electric
energy as are photovoltaic systems, whose output should
gain level of 1,3 - 3 GW up to the year 2010, which is a total
annual increase on the level of 580 MW [4], can the proposed
wind energy usage system represent economic and technical
solutions, as e.g. using the pressure tanks, a negotiable
implementation way of RER (Renewable Energy Resources)
into the energetic structures of the slovak Republic.
REFERENCES
[1] M. Horák, P. Vančura,Technika stlačeného vzduchu. Návody na
cvičenia. STU - Bratislava 1994.
[2] M. Horák, Technika stlačeného vzduchu. STU - Bratislava 1994.
[3] J. I. Šefter: Využití energie vetru. SNTL, Praha, 1991.
[4] D. Kováč, I. Kováčová: Behavior of the Voltage Measurement Transformer
during Non Harmonic signal Measuring, Power Electronics
and Motion Control (1998), 152 - 155.
[5] L. Strakoš, Technická analýza vhodnosti využití různých typů rotorů
pro pohon generátorů větrných elektráren. Větrná energie 1/07.
[6] V. Šimko, D. Kováč, I. Kováčová: Theoretical Electrotechnics I., Elfa
s.r.o. Košice (2002), 173.
[7] P. Rybár, T. Sasvári, Zem a zemské zdroje. Elfa, Košice 1997.
METALURGIJA 45 (2006) 4, 299-302

K. K. KosTúR KosTúR: REGULATIoN oF THE HEATING FURNACE IN TUBE RoLLING MILL
IssN 0543-5846
METABK 45 (4) 303-306 (2006)
UDC - UDK 621.783.2:62–55:004.94 =111
REGULATION OF THE HEATING FURNACE IN TUBE ROLLING MILL
K. Kostúr, BERG Faculty Technical University of Košice, Košice,
slovakia
Received - Primljeno: 2005-06-09
Accepted - Prihvaćeno: 2006-04-10
Preliminary Note - Prethodno priopćenje
The rolling of tube requires homogeneous heating along the tube. In steel work the difference along tube was
sometimes 80 °C. The reasons for bad homogeneousness of heating were analyzed by a simulation model of
heating furnace. Then the proposal was made for a new control system and also the proposal for reconstruction
of furnace. In this contribution also a description of some ways for improvement of heating was made. The
main contribution is the proposal of an adaptive system.
Key words: simulation model, homogeneous heating, control system
Regulacija zagrijevne peći u valjaonici cijevi. Proces valjanja cijevi zahtijeva ravnomjerno zagrijan cijevni
uložak u zagrijevnoj peći. U realnim uvjetima procesa valjanja razlike u temperaturi duž cijevi bile su i do 80
°C. Razlog neravnomjernog zagrijavanja je analiziran na simulacijskom modelu zagrijevne peći. Na toj osnovi
izrađen je prijedlog novog upravljačkog sustava kao i rekonstrukcije same peći. U okviru prijedloga dato je nekoliko
mogućih rješenja za poboljšanje postojećeg stanja. Najveća vrijednost pretpostavljenog rješenja sadržana
je u predloženom adativnom sustavu.
Ključne riječi: simulacijski model, homogena zagrijavanja, kontrolni sustav
INTRODUCTION
The heating furnace serves for heating of the semiproduct
(the tube) in front of tube rolling mill. The heated
semi-product from furnace is moved into the tube rolling
mill by a roller conveyor (see Figure 1.). The finished
product after reduction in the tube rolling mill is moved
to the storing place. The base characteristics of the furnace
are as follows:
- the dimensions of furnace - length 17000 mm,
- breadth 8370 mm,
- height 1600 mm;
- the desired temperature of heating tube 900 - 1000 °C;
- the fuel is natural gas;
- the production capacity 20 - 30 t·h –1 ;
- the diameter of tube 100 - 200 mm;
- the thickness of wall of tube 3 - 10 mm;
- the length of tube 10 000 - 16 000 mm.
The heating of tube is provided by the burner system
which consists of 26 burners. The input of fuel is regulated
with the aid of three regulation zones which are localized
on input and output sides of the furnace. The required
temperature of tube depends on the quality of steel. This
temperature would be equal along the tube. The problem
with heating the tube is the homogeneousness of the temperature
along the tube. The differences approx. 60 - 80 °C
along the tube were measured. The bad homogeneousness
of the temperature is the reason for reduction of the quality
of finished tube. Therefore, the reason for bad homogeneousness
of the temperature had to be determined and
then propose improvements of heating.
THE ANALYSIS OF
REASONS FOR BAD TEMPERATURE
HOMOGENEOUSNESS DURING HEATING
OF THE TUBE BY SIMULATION MODEL
The processes in heating furnace are very complex.
Therefore, a simulation way was chosen. The simulation
model was created on the basis of mathematical model. The
basic structure of mathematical description is similar to the
model of heating process of rotary hearth furnace [1].
Unlike old model [1] the new model solves the temperature
field of the tube according to the following system
of differential equations
dT 1
= ( Q1 −Q2
)
dτ
G ⋅ c
METALURGIJA 45 (2006) 4, 303-306 303
(1)

K. KosTúR: REGULATIoN oF THE HEATING FURNACE IN TUBE RoLLING MILL
where:
T - the temperature,
τ - the time,
G - the mass of material,
c - the specific heat capacity,
Q - the heat flow (input/output).
A new simulation model was verified on the basis of
measurements in real furnace [2]. The simulation studies
reveal the reasons of bad homogeneousness during tube
heating as follows.
Control system
The regulation zones (input of fuel) are controlled according
to signals from their own thermocouples, which
are localized approx. 1/3 of distance from output side of
furnace. They are near the opening for exhaust of combustion
products. The regulation zones on input side do not
influence the measured temperature. Therefore it is logical
to divide the regulation into:
- the regulation of the input on input side,
- the regulation of the input on output side.
Then the regulation will consist of six regulation zones
(see Figure 2.). The simulation study does not demonstrate
a marked improvement.
Heating of the beginning and end of a tube
Sometimes the temperature of the beginning/end of an
output tube is higher/lower than the required temperature.
The reason is the difference in radiant surface of a line. For
example, at the beginning of the significiant radiant heat
flow from lateral wall still exists. If the operator lowers the
required temperature then the radiant flow at the beginning
304
of the tube will be higher (side wall) than in the centre of
the tube and vice versa. Therefore, the temperature at the
beginning of the tube will be higher then in the centre (the
influence of heating inertial lining.). For solving this problem
addition (the proposal A) of burners into the horns of
furnace was proposed (see Figure 2.). These burners will be
provided by individual regulation. A second proposal (B)
METALURGIJA 45 (2006) 4, 303-306

K. KosTúR: REGULATIoN oF THE HEATING FURNACE IN TUBE RoLLING MILL
has been an exchange of refractory material, which would
be replaced with insulating material (sibral). In Figure 3. is
shown the temperature field of the tubes during their motion
in the furnace. As it can seen the temperatures along
the tubes are homogeneous.
The number of regulation zones
From Figure 3. it can be seen that the beginning of
the tube has the same temperature as the centre tube. But
the problem is the temperature of end tubes if the tube is
shorter than the breadth of the furnace. The reason is in
unequal temperature field of combustion products. Two
cases were analyzed by simulation model.
First case: The thermocouple of regulation zone is
outside the end of tube.
The fuel of all burners is controlled according to the
measured temperature T in this regulation zone. In close
neighborhood of thermocouple the heating power take-off
is lower because in this place there is not tube. Therefore,
for equal desired temperature of combustion products the
regulator should give a signal for lower mass flow rate of
fuel. The temperature of combustion products above the end
of the tube will be lower in comparison with T. Therefore,
the temperature at the end of the tube will be lower.
second case: The thermocouple of regulation zone is
above the end of tube.
In this case the regulator stabilizes the temperature of
combustion products above the end of tube. Fuel consumption
or heat flow instead consuption of heat to the right of
the end of tube is lower (the tube does exist). Therefore,
the temperature of combustion products on the right will
be higher. Radiant flow q r from this place heats the end
of tube. Therefore, the temperature at the end of tube will
be higher. The maximum of specific capacity near 750 °C
complicates this situation still more. The specific capacity
in front of 750 °C soars and then it plummets at higher
a temperature. It is reason a vehement reaction of a tube
temperature - see equation (1).
This case is shown in Table 1. The temperatures are
in a cross section under the thermocouples along breadth
of furnace.
For solving these problems the following changes
were designed:
1. Increase the number of thermocouples.
2. Increase the number of regulation zones and decrease
their range.
From the original regulation zones (1, 2 and 6, 7) 10
new regulated zones were created. Each burner zone is
individually regulated. Then regulation system consists
of 18 regulation zones.
THE ADAPTIVE SYSTEM
The control system controls the heating of the tube according
to signals from thermocouples which measured the
temperatures of combustion products. Therefore, the problem
is to define the temperatures of combustion products.
The aim is to define these temperatures so that the tube will
reach the desired temperature. It is the task of proposed
adaptation system. This algorithm is very simple.
Trj = Tj ±∆ Tj
where:
METALURGIJA 45 (2006) 4, 303-306 305
(2)
Trj - the desired temperature of combustion products at
j-th thermocouple,
Tj - the previous measured temperature at j-th thermocouple,
DT - the change (increase/ decrease) of temperature.
j
The increase/decrease can be defined as the difference
between desired and measured temperatures of the tube.

K. KosTúR: REGULATIoN oF THE HEATING FURNACE IN TUBE RoLLING MILL
Then the desired temperature of combustion products is
defined as follows:
306
tube tube ( )
Tr T a Tr Tm
j, k+ 1 j, k j k j, k
= + −
where:
(3)
j - the index of regulation zone,
k - the index of time period of adaptation,
Tr - the desired temperature of combustion products,
T - the measured temperature of combustion products,
a - the constant of adaptation,
Tr tube - the desired temperature of tube,
Tm tube - the measured temperature of tube.
The structure of control system is shown on Figure 6.
The control system consists of three levels [3]. The
optimization level computes the optimal heating regime
tube (Tr ). The adaptive level adapts the desired temperatures
j
of combustion products according to the basic equation
(3). The last level is direct digital control. Its signals (u j )
control the actuators of burners.
CONCLUSION
A model of control system (see Figure 6.) was created.
The verification of proposed control system was made with
the aid of simulation. Both models (furnace + control)
have simulated mutual cooperation for real conditions. The
contributions of this solution are the following:
- decrease of specific consumption of fuel approx. by
about 7 %,
- homogeneous temperatures along tube were attained.
The solution of the main problem (no homogeneous
heating) is shown in Table 2.
shorter tube (j = 3, …, 14) was heated. The index j is
part of tube element according length. The desired temperature
of the tube was 930 °C. The maximal deviation is
5 °C. For the tube rolling this deviation is acceptable.
REFERENCES
[1] K. Kostúr: The optimization of heating process in rotary hearth furnace
by simulation model. In: Tagungsband zum XXI. Verformungskundlichen
Kolloquium. Montanuniversität Leoben, 2002, 39 - 46.
[2] K. Kostúr, M. Pastor: Simulačný a matematický model krokovej
pece (The simulation and mathematical model of heating furnace).
Research report, OAR Košice, 2002, 81.
[3] K. Kostúr, M. Pastor, G. Trefa: Návrh regulácie a konštrukcie krokovej
pece. (The proposal of control and construction for heating
furnace). Research report, OAR Košice, 2002, 124.
Acknowledgement
This contribution is part of project VEGA No. 1/3346/06.
METALURGIJA 45 (2006) 4, 303-306

M. M. Jurković, Jurković Z. et Jurković, al.: AN ANALYSIS M. MAhMić AND MODELLING OF SPINNING PROCESS WITHOUT ... iSSN 0543-5846
METABk 45 (4) 307-312 (2006)
UDC - UDK 621.983.3:621.774.7:62–462:621.7.016.3:519.863=111
AN ANALYSIS AND
MODELLING OF SPINNING PROCESS WITHOUT WALL-THICKNESS REDUCTION
INTRODUCTION
The modelling of spinning process is similarly to the
process of deep drawing. The workpiece is flat blank.
it is obtained by this processing through simple pressing
roller the parts of complex form of good mechanical
characteristics and surface which quality is near to the
quality obtained after grinding.
it can be obtained the different axial-symmetrical parts.
The working parts are divided to symmetrical, conical with
curved drawing and combined parts. The spinning process
doesn’t enable to produce of unsymmetrical parts [1 - 7].
Tool design that are used for spinning processing is
very simple, that secure smaller price and longer the time
of explotation life. The same tools can be used for individual
operations at the different parts producing.
THEORETICAL BASIS OF SPINNING PROCESS
At the procedure of metal processing through spinning
is the main motion circular and it is made by workpiece
M. Jurković, Z. Jurković, Faculty of Engineering university of rijeka,
Croatia, M. Mahmić, Faculty of Technical Engineering university of
Bihać, Bosnia and herzegovina
Received - Primljeno: 2003-12-24
Accepted - Prihvaćeno: 2005-12-25
Preliminary Note - Prethodno priopćenje
Through the spinning process it is made the different axial-symmetrical parts by acting spinning roller on blank
of sheet metal, which is shaped through a chuck. In the paper is shown an analyse of stressed and strained
state, as well as forming force components of spinning process. On the ground of experimental results it is
made mathematical modelling of spinning forming force. The obtained mathematical model describes enough
accurate and reliable (P = 0,98) the spinning forming force.
Key words: modelling, spinning, forming force
Analiza i modeliranje procesa rotacijskog tiskanja bez stanjenja debljine stjenke. Rotacijskim tiskanjem se
dobiju različiti osnosimetrični dijelovi djelovanjem pritisnog valjka na pripremak, koji pri deformiranju prijanja uz
rotirajući trn. U radu je prikazana analiza napregnutog i deformacionog stanja, kao i komponenata sile procesa
rotacijskog tiskanja. Na osnovi eksperimentalnih rezultata izvedeno je matematičko modeliranje deformacijske
sile tiskanja. Dobiveni matematički model dovoljno točno i pouzdano (P = 0,98) opisuje silu procesa rotacijskog
tiskanja.
Ključne riječi: modeliranje, rotacijsko tiskanje, deformacijska sila
(5) together with chuck (1) while auxilary motion is made
by roller (2) (Figure 1.). The begininng material form for
processing is usually circular plate (4) pressed by follower
in tailstock (3).
The blank, in this case a plain, sheet-metal disc, is concentrically
clamped against the follower by the tailstock
and driven via the main spindle. rotating at high speed, the
workpiece is then formed by the spinning roller following a
pre-set path to produce a series of strokes or passes. Direction
of the material flowing speed (v m ) during deformation
process is the same to the axial speed (v) of pressed roller.
Geometry of spinning procedure
it is obtained by spinning the cylindrical hole parts with
bottom as is shown at the Figure 2. The part is made from
more operations by the different chucks if it isn’t able to get
desired cylindrical part from one operation (Figure 2.).
Between chuck and pressed roller (D) (Figure 1.) depending
on clearance size, the cylindrical parts can be made
by reduction and without reduction of wall thickness. The
wall thickness and cylinder bottom are the same (s 1 = s 0 )
in the first case and in the second case the wall thickness
is smaller than bottom thickness, that is preparing part
thickness (s 1 < s 0 ).
METALURGIJA 45 (2006) 4, 307-312 307

M. Jurković et al.: AN ANALYSIS AND MODELLING OF SPINNING PROCESS WITHOUT ...
Stress - strain state
The spinning process (Figure 1.), is very similar to deep
drawing process to tools at the press. The process is carried
out in one pass from circular plain preparing part. For full
analysing of strained and stressed state at the spinning it
is needed to divide workpiece into several different zones
(Figure 3.) at which are occured different schemes of strain
and stress [4, 7].
308
The stress state is treated as flat at the element wreath,
where it is considered that forming of material is acted by
absence of normal stress s Z =0. This stress state is unlike
in according to radial stress (s R ) positive and normal stress
at the tangent direction is negative (s T ).
in the element wreath for an analyse of strain and
stress is used the method of common soluting of plasticity
conditions in the form:
σR − σT = ± βk,
(1)
and balance equation:
dσR
ρ + σR − σT
= 0,
dρ
so that we get differential equation:
dσR
ρ + βk
= 0.
dρ
(2)
(3)
We get through soluting of differential equation (3)
for boundary conditions (r = R S , s R = 0) radial stressed
component that incites plastic deformation at the element
wreath:
σ = β ⋅k
R sr
where is:
ln S R
ρ
(4)
k sr - the average value of specific flow stress,
R S - the immediate value outsideed wreath radius of
cylinder (from r 1 to R 0 ),
r - radius inside of intervals r 1 ≤ r ≤ R 0 .
it is getting through involving of express (4) with condition
of plastic flow (1) the normal stress at the tangent
direction:
⎛ R ⎞
S
σT = β ⋅k ⎜
sr ⎜ln −1
⎟ ⎟.
⎜⎜⎝ ρ
⎟ ⎟⎠
(5)
At the spinning of cylindrical elements without reducing
of wall thickness the maximum axial stress is defined
helping expression:
⎛ RS s ⎞
0
σ Z = ⎜
⎜1,1k ln ( 1 1,6 )
max
sr k
⎟
⎜
+ sr
+ µ
⎜ ⎟
⎝ r1 2ρw
+ s ⎟
0 ⎠ (6)
where:
2
RS = 0,5 D0 − 4d ⎡
1sr h 0,57 ( ρw
R s0)
⎤
⎣
+ + +
⎦
.
METALURGIJA 45 (2006) 4, 307-312

M. Jurković et al.: AN ANALYSIS AND MODELLING OF SPINNING PROCESS WITHOUT ...
Maximum axial stress ( σZ
) ,
Degree of deformation
max
obtained by h = 0.
The fitted relative strain at the element wreath are:
- at the tangent direction:
ε
T
=
ρ
−1,
R + ρ − R
2 2 2
0
S
(7)
- at the radial direction (direction of sheet of metal thickness):
RS
1−2ln ρ
εR = ⋅εT
,
RS
2− ln
ρ
- at the axial direction:
ε = − ( ε + ε ).
Z T R
(8)
(9)
At the immediate strained zone it is normal strains
under pressed roller:
d
ε T = −
a
ε ε
1 1,
i
s − s
1 0
R = S = ≈
s0
0,
2hi
−( ai −d1)
εZ = εh
=
.
ai − d1
(10)
where:
2
ai = d + 4d1( hi + 0,75R)
- the immediate value of
workpiece diameter which was deformed in the cylinder
of h height.
i
Logarithmic strain at the part under pressed roller are
defined by expressions:
d s
ϕ ϕ ϕ
1 1
i
T = ln , R = ln ≈ 0, Z = ln .
ai s0 ai d1
Forming forces of the spinning process
2h
− (11)
The axial components of force is determined by
expression:
F = F = σ ⋅ A ,
Z A Zmax Z
unless the contact surface of axial force:
(12)
v
AZ = 2ls0 = 2 s0 dw
⋅ .
n
METALURGIJA 45 (2006) 4, 307-312 309
(13)
on the basis of plastic flowing condition the maximum
radial strain expresses:
σ = σ + 1,15k
Rmax Z sr
and
v v
AR = 2 dw
⋅
n n
or the maximum component of force is:
F = σ ⋅ A .
Rmax Rmax R
(14)
(15)
(16)
owing to simplifying the state of deformation it is
taken into account the plane state of deformation and the
tangent stress is:
σ
Tmax
σZ + σR
1,15k
= =
2 2
and tangent components of force:
F = σ ⋅ A
Tmax Tmax T
where the contact surface is:
1 v
AT = s0
2 ρw
⋅ .
2 n
sr
(17)
(18)
(19)
The experimental researchings are shown that the
maximum radial force occurs immediatelly at the end of
spinning of cylindrical part. The axial stress in this moment
equals zero (s Z = 0). Total force:
F F F F
2 2 2
= A + R + T .
(20)
THE EXPERIMENTAL
ANALYSIS OF THE PROCESS
The experimental analyse of spinning process is made
in the aim of measuring the forming forces which are
used for modelling and simulation ot the spinning process
(Figure 4.).
The experimental
tool for measuring spinning force components
in Figure 5. is given the presentation of force compo-

M. Jurković et al.: AN ANALYSIS AND MODELLING OF SPINNING PROCESS WITHOUT ...
nents at the spinning and Figure 6. is shown the experimental
tool for measuring spinning force components.
310
The experimental results
on the basis of acquired data for material, revolutions
numbers of the main spindle, the feed of pressed roller, roller
diameter, lubrication means are obtained the values of
force components depends on roller motion (Table 1.).
in the Figure 7. are given the obtained experimental
values for Č0148 (DiN St14) and s 0 = 1 mm.
Analyzing recorded diagrams it can be concluded the
following:
METALURGIJA 45 (2006) 4, 307-312

M. Jurković et al.: AN ANALYSIS AND MODELLING OF SPINNING PROCESS WITHOUT ...
- the pressed roller moves during the process by constant
speed,
- the tangent component has nearly constant value during
the process,
- the maximum value of radial force occurs at the end of
the process,
- the decreasing of axial force after reaching of maximum
is stepped (at the cylindrical parts obtained through combined
action) but at the parts obtained without reducing
the decreasing of axial force is extended.
FORCE MODELLING
The parameter choosing of spinning process
on the basis of the experimental results is made a
modelling of spinning force (Table 1.).
The varying parameters are defined over input variables
of process which define the experiment conditions
varying at the three levels: axial speed of pressed roller, v
/(mm/min), wall thickness of the blank, s /mm and pressed
roller path, h /mm.
The constant parameters of process are: material of
preparing part, radius of cycled tools, diameter and product,
etc. [1].
The defining of mathematical model
The number of experiment needed for modelling is
defined by expression:
N = 2 k + n 0 = 2 3 + 4 = 12,
where:
N - the total experiment number,
k - number of parameters,
n 0 - the replied experiment number at the central point of
a plan.
The force function of spinning is modelled by following
polynom function at the coded form:
Y = F = b 0 + b 1 X 1 + b 2 X 2 + b 3 X 3 + b 12 X 1 X 2 +
+ b 23 X 2 X 3 + b 13 X 1 X 3 + b 123 X 1 X 2 X 3
METALURGIJA 45 (2006) 4, 307-312 311
(21)
The further modelling action understand the determining
coefficients of mathematical model to expression:
N
1
b0 = y j,
N ∑
j=
1
N
1
bi = X ij y j,
za i = 1,2,..., k,
N −n 0 j=
1
∑
N
1
bim = X ij X mj y j,
za 1 ≤ i < m < k.
N −n 0 j=
1
∑
where:
b , b , b - coefficients of mathematical model,
0 i im
X , X - coded values.
ij mj
(22)
The values of the coefficient of mathematical models
are:
b 0 = 442; b 1 = 37; b 2 = 99; b 3 = 160;
b 12 = 2,078; b 23 = 32,58; b 13 = 13; b 123 = 0,481.
Taking in attention only significant coefficients of regression,
the mathematical model of force has the form:
Y = F = 442 + 37 X 1 + 99 X 2 +
+ 160 X 3 + 32,58 X 2 X 3
(23)

M. Jurković et al.: AN ANALYSIS AND MODELLING OF SPINNING PROCESS WITHOUT ...
The coefficient of multiple regression R = 0,993 shows
very good correlation between varying X i and spinning
force F j .
The mathematical model (23) enough correctly and reliable
(P = 0,98) describes the process force of spinning inside
the space of applied experiment what shows the comparing
of experimental and calculated values (Table 3.).
Encoding the mathematical model (23) is obtained
the physical mathematical model of the spinning force
in the form of:
Y = – 59,39 + 0,74v + 100,26s + 6,226h + 6,516s·h (24)
CONCLUSIONS
in according to deep drawing this procedure has defined
advantages:
- enable producing of complex products,
- deformation is made in the part under pressed roller,
unless at deep drawing at the whole volume of part
countour,
- the tools are more simple design than the tools of deep
drawing,
- the tool life is longer and tool costs are smaller,
- smaller forming force,
- the tool is flexibile because the same can be used for
different parts producing.
The ground failures are:
- unsymetrical parts cann’t be produce,
- smaller production in according to deep drawing.
The mathematical modelling of the force of spinning enough
correctly and reliable describes forming force, that are
confirmed by obtained model of the that has reliability P =
0,98 and the coefficient of multiple regression R = 0,993.
REFERENCES
[1] M. Jurković, Mathematical Modelling and optimization of Machining
Processes, Faculty of Engineering, university of rijeka,
rijeka, 1999, p. 151 - 176 and 335 - 386.
[2] D. Lazarević, Sile pri rotacionom izvlačenju koničnih delova,
Xviii Savetovanje proizvodnog mašinstva Jugoslavije, Mašinski
fakultet, Niš, 1984, p. 363 - 377.
[3] M. Jurković, Band Cross Section Geometry in the Function of
Thermo-Mechanical Factors and Stress State of Cold Forming
Processes, Dissertation thesis, 1981, p. 148 - 192.
[4] D. Lazarević, v. Stoiljković, Naponsko - deformaciono stanje i sile
pri rotacionom izvlačenju cilindričnih delova bez redukcije debljine
zida, Xvii Savetovanje proizvodnog mašinstva Jugoslavije,
Titograd, 1983, p. iii19 - iii22.
[5] k. Lange, Lehrbuch der umformtechnik, Band 3, Blechbearbeitung,
Springer-verlag, Berlin-heidelberg New York, 1975, p. 1 - 456.
[6] M. Jurković, Z. Jurković, Direct Determining of Stress and Friction
Coefficient on the Contact Surface of Tool and Workpiece, Proc. 1 st
int. Conf. iCiT ’97, 1 (1997), Ljubljana - Maribor, p. 127 - 132.
[7] N. i. Mogiljnji, rotacionaja vytjažka oboločkovyh detalej na stankah,
Mašinostroenie, Moskva, 1983, p. 1 - 190.
312
List of symbols
n - revolutions numbers of chuck /min –1
v - axial speed of pressed roller /(mm/min)
v - the material flowing speed /(mm/min)
m
D - diameter of workpiece (blank diameter)
0
/mm
d - diameter of rotary chuck (chuck diame-
1
ter) /mm
r - chuck radius /mm
1
d - diameter of finished product /mm
s - wall thickness /mm
s - initial sheet thickness /mm
0
d - diameter of pressed roller /mm
w
r w
- roller radius /mm
h - pressed roller path /mm
l - spinning length /mm
d - the immediate diameter of workpiece
1sr
wreath /mm
R - blank radius /mm
0
R - the immediate value outsideed wreath
S
radius of cylinder (from r to R ) /mm
1 0
a - the immediate value of workpiece
i
diameter which was deformed in the
cylinder of h height /mm
i
v/n - spinning feed of roller /mm·rev –1
k - number of parameters
k - the average value of flow stress /Pa
sr
Ds - absolute reducing of wall thickness
/mm
a 0
- angle of chuck /°
a - angle of pressed roller /°
b - Lode coefficient (b = 1,0 to 1,55)
m - coefficient of friction
r - radius inside of intervals r ≤ r ≤ R 1 0
/mm
s , s , s - radial, axial and tangent stress /Pa
R Z T
σR , σ ,
max Z σ
max T - maximum stresses in radial, axial and
max
tangent direction /Pa
e , e , e - the relative strains in radial, axial and
R Z T
tangent direction
j , j , j - logarithmic strains
R Z T
F , F , F - the force components in radial, axial and
R Z T
tangent direction /N
F , F , F - maximum force in radial, axial and
Rmax Zmax Tmax
tangent direction /N
F - total force /N
A R , A Z , A T - the pressed contact surface at the radial,
axial and tangent direction / mm 2
X ij , X mj - coded values
n 0 - the replied experiment number at the
central point of a plane
b 0 , b i , b im - coefficients of mathematical model
N - the total experiment number
MT - strain gages
METALURGIJA 45 (2006) 4, 307-312

S. S. V. DobAtkin, DobATkIn J. et Zrník, al.: nAnoSTRUCTURES i. MAMuZić bY SEVERE PLASTIC DEFoRMATIon oF STEELS ISSn ... 0543-5846
METAbk 45 (4) 313-321 (2006)
UDC - UDk 669.14:539.377:620.17=111
NANOSTRUCTURES BY
SEVERE PLASTIC DEFORMATION OF STEELS: ADVANTAGES AND PROBLEMS
S. V. Dobatkin, A. A. baikov Institute of Metallurgy and Materials Science,
Russian Academy of Sciences, Moscow, Russia, J. Zrník, Comtes
FHt, Ltd., Plzen, Czech republic, i. Mamuzić, Faculty of Metallurgy
University of Zagreb, Sisak, Croatia
Received - Primljeno: 2005-10-21
Accepted - Prihvaćeno: 2006-06-21
Review Paper - Pregledni rad
The aim of this paper is to consider the features of structure evolution during severe plastic deformation (SPD)
of steels and its influence on mechanical properties. The investigation have been carried out mainly on low
carbon steels as well as on austenitic stainless steels after SPD by torsion under high pressure (HPT) and equal
channel angular (ECA) pressing. Structure formation dependencies on temperature deformation conditions,
strain degree, chemical composition, initial state and pressure are considered. The role of phase transformations
for additional grain refinement, namely, martensitic transformation, precipitation of carbide particles during
SPD and heating is underlined.
Key words: nano- and submicrocrystalline structure, severe plastic deformation (SPD), equal channel angular
pressing (ECAP), steels
Nanostrukture dobivene intenzivnom plastičnom deformacijom: postignuća i poteškoće. Cilj članka je
razmatranje karakteristika razvitka strukture čelika uslijed intenzivne plastične deformacije (IPD) i utjecaj na
mehanička svojstva. Istraživanja su se uglavnom odvijala na niskougljičnim i austenitnim korozivno otpornim
čeilcima poslije IPD-a, primjenom visokog tlaka i torziranja (VTT), te kutno kanalnog prešanja (KKP). Tvorba
strukture zavisi od temperaturno deformacijskoh uvjeta, stupnja deformcije, kemijskog sastava, izvornog
stanja i tlaka prešanja. Ističe se uloga faznih preobražaja za dopunsku izmjenu strukture, posebice, martenzini
preobražaj, izlučivanje karbidnih čestica tijekom IPD-a i naknadnog žarenja.
Ključne riječi: nano- i submikrokristalna struktura, intenzivna plastična deformacija (IPD), kutno kanalno prešanje
(KKP), čelici
INTRODUCTION
At present, a great attention is paid to the processes of
severe plastic deformation (SPD) due to the opportunity
of the formation of nano (grain size less then 100 nm)-
and submicrocrystalline (grain size-between 100 nm and
1000 nm) structures upon deformation [1, 2]. This method
consists in severe deformation at relative low temperatures
(below (0,3 - 0,4) Tm) under high applied pressures and
provides bulk porous-free nano- and submicrocrystalline
metals and alloys [2]. Conventional deformation methods,
such as rolling, drawing, pressing, etc., reduce the
cross-sectional area of a billet and do not allow one to
obtain a high strain and grain refinement. nontraditional
methods, such as torsion under high hydrostatic pressure,
equal-channel angular pressing, multiaxial deformation,
alternating bending, accumulative roll bonding, twist
extrusion, and so on, allow one to deform a billet without
changing the cross-sectional area and to reach desirable
high strain and grain refinement. Structures obtained during
SPD have specific features: small size of grains down
to nanolevel, low density of free dislocations, high angle
misorientation of these grains, and high energy and nonequilibrium
state of grain boundaries [2]. These structures
lead to changes in physical and mechanical properties: a
significant increase in the strength at good ductility, an
increase in the wear resistance, and high-speed and lowtemperature
superplasticity [2].
Most works are related to the SPD of pure metals and
rather plastic alloys. The use of SPD for commercial steels
has been poorly studied. Moreover, now it is difficult to
widely apply severe plastic deformation in industry. nevertheless,
it is important to study the limiting structural
states of commercial steels and a combination of their
mechanical and service properties.
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The purpose of this paper is to consider the features of
structure formation during SPD and mechanical properties
of austenitic stainless and low-carbon steels.
FACTORS AFFECTING
ThE STRUCTURE FORMATION DURING SPD
Temperature
It is well known that hot deformation can cause grain
refinement due to the occurrence of dynamic recrystallization.
the lower is the temperature, the finer are the grains,
but, at the same time, the higher is the degree of deformation
required for the beginning of dynamic recrystallization
(Figure 1.). It would seem that the smallest grain size can be
obtained at room temperature, but this requires the degree of
deformation, which cannot be realized upon conventional
deformation schemes such as rolling, extrusion, forging,
etc. In reality, the grained structure with high-angle grain
boundaries was obtained at room temperature by using
methods of severe plastic deformation such as torsion under
high hydrostatic pressure (HPT) and equal-channel angular
(ECA) pressing. However, the formation of high-angle
boundaries, i.e., the process of recrystallization is thermally
activated and requires elevated temperatures. now it is already
well established that room-temperature SPD under the
high pressure cause the occurrence of diffusion-controlled
dislocations climb processes [3]. Just these processes are
responsible for the formation of new grains. Is this process
a dynamic recrystallization? In our opinion - yes, it is, since,
the new grains appear in the deformed matrix, they belong to
314
the matrix phase, but are substantially more perfect and are
separated from other grains by high-angle boundaries [4].
Thus, lowering the SPD temperature to room temperature,
we can refine the grain structure to the nanosize scale.
Degree of strain
It is conventionally assumed that the formation of predominantly
nanocrystalline structure upon SPD at lowered
temperature corresponds to the steady-stage portion in the
graph of the dependence of microhardness on the degree of
strain, i.e., to a true degree of strain ε ≈ 5 - 7 [2]. However,
one should take into account that the degree of strain, which
causes the formation of new grains with high-angle boundaries,
depends on the stacking fault energy and the degree of alloying
of the material. The required degree of strain increases
with decreasing stacking fault energy and increasing degree
of alloying. For example, the formation of submicrocrystalline
structure upon high-pressure torsion (HPT) in Armco
iron begins earlier than in the ferritic steel 0,08 % S - 18 %
Cr - 1,0 % Ti with the same bcc lattice[5].
Strain rate
An increase in the strain rate leads to the grain refinement.
However, it is unreasonable to increase the strain
rate in the case of SPD at room temperature. First, upon
cold deformation, unlike hot deformation, an increase in
strain rate insignificantly decreases grain size. Second,
an increase in strain rate causes the formation of surface
cracks and the premature failure of the sample, especially
upon ECA pressing, because of the contact of the sample
with the internal right angle of the die.
Chemical composition
nanostructure formation depends on chemical composition.
During severe deformation at room temperature, the
alloying facilitates grain refinement by slowing down the
diffusion (under high pressure, an appreciable diffusion
takes place even at room temperature [3]), by reducing the
stacking fault energy, as well as by the necessity to apply
higher deforming stresses.
For example, after SPD by torsion under high pressure
at room temperature the grain size in Armco-iron is ~ 200
nm just as in ferritic stainless 18 % Cr - Ti steel - ~ 150
nm [5]. Changes of chemical composition could initiate
phase transformations and change the structure.
Initial state
It is shown that the metastable non-equilibrium initial
state (metastable austenite, quenched oversaturated solid
solution…) results in most grain refinement during SPD
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at the expense of phase transformations (martensitic transformations,
precipitation and dissolution of carbides…)
and often helps to achieve the nanoscale grain size level
[6]. Austenitic stainless Cr-ni steel undergoes martensitic
transformation during SPD at room temperature [5 - 7].
Martensitic transformation leads to additional grain refinement
and dual phase austenitic - martensitic nanocrystalline
structure exhibits higher thermal stability because the
grain growth of one phase constituent is suppressed by the
other constituent, and vice versa.
Severe deformation of an oversaturated solid solution
can induce its decomposition in course of deformation.
Decomposition of the solid solution can also be initiated
before and after severe deformation. The second phase
particles that have precipitated during heat treatment inhibit
grain growth. Severe low temperature deformation
can lead to dissolution of the precipitates simultaneously
with the formation of nanostructure. The possibility for dis-
solving cementite Fe 3 C particles was demonstrated in cold
rolling of carbon steels with high reductions [8]. Recently,
it was shown the dissolution of carbides in quenched low
carbon 0,2 % C-Mn-b steel [9], and complete dissolution
of cementite Fe 3 C in high carbon 1,2 % C steel [10]. Subsequent
reheating can then result in re-precipitation of the
disperse particles and in stabilization of nanostructure. It
should be noted that the dissolution of the second phase
particles and their ability to stabilize the structure depends
on the size and volume fraction of precipitates.
Pressure
Structure and, correspondingly, strengthening depends
on the pressure applied upon SPD. For example, for the
low-carbon 0,1 % C-Mn-Si steel, just as for the highcarbon
0,8 % C - 6 % W - 5 % Mo steel, an increase in
pressure from 6 to 10 GPa upon room-temperature HPT
leads to a significant strengthening (Figure 2.). Moreover,
for the initially quenched state, the strengthening and the
structure refinement are higher than those observed for the
initially annealed structure.
STRUCTURE AND
PROPERTIES OF STEELS AFTER SPD
Austenitic stainless steels
Different structures can be obtained, depending on
experimental scheme. The limiting structural states are
generally realized upon high-pressure torsion (HPT) since,
in this case, the applied pressure (up to 10 GPa) allows one
to reach a high strain degree [4]. An equal channel angular
pressing (ECAP) as one of the most advantageous SPD
methods allows to prepare nano- and submicrocrystalline
samples as large as of 20 - 40 mm in diameter and 100 - 150
mm in length [2, 11, 12]. The pieces of such size can be
widely used for medical tools and implants; in particular,
they are already tested for titanium [2].
room-temperature deformation of 0,08 % С - 18,3 %
Cr - 9,8 % ni - 0,6 % Ti austenitic steel by high-pressure
torsion (HPT, P = 6 GPa) on the samples of 10 mm in
diameter and 1 mm in thickness leads to the formation of
separated structure elements with high-angle boundaries
already at e = 4,3 (1 revolution) [5, 7]. As a whole, the
oriented structure, which is formed at the initial stages, is
transformed into a rather equiaxed structure upon further
deformation. An average size of structural elements is
about of 50 nm in the 0,08 % С - 18,3 % Cr - 9,8 % ni
- 0,6 % Ti steel after deformation by HPT to e = 5.8 (5
revolutions) (Figure 3.). The character of the selected area
electron-diffraction (SAED) pattern generally indicates a
high-angle misorientation at the boundaries. Therefore, we
can define the obtained structure as nanocrystalline.
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316
Severe plastic deformation induces a martensitic transformation
in austenitic steels [5 - 7]. The martensite content
in the 0,08 % С - 18,3 % Cr - 9,8 % ni - 0,6 % ti steel
sample was 50 % already at е = 4.3 (1 revolution) and ~
60 % at е = 5,8 (5 revolutions) (Figure 4.) [5]. not only γ
→ α, but also γ →ε → α transformation was revealed. The
X-ray diffraction data on the volume fraction of martensite
were obtained without taking into account for texture [5,
6]. As we determined the martensite content with allowance
for texture formed upon deformation by torsion [7],
the same samples after е = 5,8 (5 revolutions) revealed 80
% rather than 60 % martensite shown earlier [5]. In general,
we note that the difference in the martensite contents in
austenitic steels subjected to SPD is caused not only by
the deformation scheme and applied pressure, but also, to
the greater extent, by the technique of the determination
of the α - phase content.
In any case, SPD leads to the formation of a two-phase
austenitic-martensitic structure, which should increase
the thermal stability of the obtained nanocrystalline steel.
upon heating of the nanocrystalline 0,08 % С - 18,3 % Cr
- 9,8 % ni - 0,6 % Ti steel after SPD by HPT, the initial
grain size of 50 nm remains virtually unchanged up to a
temperature of 400 °C. The grain size slightly increases
(to 250 nm) at 500 °C and begins to intensely grow at
temperatures above 600 °C (Figure 3.) [7].
This corresponds to the changes in the volume fractions
of phase constituents upon heating [7]. The martensite fraction
begins to decrease upon heating above 400 °C. After
heating to 550 °C, the phase composition corresponds to a
ratio 50%:50%. This still suppresses an intense grain growth,
which begins at 600 °C, when the austenite content is ~ 80
%. Upon heating of the nanocrystalline steel to 600 °C, the
grain size is retained in a submicrocrystalline range, remain-
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ing below 1 µm. After heating to 800 °C, the grain size was
determined by metallographic examination to be ~ 7 µm.
To determine the mechanical characteristics after SPD,
the massive samples were subjected to room-temperature
deformation by ECA pressing, since the samples deformed
by HPT are not suitable for standard mechanical tests.
An opportunity to deform a sample in the ECAP die
without failure is generally determined by the construction
of this die, which is characterized by a decreased friction in
the input channel and a back pressure in the output channel.
The die used in [7] allowed to deform a sample of 0,07 %
С - 17,3 % Cr - 9,2 % ni - 0,7 % ti austenitic steel of 20
mm in diameter and 80 mm in length for four passes, i.e.
n = 4 (one pass at an angle of 90° between channels and
three passes at an angle of 120°), to a true deformation е
= 3,2 at room temperature.
The limiting deformation achieved by ECA pressing of
0,07 % С - 17,3 % Cr - 9,2 % ni - 0,7 % ti steel is much
lower than that achievable by HPT. For this reason, we
failed to obtain an equiaxed structure after ECA pressing.
oriented structure consisting of elements of 100 - 250 nm
in size (a distance between subgrain or grain boundaries)
and separated equiaxed grains of the same size were
observed. Such oriented structure elements are presented
by shear and deformation bands, twins, martensitic plates,
and oriented subgrains (cells) [13]. it is difficult to resolve
the structure type in such a fine structure. the oriented
structures frequently cross one another at an angle. The
nucleation of equiaxed grains can occur also through the
cellular structure. With increasing strain degree, the fraction
of the grained structure increases, but even at n = 4
(е = 3,2), the structure remains far from perfection.
Unlike HPT, ECA pressing under the used conditions
induces a weak martensitic transformation, which becomes
more active only at N = 4, leading to the formation of 45
% martensite [7].
Even the imperfect and oriented submicrocrystalline
structure of 0,07 % С - 17,3 % Cr - 9,2 % ni - 0,7 % ti
steel after ECAP provides a good combination of mechanical
properties. Already at n = 2, the yield strength is 990
MPa at an elongation of 13 % (Table 1.) [7]. The further
deformation up to n = 4 monotonously increases the yield
strength up to 1315 MPa at A = 11 %. To obtain a perfect
nano- or submicrocrystalline structure, one should either
increase the degree of deformation, or heat the obtained
structure. High degree of the achievable deformation and
a high pressure used in [14] resulted in a more perfect
grained structure with a grain size of ~ 100 nm and, correspondingly,
a higher plasticity (A = 27,5 %) at a somewhat
higher strength (R e = 1340 MPa).
Low carbon steels
Cold ECA pressing
A submicrocrystalline structure in bulk billets of low
carbon steels can be produced by equal-channel angular
pressing (ECAP) at reduced deformation temperatures.
However, the lower the deformation temperature, the higher
the deformation required for the formation of high-angle
boundaries, i.e., new grains [15]. The maximum achievable
deformation without failure of a sample upon ECAP
depends substantially on the equipment used, a decrease in
the friction in the channels, and the backpressure [11, 12].
Upon cold ECAP, low-carbon steels can only be subjected
to two or three deformation cycles at the most efficient
angle of channel intersection (90°) without the failure of a
sample, which is insufficient to produce a developed grain
structure [16, 17]. The structure produced consists of cellular
and subgrain regions with a high dislocation density and a
small number of individual submicron grains.
Low carbon 0,1 % C - 1,6 % Mn - 0,1 % V - 0,08 %
Ti steel in two initial states: the ferritic-pearlitic state after
hot rolling and the martensitic (bainitic) state produced by
quenching from 925 °C (30 min.) was studied [18]. ECAP
was performed at a channel intersection angle of 90° on
samples 5 mm in diameter and 30 mm in length in two
cycles (n = 2) at room temperature for the initially ferriticpearlitic
state and at n = 2 and T def = 400 °C for the initially
martensitic state, which corresponded to the maximum
possible cold deformation without failure of a sample.
The cold ECAP of the hot rolled and quenched samples
of the 0,1 % C - 1,6 % Mn - 0,1 % V - 0,08 % Ti steel at n
= 2 results in a cellular and subgrain structure (Figures 5.a,
d). There are also areas with both an oriented structure and
equiaxed structural elements, which contain separate grains
with high-angle boundaries. After ECAP of this steel with
the initially ferritic-pearlitic structure the spheroidization of
the cementite plates was observed. The size of the structural
elements is 150 - 350 nm. The fact that the structural elements
in the quenched deformed samples are significantly
smaller than in the hot rolled deformed samples can be
due to an initially higher dislocation density in them. After
10-min heating of the deformed quenched sample at 600
°C, its structure becomes mixed: the partly polygonized
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(subgrain) structure has low-angle boundaries, whereas
the partly submicrocrystalline structure has high-angle
grain boundaries (Figure 5.e). The fact that the boundaries
are high-angle is indicated by the characteristic fringe
contrast at the grain boundaries, which is observed upon
an electron-microscopic examination, and the appearance
of individual reflections in diffraction rings. the structures
are mainly oriented. Equiaxed grains and subgrains are, as
a rule, formed inside oriented subgrains. As the temperature
of heating of the 0,1 % C - 1,6 % Mn - 0,1 % V - 0,08 %
Ti steel with the initially quenched structure after ECAP
increases from 600 to 700 °C, the structure becomes not so
oriented and the fraction of grains and their sizes increase
(Figure 5.f). The size of the structural elements increases,
on average, from ~ 0,2 to ~ 0,3µm. The regions with the
oriented structure are retained in a totally equiaxed structure
after heating at 700 °C. Heating after ECAP of the 0,1 %
C - 1,6 % Mn - 0,1 % V - 0,08 % Ti steel with the initially
ferritic-pearlitic structure at 600 °C leads to the formation
of an inhomogeneous structure (Figure 5.b). This structure
is mainly oriented and polygonized and has individual
equiaxed grains and subgrains. Areas with a cellular structure
having a high dislocation density are also retained.
Heating of the hot rolled samples after ECAP at 700 °C
results in a grain structure with a grain size of 6 - 12 µm
(Figure 5.c). Unlike heating of the deformed samples with
318
ferritic-pearlitic structure of the 0,1 % C - 1,6 % Mn - 0,1
% V - 0,08 % Ti steel at 700 °C, the formation and retention
of the submicrocrystalline structure with a grain size of ~
300 nm upon heating of the quenched samples of this steel
at 700 °C after ECAP can be explained by (1) the higher
homogeneity of the initial martensite (bainite) structure, (2)
the higher initial dislocation density, and (3) the precipitation
of fine uniformly distributed carbides upon heating.
After two ECAP cycles, the strength properties of the
0,1 % C - 1,6 % Mn - 0,1 % V - 0,08 % Ti steel increase.
Specifically, the yield strength is almost doubled: it increases
from 510 to 1000 MPa for the initially hot rolled samples
and from 600 to 1110 MPa for the initially quenched samples
(Table 2.) [18]. Under these conditions, the ductility A tot
changes only slightly for the initially hot rolled samples
and decreases for the initially quenched samples, which is
likely due to a significant increase in the dislocation density.
In the case of the initially hot rolled samples, a decrease in
the A tot induced by an increase in the dislocation density is
likely to be compensated for by an increase in A because
of the fragmentation and spheroidization of carbides in
the pearlite. Upon heating of the 0,1 % C - 1,6 % Mn - 0,1
% V - 0,08 % Ti steel after ECAP, the strength properties
decrease but in different ways: for the hot rolled samples,
R e decreases by 22 and 42 % upon heating at 600 and 700
°C, respectively, and by 10 and 27 % for the quenched
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samples upon heating at the same temperatures, respectively.
The R e of the quenched sample of the 0,1 % C - 1,6 % Mn
- 0,1 % V - 0,08 % Ti steel after ECAP, even upon heating
at 600 °C, retains its high value (R e = 1015 MPa) at the
ductility characteristics A tot = 28 % and Z = 40 %. The total
elongation upon heating of the 0,1 % C - 1,6 % Mn - 0,1
% V - 0,08 % Ti steel after ECAP increases to A tot < 30 %,
except for heating of the hot rolled sample at 700 °C, when
a completely grain structure with a grain size of 6 - 12 µm
provides A tot = 39 %. It should be noted that the values of
uniform elongation A uni are high for the initially quenched
samples after ECAP followed by heating and that those
for the initially hot rolled samples are low. The strength
properties R m and R e are substantially higher in the initially
hot rolled samples of the 0,1 % C - 1,6 % Mn - 0,1 % V
- 0,08 % Ti steel after room-temperature ECAP. From the
standpoint of the grain-subgrain structure, we would expect
the best combination of strength and ductility for the 0,1 %
C - 1,6 % Mn - 0,1 % V - 0,08 % Ti steel in the initially hot
rolled samples after ECAP followed by heating at 600 °C
and in the initially quenched samples after ECAP and heating
at 700 °C. In real practice, this combination is reached
immediately after ECAP in the former case and after ECAP
followed by heating at 600 °C in the latter case. Probably,
apart from the grain-subgrain perfection and the dislocation
density, the state of the carbides in the steel also substantially
affects the set of mechanical properties.
Warm ECA pressing
Three low carbon 0,17 % C-, 0,21 % C - 0,89 % Mn
- 0,78 % Si - 0,16 % V- and 0,23 % C - 1,24 % Mn - 0,75 %
Si-steels were studied after warm ECA pressing [19]. The
0,17 % C-steel was subjected to ECAP in the hot-rolled
state, whereas the 0,21 % C - 0,89 % Mn - 0,78 % Si - 0,16
% V- and 0,23 % C - 1,24 % Mn - 0,75 % Si-steels were
previously annealed at 950 °C for 30 min and subsequently
cooled in a furnace. In all cases, the steels had a ferriticpearlitic
structure. Warm ECAP of 0,17 % C-steel was
performed at 500 °C, whereas the 0,21 % C - 0,89 % Mn
-0,78 % Si - 0,16 % V- and 0,23 % C - 1,24 % Mn - 0,75
% Si-steels were pressed at 550 °C. The angle of intersection
of the two channels was equal to φ=90°. Samples 20
mm in diameter and 120 mm in length were subjected to
four passes n = 4; the angle of rotation of the samples
about the longitudinal axis between each pass was equal
to 180° (Route C). These conditions provide alternating
strain. Four passes under these conditions correspond to
the maximum strain before failure.
Using optical microscopy it is impossible to reveal
a substructure in the strained elongated ferritic grains
formed in the 0,17 % C-steel samples during warm ECAP
at four passes. Electron microscopic study allowed to find
both ferrite subgrains, which are formed within ferrite
grains and are separated by low-angle boundaries, and a
submicrocrystalline structure characterized by high-angle
grain boundaries (Figure 6.a). The substructure formed
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upon dynamic recovery is represented by two different
structures, namely, oriented and relatively equiaxed
structures. The submicrocrystalline structure is formed
within both ferrite grains and pearlite colonies. In both
cases, the sequence of formation of submicron grains is
the same. Within both oriented ferrite subgrains and ferrite
grains that are present between the cementite plates
of pearlite colonies, transverse subboundaries are formed
at the expense of lattice dislocations. Upon subsequent
deformation, square or parallelogram subgrains become
rounded; the subgrain boundary angle increases. Finally,
the process of increasing the subgrain boundary angle is
completed by the formation of submicron grains (less than
1 µm in size). Within the pearlitic colonies, this process is
accompanied by the fragmentation and spheroidization of
cementite plates. The sizes of the grains formed in ferrite
and pearlite are different and determined by the distance
between oriented subboundaries in the ferrite (0,3 - 0,4
µm) and the distance between cementite plates (0,1 - 0,2
µm) in the pearlite colonies, respectively. The average
size of structural elements in the ferrite of the 0,17 %
C-steel subjected to ECAP at T = 500 °C and n = 4 was
measured in the cross section for both the submicrocrystalline
structure and the substructure; it was found to be
0,35 µm. the EbSD study confirmed the presence of two
different structures with low- and high-angle grain boundaries
that are formed within the initial elongated ferrite
grains. It can be assumed that, under these conditions of
ECAP, a completely submicrocrystalline structure can be
formed after a larger number of passes. Using EbSD and
TEM (Figures 6.b, c), a similar data for the samples of
the low-alloy low-carbon 0,21 % C - 0,89 % Mn - 0,78
% Si - 0,16 % V- and 0,23 % C - 1,24 % Mn - 0,75 % Sisteels
subjected to warm ECAP at 550 °C and n = 4 was
obtained: subgrain and grain structures characterized by
structural elements 0,3 - 0,5 µm in size are formed. The
steels differ in the fractions of low- and high-angle grain
misorientations. All the samples have a mixed recovered
+ submicrocrystalline structure.
The partially submicrocrystalline structure leads to
substantial hardening of the steels as is evidenced by the
similar values of R e and R m (Table 3.) as well as the yield
drop in the stress-strain curve for the 0,17 % C-steel [20].
The yield strength of the 0,17 % C-steel (R e = 840 MPa)
subjected to ECAP is higher than that of the hot-rolled
steel by a factor of almost three; the samples exhibiting
such high yield strength are characterized by rather large
elongation (A = 10 %) [19, 20]. The low-carbon low-alloy
0,21 % C - 0,89 % Mn - 0,78 % Si - 0,16 % V- and 0,23 % C
- 1,24 % Mn - 0,75 % Si-steels exhibit different hardening
upon warm ECAP (Table 3.) [19]. Even at n = 2, the 0,23
% C - 1,24 % Mn - 0,75 % Si-steel exhibits a high yield
strength, which is virtually unchanged at n = 4. The 0,21
% C - 0,89 % Mn - 0.78 % Si - 0,16 % V-steel exhibits a
320
substantial increase in yield strength at n = 4. The yield
strength of the 0,21 % C - 0,89 % Mn - 0,78 % S i-0,16
% V- steel subjected to warm ECAP is higher than that of
the 0,23 % C - 1,24 % Mn - 0,75 % Si-steel and is equal
to 1100 MPa. In this case, its ductility is equal to 8 - 10
% (Table 3.). Unfortunately, the steels with the partially
submicrocrystalline structure are characterized by a low
impact toughness kCV at both +20 and –40 °C (Table 3.).
It is likely that the low impact toughness of the steels can
be due to both the mixed structure with a high density of
dislocations in subgrains and the low size of structural
elements, which specifies similar values of R e and R m .
Hot ECA pressing
The 0,21 % C - 0,89 % Mn - 0,78 % Si - 0,16 % V- and
0,23 % C - 1,24 % Mn -0,75 % Si-steels were subjected to
hot ECAP: T = 750 °C, n =4, ϕ = 90° and T = 750 °C, n =
8, ϕ = 110°. The degree of deformation reached after four
and eight passes, which was calculated using the shear-strain
intensity and the Mises equivalent strain, was equal to ~ 4,6
and ~ 6,5, respectively [19]. The calculations show that, if
the angle between the two channels satisfies the inequality
90° < ϕ < 120°, the average pressure and total force upon
simple shear are lower than the corresponding parameters
of the process of equivalent direct pressing by factors of
two to three and 5 - 15, respectively [11]. The samples were
heated to the deformation temperature and held for 30 min.
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The equipment used for ECAP was heated to 500 - 550 °C.
After each pass at 750 °C, the sample, whose surface was
slightly cooled, was held in a furnace at 750 °C for 10 - 15
min to level off the temperature. because of this, the total
true strain was lower than the calculated value owing to
static polygonization and possible recrystallization upon
holding in the furnace between passes.
Thus, hot ECAP was performed at 750 °C using two
tools with the angles of intersection of two channels ϕ =
110° (n = 8) and ϕ = 90° (n = 4). In the former case, it was
produced a mixed structure consisting of recrystallized 0,3
- 6 µm grains and ~ 0,5 µm subgrains, which was confirmed
by both TEM and EbSD analysis. The structure formed in
the 0,21 % C - 0,89 % Mn - 0,78 % Si - 0,16 % V- and 0,23
% C - 1,24 % Mn - 0,75 % Si-steels steels after hot ECAP
at ϕ = 110° provides their hardening to R e > 800 MPa at an
elongation A = 10 - 15 %. Moreover, the samples exhibit
a rather high impact toughness at +20 and –40 °C (Table
3.). Upon hot ECAP at ϕ = 90° (n = 4), a polygonized
structure is predominantly formed, thus providing higher
hardening; the steel exhibits R e = 905 MPa and A = 13 %
at a high impact toughness (Table 3.). It is known that the
degree of deformation that is needed for dynamic recrystallization
decreases with increasing deformation temperature.
Therefore, a completely recrystallized grain structure can be
expected to form at a very high degree of deformation; it is
calculated to be ε = 4,6 at ϕ = 90° and ε = 6,5 at ϕ = 110°.
It is likely that the calculated degree of deformation does
not correspond to the real degree of deformation because
of static polygonization and, possibly, recrystallization that
occur upon heating between ECAP passes. Thus, we failed
to produce a uniform submicrocrystalline structure with a
grain size of less than 1 µm by hot ECAP. However, the
formation of a predominantly subgrain structure allowed us
to substantially increase the impact toughness (at +20 and
–40 °C) of the steels (as compared to the steels after warm
ECAP) at high retained hardening (Table 3.).
CONCLUSIONS
Severe plastic deformation (SPD) of steels results
in grain refinement down to nanoscale. Structure is
characterized by low density of internal dislocation and
non-equilibrium state of grain boundaries. Such structure
leads to high strength and sufficient ductility. bulk nano-
and submicrocrystalline steels in equilibrium state could
be obtained by SPD and subsequent heating. A wide application
of bulk nanomaterials is thought to be limited
by the following causes: the whole set of mechanical and
service properties, including fracture toughness, impact
toughness, fatigue strength, corrosion resistance, etc., are
poorly known; the sizes of prepared billets are relatively
small; the production cost is high; there are no industrial
technologies for producing massive products with a homogeneous
structure.
REFERENCES
[1] T. C. Lowe, R. Z. Valiev (Eds): Investigations and Applications
of Severe Plastic Deformation, kluwer Academic Publishing,
Dordrecht, The netherlands, 2000, p. 395.
[2] R. Z. Valiev, I. V. Alexandrov: nanostructured Materials obtained
by Severe Plastic Deformation, Logos, Moscow, 2000, p. 272 (in
Russian).
[3] V. M. Farber, MiToM (2002) 8, 3 - 9 (in Russian).
[4] S. S. Gorelik, S. V. Dobatkin and L. M. kaputkina: Recrystallization
of Metals and Alloys, MISIS, Moscow, 2005, p. 432 (in
Russian).
[5] S. V. Dobatkin, R. Z. Valiev, L. M. kaputkina et al. Proceedings,
Forth International Conference on Recrystallization and Related
Phenomena (REX’99), Tsukuba City, Japan, 1999, T. Sakai, H.
G.Suzuki (ed.) JIM (1999) 13, 907 - 912.
[6] S. V. Dobatkin: Ultrafine Grained Materials II; Y.T.Zhu,
T.G.Langdon, R.S.Mishra, S. L. Semiatin, M. J. Saran and T. C.
Lowe (ed.), TMS (The Minerals, Metals & Materials Society) 2002,
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[7] o. V. Rybal’chenko, S. V. Dobatkin, L. M. kaputkina et al., Mat.
Sci. Eng. A387-389 (2004), 244 - 248.
[8] V. n. Gridnev, V. G. Gavrilyuk, Metallofizika 4 (1982) 3, 74 - 87
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Met. Metalloved. 77 (1994) 2, 141 - 146 (in Russian).
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[11] V. M. Segal, V. I. Reznikov, V. I. kopylov, et al., Structure Formation
in Metals, nauka i Tekhnika, Minsk, 1994, p. 232 (in Russian).
[12] V. Segal, Mater, Sci. Eng. 338A (2002), 331 - 344.
[13] A. M. Patselov, V. P. Pilyugin, E. G. Chernyshov et al.: Structure
and Properties of nanocrystalline Materials, n. noskova, G. Taluts
(ed.), Ekaterinburg 1999, 37 - 44 (in Russian).
[14] I. I. kositsyna, V. V. Sagaradze, V. I. kopylov, FMM 88 (1999) 5,
84 - 94 (in Russian).
[15] S. V. Dobatkin: Investigations and Applications of Severe Plastic
Deformation, T. C. Lowe, R. Z. Valiev (ed.), nATo Science Series,
kluwer Academic Publishers, netherlands, 2000, 13 - 22.
[16] Y. Fukuda, k. oh-ishi, Z. Horita, T. Langdon, Acta Mater. 50
(2002), 1359 - 1368.
[17] J. kim, I. kim, and D. H. Shin, Scr. Mater. 45 (2001), 421 - 426.
[18] S. M. L. Sastry, S. V. Dobatkin, S. V. Sidorova, Metally (2004) 2,
28 - 35 (in Russian).
[19] S. V. Dobatkin, P. D. odesskii, R. Pippan, et al., Metally (2004) 1,
110 - 119 (in Russian).
[20] S. V. Dobatkin, R. Z. Valiev, n. A. krasilnikov and V.n. konenkova,
Proceedings, Forth International Conference on Recrystallization
and Related Phenomena (REX’99), Tsukuba City, Japan, 1999, T.
Sakai, H. G. Suzuki (ed.), JIM (1999) 13, 913 - 918.
METALURGIJA 45 (2006) 4, 313-321 321

Časopis Metalurgija objavljuje članke iz područja metalurgije
i srodnih područja (fizike, kemije, kemijskog inženjerstva,
strojarstva, zaštite okoliša i dr.) ako su zanimljivi sa stanovišta
metalurgije.
Članak treba biti napisan i pripremljen u skladu s prema slijedećim
naputcima:
- članak mora biti neobjavljen te uredno pripremljen za tisak,
- članci se tiskaju latinicom, na hrvatskom (=163.42), engleskom
(=111) ili njemačkom jeziku (=111.2). Radovi moraju biti
napisani na standardnom književnom jeziku,
- članci se pišu na računalu, s jedne strane papira formata A4 (30
do 32 retka s približno 60 slovnih mjesta po retku). Tekst treba
biti pisan u Wordu slovima Times New Roman veličine znakova
12. Opseg članka ograničen je na 10 stranica (do približno
18 000 slovnih mjesta) uključujući slikovne materijale i
tablice. To iznosi maksimalno 4 stranice u časopisu i autori su
strogo dužni o tome voditi računa. Samo iznimno uredništvo
može prihvatiti i nešto opsežnije rukopise,
- članke treba pisati u trećem licu, pridržavajući se zakonskih
standarda i INDOK propisa. Autori su obvezni pisati metrološki
korektno koristeći odgovarajuće nazivlje Obvezna je
primjena SI jedinica. Popis upotrebljenih simbola i skraćenica
potrebno je odvojeno priložiti s nazivima i koherentnim SI
jedinicama,
- dijagrami trebaju biti izrađeni pomoću nekog programskog
paketa, najpoželjnije u Corel Draw. Veličina opisnog znakovlja
treba biti tako odabrana da nakon umanjenja slike na 8 cm svako
veliko latinično slovo bude visoko 2 mm. Dijagrami i tablice
te opisi slika i tablica na hrvatskom i engleskom (njemačkom)
jeziku šalju se na posebnim stranicama i odvojeni od teksta,
- simboli fizičkih veličina pišu se kosim velikim i malim
slovima, a jedinice uspravnim slovima,
- naslov i sažetak do najviše 110 riječi, te ključne riječi (najviše
5) na hrvatskom i engleskom (njemačkom) jeziku i
UDK broj trebaju biti odvojeno priloženi. Za autore izvan
Hrvatske prijevod naslova, sažetka, ključnih riječi te opisa
slika i tablica na hrvatski jezik sačinit će uredništvo,
- literaturu je potrebno numerirati prema redoslijedu pojavljivanja
u članku, a njen broj unijeti u tekst na odgovarajućem
mjestu u uglatoj zagradi. Citira se prema slijedećim uputama
i primjerima:
- knjiga: inicijali imena i prezime svih autora, naslov knjige,
izdavač, mjesto izdavanja, godina izdavanja, stranice
od-do s naznakom”str..”. Primjer: F. Habashi, A Textbook
of Hydrometallurgy, Metallurgy Extractive Quebec,
Quebec, 1993, str. 341-367 i 412,
- članak u časopisu: inicijali imena i prezime autora, naslov
časopisa, volumen (masno), godina izdanja (u okrugloj
zagradi), broj (ako je kontinuirana paginacija nije obvezatno),
stranica od-do. Primjer: G. G. Schlomchak, I. Mamuzić,
F. Vodopivec, Materials Science and Technology, 11
(1995) 3, 312-316,
- članak u knjizi, enciklopediji, leksikonu: inicijali imena
i prezime autora, naslov članka, naslov knjige, inicijali
imena i prezime urednika (uz naznaku “ured” u okrugloj
zagradi), svezak uz naznaku “sv.”, izdavač, mjesto izdavanja,
godina izdavanja, stranice od-do s naznakom “str.”
Primjeri: Du. Maljković, Da. Maljković, A. Paulin, Extraction
of Chlorometallic Acids with Mixed Soilvents Ether,
UPUTE AUTORIMA
U svrhu daljnjeg poboljšanja razine i izgleda časopisa Metalurgija ranije upute autorima su nadopunjene, pa se autori
umoljavaju da rukopise priprave prema novim uputama.
- Alcohol u Solvent Extraction in the Process Industries,
D. H. Logsdail, M. J. Slater (ured.), sv. 3, Elsevier Applied
Science, London, 1993. str. 1361-1368 ili P. Matković,
Tvrdi metali u Tehnička enciklopedija (D. Štefanović,
ured.), sv. 13, Leksikografski zavod “Miroslav Krleža”,
Zagreb, 1997, str. 278-282,
- članak u zborniku radova skupa: inicijali imena i prezime
autora u naslov zbornika (uključuje naziv zbornika
i/ili naziv skupa uz naznaku “Zbornik” te mjesto i godinu
održavanja ako su različiti od mjesta i godine izdavanja
zbornika), inicijali imena i prezime urednika, ako je
naveden naznakom “Ured.” u okrugloj zagradi, izdavač,
mjesto izdavanja, godina izdavanja, stranice od-do s naznakom
“str.”. Primjeri: F. Unkić u Zbornik, 34. livarsko
posvetovanje s sodelovanjem držav heksagonale, Društvo
livarjev Slovenije, Portorož, 1993, str. 213-223 ili
G. M. Ritcey, Zbornik, International Solvent Extraction
Conference, Barcelona , 1999, M. Cox, M. Hidalgo, M.
Valiente (Ured.), sv. 1, Soc. Chem. Ind., London, 2001,
str. 519-523,
- patent: inicijali imena i prezime autora ili naziv pravne
osobe vlasnika patenta, naslov patenta, zemlja patenta
s brojem patenta ili prijave patenta, datum u okrugloj
zagradi. Primjer: V. Logomerac, PELOFOS, Talijanski
patent No. 764917 (15.05.1967.).
Literatura se citira na jeziku na kojem je objavljena. Literatura
objavljena na nelatiničnom pismu se prevodi na lati-nicu
u skladu s uobičajenim pravilima.
Časopis Metalurgija razvrstava radove u slijedeće kategorije:
- izvorni znanstveni rad, u kojem se iznose rezultati istraživanja
na takav način da ih se može ponoviti ili podvrgnuti jednoznačnoj
provjeri,
- prethodno priopćenje, u kojem se iznose dotad neobjavljeni
izvorni rezultati još nedovršenih istraživanja ili najavljuje neka
nova znanstvena spoznaja koja zahtijeva brzo objavljivanje,
- pregledni rad, u kojem se iznosi originalan, kritički i sažet
prikaz nekog područja ili njegovog dijela, u kojem autor i sam
djeluje tako da je vidljiv njegov izvorni doprinos,
- strukovni rad, u kojem se daje koristan prilog iz određene
struke na osnovu vlastitog iskustva i primjene već poznatih
rezultata istraživanja,
- prikaz, u kojem se daje opis nekog znanstvenog ili stručnog
događaja (održanog skupa, predstavljene knjige i sl.).
Sve kategorije radova osim preglednog rada i prikaza trebaju
sadržavati uobičajena poglavlja: Uvod (svrha rada i stanje dosadašnjih
istraživanja), Eksperimentalni dio (metodika i tehnika
rada), Rezultati i diskusija, Zaključci, Zahvala, Popis literature,
Popis simbola, kratica, i akronima.
Autor uz svoj rukopis daje i prijedlog kategorizacije te navodi
izvorni doprinos članka. Konačnu odluku o kategorizaciji daju
recenzenti. Rukopisi se ne vraćaju. Ukoliko je autor nezadovoljan
kategorizacijom može opozvati svoj članak iz časopisa.
Radovi koji nisu pripravljeni dosljedno u skladu s uputama
neće biti razmatrani.
Radovi se dostavljaju u dvije kopije, te u elektroničkoij verziji
na CD-u, s naznakom adrese i elektroničke pošte autora za korespodenciju
na adresu uredništva:
10 000 Zagreb, Berislavićeva 6, Hrvatska (Croatia).

J. J. Zrník, ZRnIk I. et MAMuZIć, al.: REcEnT S. V. pRoGREss DobAtkInIn
hIGh sTREnGTh Low cARbon sTEELs
Issn 0543-5846
METAbk 45 (4) 323-331 (2006)
UDc - UDk 669.14.018.293:669.1.017:620.186.1:620.17=111
Recent pRogRess in high stRength low caRbon steels
J. Zrník, Comtes FHt, Ltd., Plzen, Czech republic, I. Mamuzić, Faculty
of Metallurgy university of Zagreb, Sisak, Croatia, S. V. Dobatkin, A. A.
baikov Institute of Metallurgy and Materials Science, russian Academy
of sciences, Moscow, Russia
Received - primljeno: 2005-10-13
Accepted - Prihvaćeno: 2006-04-20
Review Paper - Pregledni rad
Advanced High Strength (AHS) steels, among them especially Dual Phase (DP) steels, Transformation Induced
Plasticity (TRIP) steels, Complex Phase (CP) steels, Partially Martensite (PM) steels, feature promising results in
the field. Their extraordinary mechanical properties can be tailored and adjusted by alloying and processing. The
introduction of steels with a microstructure consisting at least of two different components has led to the enlargement
of the strength level without a deterioration of ductility. Furthermore, the development of ultra fine-grained
AHS steels and their service performance are reviewed and new techniques are introduced. Various projects
have been devoted to develop new materials for flat and long steel products for structural applications. The main
stream line is High Strength, in order to match the weight lightening requirements that concern the whole class of
load bearing structures and/or steel components and one of the most investigated topics is grain refinement.
Key words: high strength steels, phases, microstructure, mechanical properties, formability
Najnoviji napredak kod visokočvrstih niskougljičnih čelika. Progresivni visokočvrsti čelici (AHS), među
njima osobito dvofazni čelici (DP), čelici s plastičnošću induciranom transformacijom (TRIP), čelici sa složenom
fazom (CP), čelici s djelomičnim udjelom martenzita (PM), daju na tom polju obećavajuće rezultate. Njihova
izvanredna mehanička svojstva mogu se programirati i prilagoditi legiranjem i obradom. Uvođenjem čelika čija
se mikrostruktura sastoji od barem dvije različite komponente dovelo je do povećanja razine čvrstoće a da
nije došlo do narušavanja kovkosti. Nadalje, daje se pregled razvoja ultra sitnozrnih progresivno visokočvrstih
čelika i njihovih radnih karakteristika te se uvode nove tehnike. Razni projekti su imali zadatak da razviju nove
materijale za pljosnate i duge čelične proizvode za konstrukcijsku primjenu. Glavna nakana je da se postigne
visoka čvrstoća i tako zadovolje zahtjevi za smanjenjem težine koje se odnose na cijelu klasu opterećenih
konstrukcija i/ili čeličnih komponenti, a jedan od najistraživanijih problema je sitnozrnost.
Ključne riječi: visokočvrsti čelici, faze, mikrostruktura, mehanička svojstva, oblikovnost
Development of ahss
conventional high strength steels were manufactured
by adding the alloying elements such as nb, ti, V, and/or
p in low carbon or IF (interstitial free) steels. These steels
can be manufactured under the relatively simple processing
conditions and have widely been applied for weight reduction.
however, as the demands for weight reduction are
further increased, new families of high strength steel have
been developed. These new steels grades include Dp (dual
phase), trIP (transformation induced plasticity), Fb (ferrite-bainite),
cp (complex phase) and TwIp (twin induced
plasticity) steels. the critical parts of the manufacture of
the steels is to control the processing conditions so that the
microstructure and, hence, the strength-elongation balance
could be optimized. Various high added value products
are developed to satisfy increasing customer demands, as
shown in Figure 1. [1 - 3].
The terminus high strength steel (hss) is used for
cold formable steels if the minimum yield strength of the
respective steel grade is between 210 and 550 Mpa. If the
minimum yield strength is higher than 550 MPa, these
grades are called ultra-high strength steels (Uhss) [2]:
min.R e hss 210 – 550 Mpa, R m > 550 Mpa
numerous high strength steels have been developed in
the last 25 years. the conventional mechanisms to increase
the strengthening steel such as solid solution hardening or
precipitation strengthening are accompanied by a noticeably
inferior formability.
METALURGIJA 45 (2006) 4, 323-331 323

J. ZRnIk et al.: REcEnT pRoGREss In hIGh sTREnGTh Low cARbon sTEELs
conventional high strength steels (hs) in order of
increasing strength are listed in Table 1. together with
advanced high strength steels (Ahs) and high manganese
steels (hM). Ahs steels is a general term used to describe
various families of steels.
Ahs steels are multiphase
which contain phases like
martensite, bainite, and
retained austenite in sufficient
quantities to produce
unique mechanical properties.
The introduction of a
new group of steels with
microstructure consisting
of at least two different
components has led to an
enlargement of the strength
level without a deterioration
of ductility.
recently, new group of
austenitic steels with high
manganese contents has
been developed for automotive
use. These are high
manganese steels (hMs)
which combine and provide
excellent combination of
mechanical properties with
an alloying concept less
expensive than conventional
or new high strength
austenitic stainless steels.
this group is divided into transformation induced plasticity
steels (HMS-trIP) and twinning induced plasticity steels
(hMs-TwIp) due to the characteristic phenomena occurring
during plastic deformation.
the different steel grades for car body use can be characterised
by their microstructure or their alloying concept
as shown in Table 2. [1].
324
typical mechanical property ranges of these different
steels are presented in Figure 2. It can be seen that the
strength-ductility relationship of AHS steels is improved
compared to HS steels. the recently developed HM steels
show extraordinary strength-ductility relationships with a
product R m × A 80 up to 40 000 Mpa % [4, 5].
the AHS steels are characterized by the combination
of different phases with regard to microstructure description.
Smaller constituents like precipitates of microalloying
elements are not considered to be isolated phases in
this respect.
while single phase microstructers in mild steels can
be simply described by grain size and grain shape, dual
METALURGIJA 45 (2006) 4, 323-331

J. ZRnIk et al.: REcEnT pRoGREss In hIGh sTREnGTh Low cARbon sTEELs
phase, duplex, and multiphase microstructures need additional
features for quantification i.e.:
- volume fraction of different phases,
- grain size of each phase,
- hardness ration of the hard and the soft phase,
- local chemical composition,
- mechanical stability of the metastable phase.
typical microstructure features of different single and
multiphase steels are summarized in Table 5. The Dp and
trIP steels are characterized by a medium ferrite grain
size which, to some extent, can be refined by a controlled
transformation of the super cooled austenite. both steels
contain finely distributed islands of the second phase with
extraordinary small island diameters between 1 and 4 mm.
Dual phase steels
Among Ahs steels, dual phase steels are gaining the
widest usage among automakers. this is because they
provide an excellent combination of strength and ductility
while at the same time they are widely available due to the
relative ease of manufacture. The following Table 3. is a
summary of the dual phase product property requirements.
requirements for the same product sometimes vary widely;
hence only representative property targets are listed.
All the steels developed are based on annealing in
the two phase (intercritical) temperature region and the
consequent increase in carbon content in austenite comparison
with the average carbon content in the steel. Thus,
as shown in Figure 3, carbon in austenite at a lower intercritical
temperature cg 2 , is higher than carbon at a higher
temperature, cg 1 , at the same total steel carbon content.
The comparison of ccT diagrams after intercritical
annealing with CCt of the same steel after annealing in γ
region, i.e. after complete austenitization, displays some
critical features of their difference shown in Figure 4.
[6]. higher carbon content in austenite after intercritical
annealing results in a significant shift of pearlite transformation
towards lower temperature and slower cooling
rates. It is clear that the relative fraction of the formed
ferrite always increase, and significantly at certain cooling
rates. the intercritical annealing is not confined only to
higher carbon, in comparison with the fully austenitized
condition. The acceleration of “new ferrite” formation
due to the presence of pre-existing phase boundaries and
corresponding repartitioning of carbon has very important
consequences for production of Dp and TRIp steels.
The cold rolled dual phase steels have been developed
using advantages of the water quench continuous annealing.
It is clear from Figure 3. the closer to A c1 the annealing
temperatures are, the higher carbon content is in austenite
(cg) and higher its hardenability. thus, effect of annealing
temperature (T an ) and cooling rate are interrelated. The
lower the T an in the a + g region is and therefore the higher
METALURGIJA 45 (2006) 4, 323-331 325

J. ZRnIk et al.: REcEnT pRoGREss In hIGh sTREnGTh Low cARbon sTEELs
cg, the lower the permissible cooling rate is that allows
martensite transformation while avoiding pearlite and/or
bainite transformation. Direct quenching from intercritical
temperature range allows achieving the steels of very high
strength without expensive alloying. by water quenching
but without initial slow cooling, any desired volume fraction
of martensite, which will be equal to the amount of
formed austenite can be obtained [7]. The combination
of beneficial features, especially in R e /R m ratio and partly
in elongation, can be achieved using interrupted cooling
cycle involving direct quenching and relatively slow initial
cooling. Figure 5. presents effects of quenching tempera-
326
ture T q and various annealing temperatures on properties
of Dp steel. similar results were presented for various
amounts of c and Mn in work [8]. As shown, the lower the
annealing temperature (higher austenite stability), is the
larger plateau of quenching temperature is where there are
no hanges in volume fraction of martensite and therefore
Ts occur. Representative microstructures for two of the
steels grades cR 590 Dp and cR 980 Dp are presented
in Figure 6. [19].
A scheme of the metallurgical concept of obtaining
dual phase steel structure after galvannealing is presented
in Figure 7. Intercritical annealing can be used to obtain
austenite enriched by carbon. the basic idea is to have
such combination of c and Mn content as to ensure a
very high stability of gamma phase, sufficient to prevent
any decomposition of austenite during galvanizing and/or
galvannealing. the final austenite to martensite transformation
should take place during final air cooling. However,
METALURGIJA 45 (2006) 4, 323-331

J. ZRnIk et al.: REcEnT pRoGREss In hIGh sTREnGTh Low cARbon sTEELs
the higher the galvannealing temperature is, the more are
chances that the remaining austenite would decompose
partly by bainite reaction prior martensite transformation
during final air cooling.
Additional contribution to enrichment of austenite by
carbon takes place during the initial slow cooling from
galvannealing temperature, when “new ferrite” formation
initiates from austenite at sufficiently high temperatures.
At slow cooling a near-equilibrium carbon redistribution
from ferrite to remaining austenite can be achieved. This
phenomenon has some important practical consequences
such as significant decreasing the sensitivity of the final
structure and properties to annealing temperature [9]. In
fact, the higher the annealing temperature and higher the
amount of initial austenite, is the lower is its stability due
to its lower carbon content and the greater the amount of
“new ferrite” formation. the typical microstructure of
coated dual phase steels is presented in Figure 8.a [19].
concerning galvanized steels (GI in Table 3.) the dual
phase structure can be obtained using the same concept
shown in Figure 7. the key factor of this approach is
sufficient, rather high steel alloying (> 2 % Mn and/or
additions of Cr, Mo, V, which are ferrite stabilizers). on
the other side, such alloying can result in welding problems.
At the same time, the contribution to strengthening
by Si addition provides the same product strength at less
martensite volume fraction and also gives an additional
option to decrease the content of carbon or alloying elements
that could negatively affect carbon equivalent and,
therefore, weldability of steel [10]. typical microstructure
of GI steels contains a dominant portion of martensite with
a very small portion of bainite as strengthening phase in
ferrite matrix is presented in Figure 8.b [19].
multiphase steels
Multiphase steels, also referred to as complex phase
steels, provide higher level of yield strength at the same
comparable tensile strength levels of dual phase steels.
to obtain the high YS/tS ratio, different metallurgical
principles need to be used for cold rolled and for galvannealed
products. For cold rolled steels, achievement of
METALURGIJA 45 (2006) 4, 323-331 327

J. ZRnIk et al.: REcEnT pRoGREss In hIGh sTREnGTh Low cARbon sTEELs
higher R e /R m ratio of > 0,7 is possible with a higher overage
temperature on a appropriate dual phase structure.
For galvannealed steels, however, higher R e cannot be
328
obtained from an initial dual phase structure since in the
galvannealing process, martensite is formed only in the
final step of air cooling and no further overageing is possible.
the only way to gain yield strength in galvannealed
multiphase structure is to obtain appropriate mixture of
pearlite, bainite as well as ferrite straightened by grain
refinement and precipitation strengthening by nb. typical
mechanical properties of cold rolled and galvannealed
multiphase steels are given in Table 5. and structures are
displayed in Figure 9. [19].
A wide range of properties can be obtained with the
same chemical composition only by adjusting the volume
fraction of the second phases [14, 15]. steels with ferriticpearlitic
dual phase structure give properties inferior to
those having a ferritic-martensitic structure. The general
trend is an increase of yield and tensile strength with rising
volume fractions of the harder phase.
The microstructure of multiphase steels compared to
the single phase microstructures of most cold formable
steels requires additional information such as volume
fraction, size, distribution, and morphology of the different
phases, Figure 10.
while single phase microstructures in mild steel
can be simply described by grain size and grain shape,
multiphase microstructures need additional features for
quantification i.e. volume fraction of different phases,
grain size of each phase, hardness ratio of the hard and
the soft phase, local chemical composition, and mechanical
stability of the metastable phases. Concerning
individual specific steels, including dual phase, duplex,
trIP, partly martensitic steels and complex steels, the
different characteristics of phases the structure consists
of are required to define specific role of individual phase
in multiphase structure and its contribution to mechanical
properties.
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J. ZRnIk et al.: REcEnT pRoGREss In hIGh sTREnGTh Low cARbon sTEELs
tRip steels
trIP steels, based on transformation induced plasticity
effect, offer the highest combination of strength and elongation,
which is measure of high level energy absorption [13].
Simultaneously, trIP steels display high n-value strengthening
coefficient up to the limit of uniform elongation as
shown in Figure 11. [14]. In addition, they also show high
bake hardening compared to dual phase steels [15].
these steels belong to AHS group and they are characterised
by the combination of different phases with regard
to the light optical microstructure description. smaller
constituents like precipitates of microalloying elements
are not considered to be isolated phases. The TRIp and Dp
steels are characterized by medium ferrite grain size which,
to some extent, can be refined by a controlled transformation
of super cooled austenite. both steels contain finely
distributed small islands of second phase with diameters
between 1 and 4 mm.
Among the noticeable microstructural parameters
which affect the mechanical properties of TRIp steels are:
martensite volume fraction, martensite island diameter,
ferrite grain size, retained austenite volume fraction and
bainite morphology and packet size. the typical microstructure
features of different single and multiphase steels
are summarized in Table 5. [14].
Various processing routes for trIP steels are either
already in use or are subject to discussion depending on
the product [15]. The use of strip caster for processing
of high alloy steels has been put to industrial practice
already, while for low alloy multiphase and trIP steels
this is still a matter of current research. special attention
has to be paid to the cooling strategy when producing
hot rolled multiphase steels. After solutioning and different
steps of rolling in roughing and finishing mill the
microstructure and the mechanical properties are finally
adjusted in the cooling section. A variation of the cooling
intensity and the coiling temperature allows to change the
transformation behaviour and to vary the strength level.
The temperature-time schedule for the production of hot
rolled dual phase and trIP steels by continuous processing
is shown in Figure 12.
After cold rolling, to developed multiphase structure
with TRIp effect in steel, the strip has to undergo a heat
treatment that can be realized in continuous annealing lines
and hot dip galvanising lines, Figure 13. Low alloy trIP
steels are subjected to a two step heat treatment with critical
annealing in the temperature range 780 - 880 °c, fast
cooling and another isothermal annealing between 350 -
500 °C and followed by slow cooling to room temperature.
The microstructure after intercritical annealing contains
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J. ZRnIk et al.: REcEnT pRoGREss In hIGh sTREnGTh Low cARbon sTEELs
almost identical volume fractions of ferrite and austenite.
During the second isothermal holding the austenite is
mostly transformed to bainite with final retained austenite
volume fraction of 5 to 15 %. typical microstructures of
trIP steels developed by different etching procedure are
presented in Figure 13.a, b.
The description of the production process requires the
strict control of the process parameters, which is necessary
in order to produce the desired microstructure and
mechanical properties. TRIp aided steels are developed
because of their attractive combination of high strength
together with high ductility and remarkable strain hardening
[16, 17]. It is the strain hardening behaviour and the
temperature sensitivity of these steels which distinguishes
TRIp aided steels from conventional cold formable steels.
A strong temperature dependence of the strain hardening
was observed for all TRIp aided steels [18]. Due to the
strain induced formation of martensite the mechanical
properties of trIP steels respond sensitively and change
in a wide range if the test temperature is changed. The
definition of optimised structure of trIP steels for different
forming operations or forming parameters will need a
more thorough and quantitative understanding of the temperature
and stress state dependencies and microstructural
features responsible for these.
maRtensitic steels
Using water quenching in a continuous annealing
line, steels with 100 % martensite can be produced. These
steels offer very high strength although ductility is lower
than other Ahs steels. The strength of these steel is controlled
by the carbon content and complete austenitizing
temperature is used to obtain a fully martensitic structure.
The selection of martensitic steels in production and their
330
mechanical properties are given in Table 6. Martensitic
steels have also been in use for bumpers and door beams
for some time now [19].
conclusion
Advanced high strength steels are defined according
to their microstructural features. they offer extraordinary
strength-ductility relationship and are thus of prime interest
for automotive applications. Matching exact mechanical
properties of the intended steel grades the critical forming
mode requires an added level of steel suppliers’ knowledge.
the advance AHS steels have been broadly applied
to various automotive parts over the last few years. the
advanced dual and multiphase steels are already used in
production vehicles starting as early as 2005. Producing
companies have developed various hot and cold rolled
AHS steels and continue to develope new types of steels
in response to automotive demands for additional Ahs
steels capabilities. The next generation of Ahs steels is
likely to be a new class of steels based on tWin induced
plasticity, called tWIP steels. these offer very high
elongations of 60 - 80 % at comparable strength levels.
Since the trial of tWIP was successfully produced a decade
ago, the productivity improvement for cold and hot
rolled strips is now under way. the optimum materials for
each automotive part can be efficiently determined with
the help of the steel suppliers, since this provides critical
tips for successful forming of parts in many cases. As a
partner of automaker the steel supplier participates in the
full automobile production process, and must be ready to
share risks involved in the applications of new steels in
combination with advanced forming technologies.
RefeRences
[1] w. bleck, phiu-on, Iron & steel suplement 40 (2005), 91.
[2] w. bleck, proc. of International conference on TRIp Aided high
Strength Ferrous Alloys, 2002, Ghent, 247.
[3] J. s. kim, J.h. chung, posco Technical Report (1997) 2, 180.
[4] h. hofman, s. Goeklue, J. Gerlach, U. bruex, proceedings ID-
DrG International Deep Drawing 2004 Conference, Sindelfinden,
Germany, 270.
[5] r. Viscorova, J. Wendelsrorf, k. H. Spitzer, J. kross, V. Flaxa,
proceedings IDDRG International Deep Drawing 2004 conference,
Sindelfinden, Germany, 261.
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J. ZRnIk et al.: REcEnT pRoGREss In hIGh sTREnGTh Low cARbon sTEELs
[6] n. Fonstein, A. Davidiuk, proceedings of 7 th International conference
on heat Treatment of Materials, 1990, Moscow, Russia, 201.
[7] A. nishimoto, Y. Hosoya, k. nakaoka, ISIJ 21 (1981) 11, 778.
[8] I. Gupta, p. h. chang, conference proceedings, TMs-AIME 1984,
Detroit, UsA, 236.
[9] G. Eldis, conference proceedings, TME-AIME 1984, washington,
UsA, 202.
[10] I. Tsukatani, IsIJ International 31 (1991) 9, 992.
[11] J. Zrnik, o. Stejskal, Z. novy, P. Hornak, M. Fujda, Materials
science & Engineering, 2005 (in press).
[12] I. b. timochina, P. D. Hodgson, E. V. Pereloma, Metall. and Materials
Trans. A 35 (2004), 2331.
[13] V. Zackey, E. Parker, D. Fahr, r. bush, trans. of ASM 60 (1967),
252.
[14] o. Moriau, L. t. Martinez, P. Verleyzen, J. Degrieck, Proc. of
International conference on TRIp Aided high strength Ferrous
Alloys, 2002, Ghent, 247.
[15] o. Jakubovsky, n. Fonstein, D. bhattacharya, Proc. of International
Conference on trIP Aided High Strength Ferrous Alloys, 2002,
Ghent, 263.
[16] b. Engl, E. J. Drewes, Proc. IbEC’97 Congress “Automotive body
Materials”, stuttgart, 2002, 127.
[17] T. heller, b. Engl, proc. on Thermomechanical processing of steels,
London, May 2000, 438.
[18] w. bleck, s. kranz, J. ohlert, k. papamantellos, proceedings 41st
MWSP Conference, ISS, Vol. XXXVII, 1999, 295.
[19] D. bhattacharya, Proc. the Joint Int. Conf. of HSLA Steels, november
2005, hainan, china, 69.
[20] D. J. kim, s. c. baik, s. h. park, Y. R. cho, s. J. kim, proc. of
new Development in sheet Metal Forming, stuttgart, 2004, 281.
METALURGIJA 45 (2006) 4, 323-331 331

Ž E LJ E Z A R A S P L I T
STEEL WORKS SPLIT
PODUZEĆE ZA PROIZVODNJU I PRERADU ČELIKA d. d.
21 212 Kaštel Sućurac - Brižine b. b. - HRVATSKA
TELEFONI
Centrala: 385 21 202 - 111
Direktor: 385 21 202 - 104
Fax: 385 21 260 - 802
Telex: 261169 STZEL RH
Brzojav: “ŽELJEZARA SPLIT” - K. Sućurac
Poduzeće u svom sastavu ima:
Čeličanu sa elektrolučnom peći, lončanom peći i kontiljevalicom
kapaciteta 190 000 t godišnje,
čeličnih kontinuirano ljevanih gredica
100 × 100 × 2000 - 6000 mm,
125 × 125 × 2000 - 6000 mm,
u kvalitetama: - niskougljičnih čelika,
- srednjeugljičnih čelika i
- niskolegiranih čelika.
Valjaonicu godišnjeg kapaciteta 170.000 t/god. valjane
robe, uglavnom:
- betonskog čelika glatkog,
- betonskog čelika orebrenog u kolutima i šipkama,
- toplo valjane žice.
U daljnjoj fazi prerade,
Hladnu preradu čelika, koja proizvodi 35.000 t/god.
sljedećih proizvoda: Hladno valjani/vučeni betonski čelik
(glatki i orebreni, u šipkama i u kolutu), sve vrste vilica,
zavarene armaturne mreže, ogradne žičane mreže i vrata,
fine ogradne mreže za peradarstvo i mreže za poljoprivredu
(uzgoj cvijeća i povrća).
Betonski čelik i toplo valjana žica,
- valjani betonski čelik, glatki
∅ 8, 10, 12, 14 i 16 u kolutu,
∅ 8, 10, 12, 14, 16, 18, 20, 22 i 25 u šipkama dužine
12 m.
- valjani betonski čelik, rebrasti
∅ 8, 10, 12 i 14 u kolutu,
∅ 8, 10, 12, 14, 16, 19, 22 i 25 u šipkama dužine 12 m.
- toplo valjana žica
∅ 8, 10, 12 i 14 u kolutu.
Jamstvo kvaliteta naših proizvoda je trideset-petogodišnje
iskustvo i priznata kvaliteta na domaćem i stranom tržištu.
Za sve naše proizvode izdajemo tvorničke ateste.
21 212 Kaštel Sućurac - Brižine b. b. – CROATIA
Phone: 385 21 202 - 111
Fax: 385 21 260 - 802
Telex: 261169 STZEL RH
Telegram:
“STELL WORKS SPLIT” - CROATIA - K. Sućurac
The company consists of the following plants:
Steel mill with electric arc furnace, ladle furnace and
continuos cast machines,
capacity 190 000 t/year of
continuously casted steel billets:
100 × 100 × 2000 - 6000 mm,
125 × 125 × 2000 - 6000 mm.
Qualities: - low carbon steel,
- middle carbon steel and
- low alloyed steel.
Rolling mill capacity 170.000 t/year of rolled product,
mostly:
- rolled reinforcing steel plain,
- rolled reinforcing steel, ribbed,
in coils and in bars,
- hot - rolled wire.
In further phase of processing,
Cold processing steel 35.000 t/year of the following
products: Cold rolling/drawing reinforcing steel (plain
and ribbed, bars and coils), all kinds of stirrup, walded
reinforcing meshes, wire netting fences and gates, poultry
wire meshes, wire mesh for agriculture (flower and
vegetable formes).
Rolled reinforcing steel and hot - rolled wire,
- rolled reinforcing, steel
∅ 8, 10, 12, 14 and 16 in coils,
∅ 8, 10, 12, 14, 16, 18, 20, 22 and 25 in bars lenght
12 m.
- rolled reinforcing steel ribbed
∅ 8, 10, 12 and 14 in coils,
∅ 8, 10, 12, 14, 16, 19, 22 and 25 in bars lenght 12 m.
- hot - rolled wire
∅ 8, 10, 12, 14 in coils.
35 years of experience and an approved quality of our
products in domestic and foreing markets are the best
guaranty of our company.
All our products are supplied with necessary test certificates.

J. J. Dańko, Dańko M. et al.: HoLTzER THE STaTE oF aRT aND FoRESIGHT oF WoRLD’S CaSTING PRoDUCTIoN ISSN 0543-5846
METaBk 45 (4) 333-340 (2006)
UDC - UDk 7.05:621.74(100)=111
THE STATE OF ART AND FORESIGHT OF WORLD’S CASTING PRODUCTION
J. Dańko, M. Holtzer, Faculty of Foundry Engineering University of
Mining and Metallurgy, Cracow, Poland
Received - Primljeno: 2005-11-10
accepted - Prihvaćeno: 2006-06-15
Review Paper - Pregledni rad
The state of art and foresight of world’s casting production is discussed in the paper on the basis of the latest
statistical data. The progress gained during the last few years in foundry engineering is shown as a way to
further development of foundry technology.
Key words: castings, foundry, foundry production, new foundry technologies
Stanje i predmnijevanje svjetske proizvodnje odljevaka. Na temelju posljednjih statističkih izvješća, u članku
se raspravlje o stanju i predmnijavanju svjetske proizvodnje odljevaka. Probitačan napredak tijekom nekoliko
posljednjih godina u ljevačkoj industriji se pokazao kao putokaz budućeg razvitka ljevačke tehnologije.
Ključne riječi: odljevci, ljevanje, ljevačka proizvodnja, nove ljevačke tehnologije
INTRODUCTION
The casting production is considered as one of the main
factors influencing the development of world economy.
actual capacity of the world’s casting production, which
is higher than 60 million metric tones per year, is strongly
diversified. The last decade brought significant changes in
the world map of the greatest casting producers. Globalisation
and transformation of economic systems is reflected
by variations of foundry production in different countries,
moreover the globalisation of economy is regarded not
only as a chance but also as a menace for the European
foundries.
SOME COMMENTS
ON THE HISTORY OF FOUNDRY
When considering the development of foundry engineering
in a historical aspect we tend to connect it with
the development of the human civilisation and to attribute
to it the high position among the oldest world professions.
In the times, from which the written sources are available,
such as Biblical verses, Egyptian drawings or illustrations
on ancient Greek vases (Figure 1.), existed already an
advanced casting handicraft intended for religious cults,
statues and armament elements.
Foundry production of middle ages consisted first of
all of bells, baptismal fonts, temple portals, grave plates,
cannons and other equipment for war purposes. Significant
development of the production technique and work
organisation took place within guild associations of bellfounders
and smelters.
The invention of printing by Gutenberg (1420) played
certainly an important role in the development of lowmelting
non-ferrous metal casting. an intensive search for
production methods for type-metals for whole founts led
to inventing of pressure die casting and machinery casting
(W. Church - 1822, D. Bruce - 1838, J. Sturgis - 1849).
Contemporary history is a continuation - in a global
aspect - of scientific research and popularisation of inventions
of a threshold importance. For foundry engineering it
means the continuous period of introduction of enormous
amount of the new versions of technologies, new materials,
new applications and innovative metallurgical processes
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(electrometallurgy) as well as a
real revolution in the production
management.
The driving force of the foundry
engineering is currently the automotive
industry, which requires
quality castings produced by means
of practically all available technologies
and casting materials. The
transfer from production in natural
moulding sands to a serial production
in synthetic ones occurred.
The quality of castings obtained
from special alloys reaches the level,
which meets the requirements of
a cosmic technique. The progress
and advancement of the material
engineering science gained lately
allow obtaining the strength properties
of alloys and composites like
from the fantasy-land.
ESTIMATION OF THE
CURRENT SITUATION
IN THE WORLD’S
CASTING PRODUCTION
The estimation of the current
state of the world’s casting production
can be done either globally or
with dividing into kinds of casting
materials, or taking into account
factor encompassing countries of
the given continent. In this last
case it is possible to separate four
groups of the countries, producers
of castings, according to the statistical
data published in Modern
Casting [2] (see Table 1.):
The first group consists of
countries of the highest castings
production, such as: USa, Japan, China and Russia.
The second group contains highly industrialised countries
of Western Europe: Germany, France, Great Britain,
Italy and Spain.
To the third group belong the extra-European countries,
such as: India, Brazil, South korea, Taiwan, Mexico and
Turkey, in which significant increase of production occurred
during the last decade.
The fourth group consists of countries of Middle-East
Europe: Poland, Czech Republic, Slovakia, Romania and
Hungary.
annual world’s casting production and percentage
participation of group of countries in world’s volume of
334
casting over analized period of time is shown in Table 2.
Previously, the first place belonged to the USa (11,871
mln tonnes), which in 2001 was overtaken by China (14,889
mln tonnes). Russia, after the decomposition of the Soviet
Union, decreased its casting production from approximately
18,0 mln tonnes in 1991 to 6,2 mln tonnes in 2001, which
means 65 % decrease [2, 3].
Casting production in Japan was gradually decreasing
from 1991 (7,958 mln tonnes) to the level of 5,841 mln
tonnes in 2001, which caused shifting Japan to the fourth
place in the global casting production.
out of the extra-European countries of a high dynamic
of development the first place belongs to India (3,155 mln
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J. Dańko et al.: THE STaTE oF aRT aND FoRESIGHT oF WoRLD’S CaSTING PRoDUCTIoN
tonnes). Brazil is the second (1,76 mln tonnes) South korea
the third (1,683 mln tonnes) and Mexico the fourth one (1,68
mln tonnes). Taiwan (1,209 mln tonnes) and Turkey (0,905
mln tonnes) supplement the list of countries, where the total
casting production achieved in 2001 - 10,3 million tonnes.
In the countries of the former Socialistic Countries
(Czech Republic, Poland, Romania and Hungary) the
significant decrease occurred already before 1991, thus
values given in Table 1. do not fully represent the observed
production decline. However, apart from the situation in
Hungary, this decline continued in the investigated period
(1991 - 2001).
as the result of social-economic changes in Poland, the
domestic casting production in the last two decades of the
20 th century decreased by 67 % [4]. During the analysed
period the casting production decline occurred also in
Great Britain (–48,5 %), Germany (–16,38 %), Belgium
(–17,4 %) and Norway (–7,1 %).
Development of casting production in some European
countries, estimated also for the period of the last two
decades of the 20 th century, is quite interesting. Statistical
data for those countries are as follows: Finland (increase
by 0.6%), Italy (+11,26 %), Portugal (+17,0 %), Holland
(+20,8 %), austria (+38,4 %), Sweden (+152,5 %), Spain
(+165 %).
among the European Union countries the main casting
producers are still: Germany (35,4 %), France (19,25 %)
and Italy (18,2 %). The shares of Great Britain (9,0 %),
Spain (8,4 %), austria (2,3 %), Sweden and Belgium (1,3
% each) are much smaller. The remaining countries have
only 3,8 % share.
The European foundry industry, according to data
evidenced in statistical reports [2, 3], is the third largest in
the world for ferrous casting and second largest for nonferrous.
The annual production of castings in the enlarged
European Union amounts to 11,7 million tones of ferrous
and 2,8 million tonnes of non-ferrous castings. Germany,
France and Italy are the top three producers in Europe,
with a total annual production of over two million tones
of castings each. Together, the top five countries produce
more than 80 % of the total European production.
The progress of material substitution for ferrous castings
extended in recent years caused the share of iron castings
in the output total to decline slightly, dropping, from
58,9 % in 2001 to 58,2 % in 2002. Producers of nodular
iron castings held at the same time a share of 34,3 % in
the output total, making an increase of 0,5 % compared
to preceding year. analogical data for malleable castings
shown expansion of their share from 1,1 % in 2001 to 1,3
% in 2002. Share of steel castings in the output total in
2002 is dropping 0,1% (to 5,8 %).
General statement is that the total European production
tonnage of ferrous castings has been stable over past
five years, although some fluctuation have occurred for
individual countries. The analysis of the presented data
shows that the figures for Great Britain (as an instance)
indicate a general declining trend in production output,
whereas the trend for Spain is one of growth. In recent
years, Spain has taken over the fourth position from Great
Britain, with both having a production of over one million
tonnes of castings.
The non-ferrous foundry sector has undergone steady
growth since 1998. In general in most countries production
has risen. The output of non-ferrous metal alloys is
still dominated by light metal casting at a share of 75,1 %,
despite a decline by 3,5 percentage points compared to the
year before. The share of copper alloys went down from 10,1
to 9,8 %, and the share held by the producers of zinc alloys
similarly shrank from 8,7 to 7,3 %. The noticeable in last
two decades development in the market for aluminum and
magnesium castings was mainly caused by a growing shift
of the automotive industry towards lighter vehicles.
although the production volume has remained relatively
stable over the past five years, there has been a decline in the
total number of foundries. Data on the number of foundries
show that there has been a general decline in the number
of foundries since 1998, with the loss of about 5 % of the
existing foundries each year (now approximately 3000
units), which is also reflected in the employment numbers
(now about 260.000 people). However, the foundry industry
is predominantly still an SME industry, with 80 % of
companies employing less than 250 people.
The foundry production which is now undertaken
results from fewer units and less employees. This can be
explained by progressive up scaling and automation in the
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J. Dańko et al.: THE STaTE oF aRT aND FoRESIGHT oF WoRLD’S CaSTING PRoDUCTIoN
foundry units. The relationship between unit size, production
and employment is well illustrated in Figure 2.
one can notice that the larger West European producers
(Germany, France) are attaining higher productiveness
with fever people. The more labor-consumption units
are found in the Eastern and Southern
part of Europe (Poland, Hungary, and
Portugal).
The main markets served by the
foundry industry are the automotive
(about 50 % of marked share), general
engineering (30 %) and construction (10
%) sectors. While iron castings mostly
(i.e. > 60 %) go to the automotive sector,
steel castings find their market in
the construction, machinery and valve
making industries.
IS THE FOUNDRY
INDUSTRY AS THE
PRODUCTION TECHNIQUE
HAVING A FUTURE? …
analysis of the world economy and
its development trends indicates for the
constantly growing share of foundry
industry as the production and treatment
technology of metal products. The biggest
growth of casting production takes
place in the countries being the economic
leaders, in which it constitutes the
significant part of the global income.
Continuous development of technologies
and means of production did
336
not cause any elimination of castings as a production
technique, but - on the contrary - increased its importance
and resulted in treating the foundry industry as a significant
and constant element of the economic and civilisation
development of nations. Direct shaping of metal products
of practically every degree of complication, realised by
the limited number of technological procedures, eliminating
several additional operations - necessary when other
production techniques are employed - constitutes still the
basic advantage of this method, even when castings are in
the range of the so-called “high-tech” (Figure 3.).
CHANCES AND DIRECTIONS OF THE FOUNDRY
INDUSTRY FURTHER DEVELOPMENT…
The most important research directions leading to
further development of the foundry industry:
- development of new technologies and casting alloys,
- melting and liquid metal preparation,
- preparation of casting materials and composites,
- manufacturing of moulds and cores,
- pouring, solidifying and cooling of castings,
- knocking out, cleaning and finishing of castings,
- technological waste management,
- new production systems and quality control.
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J. Dańko et al.: THE STaTE oF aRT aND FoRESIGHT oF WoRLD’S CaSTING PRoDUCTIoN
The comparison concerning directions, research advancements
and their implementations into the foundry industry
in the USa, Japan, and Europe is given in Table 3.
New technologies and casting alloys
Research will concentrate on the development and inventing
new casting materials, which microstructure could
be controlled on the molecular level. Investigations on amorphic
and nanocrystalline metallic materials will be continued
since they are characterised by unique properties:
- mechanical (high strength and resistance),
- physical (favourable magnetic properties [Fe-Co alloys],
superconductivity [Mo and Nb alloys]),
- chemical (corrosion resistance).
Investigations will also concentrate on magnesium alloys,
which are characterised by low density (they are 36%
lighter than aluminium alloys), high resistance and excellent
damping properties, good flowing power, possibility
of treatment and regeneration. after solving problems
concerning corrosion they will constitute the automotive
sector future. Their application will significantly lower
the weight of vehicles thus, contributing to environment
protection by diminishing their negative influence.
Research related to aDI cast steel, which due to a high
abrasion resistance accompanied with a very good ductility
will find wide application in many industrial sectors
substituting alloy cast steel or steel after thermal treatment,
will be continued.
Casting in the semi-solid metal state (SSM)
Casting in the semi-solid metal state SSM found the
application in thixocasting, rheocasting and thixomoulding
processes [5, 8].
The thixocasting process utilises the technology of
die casting of magnesium alloys, specially prepared before
introduction into the die-casting mould. Thixotropic
properties of material enable a laminar filling of die-casting
moulds, which eliminates gaseous porosity of castings and
non-metallic inclusions. Parts made in the SSM technology
apart from good mechanical properties (resistance,
elongation) are characterised by tightness, possibility of
thermal treatment and welding. This technology allows
substitution of expensive products obtained by plastic
forming procedure by products made in conventional die
casting machines of slightly changed parameters.
The casting process utilising rheological properties
of alloys (rheocasting) was invented by the Japanese
Company UBE Technologies. The most widely known
process version is New Rheocasting (NCR) developed
by the Company in 1996. Pictorial diagram of the NCR
process is given in Figure 4.
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J. Dańko et al.: THE STaTE oF aRT aND FoRESIGHT oF WoRLD’S CaSTING PRoDUCTIoN
Thixocasting (Thixomoulding) is the third modification
of the casting process utilising thixotropic properties
of metals being in the semi-solid state. This technology
was introduced in the middle of the last decade of the 20 th
century by the american Company Thixomat and has been
constantly developing since then. Pictorial diagram and
individual production phases of the Thixocasting process
are presented in Figure 5. [5, 8].
Melting and the preparation of metal
an intensive development of induction furnaces of
medium frequency, introduction of cokeless cupolas, with
an output of 3 - 20 tonnes of cast iron per hour, as well
as research aimed at significant energy saving (which has
both economic and ecological importance) - can be noticed
presently. out of several novelties, being currently
researched worth mentioning are:
- levitation melting, intended for alloys characterised by
high chemical affinity to the furnace lining (e.g. Tial).
The melting process is performed either in a vacuum
or in special protective atmosphere, which allows producing
alloys of a good purity. Due to an inspection
of electromagnetic phenomena there is a possibility
of checking metal parameters without generating any
turbulences;
- removal of non-metallic inclusions from melting metal
by means of a constant magnetic field. Investigations
carried on in Japan confirmed the method effectiveness
in removing silicon contaminations from aluminium alloys.
This can have great significance in the aluminium
scrap processing.
338
Preparation of casting materials and composites
Procedures of material and composites preparation are
essential for the quality of castings. a majority of casting
defects is caused by an improper selection of casting
materials and means of their processing [9].
Modern moulding sands circulations, characterised by
the introduction of microprocessor process control systems
and visualisations of several operations, will enable stabilising
moulding sand parameters thus, improving qualities
of moulds and castings.
Manufacturing of moulds and cores
Further progress in the methodology of moulding
utilising air jet blown directly into moulding sands can be
foresighted. Those are, apart from blowing methods: impulse
moulding, moulding by air stream blowing through
moulding sand followed by further press compacting,
and the vacuum press moulding [10 - 12]. The renewed
interest in a dynamic press moulding and vibratory-press
moulding machines constitute a good forecast for their
further application.
Flaskless moulding will further constitute the most
economic method of serial production of moulds for the
majority of small and medium size castings. The lower
limit of serial moulds production depends solely on the
costs of the model instrumentation, since the system of
automatic changes of instrumentation enables model
changing without the production interruption [13].
In the range of core-shop equipment and instrumentation
the development trends concern mostly the technology
of cores hardened in room temperatures.
Pouring, solidifying and cooling of castings
In modern casting plant these problems are inseparably
connected with the computerisation and utilisation of new
techniques and simulating tools. Techniques of computer
assisted technologies being now-a-days useful tools of
designing and production will become a must in foundries
aspiring to survive in the market.
Computer aided techniques can be applied in:
- model designing in CaD system (aesthetic shape, geometry,
volume, weight, etc.),
- simulation of functional properties at operating conditions
(strength, resistance, durability),
- simulation of the production process (casting, thermal
treatment),
- selection of treatment procedures and production (prototype,
instrumentation, mechanical treatment, quality
control).
Simulation processes will by applied in:
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J. Dańko et al.: THE STaTE oF aRT aND FoRESIGHT oF WoRLD’S CaSTING PRoDUCTIoN
- designing and drawing of the shape of the model,
- dimensioning of the model,
- defining the boundary conditions,
- performing the simulation of pouring and solidifying
processes as well as for the interpretation of the simulation
results,
- selecting thermal treatment and determination of stresses.
Environment protection
The foundry industry is a major player in the recycling of
metals [14]. Steel, cast iron and aluminum scrap is re-melted
into new products. Most possible negative environmental
effects of foundries are related to the presence of the thermal
processes and the use of mineral additives. Environmental
effects therefore are mainly related to the exhaust and offgases
and to the re-use or disposal of mineral residues. Emissions
to air are the key environmental concern. The foundry
process generates mineral dusts, acidifying compounds.
products of incomplete combustion and volatile organic carbons.
Dust is a major issue, since it is generated in all process
steps, in varying types and compositions. Dust is emitted
from metal melting, sand moulding, casting and finishing.
any dust generated may contain metal and metal oxide. In
foundry process, emissions to air typically not to be limited
to one (or several) fixed point(s). The process involves
various emission sources (e.g. from hot castings, sand, hot
metal). a key issue in emission reduction is not only to treat
the exhaust and off-gas flow, but also to capture it.
Since foundries deal with a thermal process, energy
efficiency and management of the generated heat are important
environmental aspects. However, due to the high
amount of transport and handling of the heat carrier (i.e.
the metal) and its slow cooling, the recovery of heat is not
always straightforward.
Foundries may have a high water consumption e.g. for
cooling and quenching operations. In most foundries, water
management involves an internal circulation of water, with
a major part of the water evaporating. The water is generally
used in cooling systems of electric furnaces (induction
or arc) or cupola furnaces. In general, the final volume of
waste water is very small. Nevertheless, when wet dedusting
techniques are used, the generated waste water requires
special attention. In high pressure die-casting, a waste
water stream is formed, which needs treatment to remove
organic (phenol, oil) compounds before its disposal.
The purpose of the Directive IPPC (Council Directive
96/61/EC) to achieve integrated prevention and control
of pollution arising from the activities listed in annex I,
leading to a high level of protection of the environment
as a whole [15].
one of the most important issues of the IPPC Directive
is application of the BaT principle. The BaT descriptions
contain mainly:
- characteristics of the process technology,
- specific production of emissions, waste and by-product
generation, needs to consumptions of raw materials and
energy inputs,
- the most effective technologies related to decreasing of
emissions and waste rates and to increasing of energy
savings,
- identification of BaT technologies,
- the new and developed technologies and processes.
CONCLUSIONS
European metalcasting industry, just as most European
and USa manufacturing, suffered greatly from the early in
this decade. Moreover, substantial dynamics in the global
economy, especially off-shore sourcing of cast metal components
as well as the off-shore manufacturing of durable
goods that require castings continue to profoundly reshape
European metal casting industry. The effects of the recession
were magnified by the influx of low-priced castings from
off-shore sources including Brazil, India and particularly
China. Nowadays it is becoming clear that economic trends
and technological advances are creating an inflection point
in the growth rate for cast metals components. The growth
in the world economy, particularly in such countries like:
China, Russia, India and Brazil will fuel demand for casting
related to transportation and an industrialized infrastructure.
according to opinion of M.W. Schwatzlander and R.E.
Showman [16] from ashland Casting Solution Group,
advanced in ferrous metallurgy, extraction metallurgy and
materials processing will provide new alloys and casting opportunities
that haven’t been seen since growth of aluminum
castings in the twentieth century. Improvements in casting
design and manufacturing processes will finally convert the
“black art” of foundry into a science.
Metalcasters need to invest in technology and in
people. a meaningful improvements in casting design,
modeling, prototyping and production will be of the highest
importance if foundries want to achieve increasing the
capabilities and lower costs.
Finally foundries need to invest in people. The knowledge
and skills needed to keep pace are changing even
faster than the technology. over the next 50 years, new
skills will need to be developed every three to five years.
ongoing training and education will be a must for successful
foundries.
REFERENCES
[1] T. Gutowski, Casting http://www.mit.edu/afs/athena/course/2/2.810/
oldfiles/ts_temp/Casting.ppt
[2] “Census of World Casting Production” 1991, 2003, 2004, 2005
Modern Casting No 12, (monthly journal, edited annually with
the data concerning the number of casting houses and the world
casting production in the year preceding the issue).
METALURGIJA 45 (2006) 4, 333-340 339

J. Dańko et al.: THE STaTE oF aRT aND FoRESIGHT oF WoRLD’S CaSTING PRoDUCTIoN
[3] J. Tybulczuk, J. Piaskowski: Technological Foresight. Forecasting
of the Foundry Engineering Development Taking into account
its Significance for the Economy. Part I: analysis of the World’s
Foresight, Two-monthly Journal ‘ Foundry Engineering - Science
- Practice , 6 (2004), Special Issue No 3.
[4] D. P. kanicki.: Global casting report: past, present and future.
Modern Casting (2000) 12, 24 - 34.
[5] J. aguilar, M. Fehlbier, P. R. Sahm: SSM processing of magnesium
alloys. Diecasting Times 4 (2002) 3, 13 - 14.
[6] F. J. Edler, G. Lagrene, R. Siepe: Thin-walled Mg Structural Parts
by a Low-pressure Sand Casting Process. Proceedings, International
Congress “Magnesium alloys and their applications”,
Monachium, 2000, pp. 553 - 557.
[7] aFS 2003 Metalcasting Processes Forecast and Trends, american
Foundry Soc. Des Plaines 2002.
[8] G. Chiarmetta, P. Giordano: Rheocasting in a class of its own.
Diecasting Times 4 (2002) 3, 22.
[9] “Data relating to the European Foundry Industry”. Committee of
European Foundry assoc. http://www.caef-eurofoundry.org/industry.htm.
CaEF 2002.
340
[10] J. Dańko, R. Dańko, M. Holtzer: Reclamation of used sands in
foundry production, Metallurgy 42 (2003) 3, 173 - 178.
[11] J. Dańko, z. Górny: Casting Research in Poland in the Last Decade.
Proceedings, 3 rd Congress of the Polish Foundry Engineering,
Warsaw, 1999, pp. 18 - 42.
[12] R. Dańko: Foundry Engineering, Tradition, Modernity and Future,
Foundry Journal 54 (2004) 4, 322 - 330.
[13] W. Hespers, M. Lustig: Systematic planning of investments in
moulding plants, allowing for technical and organizational developments.
Casting Plant and Technology (1988) 4, 14 - 23.
[14] M. Holtzer, J. Dańko, R. Dańko: Possibilities and limitations of
environmenal management in domestic foundries at the moment
of Poland’s joining to the UE structures. Proceedings, The Polish-
Romanian Conference, Cracow, 2003. pp. 39-49.
[15] European Commission. Integrated Pollution Prevention and Control.
Reference Document an Best available Techniques in the
Smitheries and Foundry Industry. Sevilla 2005. Finish Report.
[16] M. W. Swartzlander, R. E. Showman: Golden age of Castings,
2005-2050, aFS Transactions 2005, paper 05-046 (14), pp. 1 - 7.
METALURGIJA 45 (2006) 4, 333-340

Z. Z. KERAn, KERAn M. et al.: SKUnCA, FInITE M. ELEMEnT MATH APPROACH TO AnALYSIS OF AXISYMMETRIC REVERSE DRAWInG...
ISSN 0543-5846
METABK 45 (4) 341-346 (2006)
UDC - UDK 539.383:539.411:621.97=111
FINITE ELEMENT
APPROACH TO ANALYSIS OF AXISYMMETRIC REVERSE DRAWING PROCESS
Z. Keran, M. Skunca, M. Math, Faculty of Mechanical Engineering and
naval Architecture University of Zagreb, Zagreb, Croatia
Received - Primljeno: 2006-01-17
Accepted - Prihvaćeno: 2006-05-30
Review Paper - Pregledni rad
The intention of this research is to make analyze of deep drawing Cr-Ni stainless steel process. The research
is related to forces that appear in machine tool during the process and also to material stress and its behaviour.
The results are taken from two sources and their comparison is made. The first source of results are experiments
made on hydraulic press, and the other source are results obtained by creation of finite element model (FEM)
and process simulation on MSC Marc Mentat program package. The measurements are made in cases of different
reduction coefficient and different tool material. Comparison that is given is related to punch and pressure
plate forces, and the state of material stress for each reduction coefficient is observed too. Datasheets and force
diagrams present the results, and material stress can be seen on figures that are result of the simulation.
Key words: FEM, reverse drawing, material stresses, cracking possibility, MSC Marc program package
Pristup metodom konačnih elemenata analizi procesa osnosimetričnog protusmjernog dubokog vučenja.
Namjera provedenog istraživanja jest načiniti analizu procesa dubokog vučenja Cr-Ni nehrđajućeg čelika.
Istraživanje se odnosi na sile koje se javljaju u alatu tijekom procesa te također na pojavu naprezanja u materijalu
i ponašanje dotičnog naprezanja. Rezultati su uzeti iz dva izvora i načinjena je njihova usporedba. Prvi izvor su
rezultati eksperimenata izvedenih na hidrauličnoj preši, a drugi izvor čine rezultati dobiveni kreiranjem modela
metodom konačnih elemenata (MKE) i simulacija procesa pomoću programskog paketa MSC Marc Mentat.
Eksperimentalna mjerenja načinjena su za različite koeficijente redukcije. Dana je usporedba rezultata koji se
odnose na silu u žigu alata i pritisak na rondelu, a također je promatrano stanje naprezanja u materijalu za svaki
koeficijent redukcije. Rezultati su prikazani u obliku tablica i dijagrama, a naprezanja u materijalu prikazana su
na slikama dobivenim kao izlazni podaci simulacije procesa metodom konačnih elemenata.
Ključne riječi: MKE, protusmjerno vučenje, naprezanja u materijalu, mogućnost pucanja, MSC Marc Mentat
programski paket
INTRODuCTION
Deep drawing of a metal sheet is a standard technique
that is widely used in order to fabricate thousands of sheet
metal structures per day in many industries, e.g. automotive,
aerospace, beverage industry etc.
One of the biggest challenges in deep drawing metal
forming is to achieve the final product by very few draws.
Thus, it makes possible to reduce time and expenses of
production. Reverse drawing is an operation developed
from the standard deep drawing process. Its purpose is
to convert two draws of the standard process into one
operation. In this way one can have greater d 1 /d 2 ratio
without stopping the process and also without taking down
the working piece. As all of these actions take time to be
done, the time and of course the expenses are automatically
saved.
Actual position of reverse drawing process in the world
is a production of aluminium and copper and their alloy
products. Deep drawing of Cr-ni stainless steel presents
an actual problem because of a great hardening of these
alloys during metal forming processes [1].
However, reliable FE models and simulations for describing
the process are of a great value in reducing much
of the tool tryout work. In this way, improvements of the
process are made before making expensive tools needed
for experimentation. In that way experiments are needed
just to verify the simulation.
THE PRObLEM ESTAbLISHMENT
As we are trying to reduce the number of needed
draws, in each draw the reduction coefficient is becoming
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smaller than before, sometimes even smaller then recommended
one.
In sheet-forming processes however, several type of
failures could occur, such as rupturing, necking, wrinkling
and too large spring back that are undesirable. In this case
they are result of the existence of inappropriate forces and
material stresses during reverse drawing Cr-ni stainless
steel process. The main task is to avoid these failures by
careful analyzing of its all-possible causes.
The scheme of the reverse drawing operation shows
the way it works and its main components.
Looking the scheme, we can assume the way this
process works: in a first draw punch is moving into a die
in order to plastically deform a blank sheet of metal into
a desired shape as it does in usual deep drawing process,
and achieves d 1 diameter. After first draw is stopped, the
second draw punch is starting its motion in the opposite
direction. It is pushing the bottom of the working piece into
hollow punch, which now becomes a die for the second
draw, giving it new diameter d 2 . The working piece gets its
final shape and is pushed out by hydraulic knockout bar.
In a deep drawing process, change of working pieces
shape is made by simultaneous activity of tensile stress
on the outside surface of the piece, compressive stress on
the inside surface of the piece (result is diameter reducement),
and by bending the piece around bottom corners
of the punch (change of direction). Bending increases
sum-total of all stresses.
In a first draw, diameter reduction, from blank sheet diameter
to first draw diameter, can be relatively large because
the bending participation is usually small. On the opposite, in
other draws, the bending participation is greater and allowed
coefficient of shape changing must be reduced. The differ-
342
ence between bending of standard second draw and second
draw in reverse drawing is in number of direction changing
that occur in it. In standard deep drawing second draw exists
triple bending (1. bending in direction of motion, 2. bending
in the opposite direction, 3. straightening), and in reverse
drawing second draw it happens four times (1. bending in
direction of motion, 2. straightening, 3. bending in direction
of motion, 4. straightening). Because of that difference, there
is also a difference in stresses that appear in material. Very
good description of stress diference is β 2 - σ z (drawing ratio
- total stress) diagrams. Beside them are schemes of the
operations that show direction changes of material.
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It is obvious that because of greater stresses, second
draw in reverse drawing, and is very much alike to produce
some of the failures. That is why stresses should be
estimated and watched very carefully.
Main parameters that need to be carefully calculated
and considered are:
- reduction coefficients in each draw, related - needed
number of draws;
- tool dimensions and shapes;
- tool forces;
- material stresses and its hardness in each draw.
EXPERIMENTATION
The intention of experiments that were carried out
was to analyze a pot producing from a 1 mm thick blank
sheet of a diameter D 145 mm to a final diameter d 2 53
mm through two draws. After first draw, calculated and
achieved diameter was d 1 80 mm. Analyzed material was
Cr-ni stainless steel. Because of very few known data
about this material’s behaviour in reverse drawing processes,
some authors suggest heating on temperature of 150
- 200 şC [3]. This experimentation was referred to carrying
out a process in a cold state. Experiments were made on
double acting hydraulic press. The double action refers
to the clamping mechanism moving independently of the
punch mechanism. This allows for the boundaries of the
sheet blank to be clamped while the punch pushes the sheet
into the die cavity. The ability to independently control
both the clamp and the punch affords the opportunity for
various modifications of the experimental procedure. It
needs to be accented that reverse drawing processes are
recommended to be drawn at triple acting presses [4], but
because such equipment is not accessible, the experiment
was performed at double acting press.
A few questions got their answers by making modifications
in experimental parameters:
1. How much reduction coefficient of the first draw can
be reduced?
2. How does the punch force act if we change reduction
coefficient (by changing blank sheet diameter D, we
change reduction coefficient of the first draw)?
3. How does the punch force change in a second draw
in relation to the change of punch force and reduction
coefficient in a first draw?
Material properties
Material that was processed is X 5 Cr Ni 18 10 with:
0,037 % C; 0,343 % Si; 1,019 % Mn; 0,031 % P; 0,0015 %
S; 18,155 % Cr; 8,927 % Ni; 0,032 % N. But, as it is well
known, the same chemical composition can have different
mechanical properties. This is a consequence of different
ways of sheet rolling (different numbers of reduction), and
also different heating treatment. Mechanical properties are
given in Table 1. The most important mechanical property in
this case is ductility, expressed with A80 : 57,3 - 60,2 %.
Sheet surface was highly polished with foil rolled on
both sides that was used as a lubricant.
Experiment and the results
In metal forming technology standard experiment
models are applied. Usually those are factor analyses
with one or more factors. In this particular case, one-factor
experiment method is used. It can be observed that
in such experiments result dependence on just one factor
is a fiction. It is possible to find several more factors that
have influence on final result. Such idealisation in complex
cases can be justified in certain circumstances:
- if factors that are not expressed are maintained in constant
level,
- if their influence is negligible,
- if their influence is accidental and is possible to use
methods of mathematical statistics to separate their influence
from controlled factor in calculated experimental
error.
In this case condition of constant level is satisfied.
A choice about the number of experiments is made
according literature [5]. Probability of 50 % with probability
level of 0,90, demands at least 7 measurements for
each factor level.
The reduction coefficient is defined by the following
expression [6]:
D
m =
D
where:
METALURGIJA 45 (2006) 4, 341-346 343
1
0
(1)
m - reduction coefficient,
D 1 - pot diameter after specific draw,
D 0 - pot diameter or a blank sheet diameter before specific
draw.
It is well known that after any cold plastic deformation,
material strength grows up and ductility decreases. There-

Z. KERAn et al.: FInITE ELEMEnT APPROACH TO AnALYSIS OF AXISYMMETRIC REVERSE DRAWInG...
fore, reduction coefficient must be bigger in each draw,
and is specifically defined for each draw and also for each
material. In a first draw, its minimum is about 0,60 and in
a second draw its minimum is about 0,80. Because this numerical
coefficient grows up, it means that deformation level
becomes smaller which is acceptable in relation to a smaller
material ductility. When reduction coefficient is changed,
blank holder force is constant, punch force is changing too.
The smaller reduction coefficient is, the punch force grows
up. Also, the stress hardening grows up with smaller reduction
coefficient, and because of greater plastic deformation,
material strength grows up too and ductility decreases. no
special lubricant was used, but instead of it a polymer foil
was applied. Punch speed was 0,020 m/s.
344
In the experiment, reduction coefficient was changed
in a first draw from 0,55 to 0,66. With smaller reduction
coefficient built-in material stresses were too large, so, in
the second draw cracking took place. By changing reduction
coefficient, punch force was changing from 270 kN to
185 kN. According to plan of experiment 84 measurements
are made. Analyse is carried out using program package
SPSS for statistical analyses.
Third question that need an answer is related to the
second draw. It is very interesting to observe how changes
of parameters in a first draw influence on the change of
parameters in a second draw. Specifically: how does the
punch force change in a second draw in relation to the
change of punch force and reduction coefficient in a first
draw? Reduction coefficient in the second draw is constant
and amounted 0,68. Punch force in a second draw related to
reduction coefficient in a first draw is shown in Figure 5.
Cracking avoidance
As it is well known, mentioned sort of stainless steel is
a material with extreme hardening in metal forming processes.
That is why those processes demand great control
of all process parameters and avoidance of any unnecessary
imposed material stress. In this particular case problem can
be created with large blankholder force. It is expressed in
case of the smallest reduction coefficient in a first draw (m
= 0,55) when all stresses reach their maximal value. All
residual stresses are remaining in second draw and cause
cracking. To avoid it blankholder force in a first draw has
to be held in smallest level that provides regular drawing
– 20 kN. In greater reduction coefficients sum total of all
stresses is becoming smaller and naturally, risk of cracking
is smaller too [4].
Change of sheet thickness is a phenomenon that needs
to be observed and mentioned in context of cracking
possibility. In the experiment that was carried out sheet
thickness was measured on final product for each reduction
coefficient. The most important change occurred at
critical points (beginning of bottom round). This change
varied from 0,1 to 0,3 mm related to change of reduction
coefficient in a first draw. It is important to notice that
change of 0,3 mm is even 30 % of sheet thickness and
occurs when reduction coefficient reaches 0,55.
RESuLTS OF THE SIMuLATION
The numerical analysis was preformed using MSC
Marc Mentat elasto-plastic program commercial package.
In the presented deep drawing problem, the full newton-
Raphson iterative procedure is chosen to solve the iteration
process and nonlinear equations of motion. This method
has quadratic convergence properties and the stiffness
matrix is reassembled in each iteration. Convergence
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Z. KERAn et al.: FInITE ELEMEnT APPROACH TO AnALYSIS OF AXISYMMETRIC REVERSE DRAWInG...
can be slowed down by some approximations, but these
computational problems are of a less importance when
iterative solvers are used. Since material elements rotate
during deep drawing process, large displacement, finite
strain plasticity and updated Lagrange procedure need to
be adopted in calculation. In the Lagrangian approach, the
element stiffness is assembled in the current configuration
of the element, and the stress and strain output is given
with respect to the coordinate system in the updated configuration
of the element [7].
The stiffness is formed using four point Gaussian
integration. Because of large displacements request, an
additional contribution needed to be made to the stiffness
matrix. By default, the analysis program uses the
full stress tensor at the last iteration, which results in the
fastest convergence [7].
3D model was created. Fourth part is used, modeled
by 3D membrane shell elements number 139. This is four
nodes, thick shell element with global displacements and
rotations. Bilinear interpolation is used for the coordinates,
displacements and rotations. The membrane strains are obtained
from the displacement field, the curvatures from the
rotation field. The transverse shear strains are calculated at
the middle of the edges and interpolated to the integration
points. This 3D model is particularly interesting because
wrinkling occurrence can be easily detected.
The main intention of a FEM simulation analysis was
a detailed follow of material stresses and punch force behaviour
through the deep drawing process in both draws. In
that way the number of experiments could be reduced.
On the Figure 6. tool with its main parts is presented.
The position of the parts is in third quarter of the process
time.
The first interesting question in simulation analysis is
behaviour of material stress in the point in which it reaches
its greatest value. Figure 7. presents equivalent Von Mises
stress in working piece. It shows both draws simulated
using 3D membrane shell elements.
Minimal stress occurs on the top of the working piece,
and it grows toward bottom of the working piece. Critical
point is placed on the beginning ob bottom round. On
Figure 8. critical point in deep drawing processes is shown.
Legend shows scale expressed in n/mm 2 .
The second question is behaviour of punch force and
maximum of needed force for specific deep drawing process.
On diagrams presented on Figure 9. and Figure 10. is
the answer to the question. The axis x shows increments of
simulation computing, that are set task. There are 100 incre-
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Z. KERAn et al.: FInITE ELEMEnT APPROACH TO AnALYSIS OF AXISYMMETRIC REVERSE DRAWInG...
ments in working cycle and 5 increments in reciprocating
motion. The axis y shows punch force expressed in n.
It is important to notice that maximal computed force
in each draw is relatively close to the force got from the
experiments.
CONCLuSION
As it is presented, reducement in number of draws is
solved by reversed drawing. Because of complexity of
346
the process and because of sensibility of the main parameters,
FE modeling showed its best face. All the changes
were done at first on the FE model, and after that on the
experimental tool and part.
It is interesting to discuss results of punch force
changing related to the reduction coefficient changing.
By growing of reduction coefficient punch force decreases
following a regression tendency curve. For the observed
Cr-Ni stainless steel minimal reduction coefficient cannot
go under 0,55 because the cracking occurs in the second
draw. Punch force in the second draw is smaller, but by
reduction coefficient changing, it also follows its own
regression tendency curve.
Criterion of process success was avoidance of cracking
occurrence. That is because by sticking to calculated
process parameters no other problems took place [8].
Important occurrence that has to be notified is that
reduction coefficient of 0,55 in a first draw is critical point
in which all process parameters reach their critical value.
That happens because of extreme hardening of material.
This is the area that still needs to be improved by possible
heat treatment.
Another thing that needs to be discussed is process
simulation. By FE model creation and its processing we
can read all the forces, displacements and stresses in process
time. Punch motion was defined in increments. By
observing each increment it is possible to have monitoring
over all important process parameters as the process occurs.
In this way all changes of parameters can be verified
virtually before they happen in the real process.
REFERENCES
[1] Doege, Meyer, Saeed, FlieβkurvenAtlas metallisher Werkstoffe,
Hanser Verlog München, Wien, 1986.
[2] G. Oehler, Schnitt-Stanz und Ziehwerkzenge, Springer-Verlag,
Berlin, 1966.
[3] H. Radtke, Technologie des Stülpziehverfahrens, Bänder Bleche
Rohre, 1971.
[4] Deep drawing Large Parts in Four Cylinder Presses, D. J. Taylor,
MetalForming Magazine, October 1996.
[5] G. M. Clarke, Statistics and Experimental Design, Edward Arnold,
London, 1980.
[6] Deep drawing with Hydraulic Presses, AP&T north America,
MetalForming Magazine, October 2002.
[7] MARC - Users guide, MARC Analysis Corporation, Palo Alto,
California, Printed in U.S.A, 1996.
[8] Z. Keran, M. Škunca, M. Math: Predviđanje naprezanja u materijalu
i mogućnosti nastanka pukotina korištenjem MKE tijekom
oblikovanja deformiranjem, MATEST 2003, Brijuni, Hrvatska,
2003.
METALURGIJA 45 (2006) 4, 341-346

P. P. VIRdzEk, VIRdzEk k. et TEPLIcká al.: PRoGREssIVE METhods In dEsIGn And ThEIR APPLIcATIon In EnGInEERInG Issn 0543-5846 ...
METABk 45 (4) 347-351 (2006)
Udc - Udk 7.05:62:681.5:004.89=111
Progressive Methods
in design and their aPPlication in engineering industry
P. Virdzek, k. Teplická, BERG Faculty Technical University of košice,
košice, slovakia
Received - Primljeno: 2005-01-25
Accepted - Prihvaćeno: 2005-10-20
Review Paper - Pregledni rad
The problem of a product‘s life cycle against R&D time has occurred due to changes in the behavior of customers.
One possibility how to solve this problem is to use Information technologies and the concept of CIM (Computer
Integrated Manufacturing) that considerably reduces R&D time, production time and the time to market. The CIM
conception is based on the utilization of single modules (CAx systems) in the Design and Production planning
area, manufacturing area (CAD/CAPP/CAM) and others, integrated together into one functional unit.
Key words: design, product’s life cycle, R&D (Research and Development), CIM (Computer Integrated Manufacturing)
Napredne metode u dizajnu i njihova primjena u strojarstvu. Problem ciklusa radnog vijeka proizvoda
prema R&D pojavio se zbog promjena nastalih u ponašanju kupaca. Jedna od mogućnosti za rješavanje tog
problema je korištenje informatičke tehnologije i ideje o CIM (proizvodnja u objedinjavanju s kompjuterom) kojom
se značajno smanjuje vrijeme proizvodnje kao i vrijeme marketinga. Ideja CIM-a se zasniva na korištenju
pojedinih modula (CA-sustava) u području projektiranja i planiranja proizvodnje (CAPP), područje izrade (CAM)
kao i drugih, ujedinjenih u jednu funkcionalnu jedinicu.
Ključne riječi: dizajn, životni ciklus produkta, R&D (Istraživanje i razvoj), CIM (proizvodnja objedinjena s kompjuterom)
introduction
during last 10 years we have seen important changes
on the market, the customer’s power was increased,
customer became the center of attention and interest of
manufacturers. The market of today is more flexible and
customer guides its progress. Mass produced products
don’t satisfy the present customers.
The result of this development is consecutive decreasing
of the serial production and increasing of the variety of the
production programme and elasticity of production. The
marketing philosophy of the firm’s management is getting
forward and it responses very flexiblly to the specified
customer’s needs. The philosophy describes the style how
to fill and supply the customer needs. Ability to realize those
customer’s needs with the minimum huge of power - time,
people, energy, material, quality is also not neglected [1].
To create successful product means to handle it in all
areas. construction, technology, processing, surface working
are very important criteria, but product is very hardly
supported without design, packing and presentation. Product
which doesn’t satisfy all criteria is unsuccessful on the
market. during standard quality of actual products design is
something, that differentiates products from each other.
research and develoPMent
of new Products, their design
Research and development of new products, their
design presents the first stage in the life cycle of product
that determinates the functional properties, but it influences
the production facilities and efficiency of production in
the second stage.
design is very important instrument which creates one
part of the price of product for consumers and decides
general financial results. The high flexibility and the low
costs of the product modification are characteristic [2].
The problem between product life and time of product
development appeared due-to the customer behavior.
The solution of this problem is to use methodology with
the information technologies that secure reduction of
development, production and implementation time of the
product.
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P. VIRdzEk et al.: PRoGREssIVE METhods In dEsIGn And ThEIR APPLIcATIon In EnGInEERInG ...
For the small and middle firms it is not profitable to
employ designer for 8 hours per day. Relationship with the
external corporations is more economically interesting that
are providing complete services for the activity of the firm
at the area of design and presentation of problem solution
by the outsourcing. Focus of activity to design products
and interior was expanded on the graphic design.
From actual analysis of the labor 70 % and 80 % of the
total labour content resulted. This valuation is involved in
the production preparation, documentation. The project and
development of product influences 70 - 85 % of production
costs, but these phases create less then 10 % of the
product’s cost [4].
Today there are used a new instruments of design for
example: CAD, CAP, CAM, CIM (Figure 1.).
Simulation and visualization plays significant role in
these processes, mainly:
- some technologies,
- activities of the machine, robots, logistic and storage
facilities,
- plan and organization of working place, production
process, installation.
Using of cIM modul allows reduction of material and
energy severity, reduction of storage, abbreviation of the
time of production and development, increasing of the time
and power of using machines, and quality of product.
The computer support of the firm’s activity is solved
by the algorithms. There are activities which are very
hard to be automatized, they haven’t punctual algorithm
of their solution.
In these activities there are important long-time experiences
of the employers, know- how, intuition about problem,
technical intelligence. For computer support artificial intelligence
and expert system of the process decision is used.
Application of information technology allows using
principle of simultaneous engineering. The nature of sI
depends on actual product development and design of
production process. The goal of the sI is to minimalize
the general time of the implementation of innovation of
product, to obtain high standard of quality through the
lower costs. From the practical experiences it results, that
the sI brings development reduction about 50 - 300 %.
Progressive methods in design and their application in
customer marketing presents Figure 2.
Application of the simultaneous engineering is suitable
especially for complex products (e.g. a car, a computer,
a camera etc.) that have a long development time. Multi
professional solution teams participate in product and parts
development as well as in production process design. The
teams are closely co-operating and working parallel on a
certain product part and its mode of production and consist
of designers, ergonomics, technologists, marketing and
other experts, solving partial and integral tasks.
characteristic features are the following [3]:
- working with always actual information through the
jointly sharing databases,
- change in certain parts is considered in all other related
parts, groups and the whole product,
- simultaneous product design and production process
design. Visual monitoring of the whole production process
of designed products through the computer allows
designers to project satisfactory products in term of
technology and to detect and directly possible eliminate
difficulties in production already in design stage. It could
be also the source of innovation plans in many areas, e.g.
change in product shape is less expensive than eventual
change in production process.
The progressive tools that could be used in product
design are:
- dFM - design for Manufacturing - design /construction/
with regard to single /simple/ production of the products
and their parts in minimal production costs. [5],
- dFA - design for Assembly - design /construction/ with
regard to single /simple/ assembly of the product, using
the minimal amount/number/ of parts, constructional
adaptation of the product to the assembly automation
possibility or disassembly in product recycling [6],
- and others: dFc (design for cost), dFE (design for
Ecology) [5].
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P. VIRdzEk et al.: PRoGREssIVE METhods In dEsIGn And ThEIR APPLIcATIon In EnGInEERInG ...
These approaches are based on the idea of constructing
the product with regard to the next stages in the product
life cycle - production, assembly, recycling, etc.
The other opportunity to increase productivity and flexibility
of an enterprise is the FAsT PRodUcTIon concEPTIon.
It is based on product modular structure which
already in design stage allows to achieve short delivery time
/time from the customer order to the product delivery to the
customer/. The product is composed of pre-manufactured
universal and standard, unified parts /modules/, produced
and delivered by supplier’s /outsourcing/. The emphasis is
put upon interconnection and cooperation with suppliers
that cover also inventory management in the customer warehouse
by JIT conception. This allows eliminating check-in
of purchased parts at the consumer.
The philosophy could be used mainly in electronic and
car industry, e.g. commission systems - PC configurations.
The one advantage is fast and flexible production /product
finalization/ exactly according to customer requirements.
The other advantage is wide range of many variants,
achieved in the final assembly stage of the modular product
by the high flexibility and short production /finalization/
and delivery time [6].
The considerable role in new product research & development
plays construction of part or product prototype, that
represents the first real vision about the object /its model/
and allows to execute different test on it /design, assembly
ability, functional options of the product/. It also can be used
in marketing activities /starting of marketing canvass before
first products manufacturing,, demand of potential customer
for future product before manufacturing and modification
features of the product according to customer needs/.
Radical time reduction of preparing and prototype
manufacturing, increasing number of design variants and
manufacturing costs cutting is possible due to RAPId
PRoToTYPInG /RP/ technologies.
The basic principle of RP is, that object /part/ computer
interpretation serves as the primary input for a technological
facility that creates physical object with features close to the
final object without preliminary phases and special tools.
RP technologies infer from 3d cAd models information
for segmentation of the volume entity on layers and using of
special technique creates the layers. The idea is information
generating layers in computer, generating of physical layers
and their connection for model /prototype/ creation.
Some of the excellent CAD/CAM/CAE systems are
suitable for using of data preparation for rapid prototyping
facilities. They are very useful, if the system contains special
module for RP technology support /e.g. Unigraphics
system by Unigraphics solutions with UG/Rapid Prototyping
module/ [7].
In comparison with conventional production methods
prototype manufacturing by using Rapid prototyping methods
takes less time - days instead of months. The advantage
350
of RP methods is not only fast prototype manufacturing
in any development phase, but especially possibility to
manufacture wide range of modifications and construction
layouts of the designed product /prototype functional
samples/, which can be then tested and adapted.
The general feature of the RP methods is that work piece
formation is not performances by material off take as it is in
conventional cutting operation, but by consecutive addition
of material in form of powder or melt. A part is created layer
by layer. In this way it is possible to manufacture also shape
complicated parts with cavities, with sloping and horizontal
down sides within very little time.
RP is an universal method for model manufacturing
/without using forms, tools/, saving costs, useable in every
production sector because of ability to produce any shape.
The advantage is fast and exact model processing [3].
RP is for its high economic investment costs suitable
especially in major industrial enterprises, e.g. automobile
industry or in company’s specializied in Research & development
area. Next possible application of RP could
be in electronic and electro technical sector, in consumer
industry /black and white consumer electronics /, but also
in health service /articular substitutes/.
It is possible to assume that RP methods will be used
more and more in future. In future parallel with prototype
manufacturing the methods could be implicated for fast
and budget-priced manufacturing of conceptual models
/Rapid Modelling/, for tools and jigs manufacturing /Rapid
Tooling/, for piece and small-lot production and service
parts production.
conclusion
Productivity is a significant tool for increasing of competitiveness
an enterprise on internal and external markets.
It is needed to evaluate productivity in the complex way,
not only in manufacturing, but also in engineering activities
in pre-manufacturing stage. only shipshape integration
of activities of the all stages in product life cycle allows
innovation of products and production processes to overshoot
in the least time, by the optimal using of enterprise
resources considering customer needs. It allows flexible
and fast response to changing customer requirements and
leads an enterprise to the success and prosperity. Information
technologies /IT/ and computers utilization at the all
process from product development, design to its packaging,
expedition and delivery to the customer is useful in
term of the objective.
In spite of intersection of IT into the manufacturing
and non-productive /engineering, service/ operations, the
main integrating element of the whole enterprise process
are and will be qualified, motivated and satisfied staff, that
play the key role in transformation of data into information
and information into knowledge.
METALURGIJA 45 (2006) 4, 347-351

P. VIRdzEk et al.: PRoGREssIVE METhods In dEsIGn And ThEIR APPLIcATIon In EnGInEERInG ...
The complex systems implementation lay stress on
multifunctional /universal/ staff and communication
among people /team work/.
references
[1] A. csikósová, z. novek, k. kameníková: The work of marketing
in the education. International seminar, košice, 1999, 17 - 20.
[2] M. havrila: new technologies - Rapid Prototyping, AT&P Journal,
Bratislava, 2001, 88 - 89.
[3] I. kuric: cAPP - computer support for design and technical documentation,
University of Žilina, Žilina, 2000, 14 - 18.
[4] M. Kováč: New technics for innovation prepare in machine industry,
Transfer innovation (2001) 2, 13 - 16.
[5] I. kuric, R. debnár: computer support system, Ware (1998) 1, 10
- 12.
[6] J. N. Marcinčin: Connections of CAD/CAM/CAE system and
system of the high speed prototype. Engineering 6, 1999.
[7] J. Peterka, A. Janáč: CAD/CAM Systems. STU Bratislava, 1996.
Acknowledgement
This paper is part of grant 1/2574/05: Application of
the modern trends in management.
METALURGIJA 45 (2006) 4, 347-351 351

I. MAMUZIć
Glavni i odgovorni urednik časopisa Metalurgija
Editor-in-chief of Journal Metallurgy
Balakin Vladimir, Ukraine
Balaž Bartolomej, Slovakia
Billy Jozef, Slovakia
Bockus Stasys, Lithuania
Bohomolov Anatolij, Ukraine
Bratutin Vladimir, Ukraine
Bukhanovski Viktor, Ukraine
Buršak Marian, Slovakia
Capko Valerij, Ukraine
Constantinescu Dan, Romania
Čigurinski Jurij, Ukraine
Dančenko Vladimir, Ukraine
Dinik Julija, Ukraine
Dobatkin Sergej, Russia
Dolžanski Aleksej, Ukraine
Dron Nikolaj, Russia
Drozdov Aleksandar, Ukraine
Fajfar Peter, Slovenia
Franz Mladen, Croatia
†
Garan Vladimir, Ukraine
Gasik Mihail, Ukraine
Gojić Mirko, Croatia
Gordienko Aleksandar, Belaruss
Gornak Jan, Slovakia
Grozdanić Vladimir, Croatia
Gubenko Svetlana, Ukraine
Guljajev Jurij, Ukraine
Hidveghy Julius, Slovakia
Holtzer Mariusz, Poland
Hršak Damir, Croatia
Jakovlev Jurij, Ukraine
Kamkina Ludmila, Ukraine
Kliber Jan, Czech Republic
Kočubej Aleksandar, Ukraine
Krivenuk Vladimir, Ukraine
352
Popis recenzenata članaka objavljenih u časopisu Metalurgija u 2006. godini
List of Reviewers of the Articles Published in Journal Metallurgy in the Year 2006
Kuzemko Vladimir, Russia
Kvačkaj Tibor, Slovakia
Lazić Ladislav, Croatia
Loboda Valerij, Russia
Lomov Ivan, Ukraine
Longauer Margita, Slovakia
Longauer Svätoboj, Slovakia
Makarenkov Eugeniy, Ukraine
Malašenko Igor, Ukraine
Mamuzić Ilija, Croatia
Math Miljenko, Croatia
Michel Jan, Slovakia
Mihok Lubomir, Slovakia
Mironenko Aleksandar, Ukraine
Musijaka Vladimir, Russia
Negovski Aleksandar, Russia
Ostrovoj Dmitrij, Russia
Pališko Aleksej, Ukraine
Pandula Blažej, Slovakia
Pobal Igor, Belaruss
Povrzanović Aleksandar, Croatia
Projdak Jurij, Russia
Roubiček Vaclav, Czech Republic
Rybar Pavol, Slovakia
Sanin Anatolij, Ukraine
Syasev Andrej, Ukraine
Syasev Valerij, Ukraine
Šatoha Valerij, Ukraine
Ševčikova Jarmila, Slovakia
Šlomčak Georg, Ukraine
Veličko Aleksandar, Ukraine
Veselovsky Vladimir, Ukraine
Vodopivec Franc, Slovenia
Zrnik Jozef, Czech Republic
METALURGIJA 45 (2006) 4, 352

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