Symposium F Nanoceramics and Ceramic based ... - EMRS

EMRS Fall Meeting 2012 – Symposium F 

Nanoceramics and Ceramic based Nanocomposites 

The aim of this Symposium is to review current state - of - the - art in the 

multidisciplinary research on nanostructured ceramics and ceramic based 

nanocomposites with the primary focus on reinforcement the relationship between 

basic science and engineering at the nanoscale level. 

Scope: 

Progress in a wide range of structural, functional and bio - medical applications of 

nanoceramics and ceramic based nanocomposites crucially depend on the development 

of new fabrication and processing technologies, along with a fundamental 

understanding of the relationship between their micro(-nano)structure and final 

properties. This will be the topic of the Symposium. 

Oxide and non-oxide nanoceramics, glass/metal/carbon-ceramic composites (particle, 

nanofibers, nanotubes, graphene reinforced), in-situ and polymer derived 

nanocomposites in the form of nanopowders, coatings and bulk materials (monoliths, 

layered composites and FGM) will be the subject of the Symposium with application 

potential as: 

Structural nanoceramics as cutting tools, engine components, etc., with improved 

hardness, strength, fracture toughness, creep, thermal shock and oxidation 

resistance, etc. 

Functional nanoceramics and composites for electronic applications, dielectrics, 

ferroelectrics, and piezoelectric materials. Ceramics for microwave and wireless 

communication technologies, etc. 

Materials for biomedical applications in orthopaedics, dentistry, drug delivery, 

bioactive coatings and interfaces, tissue engineering, etc 

Nanoceramics related to global challenges in the fields of energy and environment, 

connected with energy production, storage, batteries, photovoltaics, fuel cells, solar 

cells, supercapacitors, thermoelectrics etc. 

Hot topics to be covered by the symposium: 

Advanced synthesis and processing technologies for nanopowder preparation and 

bulk & coating nanoceramics processing – plasma & laser synthesis, spark plasma 

sintering, etc. 

Micro/nano - structure characterization of nanoceramics and composites – AFM, 

HREM, XAFS, XPS, ETEM, etc. 

Mechanical and functional properties at nano level – nanohardness, nanotribology, 

nanoscratch, etc. 

Recent and potential applications of nanoceramics and ceramic based 

nanocomposites. 

List of invited speakers: 

Manuel Belmonte, Institute of Ceramics and Glass (ICV-CSIC), Madrid, Spain 

„Carbon nanotubes/Si3N4 nanocomposites for tribological and electrical emerging 

applications” 

Ulf Jansson, Uppsala University, Uppsala, Sweden, „Design of amorphous and 

nanocomposite metal carbide“ 

Hans-Joachim Kleebe, Technische Universität Darmstadt, Germany, „Microstructure 

characterization of nanoceramics” 

Pavol Šajgalík, IICh SAS, Bratislava, Slovakia, „Si3N4+ SiC nanoceramics with 

excellent room and high temperature properties“ 

János Szépvölgyi, Research Centre for Natural Sciences, Budapest, Hungary,

„Thermal plasma synthesis of ceramic nanopowders and their characterization“ 

Richard Todd, University of Oxford, Oxford, United Kingdom, „Aligned and 

continuous MWCNT/glass-ceramic nanocomposites" 

Paula Vilarinho, University of Aveiro, Aveiro, Portugal, „Development and properties 

of functional nanoceramics“ 

Ashok Vaseashta, IASC/ICWI/NUARI and U.S. Dept. of State, Washington, DC, USA, 

„Nanoceramic based fibers for force protection and situational awareness" 

Markus Winterer, University Duisburg - Essen, Duisburg, Germany, „Nanocrystalline 

Composites based on Zinc Oxide: Preparation, Characterization and Properties“ 

Nitin P. Padture,Brown University, Providence, USA, “Perspective on Nanoceramics, 

Nanocomposites, and Carbon Nanomaterials for Structural and Functional 

Applications" 

Scientific Committee: 

Sergey Barinov, A.A. Baikov's Institute for Metallurgy and Materials Science, 

Moscow, Russia, ( barinov_s@mail.ru) 

Alida Bellosi, CNR-IRTEC, Faenza, Italy; ( bellosi@irtec1.bo.cnr.it) 

Aldo R. Boccaccini, University of Erlangen-Nuremberg, Germany; 

(aldo.boccaccini@ww.uni-erlangen.de) 

Robert Danzer, Montanuniversität Leoben, Austria, ( isfk@unileoben.ac.at) 

Gilbert Fantozzi, INSA de Lyon, France; ( gilbert.fantozzi@insa-lyon.fr) 

Irina Hussainova, Tallinn University of Technology, Estonia; (irhus@staff.ttu.ee) 

Tomaž Kosmač, „Jožef Stefan” Institute, Ljubljana, Slovenia; (tomaz.kosmac@ijs.si) 

Jakob Kuebler, EMPA; ( jakob.kuebler@empa.ch) 

Hua-Tay Lin - Oak Ridge National Laboratory, USA; ( linh@ornl.gov) 

Karel Maca, Brno University of Technology, Czech Republic; (maca@fme.vutbr.cz) 

Jose S. Moya, ICMM, Madrid, Spain; ( jsmoya@icmm.csic.es) 

Markus Niederberger, ETH Zürich, Switzerland: (markus.niederberger@mat.ethz.ch) 

Christian Mitterer, Montanuniversität Leoben, Austria; 

(Christian.Mitterer@unileoben.ac.at) 

Evagelia G. Moshopoulou, National Center for Scientific Research “Demokritos“, 

Athens, Greece; ( evagelia@ims.demokritos.gr) 

Jindrich Musil, University of West Bohemia, Plzen, Czech Republic; 

(musil@kfy.zcu.cz) 

Nitin P. Padture, Brown University, Providence, USA; ( padture.1@osu.edu) 

Mikolaj Szafran, Warsaw University of Technology, Poland; (szafran@ch.pw.edu.pl) 

Vladimir V. Srdič, University of Novi Sad, Serbia; ( srdicvv@uns.ac.rs) 

Pavol Šajgalík, IICh SAS, Bratislava, Slovakia: ( uachsajg@savba.sk) 

Gerold Schneider, TU Hamburg, Germany; ( g.schneider@tu-harburg.de) 

János Szépvölgyi, Research Centre for Natural Sciences, Budapest, Hungary; 

( szepvol@chemres.hu) 

Junichi Tatami, Yokohama National University, Japan; ( tatami@ynu.ac.jp) 

Richard Todd, University of Oxford, Oxford, United Kingdom; 

(richard.todd@materials.ox.ac.uk) 

Tseung – Yuen Tseng, National Chiao-Tung University, Taiwan; 

(tseng@cc.nctu.edu.tw) 

Ashok Vaseashta, IASC/ICWI/NUARI and U.S. Dept. of State, Washington, DC, USA; 

( prof.vaseashta@ieee.org) 

The presented lectures and posters will be published in: 

Journal of the European Ceramic Society (Impact Factor: 2.574) 

Central European Journal of Chemistry (Impact factor: 0.991) 

The reviewers will select the papers for the individual Journals.

Symposium organizers: 

Ján Dusza 

Institute of Materials Research, SAS 

Watsonova 47 

043 53 Kosice 

Slovakia 

Phone: +421 55 7922 462 

Fax: +421 55 7922 408 

jdusza@imr.saske.sk 

Csaba Balázsi 

Ceramics and Nanocomposites Department 

Research Institute for Technical Physics and Materials Science 

Konkoly-Thege M. út 29-33 

1121 Budapest 

Hungary 

Phone: +36 1 392 2249 

Fax: +36 1 392 2226 

balazsi@mfa.kfki.hu 

Witold Łojkowski 

Institute of High Pressure Physics 

Polish Academy of Sciences 

Sokołowska 29/37 

01-142 Warszawa 

Poland 

Phone: + 48 22 8880006 

Fax: +48 22 6324218 

wl@unipress.waw.pl 

Mike. J. Reece 

School of Engineering and Materials Science 

Queen Mary University of London 

Mile End Rd 

London E1 4NS 

UK 

Phone: +44 20 7882 7786 

m.j.reece@qmul.ac.uk 

Ralf Riedel 

Technische Universität Darmstadt 

Petersenstrasse 23 

64287 Darmstadt 

Germany 

Phone: +49 6151 16 6347 

Fax number: +49 6151 16 6346 

riedel@materials.tu-darmstadt.de

Symposium: F 

Nanoceramics and Ceramic based Nanocomposites 

17 September 2012 

start at Subject Num. 

Session I : - 

09:00 Perspective on Nanoceramics, Nanocomposites, and Carbon 

Nanomaterials for Structural and Functional Applications 

Authors : Nitin P. Padture 

Affiliations : Brown University, Providence, RI, USA 

Resume: There has been great interest in refining the grain 

size of polycrystalline ceramics down to the nanometer 

scale, and in introducing ceramic nanodispersoids or carbon 

nanotubes as reinforcements in ceramics. This is with the 

anticipation of improving mechanical properties of these 

nanoceramics and nanocomposites. I will present examples 

of transparent ceramics whose mechanical properties have 

been enhanced through grain refinement or incorporation of 

non-oxide ceramic nanodispersoids while maintaining optical 

transparency. I will present some results on ceramic/singlewall 

carbon nanotubes composites that possess 

unprecedented, hierarchical grain-boundary structures. 

These nanocomposites are beginning to show promising 

mechanical properties that could be tailored: contactdamage 

resistance, toughness, and high-temperature creep. 

Outstanding questions pertaining to these composites will be 

discussed. In keeping with the carbon nanomaterials theme, 

I will present some concepts where mechanics is used for 

the high-throughput nanomanufacturing of graphene for 

functional applications. 

09:45 Transmission Electron Microscopy Characterization of 

Nanostructured Polymer-Derived Ceramics 

Authors : Hans-Joachim Kleebe, Emanuel Ionescu and Ralf 

Riedel 

Affiliations : Technische Universität Darmstadt, Material- and 

Geoscience Department, Petersenstr. 23, D-64287 

Darmstadt, Germany 

Resume: The development of novel, polymer-derived 

ceramics commonly also involves a detailed characterization 

of the intrinsic micro/nanostructure of the materials with the 

overall objective to correlated characteristic microstructural 

features with corresponding properties. In this presentation, 

emphasis is placed on transmission electron microscopy 

(TEM) studies of polymer-derived ceramics, in particular, 

silicon oxycarbide (SiCO). Pronounced variations of the 

crystallite size of hafnia (HfO2) precipitates in SiOC-HfO2 

ceramic nanocomposites were observed upon annealing bulk 

samples at 1300°C for times ranging from 1 to 200 hrs. TEM 

investigations revealed homogeneous nucleation and 

crystallization of hafnia in the amorphous, Hf-bearing SiOC 

matrix upon pyrolysis at 1300°C. Unexpectedly, hightemperature 

anneal resulted in a pronounced coarsening of 

the hafnia crystallites at internal surfaces, due to a decrease 

of the C-content at surface near regions. Based on the 

F-I 

1 

F-I 

2

crystallite size, the diffusion coefficient of Hf was calculated 

via the Lifshitz-Slyozov-Wagner (LSW) theory for Ostwald 

ripening for both the bulk and internal surface regions. The 

diffusion coefficient of hafnium, DHf, in the C-depleted 

surface areas was 10-18 m²/s, while DHf of the SiOC bulk 

was three orders of magnitude lower with 10-21 m²/s. The 

present work underlines that the polymer-derived ceramics 

are in fact prone to phase separation and local chemical 

changes upon high-temperature treatment and are not as 

stable as commonly considered. Moreover, the effect of the 

local carbon content within the sample will be highlighted 

throughout the talk. In addition, the variation of the starting 

precursor (in the system SiCN) with different polymer 

architecture can result in the formation of different network 

structures and as a consequence different crystallization 

behaviour. 

10:30 Coffee Break 

Session II : - 

11:00 Aligned and continuous MWCNT/glass-ceramic 

nanocomposites 

Authors : R.I. Todd, G. Otieno, N. Grobert 

Affiliations : University of Oxford 

Resume: There are few reliable reports of significant 

toughening of inorganic matrices by the addition of carbon 

nanotubes (CNTs). Important issues include the alignment 

and dispersion of the CNTs, degree of bonding to the matrix 

and failure mechanisms. This presentation reports an 

investigation of these matters through the production of 

glass matrix composites by infiltration of CVD-grown 

multiwalled CNT carpets with a precursor sol. After 

densification, the composites contain 20% multiwall CNTs 

which are well dispersed, aligned and continuous over 

distances of several mm. The elastic properties and fracture 

behaviour have been investigated using microcantilever 

beams, milled at the surface by focused ion beams (FIB) and 

tested to failure using a nanoindenter. The CNTs were found 

to be strongly bonded to the glass matrix. Non-linear stressstrain 

response and hysteresis in subcritical loading 

indicated interwall sliding. Analysis of failure showed that 

the sliding occurred over distances of several micrometres. 

The fracture toughness was increased by a factor of 3 

compared with the unreinforced glass matrix and the 

majority of this improvement was found to be a result of 

bridging of the crack surfaces by intact CNTs. Dissipation of 

energy by pullout-type mechanisms was limited by sword in 

sheath failure of the individual nanotubes. 

Recommendations for improving the toughness of such 

composites will be made in the light of the results. 

11:35 One Dimensional (1D) Composites of MWCNT/BiFeO3 

Authors : Amit Mahajan (1), Paula M. Vilarinho (1), Angus 

Kingon (2), and Ákos Kukovecz (3) 

Affiliations : (1) Department of Materials and Ceramic 

Engineering, CICECO, University of Aveiro, 3810-193 Aveiro, 

F- 

II 

1 

F- 

II 

2

Portugal (2) Division of Engineering, Brown University, 

Providence, Rhode Island 02912, USA and (3) Department 

of Applied and Environmental Chemistry, Faculty of 

Sciences, University of Szeged, H-6720 Szeged, Hungary email: 

mahajan@ua.pt 

Resume: Top-down approaches for continuous scaling-down 

of devices and components in semiconductor industries is 

getting increasingly difficult and expensive, and thus 

bottom–up strategies, e.g., growth of functional nanostructures 

using nanowires or nanotubes are being explored. 

Carbon nanotubes (CNT) are an interesting option under 

consideration due to their extraordinary physical and 

electrical properties that make them suitable for 

microelectronic applications. In recent years, the fabrication 

of one-dimension (1D) ferroelectric (FE) nanostructures 

have been investigated as a capacitor for future 3D 

memories by using MWCNT as template or bottom electrode. 

Therefore, efforts have been made to coat MWCNT with 

barium titanate and lead zirconate titanate, among others. 

However, several difficulties need to be overcome in 

particular in the fabrication of 1D MWCNT/FE composites. In 

this work we report our approach of coating MWCNT with 

bismuth ferrite (BiFeO3, BFO), a lead free multiferroic. 

Functionalized MWCNT with diameter and length around 15- 

35 nm and ~4 µm, respectively were dispersed in the BFO 

sol gel solution and stirred at 70 -110 ºC followed by 

annealing at 350-500 ºC, to obtained the 1D composites 

having diameter of 30-100 nm and length up of few µm. The 

preliminary investigations on the coating of MWCNT array by 

BFO by sol gel were also studied. Composites were 

investigated by DTA/TG, XRD and for morphology by SEM 

and TEM. 

11:55 The Effect of CNTs on the Sintering and Grain Growth of 

Ceramics 

Authors : Ben Milsom1, Giuseppe Viola1, Zhipeng Gao1, 

Micheal Reece1,2 

Affiliations : 1. Queen Mary University of London, Mile End 

Road, London, E1 4NS 2. Nanoforce Technology Ltd, Queen 

Mary University of London, Mile End Road, E1 4NS 

Resume: The effect of carbon nanotubes (CNTs) on the 

sintering behaviour and grain growth of ceramics was 

studied using Yttria partially stabilised Zirconia and Boron 

Carbide as model systems. The CNTs simultaneously 

enhance densification and retard grain growth. The sintering 

activation energy was calculated using isothermal conditions 

produced by Spark Plasma Sintering (SPS) with a rapid 

heating rate for the monolithic materials as well as ceramic 

CNT composites (0.5 and 2 vol%). These compositions look 

at the effect both below and above the electrical percolation 

threshold respectively. A significant reduction of the 

activation energy for the ceramic 2vol% CNT composites is 

attributed to the formation of a percolating network of CNTs 

providing a lower energy diffusion pathway. The sintering 

mechanism was found to be grain boundary diffusion for all 

samples suggesting that the presence of CNTs does not 

change the sintering mechanism but does lower the 

activation energy for the rate limiting step in the sintering 

F- 

II 

3

process. The reduction in grain growth is attributed to the 

poor wetability of the CNTs acting as a physical barrier to 

prevent grain growth. 

12:10 Preparation and Characterization of Transparent Fiber 

Electrodes Based on CNT-s Metal Oxides 

Authors : Madis Paalo1, Tanel Tätte1, Medhat Hussainov1, 

Kelli Hanschmidt1, Madis Lobjakas1, Ants Lõhmus1, Uno 

Mäeorg2, Ilmar Kink1 

Affiliations : 1Institute of Physics, University of Tartu, 

Estonia; 2Institute of Chemistry, University of Tartu, Estonia 

12:30 Lunch 

Resume: During the past decade, significant efforts have 

been made to convert extraordinary and unique properties 

of carbon nanotubes (CNT-s) for bulk materials in order to 

give them some novel functionality. To take advantage of 

the unique properties of CNT-s, numerous studies have 

carried out on reinforcing different materials. Resulting 

composites combine the properties of CNT-s and the matrix 

material. CNT doping is widely acknowledged as a means of 

improving tensile strength and electrical properties of 

organic polymers [1]. Aforementioned materials may still 

not be suitable for applications under harsh conditions. 

Contrary to organic polymers, high corrosion resistance and 

thermal stability makes metal oxide ceramics very attractive 

candidates to be alternatively used as CNT composite 

matrices. A wide selection of papers have published in 

recent years, reporting nanotubes in ceramic matrices like 

SiO2, Al2O3, MgO, SiC, TiN, BaTiO3 etc. [2]. In the current 

paper we describe our studies of the preparation and 

characterization of CNT doped ceramic composites obtained 

by sol-gel chemistry. After the rheology measurements 

fiber-shape electrodes were prepared by pulling jets from 

polymerized CNT-alkoxide mass. SEM and FIB analysis 

revealed that fiber-pulling process orients CNT-s in host 

matrix. The electrical properties of the materials were 

measured by 4-point method using In-Ga alloy contacts. The 

fibers consisting 1% MWCNTs achieved electrical 

conductance up to 15 S/m, while electrical conductance of 

undoped titanium dioxide is approximately 10^-16 S/m. 

References [1] Spitalskya Z., Tasisb D., Papagelisb K., 

Galiotis C., Prog. Polym. Sci., 2010, 35, 357–401 [2] Cho J., 

Boccaccini A. R., Shaffer M. S. P., J Mater Sci, 2009, 44, 

1934-1951 

Session III : - 

14:00 Carbon nanotubes/Si3N4 nanocomposites for tribological 

and electrical emerging applications 

Authors : P. Miranzo, M.I. Osendi, M. Belmonte 

Affiliations : Institute of Ceramics and Glass (ICV-CSIC), 

Madrid, Spain 

Resume: Silicon nitride (Si3N4) based materials are well 

known for their extraordinary strength and hardness that 

make them suitable for applications under wear conditions. 

F- 

II 

4 

F- 

III 

1

However, the new demanding tribological conditions linked 

to the energy and transportation industries require new 

materials with enhanced properties. Besides, the full 

potentiality of these ceramics in emerging applications such 

as micro-turbines, MEMS, micro-reactors, and microbioimplants, 

will depend on our ability to machine them. To 

overcome these challenges, a new class of Si3N4 

nanocomposites containing carbon nanotubes (CNTs), which 

have created a great expectation due to their outstanding 

mechanical, electrical, and thermal properties, have been 

developed. In the present work, the tribological and 

electrical properties of dense good-dispersed CNTs 

containing Si3N4 nanocomposites were investigated looking 

for both a promising alternative to substitute metallic 

components in highly pressurized gasoline direct injection 

systems and manufacturing 3D intricate parts by means 

alternative machining process that requires sufficient 

electrical conductivity of the materials, such as electrical 

discharge machining (EDM). CNTs/Si3N4 nanocomposites 

exhibited an enhanced tribological performance with a raise 

of 13 orders of magnitude in the electrical conductivity 

compared to the monolithic. Based on these results, a 

micro-rotor was electrical discharge machined for the first. 

14:35 Tribological properties of Si3N4 graphene and Si3N4 CNT 

nanocomposites 

Authors : Pavol Hvizdos, Jan Dusza, Csaba Balazsi 

Affiliations : Institute of Materials Research, Slovak Academy 

of Sciences, Watsonova 47, 04353 Kosice, Slovakia; 

Ceramics and Nanocomposites Department, Research 

Institute for Technical Physics and Materials Science, 

Hungarian Academy of Science, Konkoly-Thege 29-33, H- 

1121 Budapest, Hungary 

Resume: Mechanical and tribological properties of 

nanocomposites with silicon nitride matrix with addition of 

various amounts of graphene platelets and carbon 

nanotubes were studied. Hardness and modulus of elasticity 

were measured by nanoindentation. The wear behaviour was 

observed by means of the ball-on-disk technique with a 

silicon nitride ball used as the tribological counterpart at 

room temperature in dry sliding. Coefficient of friction and 

specific wear rates were calculated and related to the 

damage mechanisms observed in the wear tracks. The 

measured properties were then assessed with respect to the 

type and volume fraction of the carbon phase additives. 

14:55 Dispersion of carbon nanostructure in silicon-nitride based 

ceramic composites 

Authors : Orsolya Tapasztó(1), Levente Tapasztó(1), Márton 

Markó(2) and Csaba Balázsi(1) 

Affiliations : (1) Research Centre for Natural Sciences 

Institute for Technical Physics and Materials Science, 

Budapest, Hungary; (2) Institute for Solid State Physics and 

Optics Wigner Research Centre for Physics of the H.A.S. 

Budapest, Hungary 

Resume: Carbon nanostructures are often employed as 

F- 

III 

2 

F- 

III 

3

filler materials for ceramic matrix composites in order to 

improve their electrical and mechanical properties. [1] One 

of the major challenges in nanocomposite preparation is that 

the nanoscale fillers have a strong tendency toward 

agglomeration, whereupon the mechanical and electrical 

properties of the resulting composites are substantially 

deteriorated. To characterize the dispersion degree of 

carbon nanostructures inside the ceramic matrix, we applied 

small angle neutron scattering (SANS) measurements, which 

are able to provide information about the dispersion of the 

nanostructures throughout the whole volume of the sample 

[2], [3], in contrast to electron microscopy investigations, 

which only provide local information. Using the SANS 

method we, demonstrate that different carbon 

nanostructures (e.g., single-wall and multi-wall carbon 

nanotubes and few layer graphene) can display strikingly 

different distribution patters within the ceramic matrix. The 

obtained results enable us to experimentally correlate the 

dispersion level of carbon nanostructures and the 

mechanical properties of the resulting composites. [1] Cs. 

Balázsi, Z. Kónya, F. Wéber, L.P. Biró , P. Arató, Mater. Sci. 

Eng. C 23 (6–8) (2003) 1133–1137. [2] O. Koszor, L. 

Tapasztó, M. Márton, Cs. Balázsi, Appl. Phys. Lett. 93 (20) 

(2008) 201910. [3] O. Tapasztó et al. Chem. Phys. Lett. 

511, 340 (2011) 

15:10 LiFePO4 /Carbon Nanocomposites as High Performance 

Cathode Materials for Lithium Ion Batteries 

Authors : N.A. Hamid1, S. Wennig2, S. Hardt1, C. 

Schulz1,3, H. Wiggers1,3 

Affiliations : 1Institute for Combustion and Gasdynamics 

(IVG), University of Duisburg-Essen, Duisburg, Germany 

2Zentrum für Brennstoffzellen Technik, ZBT GmbH, 

Duisburg, Germany 3Center for Nanointegration Duisburg- 

Essen (CENIDE), University of Duisburg-Essen, Duisburg, 

Germany 

Resume: Olivine LiFePO4 is one of the most promising 

alternatives as cathode material for Li ion battery as it 

possesses several advantageous compared to conventional 

LiCoO2. It combines highly available and affordable 

materials with improved safety and reduced toxicity. 

Conversely, its low intrinsic electric and ionic conductivity 

leads to inferior rate performance thus hampering its broad 

utilization in Li-ion batteries. Nevertheless, a few ways were 

identified in view of enhancing the rate performance and 

conductivity of LiFePO4 such as minimizing the particle size, 

doping with Mn, Al, Ti and coating with conductive carbon 

layer. Towards this idea, we used a combined gas-phase and 

solid-state reaction enabling high production rates to 

synthesize LiFePO4 with varying amount of conductive 

carbon. From the XPS and XRD measurement, we found that 

the LiFePO4/C composites were free from impurities and 

exhibited a particle size of about 26 to 88 nm. To optimize 

the impact of conductive carbon on the electrical 

conductivity, its amount was varied from 2 to 8 wt% and its 

influence towards the electrochemical performance was 

studied with electrochemical impedance spectroscopy, cyclic 

voltammetry and electrochemical cycling. We found that 

F- 

III 

4

excess as well as too low amounts of carbon leads to poor 

performances as the pathways were blocked or the electric 

conductivities were poor while about 5 wt% of carbon was 

found to yield good electrochemical properties even at high 

charge rates. Electrochemical investigations of the final 

LiFePO4/C composites show reversible capacities of more 

than 150 mAh g-1. The material supports high drain rates at 

16 C while delivering 80 mAh/g and causes excellent cycle 

stability. 


Session IV : - 

16:00 Si3N4+ SiC nanoceramics with excellent room and high 

temperature properties 

Authors : Pavol Šajgalík, Štefánia Lojanová, Miroslav 

Hnatko, Zoltán Lenčéš, Marián Gall, *Zdeněk Chlup 

Affiliations : Institute of Inorganic Chemistry, Slovak 

Academy of Sciences, Bratislava, Slovak Republic *Institute 

of Physics of Materials, Academy of Sciences of the Czech 

Republic, Brno, Czech Republic 

Resume: Dense Si3N4/SiC micro/nano composites with 

varying composition of grain boundary phase were 

fabricated by hot–pressing method at the same sintering 

conditions. Six different sintering aids (Lu2O3, Yb2O3, 

Y2O3, Sm2O3, Nd2O3 and La2O3) were used to their 

processing. Formation of SiC nano–inclusions was achieved 

by in situ carbothermal reduction of SiO2 by C during the 

sintering process. Room temperature fracture toughness, 

hardness and strength showed increasing tendency when 

the used rare-earth element in the oxide additive changes 

from a large to a small rare-earth cation (i.e. from La3+ to 

Lu3+). Besides the highest hardness and reasonably high 

fracture toughness and strength of composite material with 

Lu2O3 sintering additive also the highest creep resistance 

was observed for this micro/nano composite in the 

temperature range from 1250 to 1400 °C at the loads of the 

interval from 50 MPa to 150 MPa. GB phase strength itself 

and strength of the bond between silicon nitride grain and 

GB film were adjusted by the ab initio calculations; the role 

of the additive will be discussed. 

16:35 Creep and oxidation resistance of Si3N4-SiC nanocomposites 

Authors : Monika Kašiarová, Peter Tatarko, Ján Dusza, Pavol 

Šajgalík 

Affiliations : Institute of Materials Research, Slovak Academy 

of Sciences, Košice, Slovak Republic; Institute of Inorganic 

Chemistry, Slovak Academy of Sciences, Bratislava, Slovak 

Republic 

Resume: High temperature properties – oxidation and creep 

behaviour of carbon derived Si3N4-SiC micronanocomposites 

and monolithic Si3N4 sintered with different 

rare earth oxide additives (La2O3, Nd2O3, Y2O3, Yb2O3, 

Lu2O3) have been investigated. The strong influences of 

both the location of SiC nanoparticles and the chemical 

F- 

IV 

1 

F- 

IV 

2

composition of grain boundary phases have been observed. 

Except the Si3N4-SiC composite sintered with Lu2O3, all 

investigated materials obey the parabolic oxidation 

mechanism which has been strongly suppressed in the Ludoped 

composite because of the beneficial effect of stable 

grain boundary phase and the presence of the SiC particles 

predominantly at the grain boundaries of Si3N4. Similarly, 

significantly improved creep resistance was observed in the 

case either of composites or materials with smaller ionic 

radius of RE3+. While the cavitation formation has been 

observed only for the La2O3-containing materials, the creep 

mechanisms in all others were diffusion through the 

intergranular phases connected with the solutionprecipitation 

and grain boundary sliding. 

16:55 MICROSTRUCTURE, MECHANICAL PROPERTIES AND CREEP 

BEHAVIOR OF HOT PRESSED Al2O3/SiC MICRO/NANO 

COMPOSITES 

Authors : M. Parchovianský (1), D. Galusek (2), J. Sedláček 

(2), P. Švančárek (2), M. Kašiarová (3), J. Dusza (3) 

Affiliations : (1) Faculty of Chemical and Food Technology 

STU, Radlinského 9, 812 37 Bratislava; (2) Vitrum 

Laugaricio – Joint Glass Center of the Institute of Inorganic 

Chemistry, SAS, Alexander Dubček University of Trenčín, 

and RONA, j.s.c, Študentská 2, 911 50 Trenčín; (3) Institute 

of Materials Research, Slovak Academy of Sciences, 

Watsnova 47, SK-043 53 Košice; 

Resume: Abstract Al2O3/SiC micro/nano composites 

containing different volume fractions (3, 5, 10, 15, 20 

vol.%) of SiC were prepared by mixing a sub-micron 

alumina powder with respective amounts of either micro- or 

nano-sized silicon carbide powders. The powder mixtures 

were hot pressed 1h at 1740°C and 30 MPa in the 

atmosphere of Ar. The effect of SiC addition on the 

microstructure and mechanical properties, i.e. hardness, 

fracture toughness, and room temperature fracture strength 

were investigated. The creep behavior at temperatures up to 

1400 C, and mechanical load of 150 MPa of the composites 

was also studied, and compared to monolithic Al2O3 

reference. The fracture strength increased with increasing 

volume fraction of silicon carbide particles. The maximum 

fracture strength (655 ± 90 MPa) was achieved for the 

composite containing 20 vol. % of SiC, which is more than 

twice as high as in the Al2O3 reference. Hardness and 

fracture toughness were also moderately improved. The 

observed improvement of mechanical properties is mainly 

attributed to alumina matrix grain refinement, grain 

boundary reinforcement, and the related change of fracture 

mode from intergranular in the alumina reference to 

transgranular in the composites. The creep resistance of 

Al2O3/SiC composites was also markedly improved when 

compared to monolithic Al2O3. Long loading time before 

mechanical failure suggests diffusion controlled creep 

behavior. Enhanced creep resistance is attributed to grain 

boundary pinning mechanism by intergranular SiC 

nanoparticles. Keywords: Al2O3, SiC, nanocomposites, 

mechanical properties, creep 

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17:10 Monolithic Ceramic-based Nanocomposites from Preceramic 

Polymers: Design, Processing and Properties 

Authors : Mirna Bechelany, Wenli Zhong, Samuel Bernard, 

Philippe Miele 

Affiliations : Institut Européen des Membranes (UMR CNRS 

5635) IEM/Université Montpellier 2 Place E. Bataillon 34095 

Montpellier Cedex 5, France 

Resume: Nowdays, there is a trend toward more flexibility 

and an increased interest in "smart” and ”adaptive” 

materials with the objective to meet most industrial 

specifications. Nanocomposites can be considered as such 

strategic materials endowed with designed performance 

properties that reach far beyond those of conventional 

composites. The definition of nanocomposites has broadened 

significantly to encompass nowdays a large variety of 

systems made of distinctly dissimilar components and mixed 

at the nanometric scale. In particular, the choice of 

compositions and processing techniques has become 

enormous so that it becomes easy to select a process, 

thereby a composition that can offer solutions for most of 

the market demands. Here, we are interested by ceramicbased 

nanocomposites which are generated in an “one-pot” 

process and in particular by non-oxide ceramics/non-oxide 

ceramics nanocomposites. In particular, we based our 

concept design on two families of nanocomposites in which 

metal nitride nanocrystals (MeN with Me = Ti, Zr, Hf) are 

embedded into an amorphous nitride matrix (BN and 

Si3N4). The relatively recent Precursor-Derived Ceramics 

(PDCs) route, which is based on the shaping then pyrolysis 

of inorganic polymers into “near net shape” advanced 

ceramics, is a synthetic path which offers original and new 

preparation opportunities in advanced functional materials 

such as nanocomposites. In this presentation, we describe 

the synthesis, shaping and pyrolysis of metal-modified 

polysilazanes and polyborazylenes to prepare monolith-type 

nanocomposites for top-end functional applications. 

Corresponding author's name: Dr. Samuel Bernard; 

Samuel.Bernard@iemm.univ-montp2.fr; Tel: +33 467 149 

181; Fax: +33 467 149 119 - Institut Européen des 

Membranes (UMR CNRS 5635) IEM/Université Montpellier 2 

Place E. Bataillon 34095 Montpellier Cedex 5, France 

Poster Session 

17:30 Synthesis and Characterization of Copper oxide 

nanopowders produced with chemical methods 

Authors : Mohammad Amin Baghchesara1*, and Hossein 

Abdizadeh2 

Affiliations : 1Department of Metallurgy and Materials 

Engineering Masjed Soleyman Branch, Islamic Azad 

University, Masjed Soleyman, Iran 

*amsara2000@Gmail.com 2School of Metallurgy and 

Materials Engineering, University of Tehran, Tehran-Iran 

Resume: Copper oxide nanopowder is a black and 

incombustible material which is insoluble in water, but 

soluble in acids. This material has been used in various 

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applications such as microelectronic, microcircuits, 

nanowires, microbacteria and nanofluids. Copper oxides, 

especially, which are p-type semiconductor have been 

widely used as heterogeneous catalysts in oxidizing 

processes of organic synthesis. In this paper, 

Nanostructured CuO powders have been synthesized using 

chemical methods. Ammonium oxalate and copper nitrate 

were used as the precursor materials. The weight ratios of 

the raw materials (ammonium oxalate/copper nitrate) were 

1.1, 1.2, 1.3, and 1.4. As a result of chemical reaction 

(between them), copper oxalate was synthesized. Produced 

samples were analyzed by XRD and SEM. The results show 

that the best ratio (for ammonium oxalate/copper nitrate) is 

1.2. Produced copper oxalate powder was heated at 600, 

700 and 800oC. The final product was CuO nanopowder. 

XRD studies indicate that the highest ratio of Cu2O to CuO 

was observed in the specimen heated at 700oC. Keywords: 

CuO, nano, synthesis, oxalate, semiconductor. 

17:30 Bioactive nanocomposite hydroxyapatite / Ti-based thin 

films 

Authors : Katalin Balázsi1, Je-Yong Choi2, Seong-Gon Kim3, 

Chang-Hoon Chae4, Marta Vandrovcová5, Lucie Bacáková5, 

Csaba Balázsi1 

Affiliations : 1 Research Institute for Technical Physics and 

Materials Science, Kolkoly-Thege M. út 29-33, H-1121 

Budapest, Hungary 2 Department of Biochemistry and Cell 

Biology, Kyungpook National University,Daegu 700- 

721Korea 3 Department of Oral and Maxillofacial Surgery, 

College of Dentistry, Gangneung-Wonju National University, 

Jibyun-Dong, Gangneung, Gangwondo, 210-702 Korea 

4Department of Dentistry, Hallym University,, 

Chuncheon,Gangwon-do, 200-702 Korea 5 Institute of 

Physiology Academy of Sciences of the Czech Republic, 

Prague, Videnska 1083 CZ-14220 Prague 4 – Krc, Czech 

Republic 

Resume: Nanomaterials have wide-ranging implications in a 

variety of areas, including chemistry, physics, electronics, 

optics, materials science and biomedical sciences. 

Hydroxyapatite (HAp) and titanium compounds are found to 

be the most suitable biomaterials. The major inorganic 

constituent of bones and teeth is calcium phosphate. This 

similarity provides HAp based materials excellent 

bioactivities like bone bonding capability, osteoconductivity, 

and biocompatibility. The relatively high stiffness of 

titanium, as compared to surrounding bone, can lead to 

problems of stress-shielding and subsequent implant 

loosening. In this work, this problem was resolved by 

bioactive HAp coating on Ti-based nanocomposite thin film 

surface. The 300 nm thin TiC/ a:C nanocomposite thin films 

were prepared by dc magnetron sputtering on silicon (001) 

substrates at 25°C in argon. HAp powder was prepared from 

eggshells by attrition milling. The structure of films was 

studied by transmission and scanning electron microscopy. 

MG 63 osteoblast like cells were used for in –vitro test of TiC 

films. White New Zeland rabbits were used for in- vivo 

studies of bioactivity of nanosized HAp films. Considering the 

rapid healing in the bony defects and their easy availability, 

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nano HAp / TiC thin films could be a good new bone 

substitute for tissue engineering. Acknowledgements This 

study was supported by OTKA 76181, by the János Bolyai 

Research Scholarship of the Hungarian Academy of Sciences 

and OTKA Postdoctoral grant Nr. PD 101453 and by 

BioGreen21 Program (grant no. 200810FTH01 0103002 and 

0102001) of Rural Development Administration. 

17:30 Low thermal conductivity and high strength SiO2 

aerogel/fiber nanocomposite fabricated at ambient pressure 

drying 

Authors : Yonggang Jiang, Zilong Zhang, Jian Feng, Junzong 

Feng, Qingfu Gao 

Affiliations : Key Lab of Advanced Ceramic Fibers and 

Composites, College of Aerospace and Materials Engineering, 

National University of Defense Technology, Changsha, 

Hunan, 410073, China 

Resume: Silica aerogels are the nanoporous form of silica 

which exhibits extremely high specific surface area, low 

density and high porosity. Because of their nanoporous 

nature and tenuous solid silica network, aerogels proved 

themselves as an ideal candidate for high efficiency thermal 

insulation. However, their application as a thermal insulating 

material has been restricted due to their weak and fragile 

mechanical strength, dangerous supercritical drying 

preparing process. One of the good methods to strengthen 

aerogels is the composition of aerogel and fiber matrix under 

friendly non-supercritical drying condition. Lots of 

investigator insight into the silica aerogel through ambient 

pressure drying (APD), fewer insights into the APD silica 

aerogel/fiber nanocomposite. In the course of this work, 

SiO2 aerogel/fiber nanocomposite with low thermal 

conductivity and high strength was fabricated by sol-gel 

method at ambient pressure drying using Tetraethoxysilane 

(TEOS) as precursor, enthanol (EtOH) as solvent, muriatic 

acid and ammonia as catalysts, Hexamethyl disilazane 

(HMDZ) as modification reagent, enthanol and hexane as 

exchange solvent, ceramic fiber as reinforcement. Thermal 

conductivity and bending strength of the nanocomposite is 

0.025W/m•K (800℃) and 1.3MPa, respectively. Effect on the 

nanocomposite was studied with different amount of HMDZ, 

fiber bulk density and sol molar ratio. 

17:30 Nanoceramics incorporation in polymer during laser-assisted 

sintering 

Authors : Shishkovsky I.V., Scherbakof V.I. 

Affiliations : Lebedev Physics Institute of Russian Academy 

of Sciences, Samara branch 

Resume: Biocompatible nanooxide ceramics (TiO2, Al2O3, 

ZrO2 and hydroxyapatite) were added to bioresorbable 

polymer (polycarbonate and polyetherketone) powders for 

the layer-by-layer laser-assisted manufacturing of the 

porous tissue engineering scaffolds. The optimal regimes of 

laser sintering on the CO2 and Nd+3YAG lasers were 

determined. Comparison microstructure estimation of the 

sintered samples were conducted using scanning electron 

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microscopy (SEM) equipped with an energy-dispersive x-ray 

(EDX) analysis and evaluated with results of X-ray analysis. 

The results ascertained the potential of SLS-fabricated tissue 

engineering scaffolds. 

17:30 Crystallization Of TiO2 Sol-Gel Coatings 

Authors : Pietrzyk B., Miszczak S. 

Affiliations : Institute of Materials Science and Engineering, 

Technical University of Lodz, Poland 

Resume: Titanium dioxide (TiO2) is an important material 

because of its photocatalytical, self-cleaning, anti-corrosion, 

optical, and biomedical applications. TiO2 can be 

synthesized as amorphous or as two main polymorphs: 

metastable anatase and stable rutile. The properties of 

titanium dioxide strongly depend on the kind of phases. The 

transformation temperature between phases is influenced by 

a lot of factors like method of preparation, inpurities, size of 

grains etc. One of them is also type of substrate under the 

film of TiO2. In the present work, thin films of TiO2 were 

deposited by sol-gel method. Titanium (IV) tetrabutoxide 

was used as a precursor. Silicon (Si), austenitic stainless 

steel (304) and Co-Cr-Mo alloy (Vitallium) were used as 

substrates. The temperature of crystallization as well as 

temperature of anatase rutile phase transformation were 

investigated by X-Ray Diffraction (XRD) studies of films on 

different substrates. The results were compared with 

transformations temperature of TiO2 powders obtained by 

analogous sol-gel process. It was found that as a result of 

crystallization anatase occurred in all investigated cases, at 

the similar temperature. The temperature of anatase rutile 

phase transformation changed from 600-700oC for sol-gel 

powder to more then 1000oC for film deposited on Si. The 

temperature of anatase rutile phase transformation strongly 

depend on kind of substrate. 

17:30 Effects of Rapid Thermal Process on Electrical Properties, 

Electronic Structure and Microstructure of Sol-Gel-Derived 

TiSiOx Films 

Authors : Seung Muk Lee, Geun Chul Park, Soo Min Hwang, 

Jun Hyuk Choi, Tae Woong Kim, Jinho Joo 

Affiliations : School of Advanced Materials Science and 

Engineering, Sungkyunkwan University, 300 Cheoncheondong, 

Jangan-gu, Suwon, Gyeonggi-do, 440-746, Korea 

Resume: Sol-gel-derived TiSiOx films were fabricated and 

their electronic structure, microstructure, and electrical 

properties were evaluated by adjusting rapid thermal 

process (RTP) temperature from 700oC to 1000oC. Ti-O-Si 

bonds were found for all the films by Fourier transform 

infrared spectroscopy and O 1s X-ray photoelectron 

spectroscopy spectra clearly revealed that the film before 

RTP consisted of amorphous Ti- and Si-rich silicate phases. 

These phases decomposed toward TiO2 and SiO2 and 

crystallized during RTP. Furthermore, for the 1000oC 

sample, in spite of well crystallized nature (generally 

regarded as TiO2), the binding energy of the Ti-rich phase 

was relatively higher than that of pure TiO2 while that of the 

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Si-rich phase agreed well with that of pure SiO2. This 

suggested that the film was probably constituted of pure 

SiO2 and TiySizO2 phase (y>>z), implying that TiSiOx was 

not completely decomposed despite high temperature. In 

addition, secondary ion mass spectrometry exhibited that Ti 

diffused towards the Si substrates by heat treatment, 

resulting in higher permittivity (k) of interfacial layer than 

that of SiO2. The k and energy band gap for the 1000oC 

sample was ~36 and ~3.9 eV, respectively. 

ACKNOWLEDGEMENT: This research was supported by Basic 

Science Research Program through the National Research 

Foundation of Korea (NRF) funded by the Ministry of 

Education, Science and Technology (Grant No. 2012- 

0002923). 

17:30 Phase Stability and Microstructure of Sol-Gel-Derived 

Nanoscale-Thick ZrO2/Si Films 

Authors : Soo Min Hwang, Seung Muk Lee, Jun Hyuk Choi, 

Geun Chul Park, Tae Woong Kim, Jinho Joo 


Engineering, Sungkyunkwan University 

Resume: Nanoscale-thick (~15 nm) ZrO2/Si films were 

fabricated by sol-gel method and the phase and 

microstructural evolution by thermal annealing were studied. 

The ZrO2 films were prepared by synthesis of the precursor 

sol (0.2 M) using a Zr-acetylacetonate (Zr-acac), spincoating 

of the solution on Si substrates and drying, followed 

by annealing at 300-950oC in ambient air. Microstructure 

and surface morphology were observed by transmission 

electron microscopy (TEM) and atomic force microscopy 

(AFM). Phase identification was performed by using X-ray 

diffraction (XRD), Raman spectroscopy, and selected area 

electron diffraction (SAED). Thermal annealing resulted in 

the phase evolution from the amorphous to tetragonal (t-) 

phase which was retained without a conspicuous transition 

to monoclinic phase despite the high-temperature annealing 

at ~950oC. The mechanism of the t-phase stability was 

suggested on the basis of the microstructural changes: the 

film thickness was reduced, whereas the in-plane grain size 

and surface/interface area were increased with increasing 

annealing temperature. 

17:30 Tm2O3 nanopowders preparation by precipitation for 

Tm:YAG reactive sintering 

Authors : Agata Sidorowicz 1,2, Helena Węglarz 1, Anna 

Wajler 1, Henryk Tomaszewski 1, Andrzej Olszyna 2 

Affiliations : 1) Institute of Electronic Materials Technology, 

Wólczyńska 133, 01-919 Warsaw, Poland; 2) Warsaw 

University of Technology, Wołoska 141, 02-507 Warsaw, 


Resume: In this study thulium oxide powder has been 

prepared by thulium nitrate precipitation using ammonia or 

ammonium hydrogen carbonate as a precipitating agent. 

The aim of this work was investigation of relation between 

precipitation parameters (pH, precipitation temperature) and 

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the properties of thulium oxide nanopowders obtained after 

precursors calcination. Tm2O3 powders and precursors were 

characterized by XRD, SEM and BET techniques. The 

mixtures for reaction sintering of Tm:YAG, containing the 

powders produced and commercially available, were 

prepared and consolidated. Finally, Tm:YAG ceramics 

obtained by reactive sintering (1830oC/6h) using different 

powders have been compared in respect to microstructure 

and transmittance. The project was financed by the National 

Science Centre Fund granted based on the decision no. DEC- 

2011/01/N/ST8/02648. 

17:30 Amorphous aluminium oxide-nitride coatings for solar 

thermal applications 

Authors : R. Romero, B. Gavil?, F. Martin, J.R. Ramos- 

Barrado, D. Leinen 

Affiliations : Dpto. F?sica Aplicada I & Dpto. Ingenier?a 

Qu?mica, Universidad de M?laga, E-29071 M?laga, Spain. 

Resume: Amorphous aluminium oxide-nitride coatings have 

been deposited in air (open atmosphere) from aqueous 

aluminium nitrate solutions onto raw rolled 304 stainless 

steel sheet by the spray pyrolysis technique. It is shown by 

XPS and FTIR analysis that the nitride to oxide ratio in the 

composite film is determined by the substrate temperature 

during deposition. Thereby substrate surface temperatures 

can be hold as low as 200 ?C yielding amorphous thin films 

of highly compact deposit observed with cross-section 

scanning electron microscopy (SEM-FIB). In view to 

application of these coatings as antireflective and protective 

top coating on solar thermal devices based on metallic 

substrates to work, particularly, in sea near areas, the solar 

absorptance and the thermal emittance as well as the 

corrosion resistance in saline conditions have been 

determined showing appropriate values. 

17:30 Mechanical behaviour of Al/Si3N4 metal-ceramic multilayers 

under nanoindentation 

Authors : Ming Wang, Dong Wang, Marcus Hopfeld, Diana 

Rossberg, Peter Schaaf 

Affiliations : Ilmenau University of Technology, Institute of 

Materials Engineering and Institute of Micro- and 

Nanotechnologies MacroNano®, Chair Materials for 

Electronics and Electrical Engineering, Gustav-Kirchhoff-St. 

5, 98693 Ilmenau, Germany 

Resume: The mechanical properties of ceramic films in the 

nanometer thickness range have attracted an increased 

attention due to microelectronics and high-speed 

technologies. In this work, nano-indentation measurments 

were performed on metal-ceramic multilayers as a function 

of the individual layer thicknesses. Therefore, Al/Si3N4 

multilayers with individual layer thickness from 10 nm to 

500 nm were investigated by nanoindentation using Vickers 

and Brinell indenters. For these metal-ceramic multilayers, 

the hardness increases when decreasing the individual layer 

thickness from 500 nm to 10 nm. This indicates a significant 

size effect in their mechanical behaviour. As the individual 

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layer thickness decreases from sub micro to the nanometer 

scale, a different deformation behaviors in the multilayers is 

observed in cross-section scanning electron micropcopic 

observation. These differences are discussed in terms of 

plasticity, crack formation and bond strength. Also 

differences between the two indenters are observed and are 

presented. 

17:30 Controlling the shape and size of ceria nanoparticles for 

application as catalyst in energy systems 

Authors : Inderjeet Singh(1), Rafael Munoz-Espi(2), 

Katharina Landfester(2) and Amreesh Chandra(1) 

Affiliations : (1)Department of Physics and Meteorology, 

Indian Institute of Technology, Kharagpur-721302, West 

Bengal, India; (2)Max Planck Institute for Polymer Research, 

Ackermannweg 10, 55128, Mainz, Germany 

Resume: Improved physiochemical and catalytic properties 

of metal-oxide nanoparticles due to higher surface has been 

a major focus area over the last few decades. The 

importance of such catalysts has increased further due their 

critical role in alternative energy systems such as fuel cells, 

batteries and supercapacitors. Especially, investigations on 

ceria as catalyst have become very important owing to its 

low cost, abundance and relatively low toxicity. In the 

present study, ceria nanoparticles were synthesized using 

two techniques namely, a conventional sol-gel process and a 

water-in-oil miniemulsion technique. Conventional sol-gel 

allows large scale production of CeO2 powders but with 

inhomogeneous particle size distribution, while miniemulsion 

give a route to synthesize homogeneous nanoparticles but 

the yield is low. Ceria nanoparticles were characterized using 

XRD, SEM, TEM, XPS and BET measurements. The prepared 

ceria powders were used as a cathode material in a 

microbial fuel cell (MFC) to enhance the kinetics of oxygen 

reduction reaction at cathode and improving the output 

power densities of the cell. Contrary to expected, the 

continuous reduction in particle size results is performance 

degradation. The reduction is particle size causes the 

transformation of CeO2 to CeO2−δ along with stabilization 

of Ce2O3. Such condition makes the system behave more 

like O-storage rather than a catalytic material. The 

performance of fuel cells has been evaluated by obtaining 

power density. 

17:30 Ytterbium and thulium co-doped YSZ for infrared emitters 

Authors : M.R.N. Soares, M. J. Soares, T. Monteiro, F. M. 

Costa 

Affiliations : Department of Physics, i3N, University of 

Aveiro, 3810-193 Aveiro, Portugal 

Resume: Incorporated in wide band gap materials, optically 

activated rare earth (RE) ions lead to widespread transitions 

among the intra-4fn electronic levels permitting spanning 

the luminescence from the ultraviolet to the infrared by an 

appropriate selection of the lanthanide dopant. This is the 

case for the yttria stabilized zirconia (YSZ) host which, with 

a bandgap in the ultraviolet region, constitutes a suitable 

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material for visible RE-based activated phosphors. Besides 

the obvious interest in visible solid state lighting, efficient 

infrared emitters for mid-infrared optical communication 

systems and biological sensing applications is still a demand 

in nowadays. YSZ fibers grown by the laser floating zone 

(LFZ) technique and nanoparticles prepared by solution 

combustion synthesis (CS) were intentionally co-doped with 

ytterbium and thulium ions in order to enhance the infrared 

luminescence intensity in the mid-infrared spectral region. 

The crystalline quality of both samples was characterized by 

X-ray diffraction (XRD) and Raman Spectroscopy. The 

optical transitions among the distinct 2S+1LJ multiplets 

were analyzed by photoluminescence (PL) and 

photoluminescence excitation (PLE) spectroscopy. Besides 

the Tm3+-related blue light, a noticed enhancement of the 

mid-infrared luminescence was observed by increasing the 

temperature between 14 K and RT open the way to explore 

the potentialities of co-doped YSZ as infrared emitter. 

17:30 Deposition and structural characterization of verticallyaligned 

La0.8Sr0.2CoO3/(La0.5Sr0.5)2CoO4 composite thin 

films 

Authors : Yener Kuru, Wen Ma, Yan Chen, Zhuhua Cai, Jae- 

Jin Kim, Harry L. Tuller, Bilge Yildiz 

Affiliations : Department of Nuclear Science and 

Engineering, Massachusetts Institute of Technology, 77 

Massachusetts Avenue, MA 02139, United States 

Department of Materials Science and Engineering, 

Massachusetts Institute of Technology, 77 Massachusetts 

Avenue, MA 02139, United States Department of Materials 

Science and Engineering, Akdeniz University, Dumlupinar 

Bulvari, 07058 Antalya, Turkey; Department of Nuclear 

Science and Engineering, Massachusetts Institute of 

Technology, 77 Massachusetts Avenue, MA 02139, United 

States; Department of Nuclear Science and Engineering, 


Avenue, MA 02139, United States; Department of Nuclear 



States; Department of Materials Science and Engineering, 


Avenue, MA 02139, United States; Department of Materials 



States; Department of Nuclear Science and Engineering, 


Avenue, MA 02139, United States 

Resume: It has recently been reported that the 

La0.8Sr0.2CoO3/(La0.5Sr0.5)2CoO4 (LSC113/LSC214) 

interface has drastically improved oxygen reduction kinetics 

compared to the both of the cobaltite phases [M. Sase et al. 

Solid State Ionics 178, 1843-52, 2008]. In order to clarify 

the mechanism(s) behind this result, we deposited 

LSC113/LSC214 composite thin films on (001) SrTiO3 

substrates by pulsed laser deposition from a composite 

target in the present study. The structure of the composite 

film is called ‘vertically aligned nanostructure, VAN’ since the 

interfaces separating the two phases in the composite are 

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perpendicular to the film surface and the grains are 

columnar. Such a VAN structure allows to obtain reliable 

information about the electrical transport properties of the 

LSC113/LSC214 interfaces since these interfaces are 

exposed directly to the oxygen environment and the current 

path in an out-of-plane measurement using LSC113/LSC214 

VAN structure is better defined compared to the one in an 

in-plane measurement performed employing a 

LSC113/LSC214 multilayer. Microstructural characteristics of 

the specimens were examined by high resolution X-ray 

diffraction, focused ion beam microscopy and scanning 

tunneling microscopy. The films consist of homogenously 

distributed LSC113 islands having a screw dislocation per 

island, and the LSC214 phase connects these islands and 

has a smaller grain size. The electronic structure of the 

hetero-phase domains and their interfaces is being 

investigated by scanning tunneling spectroscopy. 

17:30 Impact of I-ZnO layer and CIGS on oxygen concentration 

changes. 

Authors : Tae-Young Yun*, Ju-Young Beak, Jun-Seung Park, 

Soon-Rok Park, Chan-Wook Jeon 

Affiliations : Department of Chemical Engineering; 

Yeungnam University; Gyeongsan; Gyeongbuk; 712-749; 

Korea 

Resume: Abstract CIGS solar cell junction is important. In 

particular, the receiving buffer layer of oxygen plasma 

damage and Intrinsic Zinc Oxide (i-ZnO) layer junction are 

very important of CIGS solar cell performed. Impact of 

oxygen concentration changes on the i-ZnO layer and the 

CIGS solar cells is to analyze. Introduction The undoped ZnO 

is a common choice for the insulating layer and it is believed 

to eliminate the shunt paths possibly left by the notconformal 

coverage of CIGS surface by a buffer layer 

deposited by a chemical bath deposition. But, CIGS solar cell 

is damaged by plasma. Especially, insulating layer undoped 

ZnO on buffer layer. Plasma damage is a major cause of 

oxygen. Experimental The CIGS absorbers were deposited 

by molecular beam epitaxy.The CdS thin films were 

deposited by the chemical bath deposition. The i-ZnO layer 

was deposited by RF magnetron sputter. The oxygen flow 

rate adjustable from 0 to 10% for the i-ZnO films were 

deposited. Subsequently AZO were deposited by DC 

magnetron sputter. The evaluation of photovoltaic 

performance of CIGS solar cell has been performed using 

solar simulator under AM1.5, 100mW/cm2 illumination at 

25℃. i-ZnO thin film was analyzed by XRD, AFM. Result and 

Discussion I-ZnO layer, depending on the oxygen 

concentration was changed by the XRD results. CIGS solar 

cells is also dependent on oxygen concentration. Reference 

Applied Surface Science 245 (2005) 273–-280 Journal of 

Alloys and Compounds 509 (2011) 1774–.1776 

17:30 Synthesis and studies on LiMnPO4/Ag nanocomposite for 

lithium ion secondary batteries 

Authors : Monika Michalska1, Ludwika Lipińska1, Krzysztof 

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Korona2 

Affiliations : 1Institute of Electronic Materials Technology, 

Wólczyńska 133, 01-919 Warsaw, Poland 2Faculty of 

Physics, University of Warsaw, Hoża 69, 00-681 Warsaw, 


Resume: Compounds of olivine structure like LiMnPO4, 

LiFePO4 are very promising as cathode materials for lithium 

ion batteries because of low cost, low toxicity and higher 

safety. Unfortunately they suffer from a low intrinsic 

electronic conductivity. This drawback can be overcome by 

mixing olivines with conducting compounds e.g. carbon or 

doping by metal ions. In this work silver deposition on the 

olivine particles was applied in order to improve 

electrochemical performance. Firstly the nanocrystalline 

powder was synthesized by modified sol-gel method. 

Secondly LiMnPO4/Ag composite was prepared by adsorbing 

silver nanoparticles on LiMnPO4 powders. Silver salt was 

dissolved in an alcohol – deionized water solution and then 

the single phase LiMnPO4 nanopowder was added to obtain 

homogenous suspension. The gel were dried at 150°C for 

several hours and then ground in an agate mortar to obtain 

fine powder. The powders were calcined at 450°C for few 

hours in the air. The crystal structures of powders: LiMnPO4 

and LiMnPO4/Ag composite were characterized by X-ray 

powder diffraction (XRD). The size and morphology of 

nanocrystalline powder LiMnPO4 and LiMnPO4/Ag composite 

were analyzed by scanning electron microscopy (SEM) and 

high resolution scanning electron microscopy (HRSEM). Also, 

the differential scanning calorimetry (DSC) analysis have 

been done. Raman scattering spectra of LiMnPO4 and 

LiMnPO4/Ag composite were studied. In both materials 1, 

2 and 4 oscillation modes are clearlyvvisible. The main 

lines were sharp (20 cm-1) what confirms good quality of 

the samples. It was found that in the LiMnPO4/Ag composite 

the intensity of B1g 4 mode related to Ag 4 mode is 

significantly higher than in the pure material. It could be 

related to direct interaction between PO4 and silver, what 

means that some silver was incorporated into the LiMnPO4 

crystal lattice. Moreover, strong phonon–plasmon coupling 

was observed for Ag 1 and Ag 3 modes. It is suggested that 

the silver nanoparticles were in close contact with LiMnPO4 

crystals, so the LiMnPO4 phonon modes can be electrically 

coupled to electron plasma in silver. 

17:30 Microstructural and biological characterization of spark 

plasma sintered hydroxyapatite-zirconia composites 

Authors : Gréta Gergely, Zsuzsanna Litván, Andrea Szegő, 

Zsombor Lacza, Filiz Cinar Sahin, Gültekin Göller, Onuralp 

Yücel, Csaba Balázsi 

Affiliations : gergely.greta@ttk.mta.hu 

Resume: Nano hydroxyapatite (HAp)-zirconia (ZrO2) 

composites were produced by spark plasma sintering (SPS). 

The HAp was reinforced with the bioinert yttria stabilized 

zirconia. The composites were fabricated by SPS, which can 

be characterized as a fast and direct sintering process. 

During the SPS process low temperatures (650-950oC) and 

short dwelling time (5 minutes) were applied to avoid the 

decomposition of HAp and the reaction between HAp and 

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ZrO2. The grain size of the sintered composites were 200- 

1000 nm. The microhardness decreased, whereas the 

bending strength increased with increasing the sintering 

temperature. A grain coarsening was observed in the case of 

high HAp content (90, 95, 100wt%) and higher sintering 

temperatures (700 and 800oC) . The microstructure of 

composites (grain size 200-300nm) was preserved in the 

case of lower HAp content (60 wt%) even if the temperature 

was relative high (825, 950oC). The biocompatibility of HAp- 

ZrO2 was tested under in vitro cell culture conditions. 

Human bone marrow derived mesenchymal stem cell 

(hBMSC) attachment and proliferation was slightly increased 

on Hap-ZrO2 surfaces compared to regular HAp. Our results 

show that SPS sintered Hap-ZrO2 composites may be 

suitable for bone implant materials. 

17:30 Synthesis and characterization of kesterite nanopowder, 

microcrystals and single monocrystals 

Authors : Krzysztof Łyżwa, Maciej Zieliński, Marta Serafin, 

Monika Guzowska, Paweł Łężak 

Affiliations : Warsaw University of Technology, Faculty of 

Chemistry 

Resume: Kesterite Cu2znSnS4 is a semiconductor material 

that can be used as a light absorbing layer in novel 

photovoltaic devices. It can replace expensive and rare 

materials such as chalcopyrite type Cu(In, Ga)Se2 or zinc 

blende type CdTe. Our research focused on methods of 

kesterite production using the solvothermal and high 

temperature furnace processes. The solvothermal method is 

based on a reaction between inorganic salts and sulphur in 

organic solvents. The reaction was carried out at high 

temperatures ranging from 130 to 250 oC. Due to its high 

boiling point and good solubility properties, oleylamine was 

used as a solvent. The reaction was carried out in an inert 

gas atmosphere to avoid oxidation of the reagents. The 

solvothermal method resulted in kesterite nanopowder with 

an average granule size of 5 nm. The influence of 

temperature and duration of the process on the end product 

was studied. Characterization of the end product was 

performed using XRD, TEM and Raman Spectroscopy. The 

high temperature furnace method was based on the reaction 

between the sulfides CuS, ZnS and SnS. The reagents were 

sealed in a quartz ampoule under high vacuum. The 

ampoule was placed in a furnace and heated to 750 oC. The 

reaction was allowed to carry on for 24 to 336 hours. At the 

conclusion of the reaction the ampoule was cooled down and 

opened. This method yielded kesterite microcrystals and 

single monocrystals. The end product was studied using 

XRD, SEM and Raman Spectroscopy. 

17:30 Effect of growth temperature of Cu(In,Ga)Se2 on solar cell 

performance 

Authors : Soon-Rok Park, Ju-Young Baek, Tae-Young Yun, 

Hye-Jin Han and Chan-Wook Jeon 

Affiliations : Optoelectronic Devices Laboratory, School of 

Display and Chemical Engineering, Yeungnam University 

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Resume: Solar cells based on the Cu(In,Ga)Se2 compound 

semiconductor have recorded the highest conversion 

efficiency in thin film solar cells. The most successful 

absorber deposition method for high efficiency small-area 

devices seems to be the three-stage co-evaporation of CIGS 

from elemental sources in the presence of excess Se vapor. 

In three-stage co-evaporation, the orientations of CuInSe2 

depend strongly on the orientation of the underlying 

(In,Ga)2Se3 precursor layer at the first stage. In this study, 

CIGS absorber layer was grown using the three-stage coevaporation 

process. The solar cells made of CIGS grown at 

different substrate temperatures in the first stage were 

experimentally compared and the effect of variation growth 

temperature analyzed. On the Mo (600nm) coated glass, the 

CIGS absorber layer was grown by three-stage coevaporation. 

In the first stage, the substrate temperature 

were regulated ranging from 300℃, 350℃ and 400℃. A 

50nm thick CdS layer was deposited by CBD and i-ZnO 

(80nm)/ n-Zno:Al (500nm) were deposited by RF sputtering. 

An Al grid (750nm) was deposited by DC sputtering. In this 

research, the solar cell grown at lower temperature in the 

first stage was found to have better conversion efficiency 

according to I-V curve. For the reason of the results, IPCE, 

C-V, XRD, SIMS, XRD, SEM were analyzed. Based on the 

extensive analytical results, the prefer-orientation (220/204) 

was suggested for high conversion efficiency and more will 

be discussed. 

17:30 Influence of Sintering Temperature on the Properties of 

Pulsed Electric Current Sintered Hybrid Coreshell Powders 

Authors : Norsuria Mahmed, Juha Larisma, Oleg Heczko, 

Mehmet Erkin Cura, Simo-Pekka Hannula 

Affiliations : Norsuria Mahmed; Juha Larisma; Mehmet Erkin 

Cura; Simo-Pekka Hannula; Aalto University School of 

Chemical Technology, Department of Materials Science and 

Engineering, P.O.Box 16200, FI-00076 Aalto, Finland. Oleg 

Heczko; Institute of Physics, Academy of Sciences, Czech 

Republic Na Slovance 2, CZ-182 21 Praha 8, Czech Republic. 

Resume: The influence of process temperature of pulsed 

electric current sintering (PECS) on the properties of bulk 

materials consolidated from three different types of hybrid 

powders was studied. The starting powders consisted of iron 

oxide-silica coreshell structure with and without silver 

nanoparticles doping, and iron oxide-free silica particles with 

silver doping. The powders were prepared based on a 

modified Stöber method. The sintering temperature was 

varied from 773 K up to 1273 K while 50 MPa of pressure 

and 15 minutes of sintering time were constant. Results 

showed that the sintering temperature induced the growth 

of silver nanoparticles on the silica surfaces, with particle 

size evolution depending on the temperature. Iron oxide 

nanoparticles were found to influence the oxidation of silver 

during the compaction. The sintering environment also 

influenced the stability of iron oxide nanoparticles. Iron 

oxide was found to be reduced into the pure iron (Fe) when 

the temperature was higher than 1173K and showed 

ferromagnetic behavior. At the same temperature 

crystallization of the amorphous silica matrix occurred. 

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17:30 Plasma enhanced aerosol-gel deposition of Al2O3 coatings 

Authors : Gawronski Z., Miszczak S., Pietrzyk B., 

Szymanowski H., Kucharski D. 

Affiliations : Institute of Materials Science & Engineering, 

Technical University of Lodz, Poland 

Resume: The new plasma enhanced aerosol-gel technique 

has been used for films preparation in this work. This 

process integrates aerosol-gel deposition of films and their 

plasma treatment in one reactor. The alumina films aerosolgel 

deposited on Si substrate were plasma and thermally 

treated. The influence of deposition and condensation 

conditions on properties of the films has been studied. The 

morphology of films was investigated using optical 

microscope, SEM and AFM . The chemical and crystalline 

structure of the coatings was analyzed by FTIR and XRD 

techniques, respectively. Optical properties were determined 

by elipsometer measurements. It was found that plasma 

treatment influenced on all investigated properties of 

aerosol-gel deposited alumina films. 

17:30 Nanopowders preparation and spark plasma sintering of 

Co:MgAl2O4 transparent ceramics 

Authors : Anna Wajler1, Agata Sidorowicz1,2, Piotr Putyra3, 

Helena Węglarz1, Katarzyna Jach1, Urszula Zagrajek1, 

Henryk Tomaszewski1 

Affiliations : 1) Institute of Electronic Materials Technology, 

W?lczyńska 133, 01-919 Warsaw, Poland; 2) Warsaw 

University of Technology, Wołoska 141, 02-507 Warsaw, 

Poland; 3) Institute of Advanced Manufacturing Technology, 

Wroclawska 37A, 30-011 Cracow, Poland 

Resume: In this study cobalt doped magnesium aluminate 

nanopowders (Co:MgAl2O4) of 0.1 at.%-5 at.% doping level 

were prepared by co-precipitation and two steps 

precipitation using ammonium hydrogen carbonate. As 

found, the morphology of obtained precursors and calcined 

powders was strongly dependent on applied preparation 

technology. Moreover, sintering studies proved that despite 

the powders exhibited very similar surface area values (BET) 

and grain size (SEM) their sinterability were very different. 

High density translucent Co:MgAl2O4 ceramics have been 

prepared without the use of sintering aids by classical 

pressureless sintering and spark plasma sintering (SPS). The 

work is financed by the Polish Science Funds in the years 

2010-2013 as a research project no. N N507 5902 38 

17:30 Preparation and characterization of brand new boron nitride 

nanotubes reinforced Bioglass scaffold for bone substitution. 

Authors : L. Bertolla, I. Dlouhy, A.R.Boccaccini. P. Tatarko. 

Affiliations : Institute of Physics of Materials of the Academy 

of Sciences of the Czech Republic, v. v. i.; Institute of 

Physics of Materials of the Academy of Sciences of the Czech 

Republic, v. v. i.; Friedrich-Alexander-Universität Erlangen- 

Nürnberg Department Werkstoffwissenschaften Lehrstuhl 

Biomaterialien, nstitute of Physics of Materials of the 

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Academy of Sciences of the Czech Republic, v. v. i. 

Resume: Bioglass 45S5 foams containing different weight 

percentage of BNNTs were produced by foam replica 

process. Tensile and compression tests were performed on 

produced scaffolds. Compressive and tensile elastic modulus 

were measured and compared with literature references. 

Toughening contribution of BNNTs within the glass matrix 

were evaluated both from a qualitatively and quantitatively 

point of you. 

17:30 Microstructural changes in Ni-ScSZ SOFC anode upon 

reduction in hydrogen 

Authors : M. Andrzejczuk1, O. Vasylyev2, I. Brodnikovskyi2, 

V. Podhurska3, B. Vasyliv3, O. Ostash3, M. Lewandowska1, 

K. J. Kurzydłowski1 

Affiliations : 1 Warsaw University of Technology, Warsaw, 

Poland 2 Institute for Problems of Materials Science, Kyiv, 

Ukraine 3 Physical-Mechanical Intitute, Lviv, Ukraine 

Resume: Ni-ScSZ cermet is a perspective material for 

anode of solid oxide fuel cells (SOFC) because of its good 

electrochemical properties. However, it is also susceptible to 

degradation processes taking place during operation. The 

shrinkage during transformation of NiO into Ni is not 

reversible and re-oxidation brings a large volume expansion 

which cannot be fully accommodated by porous structure. 

This may result in stress generation and fracture. In this 

work, to model degaradtion behavior of Ni-ScSZ anode, it 

has been subjected to reduction in hydrogen and the 

resulting microstructure changes of cermet anode have been 

investigated using advanced electron microscopy 

techniques, i.e. scanning transmission electron microscope 

Hitachi HD-2700 equipped with X-ray energy dispersive 

spectrometer (EDS) and electron energy loss spectrometer 

(EELS). An attempt of three dimensional morphology 

reconstruction was done using dual-beam focused ion 

beam/scanning electron microscopy (FIB/SEM) facility. The 

results revealed high porosity of reduced nickel phase and 

changes of anode microstructre after redox cycles. 

17:30 Electrical and thermal properties of nano- and micro-sized 

powders of Y2O3 type 

Authors : Grzegorz Moskal, Marta Mikuśkiewicz, Anna 

Starczewska, Gabriela Tomczykiewicz 

Affiliations : Silesian University of Technology, Department 

of Materials Science, 40-019 Katowice, ul. Krasińskiego 8, 


Resume: Results of electrical and thermal properties 

evaluation of Y2O3 powders were presented in this article. 

The tests were made on the two different types of powders. 

First of them was a powder of the "micro-size" type with the 

particle sizes not crossing10 µm, however the size of 

particles of the second powder was located in range 30 - 50 

nm. Totally different was a morphology of both powders as 

well. In the first case the form of dense polyhedrons about 

the smooth surface was observed. However the powder of 

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the type “nano” was characterized by spongy 

conglomeration of “nano” particles type of morphology. The 

range of investigations included the evaluation of electric 

properties by impedance spectroscopy and thermal 

properties by laser-flash method. The obtained results 

showed that “nano” powders of oxide Y2O3 is different in the 

morphology of individual particles, but he is also better ionic 

conductor in the temperature of 20°C comparing to powder 

the micro type. In the case of thermal properties we 

observed that at temperature 20°C the “nano” type of 

powder is characterized by lower value of thermal diffusivity 

in comparison to “micro-sized” powder. 

17:30 Influence of additional gases on nanohardness and 

tribological properties of PECVD WC/C coatings 

Authors : Peter Horňák, Milan Ferdinandy, František Lofaj 

Affiliations : Institute of Materials Research, SAS, Watsonova 

47, 043 53 Kosice, Slovak Republic 

Resume: The influence of additional gases parameters on 

nanohardness and tribological properties of PECVD WC/C 

coatings was studied to optimize the deposition conditions to 

reach high hardness and low coefficient of friction (COF). 

WC/C coatings were deposited on C45 steel substrates by 

PECVD process using W(CO)6 powder as a precursor. 

Deposition parameters were total gas pressure and partial 

pressure of several gases at constant bias and current 

density. Total deposition pressure consists of carbonyl 

vapour pressure and additional gas pressure of Ar, C2H2, N2 

or H2. Indentation hardness was measured using 

instrumented indentation in sinusoidal loading mode up to 

10 mN. The tribological properties were studied using ballon-disc 

method under the load of 0.5N at 3 different sliding 

rates (5-15 cm/s). The wear tracks were observed by 

confocal microscopy and SEM. The optimization resulted in 

the increase of the hardness up to 28.5±2 GPa and 

indentation modulus up to 351±28 GPa when using Ar 

atmosphere. The lowest COF of 0.12 was obtained using 

C2H2. Generally, coatings with low hardness exhibit low 

values of COF = 0.12 (HIT ≈ 15 GPa), while the coatings 

with high hardness have the COF of around 0.8. Influence of 

C2H2 as an additional carbon source during PECVD seems to 

be the most important for the formation of graphite 

lubricant, which decreases COF and HIT as well. 

17:30 Influence of the processing on the fracture toughness of 

Si3N4 + graphene platelet composites. 

Authors : Lenka Kvetková(a), Jerzy Morgiel(b), Annamaria 

Duszová(a), Monika Kašiarová(a), Františka Dorčáková(a), 

Ján Dusza(a), Péter Kun(c), Csaba Balázsi(c). 

Affiliations : (a) Institute of Materials Research, Slovak 

Academy of Sciences, Watsonova 47, 04353 Košice, Slovak 

Republic; (b) Institute of Metallurgy and Materials Science of 

Polish Academy of Sciences, Reymonta 25, 30 059 Krakow, 

Poland; (c) Research Institute for Technical Physics and 

Materials Science, Ceramics and Nanocomposites 

Department, Budapest, 49, H-1525, Hungary; 

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Resume: Silicon nitride + 1 wt% graphene platelet 

composites were prepared using various graphene platelets 

(GPLs) as filler. Two different sintering routes have been 

applied; hot isostatic pressing at 1700 0C and 20 MPa with 3 

h holding time and gas pressure sintering at 1700 0C and 2 

MPa without holding time. The influence of the addition of 

GPLs and processing routes on the microstructure 

development and on the fracture toughness of Si3N4 + GPLs 

composites was investigated. The GPLs with thickness from 

5 nm to 50 nm are relatively homogeneously distributed in 

the matrix of all composites, however overlapping/bundle 

formation of GPLs was found, containing 2-4 platelets as 

well. The single GPLs and overlapped GPLs are located at the 

boundaries of Si3N4, and hinder the grain growth and 

change the shape of the grains. The fracture toughness was 

significantly higher for all composites in comparison to the 

monolithic Si3N4 with the highest value of 9.92 MPam0.5for 

the composite containing the GPLs with smallest dimension. 

The composites prepared by hot isostatic pressing exhibits 

higher fracture toughness than the spark plasma sintered 

composites. The main toughening mechanisms originated 

from the presence of graphene platelets, and responsible for 

the increase in the fracture toughness values are crack 

deflection, crack branching and crack bridging. 

17:30 Nanoindentation and grid analysis of WC ? Co hardmetals 

Authors : Annam?ria DUSZOV?, Pavol HVIZDO?, Franti?ek 

LOFAJ, J?n DUSZA 

Affiliations : Institute of Materials Research of SAS, Ko?ice, 

Slovak Republic 


Resume: The hardness and indentation modulus of 

individual phases have been studied in WC ? Co cemented 

carbides with different microstructure paramaters. Grid 

indentation technique (GIT), has been applied for the 

statistical analyses of experimental data with the maximum 

applied loads from 0.63 to 5 mN. SEM, EBSD and AFM 

methods were used for microstructure characterization and 

for the identification of WC grains with different 

crystallographic orientation. The statistical evaluation of the 

results of GIT experiment revealed clear maxima of 

hardness of individual phases. However, these are shifted to 

higher values at lower indentation loads, which is probably 

connected with the indentation size effect.The hardness of 

the individual phases were in the range from approximatelly 

8 - 12 GPa for Co binder up to approximatelly 31 - 42 GPa 

for WC grains. Significant scatter in mechanical properties of 

WC ? Co is caused by the orientation dependence of 

hardness in WC and by the ratio of the indentation 

depth/mean free path in binder phase. The comparison of 

hardness values from individual WC grains and their 

crystallographic orientation obtained by EBSD revealed 

significant anisotropy of hardness and elastic modulus. Thus, 

GIT combined with instrumented indentation on individual 

WC grains with known orientation is a convenient method 

for the investigation of mechanical properties of individual 

phases as well as for the study of anisotropy of each phase. 

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Session V : - 

09:00 Nanocrystalline Composites based on Zinc Oxide: 

Preparation, Characterization and Properties 

Authors : Devendraprakash Gautam, Carolin Schilling, Alice 

Sandmann, Alexander Kompch, and Markus Winterer 

Affiliations : Nanoparticle Process Technology Faculty of 

Engineering Center for Nanointegration Duisburg-Essen 

(CENIDE) University of Duisburg-Essen Lotharstr. 1 47057 

Duisburg Germany 

Resume: The preparation of nanocomposite ceramics from 

powders is challenging since homogeneous mixing of (dry) 

powders on the nanoscale is hindered due to interparticle 

forces. Chemical Vapor Synthesis provides a route to 

produce nanoparticles consisting either of (metastable) 

solid solutions or core-shell particles. Sintered ceramics are 

prepared by pulsed electric current sintering. Structural 

characterization is performed using X-ray diffraction and 

electron microscopy. The control of distribution of two 

components at the particle level as well as the content of 

the second phase has substantial influence on 

microstructure and physical properties of the ceramic 

materials. Zinc oxide ceramics containing aluminum are 

interesting as transparent conducting and thermoelectric 

materials. 

09:35 Multiferroic composite ceramics: influence of synthesis 

parameters of core/shell SrTiO3/NiFe2O4 nanoparticles on 

final structural and functional characteristics 

Authors : Bojana Mojić1; Jelena Vukmirović1; Konstantinos 

P. Giannakopoulos2; and Vladimir V. Srdić1 

Affiliations : 1 Department of Materials Engineering, 

Faculty of Technology, University of Novi Sad, Serbia 2 

Institute of Material Sciences, NCSR “Democritos“, Greece. 

Currently at the Institute of Microelectronics, NCSR 

«Demokritos», Greece 

Resume: Composite multiferroic ceramics (consisting of 

ferroelectric and ferromagnetic separate phases) have 

drawn increasing attention in recent years, due to the wide 

variety of design possibilities and promising functional 

characteristics they posses. One of the most attractive 

ways to combine materials with ferromagnetic and 

ferroelectric properties is the core/shell structure. In this 

work, strontium titanate/nickel ferrite core/shell 

nanoparticles were prepared by the combination of sol-gel 

and co-precipitation methods. Possible routes for achieving 

complete core coverage, good control of shell thickness 

and decrease of agglomeration and thus particle size and 

size distribution were examined. Synthesized nanoparticles 

were further processed into dense ceramics and 

characterized in order to systematically examine the 

influence of the morphology and particular synthesis 

procedure on the final structural and functional 

characteristics of composite ceramics. Influence of 

processing parameters (uni-axial pressure, temperature 

and the type of sintering) on the characteristics of obtained 

dense ceramics was also investigated. Characterization of 

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synthesized particles and corresponding ceramics showed a 

close relation of synthesis parameters (pH, core/shell mass 

ratio, surfactant concentration) of core-shell particles to 

the structural (density, homogeneity, phase composition) 

and functional (electrical, magnetic) characteristics of 

obtained multiferroic ceramics. 

09:55 Surface properties of ceramic nanopowders and their 

influence on rheological properties of nanosuspension 

Authors : Anna Danelska, Mikolaj Szafran 

Affiliations : Department of Inorganic Technology and 

Ceramics, Faculty of Chemistry, Warsaw University of 

Technology, 3 Noakowskiego St, 00-664 Warsaw 

Resume: Surface characterization of ceramic nanopowders 

is crucial to determine their applicable potential. Surface 

properties are highly significant and intensified in 

nanoscale due to the developed surface of the powders. 

Nanopowders are found to be of great surface reactivity 

what is generally profitable but is a serious obstacle when 

the powders are manufactured or processed. Highly 

developed and metastable nanosurface becomes easily 

modified or contaminated during processing what often 

provides an unexpected behaviour of the substance. Such 

specific surface phenomena are usually noticed during 

aqueous processing of nanopowders, particularly when 

deflocculation of nanodispersions is carried out. Effectively 

working deflocculants are definitely required by colloidal 

processing of nanopowders. The additives are responsible 

for some favourable rheological properties of dispersions, 

like stability or decreased viscosity. Deflocculants work via 

some different mechanisms, but their majority work due to 

adsorption process on nanopowder surface. The adsorption 

changes electrostatic and/or steric interactions among 

nanoparticles. Contaminated or intentionally modified 

nanosurfaces do not cooperate properly with some 

deflocculants. Surface properties of ceramic nanopowders 

have to be defined and/or modified when rheological 

behaviour of nanosuspensions is to be controlled. Such a 

treatment would allow obtaining green and sintered bodies 

of satisfactory properties. 

10:10 Solution-based synthesis and characterization towards 

ceramic BaZrO3 nanocrystals 

Authors : K. De Keukeleere, M. Meire, J. Feys, P. 

Lommens, I. Van Driessche 

Affiliations : Ghent University, department of Inorganic and 

Physical Chemistry, SCRiPTS, Krijgslaan 281 – S3, Ghent, 

Belgium. Katrien.DeKeukeleere@ugent.be, 

Isabel.VanDriessche@ugent.be 

Resume: The versatile properties of ceramic oxides, make 

them very interesting candidates for multiple applications 

in the field of fuel cells, sensors, thermal barrier coatings 

and superconductors. Moreover, nanocrystals of these 

oxides exhibit very interesting size-dependent properties, 

which cannot be achieved by their bulk counterparts. 

Therefore, our research focuses on the synthesis and 

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characterization of BaZrO3 nanocrystals, for the 

incorporation as pinning centers in YBa2Cu3O7-δ (YBCO) 

high-temperature superconductors. YBCO superconductors 

have reached the level of high performance applications, 

like magnets, generators and transformers. However, the 

extent of the critical current density Jc and its dependence 

on the orientation of the magnetic field poses problems for 

practical applications. These problems can be circumvented 

by the introduction of structural and morphological defects, 

or pinning centers, like BaZrO3 nanocrystals, in the YBCO 

film. We explored a solvothermal and microwave assisted 

treatment to synthesize BaZrO3 nanostructures, starting 

from water and/or organic precursors. Afterwards, the 

particles are characterized by XRD and TEM analysis. In 

this research, the as-prepared nanocrystals are added to 

an YBCO precursor solution, which can be deposited on a 

substrate through the up scalable deposition technique, 

ink-jet printing. This brings us one step closer to the 

incorporation of these superconductors in applications for 

alternative energy generation. 


Session VI : - 

11:00 Thermal plasma synthesis of ceramic nano-powders and 

their characterization 

Authors : János Szépvölgyi, Zoltán Károly, Szilvia Klébert 

Affiliations : Institute of Materials and Environmental 

Chemistry, Research Centre for Natural Sciences, 

Hungarian Academy of Sciences 

Resume: Thermal plasma reactors provide special 

conditions for the synthesis of nanosized powders such as 

very high temperature, high heating rate of precursors and 

very rapid cooling of products. In particular systems 

ceramic powders of special composition, microstructure 

and morphology can be produced from a wide range of 

precursors. In this paper correlation among the 

composition, microstructure, macroscopic properties and 

synthesis conditions are presented and discussed for 

different model systems. The models include simple and 

composite oxide, nitride, carbide and boride ceramic 

powders produced in RF thermal plasma reactor. The 

powders are characterized by different advanced methods 

for bulk and surface chemical composition, purity, phase 

composition, morphology and application-related 

macroscopic properties. Their sintering behavior on hot 

pressing and spark plasma sintering was studied, as well. 

11:35 SYNTHESIS AND CHARACTERIZATION OF A VARISTOR 

POWDER USING A SOFT CHEMISTRY PROCESS 

Authors : Geoffroy GADACZ, Sophie BEAUDET-SAVIGNAT, 

Jean-Louis LONGUET, Laurence LONGUET 

Affiliations : CEA/DAM, Le Ripault BP 16, 37200 MONTS 

Resume: Synthesis of oxide powders using coprecipitation 

processes is a robust alternative to traditional 

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ceramic powder preparation. This method allows indeed an 

easier doping with different elements because of the lower 

grain size produced. It results in powders with a higher 

purity, more homogeneous composition and higher 

reactivity to sintering. The aim of this work is to produce 

varistor powders of ZnO doped with Co and Mn using a coprecipitation 

process. Bismuth oxide is also added as a 

varistor former. In this way, ceramic powders have been 

prepared in a two step process. First, Zn, Mn and Co 

precursors solutions were co-precipitated using 

concentrated NaOH. Since the obtained hydroxides 

contained a high quantity of impurities, they were 

converted into oxalates using oxalic acid addition. After 

filtration, the oxalates were washed, dried, and fired. 

Secondly, the obtained powders were mixed with an acidic 

bismuth nitrate solution. After precipitation of the bismuth 

ions, powders were again washed and fired after filtration. 

Here we present a study of the influence of the first step 

firing procedure and the the precursor type (chloride or 

nitrate) on the powder and ceramics properties. ICP-AES, 

MEB, BET and electric field measurements were performed. 

The results show that the powders are extremely pure, 

have a specific surface area around 7-16 m².g-1 and sinter 

at temperatures around 730-750°C. Breakdown field 

measurements show that, depending on the powders, 

values between 40 and 70 kV.cm-1 can be obtained. 

11:55 Microwave assisted synthesis of zirconia and YSZ colloidal 

solutions 

Authors : K. Vernieuwe, P. Lommens, J. Martins, I. Van 

Driessche, K. De Buysser 

Affiliations : Ghent University, department of Inorganic and 

Physical Chemistry, SCRiPTS, Krijgslaan 281 S3, Ghent, 

Belgium. Kenny.Vernieuwe@ugent.be, 

Klaartje.DeBuysser@ugent.be 

Resume: In the world of ceramic materials, zirconia and 

YSZ are well-know materials with very specific properties. 

Cubic zirconia is famous for its low thermal conductivity 

and yttria-stabilised zirconia is an excellent oxygen ion 

conductor. Nowadays, the synthesis of nanoparticles and 

colloidal solutions gained more and more interest because 

the material properties can be tuned accurately. Also, 

scaling down the dimensions of these ceramics results in 

faster sinter processes at lower temperatures which is a 

first step towards low energy consuming and 

environmental friendly synthesis processes. The 

advantages of microwave assisted solvothermal synthesis 

routes in comparison with more traditional solid state 

reactions or solvothermal synthesis routes make it a very 

attractive synthesis route. The modern microwave 

equipment allows a fast screening of several parameters 

due to the short reaction time. Even the production of high 

quality nanomaterials on industrial level is possible. 

Aqueous solutions, containing Zr4 or Y3 and Zr4 ions can 

be transformed into colloidal solutions via microwave 

treatment. Several parameters can be studied such as 

reaction time, reaction temperature, complexingagents, pH 

level, etc. The particle size of the obtained particles varied 

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from 40 ? 400nm. The crystallinity is studied by X-ray 

diffraction. The stability and possible ligand exchange of 

these particles is studied through NMR (1D proton 

combined with 2D NOESY) and TGA-DTA. 

12:10 Simple and rapid synthesis of giant dielectric constant 

CaCu3Ti4O12 ceramics using novel Electric Discharge 

Assisted Mechanical Milling 

Authors : A.Calka1,#, A. A. Chowdhury1, D.Wexler1 and K. 

Konstantinov2 

Affiliations : 1 School of Mechanical, Materials and 

Mechatronic Engineering, Faculty of Engineering, University 

of Wollongong, NSW 2522, Australia 2 Institute for 

Superconducting and Electronic Materials, University of 

Wollongong, NSW 2522, Australia 

12:30 Lunch 

Resume: The conventional method to prepare functional 

oxides is ceramic-powder-based processing, i.e., through 

solid-state reaction at high temperatures. This process has 

several disadvantages, such as high-temperature reaction, 

limited degree of chemical homogeneity, and low sintering 

ability. Various chemical-based processing routes have 

been developed to prepare powders with more 

homogeneous composition, improved reactivity, and 

sintering ability at low temperatures. Regardless of the 

route chosen to synthesize complex oxides, almost all of 

them require lengthy heat treatment schedules that usually 

exceed 10 h, as well as multi-stage processing steps. The 

EDAMM technique has successfully been applied for the 

rapid synthesis of oxide capacitor materials. By using 

EDAMM, nanocrystalline precursors of high dielectric 

constant ceramics can be formed in as little as 0.1% of the 

processing time required in conventional solid-state 

techniques. In this study we present for the first time that 

using nanocrystalline precursor of CaCu3Ti4O12 made by 

EDAMM and subsequent annealing, dielectric constant of 6 

x105 can be achieved at room temperature and @50Hz 

frequency. In this study we discuss process parameters 

that lead to formation of nanostructured CaCu3Ti4O12 . 

Characterization of samples after EDAMM and after 

sintering was carried out using XRD, TEM and SEM. The 

dielectric properties of prepared samples were studied by 

LCR meter. 

Session VII : - 

14:00 Nanoceramic based fibers for force protection and 

situational awareness 

Authors : Prof. Dr. Ashok VASEASHTA, Dr. Nimet BOLGEN 

Affiliations : Institute for Advanced Sciences Convergence 

& Intl' Clean Water Institute NUARI, 13873 Park Center Rd. 

Suite 500 Herndon, VA 20171 USA 

Resume: The objective of this investigation to develop a 

systematic and progressive methodology to develop 

micro/nanofibers using electrospinning employing ceramers 

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1

and other novel materials mixed in solutions of highperformance 

polymers. The methodology involves 

identification and selection of novel combinations of loading 

and high-performance polymers. The resulting 

nano/microfibers with properties leading to increased 

mechanical strength, improved sensitivity to contaminants, 

better filtering capabilities, improved response to 

electromagnetic stimuli, and desired conductivity. Also, 

high surface area/volume ratio and fibers with varying 

functionality, combined with its potential biocompatibility 

and biodegradable nature, offers tremendous promise for 

diverse applications in tissue engineering, targeted vaccine 

delivery, non-thrombogenic materials for blood contacting 

applications, chemical and biological sensors, system-onfibers 

(SoF) and e-textiles. Such characteristics will allow 

for the creation and improvement of barrier materials for 

force protection, embedded informational and 

communication technologies (ICT) devices - signal 

receiving/communication capability, sensors that respond 

to environmental contaminants, built-in timed-release or 

physiological condition based-release therapeutics, filtering 

of contaminants, biological mimicking for sensing, and 

optical cloaking – all of which promise direct applications of 

loaded micro/nano fibers in outerwear used in combat 

theatre. In addition, a selected application of the loaded 

electrospun nanofibers in biomedicine will be presented. It 

was shown that antibiotic loaded biodegradable and 

biocompatible polymeric electrospun nanofibrous 

membranes can prevent post surgery induced intraabdominal 

adhesions by providing a physical barrier during 

wound healing process and at the same time a functional 

barrier against strains of microorganisms thereby reducing 

the local inflammatory response. The results of our 

previous studies including synthesis of biocompatible and 

biodegradable polymers, production and characterization of 

electrospun nanofibers from those polymers, their loading 

with drugs and the release of the drugs from the produced 

matrices would provide a linkage for the development of 

new functional barriers for protection applications. The 

work is complemented by using advanced science 

convergence methodologies such as automated data 

analysis, mining and surveillance (ADAMSTM) and 

technology foresight and road-mapping (TechFARMTM) to 

provide additional knowledge base. Preliminary data of 

fibers using loaded high performance polymers will be 

presented with the objective to fabricate ceramers 

embedded multi-functional nano/micro fibers for military 

outerwear and gears that provide an integrated solution 

path through a revolutionary approach of using ceramers 

embedded in high performance polymers as materials for 

suits, masks, and embedded sensors for situational 

awareness. Keywords: e-spin, nano-fibers, filtration, 

mechanical strength, sensors 

14:35 CHARACTERIZATION OF ZnO/CuO2 HETEREOSTRUCTURE 

NANOPILLAR ARRAYS 

Authors : Gariné Guerguerian1, Fernando Elhordoy1, 

Carlos J. Pereyra1, Ricardo E. Marotti1, Francisco Martín2, 

Dietmar Leinen2, José R. Ramos-Barrado2 and Enrique A. 

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Dalchiele1 

Affiliations : 1. Instituto de Física & CINQUIFIMA, Facultad 

de Ingeniería, Herrera y Reissig 565, C.C. 30, 11000 

Montevideo, Uruguay.  Laboratorio de Materiales y 

Superficie (Unidad Asociada al CSIC). 2. Departamentos de 

Física Aplicada & Ingeniería Química, Universidad de 

Málaga, Campus de Teatinos s/n, E29071 Málaga, Spain. 

Resume: Vertically aligned ZnO/Cu2O heterostructure 

nanopillar arrays consisting of a ZnO core and a Cu2O shell 

were fabricated by a two-step electrochemical deposition 

method. Morphological, structural and optical properties of 

the nanopillar heterojunctions were investigated. The 

surface of the single-crystalline ZnO nanopillars has been 

coated uniformly, conformally and densely over the entire 

nanopillar length by numerous Cu2O nanocrystals (25-35 

nm mean diameter), constituting a conformal shell layer 90 

nm thick, integrating these two materials into an 

electronically intimate composite. The optical properties 

can be interpreted, by appropriate fittings of each feature, 

as being due to the properties of the bare ZnO nanopillar 

array plus the increased absorption of Cu2O. This study 

demonstrates that electrodeposition is a suitable and 

accessible technique for large-scale fabrication of nanopillar 

heterostructures and to achieve conformal coverage of 

nanostructured samples. 

14:55 Spark plasma sintering of ZrC-based nanocomposites 

Authors : Irina Hussainova1, Nikolai Voltšihhin1, Der-Liang 

Yung1, Erkin Cura2, Simo-Pekka Hannula2 

Affiliations : 1Department of Materials Engineering, Tallinn 

University of Technology, Ehitajate 5, 19086 Tallinn, 

Estonia 2Department of Materials Science and Engineering, 

Aalto University School of Chemical Technology, POB 

16200, Aalto 00076, Finland 

Resume: The potential applications for ZrC span a wide 

number of needs arising from future military, industrial, 

and space based projects. The study is aimed at 

development, processing and characterization of ZrC - 

based ceramics for high temperature applications. ZrC 

matrix composites added by nanosized partially stabilized 

zirconia and titanium carbide were spark plasma sintered 

to >98% of theoretical density at temperatures between 

1700 and 2000 0C and pressure of 50 MPa. The weight 

fraction of additives varied from 40 to 20% in the 

precursor powder blend. ZrC powders were produced by 

cost-effective in situ reactive sintering of nano-sized 

zirconium oxide and graphite. Mechanical activation by ball 

milling technology and reactive vacuum sintering were 

used to synthesize ZrC nanopowder. The major drawbacks 

for bulk ZrC is low sinterability of the powder and relatively 

low fracture toughness, making it a less than ideal 

candidate for use in high temperature applications where 

mechanical stresses are prevalent. Microstructural analysis 

shows the fine-structured composites of quite uniform 

phase distribution. The presence of the retained tetragonal 

zirconia in ZrC-ZrO2 composite results in some increase in 

fracture toughness due to stress induced transformation 

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3

toughening while the effect of zirconia phase 

transformation is most pronounced under conditions of 

impact wear. Introduction of TiC particles inhibits ZrC grain 

growth and improve sinterability. 

15:10 Effect of oxide nanofillers on fabrication, structure and 

properties of zirconia based composites 

Authors : Igor Danilenkoa, Fedor Glazunov, Tetyana 

Konstantinova, Galina Volkova, Valerii Burkhovetski 

Affiliations : Material science department of Donetsk 

Institute for Physics and Engineering NAS of Ukraine, 

Donetsk, Ukraine 

Resume: Oxide ceramics have wide applications as 

alternative materials to traditional metallic tools, due to 

their combination of strength and wear resistance. ZrO2 

has an outstanding combination of mechanical properties of 

all ceramic materials, but it not enough for modern 

technique. One of the promising means used for solving of 

this problem is application of ceramic based composites. 

The addition of second-phase inclusions that stopped the 

cracks propagation in the material is one much studied 

approach. There are widely studied ZrO2- Al2O3 

composites. Much attention also focused on the 

development of ceramic nanocomposites with nano-sized 

metal dispersion, in particular, ZrO2 - Ni composites. In 

this material the toughness enhancement is due to the 

plastic deformation of the ductile inclusions. In this work 

the influence of oxide and metallic inclusions on fracture 

toughness of zirconia based composites was studied. The 

reversible transformation of NiO to Ni under reduction – 

oxidation environment allow to varying the nature of 

inclusions and study the structure and properties of 

nanocomposite materials in the system ZrO2-NiO(Ni). It 

was shown that fracture toughness of sintered 

nanocomposite ZrO2-NiO(Ni) increased more that two 

times in comparison with zirconia ceramics. Also was 

shown that the increase of the oxide component leads to 

effective inhibition of crack propagation in composite 

material. 


Session VIII : - 

16:00 Porous zirconia nanoceramics with hierarchical 

heterogeneities 

Authors : Andraz Kocjan(1,2), Zhijian Shen(1) 

Affiliations : (1) Department of Materials and 

Environmental Chemistry, Arrhenius Laboratory, Stockholm 

University, S-10691 Stockholm, Sweden (2) Engineering 

Ceramics Department, Jo?ef Stefan Institute, Jamova 39, 

SI-1000, Ljubljana, Slovenia 

Resume: The demand for porous zirconia ceramics is 

growing, due to their potential application in the fields of 

fuel cells, catalysis, filtration, and bio-implants. In the 

latter case, its porous characteristics could provide a nano- 

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1

textured surface that might enhance the bioactivity of an 

otherwise bioinert material. However, it is not trivial to 

process zirconia ceramics exhibiting a high surface area 

and tailor-made pore structures in the meso-scale region. 

In general, porous ceramics are prepared either by packing 

the powder and sintering them to moderate densities or by 

inserting pore-forming agents, which, however, results in 

micro- rather than meso-porous materials. In the first 

approach more often than not the migration and 

coalescence of the non-homogeneously distributed pores in 

the ceramic body result in an increase of the pore 

coordination number and thus in a smaller interparticle 

contact area and/or the formation of detrimental strengthlimiting 

point defects, which are hard or impossible to 

eliminate, even with higher sintering temperatures. In the 

present work an attempt was made to prepare porous 

zirconia ceramics by the processing of a mesoporous 

zirconia powder. The powder consists of about 200nanometer-sized 

(d50) particles, which are initially 

composed of ten times smaller, loosely aggregated 

crystallites. The consolidated green compacts thus 

exhibited hierarchical heterogeneities in terms of the 

bimodal distribution of pores, originating from intra- and 

inter-particle packing. It is a challenge to sinter this type of 

microstructure while retaining the bimodal pore structure. 

The pore structure development and neck formation 

between the intra- and inter-particles during the sintering 

of as-prepared green compacts will be discussed. It will 

also be shown that the uniform packing and coordination of 

aggregated nanoparticles can lead to a superior 

microstructural evolution of ceramics. Using this process, 

i.e., making porous ceramics exhibiting hierarchical 

heterogeneities, we meet the conflicting demands of 

developing reasonable mechanical properties, while 

maintaining the high porosity, which offers a high pore 

surface area and beneficial textured surfaces. 

16:20 Two-Stage Master Sintering Curve for description of Two- 

Step Sintering 

Authors : Vaclav Pouchly 1, Karel Maca 1+2 , Zhijian 

James Shen 3 

Affiliations : 1 Department of Ceramics and Polymers, 

Faculty of Mechanical Engineering, Brno University of 

Technology, Technicka 2896/2, 616 69 Brno, Czech 

Republic; 2 Department of Ceramics and Polymers, CEITEC 

BUT, Technicka 3058/2 616 69 Brno, Czech Republic; 3 

Department of Materials and Environmental Chemistry, 

Arrhenius Laboratory, Stockholm University, S-106 91 

Stockholm, Sweden; 

Resume: The Master Sintering Curve (MSC) is a useful tool 

for sintering description and prediction. Fine-grained 

(tetragonal and cubic) zirconia and alumina powders were 

shaped by cold isostatic pressing and then sintered by 

different Constant-Rate of Heating (CRH) schedules as well 

as by Two-Step Sintering (TSS) regimes in hightemperature 

dilatometer. It was found that the shape of 

MSC created with TSS data deviates significantly from that 

constructed with CRH data. Our newly developed Two- 

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2

Stage Master Sintering Curve addressed this deviation to 

another sintering mechanism with lower activation energy 

acting in the final sintering stage. The influence of different 

sintering and grain growth activation energies on final 

microstructure of sintered ceramics is discussed. 

16:35 Structural and dielectric properties of yttrium substituted 

nickel ferrite nanoceramics 

Authors : Stevan M. Ognjanović1, Stevan Jankov2, Srdjan 

Rakić2, Željka Cvejić2, Goran Stojanović3,Akos Kukovecz4, 

Vladimir V. Srdić1 

Affiliations : 1 Department of Materials Engineering, 

Faculty of Technology, University of Novi Sad, Serbia 2 

Institute of Physics, Faculty of Natural Sciences, University 

of Novi Sad, Serbia 3 Faculty of Technical Sciences, 

University of Novi Sad, Serbia 4 Department of Applied and 

Environmental Chemistry, University of Szeged, Hungary 

Resume: A lot of attention was dedicated in recent years 

to trivalent ion substituted nickel ferrites due to their 

excellent properties and potential applications as core 

materials in telecommunications and other high frequency 

applications. A lot of research has been done on Gd3+ and 

Tb3+ substituted ferrites, while Y3+ has received little 

attention. Therefore, in this work nickel ferrite 

nanopowders containing different amounts of Y (NiFe2xYxO4, 

where x = 0, 0.05, 0.15, 0.2 and 0.3) were 

synthesised by the co-precipitation method. The spinel 

structure was confirmed using X-ray diffraction, while 

additional structural characterisation was done by SEM, 

TEM, FTIR and low temperature nitrogen adsorption. The 

powders were then annealed, uniaxially pressed into pellets 

and sintered at optimal temperature in order to obtain 

dense ceramics. Structural and dielectric properties of the 

pellets were examined before and after sintering, and 

correlated to the concentration of Y in order to determine 

the influence of Y3+ ions on the applicability of substituted 

nickel ferrite ceramics. 

16:55 Functionalization of nitride engineering ceramics by 

polymer derived sintering aids 

Authors : Z. Lenčéš, P. Šajgalík, T. Plachký, R. Riedel,* 

H.J. Kleebe* 

Affiliations : Institute of Inorganic Chemistry, Slovak 

Academy of Sciences, Bratislava, Slovakia *Technische 

Universität Darmstadt, Darmstadt, Germany 

Resume: Densification of silicon carbide and/or silicon 

nitride ceramics is usually reached by the addition of some 

oxide additives which together with SiO2 as a main 

impurity in nonoxide ceramics powders create a liquid 

phase at the temperatures of sintering. This temporary 

liquid helps to densify the samples at reasonable sintering 

temperatures and times. The selection of particular oxides 

affects not only the sintering conditions but also the 

highest temperature limit of their application. As less 

viscous liquid phase we are able create at the sintering 

conditions as low can be the sintering temperature. On the 

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4

other hand, these low viscous liquids produce also a low 

temperature melting glasses, which are distributed on the 

grain boundaries and thus dictates the temperature of 

ceramics application. It seems to be beneficial to replace 

the binary oxide sintering additives by other more viscous 

systems. The replacement of the binary oxide additive by 

SiOC and/or SiOAlC sintering additives is one of the 

solutions. SiOC and SiOAlC sintering additives were 

prepared from organometalic precursor by cross-linking 

and subsequent pyrolysis. Prepared ceramic composites 

consist of the major crystalline phase and residual glass 

located along the grain boundaries and multi grain 

junctions. This glass is partly crystallized with the SiC 

nano-inclusions as a main phase. Room temperature 

hardness and fracture toughness of both materials are 

similar to those for the liquid phase sintered silicon nitride. 

The presence of this matter at grain boundaries affects not 

only the mechanical properties but also the thermal 

properties. E.g. addition of 7 vol % of SiOC increased the 

thermal conductivity of ceramics up to 80 W/m.K. On the 

other hand O´-sialon was prepared by the addition of 

SiAlOC precursor to the crystalline silicon nitride powder. 

Eu-doped O´- sialon showed luminescent properties. This 

type of phosphor synthesized at 1650 °C emitted greenyellow 

light, when excited by UV light. 

17:15 Negative capacitance of nanocomposites containing CoFeZr 

nanoparticles embedded into ferroelectric PZT matrix 

Authors : J.A. Fedotova, T N Kołtunowicz, P. Zhukowski, A. 

Saad, A.K. Fedotov, ?.V. Mazanik, A.V. Larkin, Yu.E. 

Kalinin, A.V. Sitnikov, V.V. Fedotova 

Affiliations : National Centre for Particles and High Energy 

Physics of BSU, 220040 Minsk, Belarus; Lublin University of 

Technology, 20-618 Lublin, Poland; Al-Balqa Applied 

University, 11953 Amman, Jordan; Belarusian State 

University, 220030 Minsk, Belarus; Voronezh State 

Technical University, 250770 Voronezh, Russia; Practical- 

Scientific Center of NASB on Material Science, 220078 

Minsk, Belarus 

Resume: We studied frequency/temperature dependences 

of real part of admittance G(T, f) in 

(Fe0.45Co0.45Zr0.10)0.28(PZT)0.72 composite films 

containing FeCoZr nanoparticles embedded into 

ferroelectric PZT matrix. The films with x = 0.28 and 3 m 

thicknesses were deposited in vacuum chamber with Ar O2 

atmosphere using ion-beam sputtering technique. 

Admittance measurements in frequency range of 0.1-100 

kHz were performed at the temperatures of 77 - 330 ?. The 

films were also characterized by Mössbauer and Raman 

spectroscopies, scanning electron microscopy and 

magnetization studies. It was revealed by Mössbauer 

spectroscopy and magnetization measurements that 

FeCoZr nanoparticles were in superparamagnetic state. The 

observed G(f, T) dependencies for the studied films have 

shown dielectric regime of carrier transport and observed 

an negative capacitance effect (inductive-like contribution) 

on G(T, f) dependencies. This effect was explained by a 

specially developed model of AC/DC hopping conductance 

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5

of electrons over FeCoZr nanoparticles covered with 

complicated CoFe-oxides and embedded into PZT matrix. 

In particular, at the determined conditions such a structure 

of nanocomposite resulted in the increase of hopping 

electron mean life time on nanoparticles and delay its 

returning jump under subjection of alternating electric field 

that created the possibility for positive angles of the phase 

shifts and properly NC (inductive-like contribution) effect 

even at room temperatures. 

17:20 Functional Nanoceramics for Intermediate Temperature 

Solid Oxide Fuel Cells and Oxygen Separation Membranes 

Authors : V. Sadykov, V. Usoltsev, N. Yeremeev, N. 

Mezentseva, T. Krieger, A. Ishchenko, Yu. Okhlupin, N. 

Uvarov, O. Smorygo, A. Arzhannikov, M. Korobeynikov, 

Ma. K. A. Thumm 

Affiliations : Boreskov Institute of Catalysis, Novosibirsk 

State University, Novosibirsk, Russia; Institute of Solid 

State Chemistry, Novosibirsk, Russia; Powder Metallurgy 

Institute, Minsk, Belarus; Budker Institute of Nuclear 

Physics, Novosibirsk State University, Novosibirsk, Russia; 

Karlsruhe Inst. Technol., Karlsruhe, Germany 

Resume: This work reviews results of research aimed at 

design and characterization of mixed ionic-electronic 

conducting perovskite-fluorite nanocomposite ceramics as 

functional cathode layers in solid oxide fuel cells (SOFC) 

and oxygen –permeable layers in asymmetric supported 

membranes. Nanocrystalline complex oxides with ionic 

conductivity (YSZ, ScCeSZ, GDC, etc) and mainly electronic 

conductivity (Ln1-xSrxMe11-yMe2yO3, Ln2MeO4, Ln= La, 

Pr; Me = Mn, Co, Ni, Cu) were prepared via polymerized 

polyester precursors (Pechini) route, their nanocomposites 

–via powerful ultrasonic dispersion of their mixture in 

organic solvents with addition of surfactants. Thin 

functional nanocomposite layers were supported on 

electrolyte layers and Ni-Al foam membrane substrate by 

slip casting, screen-printing and air brushing. New sintering 

techniques (microwave heating or e-beams radiationthermal 

treatment) were shown to provide a higher density 

of nanocomposite ceramics at lower temperatures as 

compared with conventional sintering. Genesis of the real 

structure of sintered functional layers was studied in details 

by high resolution transmission electron microscopy and 

scanning electron microscopy with local elemental analysis 

by EDX, X-ray powder diffraction, XPS. Applied preparation 

procedures ensured nano-sizes of domains even in dense 

ceramics and a high spatial uniformity of constituting 

phases distribution. Redistribution of elements between 

perovskite-fluorite domains without formation of new 

phases was revealed. Characterization of nanocomposite 

transport properties by oxygen isotope heteroexchange 

and analysis of dynamics of conductivity or weight variation 

after changing the oxygen partial pressure in the gas phase 

demonstrated that perovskite-fluorite interfaces are paths 

for fast oxygen diffusion with oxygen diffusion coefficients 

exceeding those within perovskite or fluorite domain by up 

to 6 orders of magnitude. Best perovskite-fluorite 

combinations providing the highest oxygen mobility were 

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7

selected, and their composition was optimized. For buttonsize 

thin film fuel cells with nanocomposite cathode layers 

on YSZ electrolyte, the maximum power density was up to 

600-800 mW/cm2 at 700 °C using wet H2/air feeds. For 

supported oxygen separation membranes the oxygen flux 

achieved under air/CH4 gradient was up to 10 cm3 O2 

(STP)/cm2min. Hence, developed mixed ionic-electronic 

nanoceramics is promising for the practical application in 

the hydrogen energy field. Support by by OCMOL FP7 

Project, Integration Projects SB RAS- Belarus NAS, Russian 

Federation Government Grant N 11.G34.31.0033 and 

Federal Program “Scientific and Educational Cadres of 

Russia” is gratefully acknowledged. 

Poster Session 

17:30 Forming of Protecitve Nanostructure Coatings on Metals an 

Glasses and Their Properties Investigation 

Authors : Alla Deshkovskaya, Leonid Lynkov, Andrey 

Nagibarov, Vasiliy Glybin, Edgar Richter, M. Pham 

Affiliations : Belarusian State University of Informatics and 

Radioelectronics, Minsk, Belarus; Belarusian State 

University of Informatics and Radioelectronics, Minsk, 

Belarus; "Para la Oro Inc.", Minsk, Belarus; Belarusian 

Technological University, MInsk, Belarus; R&D center, 

Rosendorf, Germany; R&D center, Rosendorf, Germany 

Resume: 10…30 nm transparent heat-resistant coatings 

described by (ZrO2)x•(Y2O3)y composition are formed on 

the surface of metals and glasses by a thermolysis 

technique. The deposited coatings are characterized by a 

high adhesive strength, high corrosive and abrasive 

resistance. The nanocrystalline formations are revealed on 

the sample surfaces, with the quantity of these formations 

depending on the basic solution concentration, number of 

the layers formed, and mode of the thermal treatment. The 

ion-beam modification of the obtained coatings in the 

conditions of the mixing mode enables the said properties 

to enhance owing to formation of zirconium oxiboride 

within the coating as a result of ion-beam synthesis. 

17:30 Nb-doping effects on the hydrophilicity of TiO2 coatings 

prepared by sol-gel method 

Authors : A. V. Manole 1, M. Dobromir 2, M. Gîrtan 3, R. 

Mallet 4, G. Rusu 1, D. Luca 1 

Affiliations : 1 Faculty of Physics, “Alexandru Ioan Cuza” 

University, 700506 Iaşi, Romania; 2 Department of 

Sciences, “Alexandru Ioan Cuza” University, 700506 Iaşi, 

Romania; 3 Photonics Laboratory, Angers University, 

49045 Angers, France; 4 SCIAM, Angers University, 49045 

Angers, France 

Resume: The high hydrophilicity exhibited by TiO2 under 

UV exposure associated with its photocatalytic activity 

makes this material most suitable for coating applications 

like self-cleaning, self-sterilizing and antifogging surfaces. 

In this work, we studied surface wettability of pure and Nbdoped 

TiO2 synthesized using a sol-gel method and 

F 

28 

F 

29

deposited as thin films by spin-coating and annealing at 

500°C. The surface hydrophilicity was evaluated from 

contact angle data. The surface elemental composition was 

derived from X-ray photoelectron spectra, while structure 

and surface morphology were investigated using grazingincidence 

X-ray diffraction and atomic force/scanning 

electron microscopy. Finally, the optical properties were 

investigated by means of UV-Vis spectroscopy and 

spectroscopic ellipsometry. The XRD patterns of the 

deposited films, with about 30 nm thickness, showed no 

diffraction peaks. Doping TiO2 samples with Nb modified 

the surface morphology and hydrophilicity: the surface 

roughness increases with Nb content (1.8 - 4.3 at.%), 

resulting in a decrease of the contact angle. This is 

accompanied by a decrease in the refractive index and an 

increase of the band gap of the TiO2 films. Our findings are 

discussed in terms of recent results from the literature. 

Acknowledgements The financial support from the 

Romanian Ministry of Education, Research and Youth 

through PCCE ID_76 project and from the EU Structural 

Funds through POSDRU 89/1.5/S/49944 project is 

acknowledged. 

17:30 THE INFLUENCE OF SiO2 ADDITION ON THE 

MICROSTRUCTURE, MECHANICAL PROPERTIES AND CREEP 

BEHAVIOR OF HOT PRESSED Al2O3/SiC NANOCOMPOSITES 

Authors : M. Parchovianský1, D. Galusek2, J. Sedláček2, P. 

Švančárek2, M. Kašiarová3, J. Dusza3 

Affiliations : 1Faculty of Chemical and Food Technology 

STU, Radlinského 9, 812 37 Bratislava; 2Vitrum Laugaricio 

– Joint Glass Center of the Institute of Inorganic 

Chemistry, SAS, Alexander Dubček University of Trenčín, 

and RONA, j.s.c, Študentská 2, 911 50 Trenčín; 3Institute 

of Materials Research, Slovak Academy of Sciences, 

Watsnova 47, SK-043 53 Košice; 

Resume: The incorporation of small amount of silicon 

carbide particles into alumina matrix could significantly 

enhance mechanical properties, especially strength, 

fracture toughness, hardness and also wear and creep 

resistance. However, the exact mechanism of 

strengthening is not clear, and some results indicate that 

purely mechanical explanation does not suffice if the 

chemical influence, especially the presence of silica, which 

is always present as oxide layer at the surface of SiC 

nanoparticles, at grain boundaries, is not taken into 

account. In order to elucidate the silica influence on 

mechanical properties of Al2O3-SiC micro-nanocomposites 

the materials with 5 vol. % of silicon carbide nanoparticles 

were prepared by hot pressing the composite powder in 

graphite die for 1 hour at 30 MPa in the Ar atmosphere and 

the temperature 1740 °C. Silica free specimens were 

prepared by removing the oxidized silica layer from SiC 

powder by washing in HF. The Al2O3-SiC nanocomposited 

with controlled silica contents (0; 0,5; 1 and 5 wt.% SiO2) 

were also prepared with tetraethylortosilicate (TEOS) as 

the source of silica. The influence of the silica addition on 

microstructural development, mechanical properties, 

including hardness, fracture toughness, fracture strength 

F 

30

and creep resistance of 5 vol. % SiC-Al2O3 

nanocomposites is discussed and evaluated. Keywords: 

Al2O3/SiC nanocomposites, SiO2, mechanical properties, 

creep 

17:30 Silicon oxycarbide black glasses prepared from the 

precursor system polydimethylosiloxane/toluene-soluble 

fraction of coal tar pitch 

Authors : Cezary Czosnek 1, Mariusz Drygaś 1, Zbigniew 

Olejniczak 2, Patrycja Winiarczyk 1a, Krzysztof Paterak 1a, 

Jerzy F. Janik 1 

Affiliations : 1 AGH University of Science and Technology, 

Faculty of Energy and Fuels, al. A. Mickiewicza 30, 30-059 

Krakow, Poland, a - student 2 Institute of Nuclear Physics, 

Polish Academy of Sciences, ul. Radzikowskiego 152, 31- 

342 Krakow, Poland 

Resume: Silicon oxycarbide glasses possess many 

advantageous properties such as high thermal and 

chemical stabilities, low density, and good electrical 

properties, the latter resulting from the presence of free 

carbon often in the graphitic form. These materials 

frequently show higher electric charge capacity than that of 

graphite and for this reason are considered potential 

sources for anode production in lithium-ion batteries. We 

present here a part of our study on the preparation of 

silicon oxycarbide black glasses from the precursor system 

composed of silicone oil and toluene-soluble fraction of a 

coal tar pitch. We applied two commercially available types 

of silicone oil as received. A toluene-soluble coal tar pitch 

fraction was obtained by a standardized extraction workup. 

After mixing an oil with the coal tar pitch fraction under 

reflux, the solvent was removed by distillation and each of 

the binary precursor mixtures was initially subjected to 

curing in air. This step was followed by a two stage 

pyrolysis under argon at 600 °C and 1300 °C. The black 

solid products of the pyrolyses were at this point 

investigated/characterized mainly with the powder XRD, 

SEM, 29Si MAS NMR, and FT-IR spectroscopy. 

Acknowledgment. This work was supported by AGH 

University of Science and Technology Grant No. 

11.11.210.213 

17:30 VUV Synchrotron Radiation Spectroscopy of Li2B4O7 glass 

ceramics 

Authors : A.I. Popov (1) , V. Savchyn (2), V.Pankratov (1), 

V.T.Adamiv (3), Ya.V. Burak (3), I.M.Teslyuk (3) 

Affiliations : (1) Institute of Solid State Physics, University 

of Latvia, Kengaraga 8, 1063 Riga, Latvia, (2) Department 

of Electronics, Ivan Franko National University of Lviv, 107 

Tarnavskogo str, 79017 Lviv, Ukraine, (3) Institute of 

Physical Optics, 23 Dragomanov str., 79005, Lviv, Ukraine 

Resume: Lithium tetraborate Li2B4O7 is considered to be 

a perspective material for neutron detection. In this report, 

for the first time the luminescence properties of Li2B4O7 

ZnS AgI glass compounds were studied under vacuum 

ultraviolet (VUV) and ultraviolet (UV) synchrotron radiation 

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(3.6 ? 25.0 eV) emitted from DORIS III storage ring at 

SUPERLUMI station at HASYLAB, DESY, Hamburg, in the 

wide temperature range of 10?293 K. As it is known for 

many materials, the use of synchrotron radiation provides 

ideal conditions for the multiplication of electronic 

excitations, when each absorbed photon produces two or 

more electronic excitations. To study this effect, we have 

measured the appropriate excitation spectra of the intrinsic 

emission (~500 nm). In all cases, a prominent threshold 

for excitation multiplication at ca. 20.0 eV (as high as (3-4) 

Eg) was discovered. 

17:30 Colour Tuning of Niobium Oxides Core-Shell Structures 

Authors : C. Nico(1), M. Matos(2), R. Monteiro(2), M.A. 

Valente(1), F.M. Costa(1), T. Monteiro(1), M.P.F. Graça(1) 

Affiliations : (1) Department of Physics & I3N, University of 

Aveiro, Campus Universitário de Santiago 3810-193 Aveiro, 

Portugal (2) KEMET Electronics, Évora, Portugal 

Resume: Niobium oxides have been reported to be an 

alternative to tantalum, and its oxide, for the production of 

solid electrolytic capacitors. Regardless the increasing 

number of works on niobium oxides in the past decade, 

these materials still require a further and exhaustive study. 

The understanding of the dynamics of the oxidation 

process from NbO to Nb2O5 is essential to explain and 

control the properties of a niobium oxide based capacitors. 

In-situ XRD analysis of NbO powders was performed from 

100 to 1100 ºC, which showed a temperature range where 

only amorphous phase was present between the NbO and 

T-Nb2O5 crystallization. The capacitor anodes, formed from 

the same type of NbO powders, were then treated in air 

from room-temperature (RT) to 450 ºC with different 

heating rates and recorded with a video camera to see the 

colour shift with the temperature. Under the same 

conditions, in-situ Raman spectroscopy analysis was 

performed. Some anodes were also treated at different 

temperatures between 300 and 400 ºC and analysed by 

SEM and absorption spectroscopy. The presence of coreshell 

structures and the increase of the shell 

thickness/amount with temperature are visible in SEM and 

justify the shifting of the anodes colours. 

17:30 Development and characterization of bulk aluminumalumina 

nanocomposites - study of their nanosintering with 

respect to densification and grain growth 

Authors : C. Balázsi , Ajay Dhar 

Affiliations : Hungarian Academy of Sciences, Research 

Centre for Natural Sciences, Institute for Technical Physics 

and Materials Science, 1121 Budapest, Konkoly-Thege út 

29-33, Hungary National Physical Laboratory, Dr. K.S. 

Krishnan Road, New Delhi, 110070 Delhi, India, 

Resume: The property improvements of nanocrystalline 

materials have been attributed to the novel characteristics 

of grain boundaries coupled with drastic refinements in 

grain size. The added advantage of nanocomposites is that 

their properties can be tailored by varying their 

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composition and grain microstructure to suit a particular 

application making their applications more wide and 

versatile with improved performance. Al-Al2O3 

(aluminium-alumina) are important metal-ceramic 

composites possessing high wear resistance, low CTE and 

improved mechanical properties over a wide range of 

temperatures. In view of the background mentioned, this 

project proposes to synthesize bulk nanocomposites of Al- 

Al2O3 (with varying weight fraction of Al2O3) in two stages 

(i) synthesize Al-Al2O3 nanocrystalline composite powders 

using high energy ball milling followed by (ii) consolidation 

of these nanopowders using rapid sintering at high 

pressures. An expected outcome of this research work is 

the development of “rapid sintering at nearly-isostatic high 

pressures” as a consolidation technique of nanopowders, 

which is economical, fast and yields nanocomposites with 

near-theoretical density with minimal grain growth leading 

to improved properties. 

17:30 Effect of laser irradiation on properties and gas sensor 

performance of aluminum doped ZnO thin films 

Authors : Yue Hou, Ahalapitiya H. Jayatissa 

Affiliations : Mechanical, Industrial and Manufacturing 

Engineering Department The University of Toledo, OH 

43607, USA 

Resume: Aluminum doped ZnO thin films were 

synthesized on alkali free glass substrate using sol-gel 

spin-coating technique. The structure characterization, 

electrical property, surface morphology, optical properties 

and hydrogen gas sensor performance of aluminum doped 

ZnO thin films under different laser energy were 

investigated. XRD pattern showed that all the thin films 

had a (002) preferred orientation. It was also observed 

that low laser energy slightly increased the grain size and 

produced higher crystallinity, however, high laser energy 

slightly decreased the grain size and densified the thin 

films. The electrical property was tested in vacuum in the 

temperature range of 40 oC to 180 oC. The result showed 

that the conductivity of the thin film was enhanced by laser 

irradiation treatment. The conductivity decreased with low 

laser energy and increased with high laser energy. The 

SEM images exhibited a more porous surface with low laser 

energy irradiated film and denser surface with high laser 

energy irradiated film, which is a good agreement with the 

XRD results. The optical transmittance of all the thin films 

was measured. It indicated that the transmittance of laserirradiated 

films was improved in the visible region. The gas 

sensor performance of laser-irradiated films exposed to 

various hydrogen concentrations were measured at 150 oC 

in the dry air. All aluminum doped ZnO thin films were 

sensitive to hydrogen gas. As-deposit ZnO film showed a 

fast resistance change in response and a slow resistance 

change in recovery when expose to hydrogen gas. The gas 

sensor performance of laser-irradiated thin films was 

compared with as-deposit thin film. It was observed that 

the resistance change in recovery was significantly 

improved under laser irradiation. However, the sensitivity 

decreased under high laser energy irradiation. The 50 

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mj/cm2 laser-irradiated thin film showed highest sensitivity 

and shortest response and recovery time. 

17:30 Ammonia Gas Sensing Behavior of Lithium Doped Nickel 

Oxide Thin Films 

Authors : A. M. Soleimanpour, Ahalapitiya. H. Jayatissa 

Affiliations : Department of Mechanical Industrial and 

Manufacturing Engineering, University of Toledo, Toledo, 

Ohio, USA 

Resume: In industrial applications, hydroxylation of urea 

results in the formation of ammonia (NH3) gas. This gas is 

caustic and hazardous to human body above a threshold 

limit value (TLV) of 25 ppm. Therefore fabricating and 

development of a sensor to detect NH3 gas in a ppm level 

is important for industrial applications. NiO is an interesting 

p-type semiconductor material which has been used as gas 

sensor applications. The stoichiometric NiO is an insulator, 

but its resistivity can be decreased with increasing the hole 

concentration by increasing the numbers of nickel 

vacancies or monovalent dopant atoms like Lithium (Li) in 

the NiO crystalline. In this study, Li dopant was used to 

improve the structural, electrical and gas sensing behavior 

of the NiO thin films. Li doped nickel oxide thin films were 

fabricated with a sol-gel technique on a alkali free glass 

substrate. The structural properties and surface 

morphology of samples were studied with X-ray diffraction 

and scanning electron microscopy. It was found that the 

NiO samples were nanocrystalline and the grain size 

slightly increased with increasing the Li concentration. The 

minimum electrical resistivity was observed for the sample 

with 3%at of Li. The activation energy of samples was in 

the range of 0.39-0.42 eV. The NH3 gas sensing property 

of samples was collected at 140 oC and sample with 2%at 

showed highest response of 39 percent to 50 ppm of NH3 

gas. The analysis confirmed that Li ions occupy the 

substitutional sites in the film which enhanced p-type 

conductivity and as a result the gas sensing characteristic 

of NiO film improved using Li doping concentration. 

Keywords: Nickel oxide, Lithium doped, Gas sensor, 

Ammonia, Sol-gel. 

17:30 Luminescent properties of ZnO nanoceramics sintered with 

a flux 

Authors : V.I. Kushnirenko 1, I.V. Markevich 1, T.V. 

Zashivailo 2 

Affiliations : 1 V. Lashkarev Institute of Semiconductor 

Physics, NASU, Pr. Nauky 45, Kiev, 03028, Ukraine 2 

National Technical University of Ukraine "КРI", Pr. Pobedy 

37, Kiev, 03056, Ukraine 

Resume: Nanoceramics are attractive materials for device 

application due to simplicity of fabrication. It is known that 

adding of a flux to the starting materials can both lower 

sintering temperature TS and improve parameters of 

nanoceramics. In this work, ceramics of ZnO nanopowder 

with and without a flux were prepared and their 

photoluminescence (PL) characteristics were investigated. 

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The samples were sintered in air for 2h at TS = 800- 

1200°C. It was found that adding of the flux resulted in TS 

lowering, firm and dense nanoceramics being formed even 

without pressing of the starting mixture. PL and PL 

excitation (PLE) spectra of obtained samples were 

measured at 300 and 77K. In PL spectra, bright exciton 

luminescence as well as relatively weak green (500 nm) 

and orange (620 nm) bands were observed. The most 

intensive exciton luminescence took place in the samples 

sintered with the flux at TS = 800-900°C. In PLE spectra of 

green and orange bands, a number of peaks were present 

in 367-450 nm wavelength range. 

17:30 TiO2-SnO2 nanomaterials for gas sensing and 

photocatalysis. 

Authors : 1A.Kusior, 1J.Klich-Kafel, 1A.Trenczek-Zajac, 

1M.Radecka and 2K.Zakrzewska 

Affiliations : 1AGH University of Science and Technology, 

Faculty of Materials Science and Ceramics, al. A. 

Mickiewicza 30, 30-059 Krakow, Poland 2AGH University of 

Science and Technology, Faculty of Electrical Engineering, 

Automatics, Computer Science and Electronics, al. A. 

Mickiewicza 30, 30-059 Krakow, Poland 

Resume: Nanomaterials of TiO2-SnO2 system, including 

solid solution and composites, have been studied for 

applications in the field of gas sensing and photocatalysis. 

Nanopowders of TiO2 – SnO2 over a full compositional 

range extending from TiO2 to 100 were obtained by sol – 

gel method from TTIP and SnCl2∙2H2O precursors of Ti and 

Sn, respectively. The samples are characterized by 

nitrogen adsorption method, BET, X-ray diffraction, XRD, 

and Transmission Electron Microscopy, TEM. Electrical and 

optical properties of the prepared materials are 

determined. TEM images indicate that the particles 

obtained in the sol-gel process are mainly sphericalshaped. 

The specific surface area SSA of TiO2 is 95 m2/g 

while that of SnO2 amounts to 129 m2/g. In the case of 

Sn1-xTi1-xO2 with x=0.2 and 0.5 the highest SSA of 150 

m2/g is achieved. The phase structure of nanopowders 

depends on their chemical composition. The samples of 

Sn1-xTi1-xO2 with x up to 0.5 crystalize in the rutile 

structure. TiO2 contains the anatase phase while for TiO2rich 

specimen formation of a mixture of anatase, brookite 

and solid-solution phases is proposed. The crystallite size 

derived from X-ray diffraction is found to be over the range 

of 4-10 nm. Optical and electrical measurements reveal the 

influence of composition of the nanomaterials on the 

semiconducting properties of TiO2-SnO2 system. 

Acknowledgement The project was financed from the 

National Science Center based on the decision number 

DEC-2011/01/D/ST5/05859. 

17:30 PREPARATION AND DIELECTRIC CHARACTERIZATION OF 

CCTO FILMS BY A MODIFYED PECHINI METHOD 

Authors : J.L.P. Santos1, L. C. Costa1, F. Amaral1,2, M.A. 

Valente1*, M.P.F. Graça1 

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Affiliations : 1Department of Physics and I3N, University of 

Aveiro, Campus Santiago, 3810-193 Aveiro, Portugal; 

2College of Technology and Management of Oliveira do 

Hospital, 3400-124 Oliveira do Hospital, Portugal 

Resume: The uncommon dielectric properties of 

CaCu3Ti4O12 (CCTO) are of considerable scientific and 

technical interest. The material has a distorted, complex 

cubic perovskite (ABO3)-like structure and exhibits a very 

large dielectric constant ( ´>104) nearly temperature 

independent in the range between 200 and 300 K. Such 

large ´ values make CCTO an attractive material for ultrahigh 

energy density capacitors. In this work, films of CCTO 

were prepared by spin-coating. The CCTO solution was 

prepared by a modified Pechini method, using 

ethylenediaminetetraacetic acid (EDTA) as the complexing 

agent. The obtained blue transparent gel was stable for 

more than 2 month, showing a viscosity of 0.14 Pa.s, at 

25ºC. The thin films were deposited on Si(111) substrates, 

doped with boron,. The layer-by-layer technique was 

applied and the obtained films properties were analysed in 

function of the number of layers. The structure of the films 

was studied using XRD and Raman spectroscopy. The 

morphology was analysed by SEM. The dc electrical 

conductivity and the broadband dielectric spectroscopy 

were measured as function of the temperature (100 K < T 

< 360 K). The dielectric constant, at room temperature, 

show values in the order of 105. The dielectric loss, at 

room temperature and at 1 kHz, is always lower than 0.25. 

17:30 Fabrication Technique of Porous Tungsten Oxide Nanofibers 

for Gas Sensors 

Authors : István Endre Lukács, Áron Kázmér Nagy, Csaba 

Balázsi 

Affiliations : Hungarian Academy of Sciences Research 

Centre for Natural Sciences 

Resume: Detection of nitrogen oxides is an important 

environmental and health issue. Hexagonal tungsten oxide 

shows excellent gas sensing properties in detection of NOx. 

For advanced performance the active structure of sensory 

should have large specific surface area and low volume. In 

this paper we report on a technique for fabrication of 

porous tungsten oxide nanofibers with a diameter under 

200 nm and a macroscopic length. The decisive element of 

the production is electrospinning. A technique has been 

developed to evenly disperse tungsten oxide nanoparticles 

in polymer solution for electrospinning. The ideal mass 

ratio of solvents, polymer and the maximum amount of 

tungsten oxides have been determined by a series of 

experiments. A solution of polymer (polyvinyl alcohol) and 

dopant is put in a syringe, which is controlled by a stepper 

motor. The solution leaves the needle, and flies to the 

target (metal plate) driven by the high voltage switched 

between the target and the needle. A microchip specially 

developed for gas sensing is fixed on the target. At tis 

state the hexagonal tungsten oxide nanoparticles are 

coated with polymer, we developed methods for eliminate 

the polymer whilst the nanofibers remain and the tungsten 

oxide nanoparticles form porous nanofibers on the surface 

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of gas sensor chip. The resulted samples were analyzed by 

XRD and by FTIR, their morphology was studied by SEM. 

The distribution of the tungsten content in the fibers was 

mapped by EDS. 

17:30 MAGNETIC PROPERTIES OF LIFe5O8 POWDERS PREPARED 

BY SOLID STATE REACTION 

Authors : S. Soreto Teixeira, M.P.F. Graça, L. C. Costa, 

M.A. Valente 

Affiliations : University of Aveiro 

Resume: Lithium ferrite (LiFe5O8) is one of the most 

known cubic ferrites which belong to the group of soft 

ferrite materials with high Curie temperature, presenting a 

square hysteresis loop and high magnetization. It has 

attracted special attention due to its numerous 

technological applications in microwave devices, magnetic 

recording, transformer cores, rod antennas and possible 

applications in biomedics. It is also a promising candidate 

for cathode materials in rechargeable lithium batteries as 

well as low cost substitutes to garnet materials in 

microwave frequency applications. In the present work, 

amorphous Li2O-Fe2O3 powders were mixture via wet ball 

milling method. The as-prepared powders were heattreated 

at temperatures between 200 and 1400 ºC and 

their structure analyzed by X-ray diffraction and FTIR 

spectroscopy. The morphology was analyzed by scanning 

electron microscopy. The magnetic properties were 

measured using a vibrating sample magnetometer (VSM). 

The dc magnetic susceptibility was recorder under zero 

field cooled (ZFC) and field cooled (FC) sequences under 

0.1 T, between 5 and 300 K. Typical hysteresis curves were 

obtained at several temperatures. The saturation 

magnetization increases with the increase of the heattreatment 

temperature until 1200 ºC. This sample 

presents, at 5 K, a magnetic moment of 73 emu/g and, at 

300 K, of 66 emu/g. The decrease of the magnetic moment 

for the sample heat-treated at 1400 ºC is related with the 

decrease of LiFe5O8 content. 

17:30 Internal composite fibers as SOFC cathode materials 

Authors : Jinyi Choi a, Byeongseok Kim b and Dongwook 

Shin a,b* 

Affiliations : a Department of Fuel Cells and Hydrogen 

Technology, Hanyang University b Division of Materials 

Science & Engineering, Hanyang University, 

Resume: The fibrous cathode offers a continuous path for 

charge transport and an increased number of triple-phase 

boundary sites. SSC and SDC composite fibers were 

successfully fabricated by electrospinning method using 

SDC commercial nanopowders and a SSC precursor 

solution that contained polyvinyl alcohol (PVA) and 

aqueous metal nitrate. The as-spun and calcined composite 

fibers were characterized by TG-DTA, X-ray diffraction, 

SEM and TEM, respectively. After calcination of the 

composite fibers in microwave furnace at 800 oC, the fibers 

of 300 ± 50 nm in diameter having well-developed SSC 

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cubic-perovskite structure and fluorite SDC were 

successfully obtained. A single cell with the internal 

composite fibers shows improved performances at 

intermediate operating temperatures (550–700 oC) as 

compared with the conventional powder composites. The 

polarization resistance at 650 oC of fibrous composite 

cathodes was about 51% lower than powder composite 

cathodes and maximum power densities of fiber and 

powder cathodes were 1,260 mW/cm2 and 866 mW/cm2 

at 700 oC, using H2 at a flow rate of 200 sccm as fuel and 

air at a flow rate of 300 sccm as oxidant. 

[Acknowledgements] This work was supported by Solid 

oxide fuel cell of New & Renewable Energy R&D program 

(20093021030010) under the Korea Ministry of Knowledge 

Economy (MKE). 

17:30 Bias dependent NO2 sensitivity of SnO2 thin films at room 

temperature 

Authors : M. Kodu, T. Avarmaa, A. Floren, R. Jaaniso 

Affiliations : Institute of Physics, University of Tartu, Riia 

142, 51 014 Tartu, Estonia 

Resume: Lowering the power consumption of 

semiconductor gas sensors is an essential task for 

developing advanced e-noses and wireless applications. 

One possibility is the reduction of working temperature, as 

the power is mainly consumed for heating the sensor 

element. At the same time, the materials, which gas 

sensitivity can be controlled by external fields are of 

interest, as allowing to improve the selectivity of sensors or 

sensor arrays. The electrical and gas sensing properties of 

SnO2 thin films, made by pulsed laser deposition, were 

studied. Large and reversible response to NO2 gas was 

observed at room temperature for amorphous but granular 

films. It was demonstrated that the nonlinear electrical 

characteristics and bias dependent gas sensitivity were 

inherently the properties of thin films and the contacts 

were ohmic. The underlying transduction mechanism of gas 

sensitivity, as well as its relation to the structure of thin 

films was discussed. 

17:30 Microstructural characteristics of RE2Zr2O7 type powders 

obtained by spray drying method 

Authors : Grzegorz Moskal 

Affiliations : Silesian University of Technology, Department 

of Materilas Science, 40-019 Katowice, ul. Krasińskiego 8b 

Resume: The paper presents the study results concerning 

microstructural characteristics of the spry dried powders on 

the basis of rare earth zirconates with RE2Zr2O7 type 

pyrochlore structure. Powders on the basis of Gd, La, Sm 

and Nd zirconates were used as the study material. The 

assessment of surface morphology and inner structure of 

powders (SEM) was made. Chemical composition (EDX, 

OES-ICP) of the powders was determined, with special 

attention being paid to uniformity in arrangement of alloy 

elements and content of carbon, sulphur, oxygen and 

nitrogen. Phase composition by using XRD and EBSD 

methods was also analysed. The study performed showed 

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that the analysed powders are predominantly characterized 

by a spherical shape. Powder surface shows low 

smoothness and high porosity both surface and inner 

porosity. Single particles of ?hollow spheres? type are 

made up of only outer hollow shell. The particles were 

predominantly filled with the material in a form of ultrafine 

dispersion and nanozised polyhedrons with uniform 

chemical composition. The analysis of phase composition 

showed predominant share of RE2Zr2O7 type cubic phases 

with low quantities of rare earth oxides and ZrO2. 

17:30 Structural and magnetic studies on Fe-doped NiO 

nanoparticles synthesized by combustion method 

Authors : Samar Layek and H. C. Verma 

Affiliations : Department of Physics, Indian Institute of 

Technology, Kanpur, 208016, India. 

Resume: Transition metal oxides (TMOs) are one of the 

mostly investigated materials not only because of their 

wide range of material and industrial applications in science 

and technology, but also interesting and diverse physical 

properties. Such applications in different fields and/or the 

physical properties can be tuned by decreasing the particle 

size down to nanoscale range. Among these TMOs, 

stoichiometric nickel oxide (NiO) is well known as a 

strongly correlated Mott-Hubbard insulator with optical gap 

of about 4 eV [1, 2]. It undergoes antiferromagnetic 

ordering below TN= 523 K which is well above room 

temperature [3, 4]. Ferromagnetic sheets of Ni2+ atoms 

which are parallel to the (111) plane with opposite spin 

direction in the neighboring sheets consists the magnetic 

structure of the NiO. As t2g orbitals are filled, no direct 

cation-cation exchange is possible in NiO. But there is 

possibility of Ni-O-Ni interactions through the oxygen 2s 

and 2p orbitals [5]. Anomalous large magmatic moment 

along with noticeable coercivity and loop shift have been 

found in 31nm or less sized NiO nanoparticles which are 

believed to be due to finite size effect [6, 7]. Though pure 

NiO in the bulk form is an insulator, it can be transformed 

into p-type semiconductor after the development of Ni2+ 

vacancies or by doping with other cations [8, 9]. Fe-doped 

NiO samples have been synthesized by many methods like 

solid state reaction method [10], sol-gel method [11, 12], 

co-precipitation method [13-15], hydrothermal method 

using ethylenediamine [16] etc. Room temperature 

ferromagnetism along with exchange bias has been found 

in some of these samples. Li and Fe co-doped NiO samples 

have also been prepared by sol-gel method [12] and PVA 

sol-gel route [17] in order to investigate the effect of 

further Li-doping on the magnetic properties of NiO. 

Enhancement of the magnetic properties has been founded 

in Li and Fe doped NiO thin films [18, 19]. The structural, 

magnetic and electrical properties of nonmagnetic Mndoped 

NiO particles have also been investigated [20, 

21].The structural and magnetic properties in doped NiO 

systems greatly depend on the morphology, particle size 

etc., which indirectly depend on the methods used to 

synthesize the samples. Combustion method is a very 

efficient method for preparing bulk samples and 

nanoparticles. It has been used quite successfully for 

synthesis of oxides, ferrites etc [22]. Combustion method 

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has not been used so far for preparation of Fe-doped NiO 

particles to the best of our knowledge. Fe-doped NiO 

nanoparticles of the series Ni1-xFexO (x= 0.00, 0.01, 0.02, 

and 0.04) nanoparticles had been prepared by a 

combustion method using metal nitrate solution in 

presence of glycine following the procedure reported in the 

literature [22]. Nickel and ferric nitrate were taken in 

appropriate stoichiometric ratio and mixed together in 

100ml double distilled water in a glass beaker for about 30 

minutes using a magnetic stirrer at 80 0C. Glycine was 

added to the mixed nitrate solution and stirred at 80 0C for 

about 30 minutes. Finally, the solution was heated at 150 

0C to for about 30 minutes and combusted into black 

colored precursor. The precursors were grounded into 

powders using mortar and pastel. Small part of the 

powders were annealed using quartz crucibles in air at 600 

0C for 4 hours each inside a programmable box furnace 

with heating rate 100 0C per hour and then slowly cooled 

down to room temperature. Small amount of each 

annealed powder sample was characterized by XRD on a 

Seifert Iso-Debyeflex 1001 Diffractometer using Cu- Kα 

radiation (wavelength =1.54 Å) in order to check the phase 

purity and calculate average crystallite size. All the XRD 

peaks can be indexed in the fcc structure with space group 

Fm-3m. The values of the ionic radius for Ni2+, Fe2+ and 

Fe3+ are 0.69 Å, 0.74 Å and 0.64 Å respectively. As the 

deference in the ionic radius between the Ni2+ and Fe2+ 

or Fe3+ in not so much, Fe-ions can replace the Ni2+ ions 

without changing the crystal structure. No evidence of 

impurity phases (like Fe in metallic form, iron oxides like 

α–Fe2O3, γ–Fe2O3, and Fe3O4 and ferrite like NiFe2O4) 

has been found even upto 4% of Fe-doping. The average 

crystallite sizes calculated from the XRD peak broadening 

after correction from the instrumental broadening are in 

between 58 to 49 nm and decreases with increasing Fedoping. 

Morphology and size of the particles are 

investigated by transmission electron microscope (TEM). 

The particles size calculated from the TEM studies are 

nearly same as obtained from the XRD measurements. 

Room temperature magnetization as a function of applied 

magnetic field was taken using a vibrating sample 

magnetometer (VSM, ADE Technologies, USA) upto applied 

field of 1.75 T. Pure NiO nanoparticles shows weak 

ferromagnetic behavior with coercive field of about 109 Oe. 

The magnetization increases with increasing magnetic field 

but does not saturate upto highest applied magnetic field. 

Substitution of Fe-atoms in place of Ni2+ in NiO matrix 

improves the magnetic properties significantly in these 

compounds. The net value of the magnetization increases 

with increasing Fe-doping concentration whereas the 

coercive field value is highest for 2% Fe-doped 

nanoparticles. The increase in the magnetization may be 

due to increase in the Fe-Fe exchange interaction with 

increasing iron concentration in NiO matrix. Reference: [1] 

R. J. Powell and W. E. Spicer, Phys. Rev. B 2, 2182 (1970). 

[2] G. A. Sawatzky and J. W. Allen, Phys. Rev. Lett. 53, 

2339–2342 (1984). [3] V. G. Bhide and G. K. Shenoy Phys. 

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Phys. Rev. B 3, 1039 (1971). [5] M. Corti, S. Marini, A. 

Rigamonti, F. Tedoldi, D. Capsoni, and V. Massarotti, Phys.

Rev. B 56, 11056 (1997) [6] R. H. Kodama, S. A. 

Makhlouf, and A. E. Berkowitz, Phys. Rev. Lett. 79, 1393 

(1997). [7] S. A. Makhlouf, F. T. Parker, F. E. Spada, and 

A. E. Berkowitz, J. Appl. Phys. 81, 5561 (1997). [8] J. Wu, 

C.-W. Nan, Y. Lin, and Y. Deng, Phys. Rev. Lett. 89, 

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Phys. D: Appl. Phys. 42 (2009) 145001 [11] Jinda 

Khemprasitn, Suriyasit Kaen-ngam,Bualan Khumpaitool, 

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,Teerapon Yamwong,Santi Maensiri, 

MaterialsChemistryandPhysics 123 (2010) 56–61. [13] J. 

H. He, S. L. Yuan, Y. S. Yin, Z. M. Tian, P. Li, Y. Q. Wang, 

K. L. Liu, and C. H. Wang, J. Appl. Phys. 103, 023906 2008 

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Condens. Matter 19 (2007) 436203 [15] J. H. He, S .L. 

Yuan, Z. M. Tian, Y. S. Yin, P. Li, Y. Q. Wang, K. L. Liu, S. 

J. Yuan, X. L. Wang, L. Liu, J. of Mag. and Mag. Mat. 320 

(2008) 3293–3296 [16]S. Manna, A. K. Deb, J. Jagannath, 

and S. K. De, J. Phys. Chem. C 2008, 112, 10659–10662 

[17]S. Manna, S. K. De, Solid State Communications149 

(2009) 297. [18] Y. –H. Lin, R. Zhao, C. –W. Nan, M. Ying, 

M. Kobayashi, Y. Ooki, and A. Fujimori, Appl. Phys. Lett. 

89, 202501 (2006). [19] W. Yan, W. Weng, G. Zhang, Z. 

Sun, Q. Liu, Z. Pan, Y. Guo, P. Xu, S. Wei,0Y. Zhang, and 

S. Yan, Appl. Phys. Lett. 92, 052508 2008. [20] P. Mallick, 

C. Rath, A. Rath, A. Banerjee and N. C. Mishra, Solid State 

Communication, 150 (2010) 1342-1345. [21] S. P. Raja 

and C. Venkateswaran, J. Nanoscience and Nanotech., 11 

(2011) 2747-2751. [22] C. –C. Hwang, T. –Y. Wu, J. Wan, 

J. –S. Tsai, Materials Science and Engineering B111 (2004) 

49–56. 

17:30 Synthesis and characterization of porous titanium- 

hydroxyapatite nanocomposites 

Authors : Katarzyna Niespodziana, Mieczysław Jurczyk 

Affiliations : Poznan University of Technology, Institute of 

Materials Science and Engineering, Poznan, Poland 


Resume: Titanium-20wt% hydroxyapatite nanocomposites 

were produced by the combination of mechanical alloying 

(MA) and powder metallurgical process with the addition of 

titanium hydride particles as the pore forming agent. The 

powder mixture of Ti, HA and spacer particles were milled, 

pressed and heat treated to burn out the spacer particles 

and to sinter into highly porous Ti-HA materials. The 

resulting microstructures were characterized using X-ray 

diffraction and scanning electron microscope with energy 

dispersive spectrometry. The properties of the porous 

nanocomposites were investigated by mechanical studies. 

The results show that the porous Ti-HA nanocomposites are 

promising scaffold biomaterials for bone tissue engineering 

because of their good mechanical properties and highly 

porous structure. 

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Session IX : - 

09:00 Design of amorphous and nanocomposite metal carbide films 

Authors : Ulf Jansson 

Affiliations : Department of Chemistry-Angstrom Laboratory 

Resume: Magnetron sputtering gives unique possibilities to 

design different types of functional carbide-based films. By 

tuning the growth parameters it is possible to obtain 

amorphous structures as well as nanocomposites with 

nanocrystalline carbide grains in an amorphous matrix. Such 

coatings may exhibit excellent mechanical, tribological and 

electric properties and have a use in a wide range of 

applications. The present paper will summarize some 

approaches to control the microstructure by a designed 

alloying of additional elements in, for example, the Ti-Me-C 

(Me = 3d transition metals) and Me-X-C systems (Me = Ti, 

Nb, Zr and X= B, Si, S). Such alloying can lead to 

metastable solid solutions into the carbide phase. During 

annealing, the metastable structures can decompose to 

more stable structures. A potential use of such a concept is 

self-adaptive coatings which spontaneously form a lowfriction 

graphitic or sulfide interfaces in a tribological 

contact. Another approach is to add glass-forming pelements 

to a binary metal carbide phase. By a careful 

tuning of the composition it is possible to form metal glass 

coatings or coatings with both an amorphous and a 

nanocrystalline component. Potential applications of these 

materials as corrosion- or wear- resistant coatings will be 

discussed. 

09:35 Friction and wear mechanisms in magnetron sputtered and 

PE CVD W-C based coatings 

Authors : Frantisek Lofaj, Milan Ferdinandy, Peter Hornak 

Affiliations : Institute of Materials Research of the Slovak 

Academy of Sciences 

Resume: Friction and wear mechanisms were investigated 

on magnetron sputtered and PE CVD nanocomposite W-C 

based coatings to elucidate the effects of deposition 

technology on their tribological performance. The work is 

focused is on the understanding of relationships among 

deposition conditions, chemical composition, structure and 

their properties, including hardness, coefficient of friction 

(COF) and wear resistence. PECVD W-C based coatings were 

prepared from the volatile tungsten carbonyl precursor. The 

deposition conditions including total pressure, current 

density and bias were optimized to obtain maximum 

hardness. In case of DC and RF magnetron sputtering from 

WC target, total pressure and energy were optimized from 

the same viewpoint. The topography of all coatings was 

investigated using SEM and AFM. Their properties were 

determined using nanoindentation and ball-on-disc testing, 

respectively.The differences in carbon state among the 

compositions were detected using Raman spectroscopy and 

correlated with the spectroscopic Raman data. The results 

indicate strong correlation among deposition conditions, 

phase composition, carbon bonding and resulting mechanical 

and tribological properties. Understoichiometric W-C 

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compositions with the lack of carbon phase exhibit high 

hardness and high coefficient of friction whereas an increase 

of free carbon content reduces both parameters regardless 

of the deposition technology. The lowest COF values of 

around 0.11 were obtained in the case of PE CVD W-C 

coatings, DC and RF sputtered coatings exhibited slightly 

higher COF values accompanied by higher hardness possibly 

due to the differences in the structure of the coatings. 

09:55 Phase Stability and Microstructure of Sol-Gel-Derived 

Nanoscale-Thick ZrO2/Si Films 

Authors : Soo Min Hwang, Seung Muk Lee, Jun Hyuk Choi, 

Geun Chul Park, Tae Woong Kim, Jinho Joo 


Engineering, Sungkyunkwan University 

Resume: Nanoscale-thick (~15 nm) ZrO2/Si films were 

fabricated by sol-gel method and the phase and 

microstructural evolution by thermal annealing were studied. 

The ZrO2 films were prepared by synthesis of the precursor 

sol (0.2 M) using a Zr-acetylacetonate (Zr-acac), spincoating 

of the solution on Si substrates and drying, followed 

by annealing at 300-950 o C in ambient air. Microstructure 

and surface morphology were observed by transmission 

electron microscopy (TEM) and atomic force microscopy 

(AFM). Phase identification was performed by using X-ray 

diffraction (XRD), Raman spectroscopy, and selected area 

electron diffraction (SAED). Thermal annealing resulted in 

the phase evolution from the amorphous to tetragonal (t-) 

phase which was retained without a conspicuous transition 

to monoclinic phase despite the high-temperature annealing 

at ~950 o C. The mechanism of the t-phase stability was 

suggested on the basis of the microstructural changes: the 

film thickness was reduced, whereas the in-plane grain size 

and surface/interface area were increased with increasing 

annealing temperature. 

Acknowlegment: This research was supported by Basic 

Science Research Program through the National Research 

Foundation of Korea (NRF) funded by the Ministry of 

Education, Science and Technology (2012-0002923). 

10:10 Superhard ZrC thin films grown by pulsed laser deposition 

Authors : D. Craciun1, G. Socol1, S. Niculaie1, G. 

Dorcioman1, E. McCumiskey2, M. Hanna2, C. R. Taylor2, G. 

Bourne3, E. Lambers4, and V. Craciun1, 4 

Affiliations : 1National Institute for Laser, Plasma, and 

Radiation Physics, Bucharest, Romania 2Mechanical and 

Aerospace Engineering, University of Florida, Gainesville, 

USA 3Metallurgical and Materials Engineering, Colorado 

School of Mines, Golden, USA 4Major Analytical 

Instrumentation Center, University of Florida, Gainesville, 

USA 

Resume: ZrC is well known for its excellent mechanical, 

electronic, optical, and thermochemical properties, being 

used for hard and protective coatings, field emission tips, 

outer space thermal radiators, nuclear fuel coatings, or 

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diffusion barriers in microelectronics. ZrC films thinner than 

500 nm were grown on (100) Si substrates from room 

temperature up to 500 oC by pulsed laser deposition using a 

KrF excimer ( =248 nm, pulse duration τ = 25 ns, 6-10 

J/cm2 fluence, 40 Hz repetition rate). Simulations of the Xray 

reflectivity curves acquired from the deposited ZrC films 

showed that the mass densities were around bulk values and 

the surface morphology was very smooth, as also confirmed 

by atomic force microscopy investigations. X-ray diffraction 

investigations showed that the films were nanocrystalline, 

with a slight (111) texture. Williamson-Hall and sin2(psi) 

plots indicated that the films are both microstressed as well 

as under a uniform high compressive stress. The oxygen 

content, measured by Auger electron spectroscopy was 

below 2 at. %. Nanoindentation measurements found 

hardness values between 35 and 47 GPa, significantly higher 

than the best values reported so far for this material. Such 

high hardness values could be explained by the use of a high 

laser fluence for ablation, which generates energetic species 

that bombarded the substrate and film during growth, 

resulting in the deposition of very dense, adherent, 

nanostructured and micro-stressed films. 


Session X : - 

11:00 The materials and processing of polymer-derived Si/C/N 

ceramics: From MEMS to medical components 

Authors : (a) Jakob Kuebler , Vadym Bakumov, Federico 

Dalcanale, Gurdial Blugan (b) Vahid Fakhfouri, Jonas 

Grossenbacher, Maurizio Gullo, Juergen Brugger 

Affiliations : (a) Empa, Swiss Federal Laboratories for 

Materials Science and Technology, Laboratory for High 

Performance Ceramics, Ueberlandstrasse 129, CH-8600 

Duebendorf, Switzerland (b) EPFL, Microsystems Laboratory, 

CH-1015 Lausanne, Switzerland 

Resume: Polymer-derived ceramics (PDCs) are gaining 

increasing attention from research and industry. The soft 

nature of the starting polymeric materials provides a unique 

opportunity for fabrication, next to e.g. coatings and fibers, 

of highly precise and structured shapes, which are converted 

into ceramic structures upon curing and subsequent pyrolytic 

treatment. As the ceramics can be functionalized, e.g. to be 

electrical conductive or non-conductive, they have not only a 

high potential for producing small components to be used in 

small devices (MEMS) but also for sensors and actuators, 

e.g. in medical devices. In this presentation the materials 

and processing development for the production of aesthetic, 

wear resistant and conductive MEMS for mechanical, sensor 

and medical applications is highlighted. The materials 

properties and micro-structure of these Si/C/N-MEMS 

ceramics are presented. 

11:20 Effect of Y doping on AlTiTaN hard nanocomposite coatings 

Authors : Vishal Khetan(1), Baptiste Girault(1), Nathalie 

Valle(1), David Duday(1), Patrick Choquet(1), Claude 

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Michotte(2), Marianne Penoy(2), Christian Mitterer(3), 

Marie-Paule Delplancke(4) 

Affiliations : (1) CRP - Gabriel Lippmann, Belvaux, 

Luxembourg; (2) CERATIZIT, Mamer, Luxembourg; (3) 

Montanuniversität Leoben, Leoben, Austria; (4) Université 

Libre de Bruxelles, Brussel, Belgium 

Resume: TiAlN based nanocomposite coatings have gained 

high importance in the field of wear and oxidation resistant 

hard coatings. Nevertheless, their use regarding high 

temperature (>850ºC) applications such as dry high speed 

machining remains a challenging issue. Additional alloying 

elements such as Si or Ta have shown a beneficial impact on 

those properties although oxidation resistance at high 

temperature is still problematic. This work proposes to 

investigate effects of Y addition on AlTiTaN nanocomposite 

coating in order to achieve better wear and oxidation 

properties at high temperature. Y doped AlTiTaN samples 

were deposited from Al46Ti42Ta12 and pure yttrium targets 

using DC magnetron sputtering in a reactive Ar+N2 

discharge. Different doping concentrations of Y have been 

used ranging from 0 to 3 at.%. Bias voltage effects (from 0V 

to -200V) on coating properties have also been investigated. 

X-ray diffraction studies have shown that addition of Y leads 

to a progressive preferential crystallographic orientation 

switch from {111} to {200} and a decrease of grain size. 

TEM analysis on 2.4 at.% Y-doped sample revealed a mixed 

columnar-superlattice microstructure. The Y doped samples 

have shown nanohardness values as high as 35 GPa. The 

effect of Y doping on oxidation behaviour and tribological 

properties was also studied. The study provides us a direct 

correlation between the chemical composition, 

microstructure, tribological and mechanical properties of the 

samples deposited. 

11:35 Evaluation of non-hydrogenated and hydrogenated carbonrich 

silicon-carbon alloy thin films as protective coating and 

functional material 

Authors : A.V. Vasin*, A.V. Rusavsky*, A.N. Nazarov*, V.S. 

Lysenko*, V.P. Kladko*, O.Yo. Gudymenko*, C. Nouveau** 

Affiliations : *Lashkaryov Institute of Semiconductor Physics, 

Kiev, 03028 Ukraine; **LaBoMaP, CER Arts et Métiers 

ParisTech, Rue Porte de Paris, F-71250, Cluny, France 

Resume: Amorphous silicon-carbon alloy films were 

deposited on silicon substrates at 200 0C by RF-magnetron 

sputtering of SiC target in argon or argon/methane gas 

mixture. Hydrogenated and non-hydrogenated layers were 

examined in terms of density, mechanical stresses as well as 

oxidation and wear resistance. Density of the films was 

varied in range of 1.6-3.4 g/cm3 by varying magnetron 

discharge power and working gas composition. FTIR and 

Raman spectroscopy identify the structure of as-deposited 

films as amorphous SiC matrix with incorporated carbon 

nano-clusters. As-deposited films exhibited compressive 

stresses that were partially relaxed after annealing in pure 

argon. Annealing in oxygen flow resulted in drastic evolution 

of compressive stresses into tensile. It was found that 

oxidation resistance directly correlates with density of the 

films. Significant oxidation was observed in low density films 

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after annealing in oxygen at temperature as low as 550 0C 

while samples with density above 3 g/cm2 exhibited no 

oxidation up to 1000 0C. Mechanism of stresses evolution 

and possibility of stresses engineering are discussed. Ballon-plate 

tribology wear testes using stainless steel and 

alumina balls have been performed. Polycrystalline SiC layer 

deposited by CVD method at 1300 0C was used as a 

standard for comparative evaluation of wear rates. 

Surprisingly dense a-SiC layers exhibited superior wear 

resistance in comparison to CVD SiC when using ceramic 

ball. 

11:55 Stainless steel modified by surface functionalization using 

sol-gel method for bone implants 

Authors : Anna Donesz-Sikorska, Justyna Krzak-Roś, Jakub 

Grzesiak, Krzysztof Marycz 

Affiliations : Wroclaw University of Technology; Wroclaw 

University of Technology; Wroclaw University of Life 

Sciences; Wroclaw University of Life Sciences 

Resume: Introduction Steel Cr-Ni-Mo ASI 316L is a basic 

material for bone implants, characterize good mechanical 

properties, high resistance to corrosion and with composition 

and structure making possible shaping in the technological 

processes. Unfortunately, steel 316L like all metallic 

biomaterials contain a toxic chemical elements. For these 

reason we decided to synthesize functionalized silica 

coatings using sol-gel method to forming biocompatibility 

diffusion barrier used on metallic implants. Materials and 

Methods Thin silica films were synthesis using the sol- gel 

method that is based on the hydrolysis of alkoxide 

precursors at room temperature. Silica coatings was 

synthesized from: silica precursor-tetraethoxyorthosilicate 

(TEOS), solvent- ethanol (EtOH) and catalyst- hydrochloric 

acid (HCl). For functionalization we used silica precursors 

containing: amine, thiol, fluorine and chlorine grups. 

Obtained mixtures were dip-coated onto the cleaned metallic 

substrates with controlled process parameters. The 

deposited films were dried at room temperature on air and 

then annealed at 250C for 12hrs. Obtained materials were 

examined: structurally (SEM-EDX), mechanically (scratch 

test) and biologically (tests in vitro). Obtained coatings are: 

nano size, transparent, homogeneous and uniformly cover 

the substrate- steal 316L. SEM-EDX mapping image of silica 

functionalized layers shows the uniform distribution obtained 

coatings on steal. Results of scratch tests showed good 

adhesion of most sol-gel layers to the substrate. 

Observations of the macro-edge cuts showed no cracks or 

splinters. It has been found only a uniform wipes of coating 

in analyzed areas. Tests in vitro showed a stimulating effect 

of obtained coatings onto stem cells isolated from adipose 

tissue. 

12:15 Surface functionalisation of hydroxyapatite for increased 

protein loading 

Authors : Vinayaraj Ozhukil Kollath, Steven Mullens, Jan 

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12:30 Lunch 

Luyten, Karl Traina, Rudi Cloots 

Affiliations : Vinayaraj Ozhukil Kollath; Steven Mullens - 

Materials Technology, Flemish Institute for Technological 

Research (VITO), 2400 Mol, Belgium; Jan Luyten - MTM, 

KULeuven, 3001 Heverlee, Belgium; Vinayaraj Ozhukil 

Kollath, Karl Traina, Rudi Cloots - GREENMAT, Dept of 

Chemistry, University of LIège, 4000 Liège, Belgium 

Resume: Introduction: Protein and biomolecule delivery via 

oral route is a safer way of administration and has been a 

topic of interest in the pharmaceutical industry[1]. Nano and 

microparticulate calcium phosphate can be used as a carrier 

for protein delivery due to its biocompatibility[2-4]. However 

bioavailability of such inorganic carriers is less compared to 

organic or viral carriers[5]. In this study we compared the 

surface functionalisation of hydroxyapatite (HA) powder 

using different amino acid entities (AA). This approach aims 

at increasing the protein loading by improving the 

electrostatic interaction between the protein and the HA, 

which require increasing the positive surface charge of HA in 

physiological pH. Both powder characteristics and protein 

loading are characterised qualitatively and quantitatively. 

Methods: The HA (Merck) powder was characterised 

extensively. HA powder was magnetically stirred in AA 

solutions and collected by centrifugation. This powder was 

washed and then mixed with bovine serum albumin (BSA) 

suspensions. BSA adsorbed HA was centrifuged and 

supernatant was quantified. Results and Discussion: The 

zeta potential measurements (figure below) show that two of 

the AA entities shifted the isoelectric point (IEP) of the 

powder to higher pH, enhancing positive charge on the 

surface. Further XPS results proved the presence of nitrogen 

on the surface of these modified powders. Thus the presence 

of amine group on the surface could be the reason for the 

shift in IEP. The adsorption isotherms of functionalised 

powder was in accordance with the zeta potential 

measurments. Functionalisations which showed a shift in IEP 

to higher pH, also show a significant increase in protein 

adsorption. The combination of the zeta potential profiles 

and the BSA adsorption isotherms points to a protein-HA 

interaction mainly governed by electrostatic forces. 

Adsorbing even relatively small quantities of amino acids will 

change the chemical composition of the HA surface 

substantially. REFERENCES 1. J.L. Cleland, A. Daugherty, R. 

Mrsny. Curr. Opin. Biotechnol. 12 (2001) 212. 2. B. Mueller, 

M. Zacharias, K. Rezwan. Adv Eng Mater. 12 (2010) 53. 3. 

S. Dasgupta, A. Bandyopadhyay, S. Bose. Acta Biomater. 5 

(2009) 3112. 4. N. Brandes, P.B. Welzel, C. Werner, L.W. 

Kroh. J Colloid Interface Sci. 299 (2006) 56. 5. Z.P. Xu, Q.H. 

Zeng, G.Q. Lu, A.B. Yu. Chem. Eng. Sci. 61 (2006) 1027. 

Session XI : - 

14:00 Densification and grain growth of fine-grained alumina F-

ceramics doped by magnesia, yttria and zirconia 

Authors : Karel Maca1, Vaclav Pouchly1, K. Ghillányová2, 

P.Švančárek3, D. Galusek3 

Affiliations : 1 Brno University of Technology, Brno, Czech 

Republic; 2 Institute of Inorganic Chemistry, Slovak 

Academy of Sciences, Bratislava, Slovakia; 3 Joint Glass 

Centre of the IIC SAS, TnU AD, FChFT STU, and RONA j.s.c., 

Trencin, Slovakia 

Resume: The influence of various dopants (500 ppm of 

MgO, Y2O3 or ZrO2) on sintering kinetics of fine-grained 

alumina ceramics was evaluated by means of hightemperature 

dilatometry. The apparent activation energy of 

sintering was estimated with the help of Master Sintering 

Curve concept. The lowest value of activation energy was 

determined for the undoped alumina (690-700 kJ/mol). The 

addition of MgO increased this value only slightly (710-720 

kJ/mol). The addition of Y2O3 and ZrO2 inhibited the 

densification, which was reflected by higher values of 

sintering activation energies (810 kJ/mol for zirconia, resp. 

860 kJ/mol for yttria doping). All three additives suppressed 

the grain growth when compared to pure alumina. The effect 

of doping on the efficiency of two-step sintering of alumina 

ceramics in comparison to conventional heating of aluminas 

with identical compositions was evaluated. 

14:20 Medical fine-grained ceramics based on ultra dispersed 

Ce0.09Zr0.91O2 and Al2O3-MgO powders 

Authors : E.A. Trusova A.A. Khrushcheva K.V. Vokhmintcev 

Affiliations : Institution of Russian Academy of Sciences, A.A. 

Baikov Institute of Metallurgy and Material Science of RAS 

Resume: The presentation is related to the development of 

fine-grained medical ceramics (IV generation) for the 

endoprosthesis with grain size not more than 2 microns. 

Laboratory technology based on modified sol-gel technique 

was developed for obtaining of ultra dispersed compositions, 

containing the previously developed solid-solution 

Ce0.09Zr0.91O2 [J. Eur. Cer. Soc. 32 (2012) 1977-1981] 

and Al2O3-MgO. The particle size of powdery composition 

was 2-30 nm. Dilatometric study of the compacted samples 

Ce0.09Zr0.91O2/Al2O3-MgO (20/80, wt.) was carried out by 

using of device NETZSCH DIL 402 C. The behavior of finegrained 

ceramics formation during sintering was 

investigated. It was determine, that MgO role is to reduce 

the sintering temperature due to higher saturated vapor 

pressure than that of Al2O3 at the same temperature. We 

propose a working model of a fine-grained ceramics 

formation from ultra dispersed metal oxide particles. 

14:35 Nano particles as a binder for strong ceramic green body 

Authors : David Salamon, Zdeněk Chlup 

Affiliations : CEITEC - Central European Institute of 

Technology, Brno University of Technology, Technicka 

3058/10, 61600 Brno, Czech Republic; Institute of Physics of 

Materials, Academy of Sciences of the Czech Republic, 

Zizkova 513/22, 616 62 Brno, Czech Republic 

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Resume: There are several forming processes for advanced 

ceramics based on shaping of green body. The near-netshape 

forming of advanced ceramics are on the top of the 

interest. Both, wet and dry forming processes have 

limitations in a possible desired shape. The wet method 

such as slip casting has an ability to form green bodies with 

complex shape, but it needs a porous mold, binder and 

tailoring of drying conditions. Contrary, die pressing is the 

dry method, when pressed green bodies can be then fired 

directly after the process; however the main limitations are 

in variability of a shape and formation of a density gradient 

inside the green body. In this work we present a possibility 

to form strong green body suitable for mechanical machining 

without a binder. Water based suspensions of ceramic nano 

powder with submicron powder (both alumina) were 

prepared and dried in ambient conditions. After drying, the 

strong green body without any binder was able to be 

machined. Further heat treatment increased the mechanical 

strength four times. The obtained results demonstrated an 

ability of nano particles act as a binder between submicron 

particles. This process is energy saving and allows recycling 

of powder after the green body machining. 

14:55 INVESTIGATING THE MECHANICAL COUPLING IN 

COMPOSITE MULTIFERROICS VIA MAGNETOCAPACITANCE 

Authors : Mohsin Rafique1, Syed Qamar ul Hasan1, 

Muhammad Saif Ullah Awan2 and Sadia Manzoor1,2 

Affiliations : 1 Department of Physics, COMSATS Institute of 

Information Technology, Park Road, Islamabad, Pakistan 

2Center for Micro and Nano Devices (CMND), Department of 

Physics, COMSATS Institute of Information Technology, Park 

Road, Islamabad, Pakistan 

Resume: The role of magnetostrictive content and interface 

density of cobalt ferrite (CFO) and barium titanate (BTO) 

phases on the magnetoelectric (ME) response has been 

investigated in composites comprising of nanoparticles of the 

magnetostrictive material (cobalt ferrite) embedded in a 

continuous matrix of a piezoelectric material (barium 

titanate). When the sample capacitor of such a composite is 

placed in the magnetic field, the magnetostrictive (CFO) 

phase gets strained. This strain, when transfers to the 

piezoelectric (BTO) phase, due to the interfacial coupling, 

induces polarization in it which can be detected from the 

increased capacitance. A linear dependence of 

magnetocapacitance on the magnetic field has been obtained 

which is most likely due to a similar dependence of the 

magnetostriction on the applied magnetic field. The 

magnetocapacitance increases with the increase of CFO 

content non-linearly. This, we believe is due to the 

compounded effect of the increase in the magnetostrictive 

phase content as well as increase in the interface density per 

unit volume in the composite with increasing CFO content. 

The magnetoelectric susceptibility coefficient calculated from 

MC for our samples range from 0.02 to 0.8 mV.cm-1Oe-1. 

The sharp increase in the MC and the ME susceptibility with 

CFO content is a direct consequence of ME coupling. 

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15:10 Scaling Behavior and nearly constant loss effects in AgI- 

LiPO3 composite glasses 

Authors : D. P. Singh, K. Shahi, K. K. Kar 

Affiliations : Indian Institute of Technology Kanpur, India 


Resume: xAgI-(1-x)LiPO3 composite glass electrolytes were 

prepared by melt quenching technique using a twin roller 

assembly operated at 2000 rpm. The composite glasses with 

x0.2, micron size cluster particles of gamma-AgI 

nanocrystallytes were observed embedded in the glass 

matrix. This was confirmed by XRD and SEM studies. The 

conductivity of composite glasses increased by several 

orders of magnitude in comparison to pure LiPO3 glasses. 

Maximum conductivity of ~10-3 S/cm was found for x=0.5 

composition. FTIR studies suggest that AgI acts as 

plasticizing agent reduces the polymeric chain lengths of 

phosphate glasses. In addition AgI provides silver ions which 

contribute to the total ionic conductivity. It was shown using 

Summerfield scaling law that glass with x0.2 obeyed the 

Summerfield scaling and it was deduced that in these 

glasses the conduction is predominantly due to silver ions 

and any conduction due to lithium ions if at is negligible. 

Also nearly constant loss effects were observed in low AgI 

(x0.2) glasses. It is expected that 

presence of NCL is due to lithium ions only since NCL have 

been found in pure LiPO3. 

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Session XII : - 

09:00 Titanate based ferroelectric nanocomposites 

Authors : Paula Maria Vilarinho 

Affiliations : Department of Materials and Ceramic 

Engineering, Centre for Research In Ceramics and 

Composites (CICECO), University of Aveiro, 3810-193 

Aveiro, Portugal 

Resume: This talk is about approaches to produce novel 

nano-composite structures aiming at engineered properties 

of functional nanostructures. Combining different materials 

at the nanoscale permits creating multifunctional nanocomposites 

and novel properties may occur from the scale, 

interface and interactions. This is the case of ferroelectrics. 

Controlling the morphology of ferroelectrics at the 

nanoscale and synthesizing one-dimensional structures, 

such as nanorods, nanowires and nanotubes, as well as 

self-assembly of zero-dimensional nanoislands of 

ferroelectrics have been reported, for fundamental studies 

and novel applications. Also, ferroelectric-based nanocomposites 

with other functional components, such as 

metals and ferromagnetic phases are currently being 

studied for ultra-high dielectric constant, power storage, or 

magnetoelectric applications. Within this context we have 

been exploiting porosity at the nanoscale as a strategy to 

create ferroelectric nanocomposites. In this presentation 

different strategies to synthesise nanoporous ferroelectrics 

are presented and discussed. The combination of 

conventional ferroelectrics with recent developed 

mesoporous carbon materials is described. Our last results 

on the use of nanoporosity to develop ferroic structures will 

be presented as well. 

09:35 Nanostructured Zeolite LTA-Polyimide Nanocomposite 

Membranes for Natural Gas Separations 

Authors : Megan Lydon, Sankar Nair, Christopher Jones 

Affiliations : School of Chemistry & Biochemistry, Georgia 

Institute of Technology, Atlanta, GA, USA; School of 

Chemical & Biomolecular Engineering, Georgia Institute of 

Technology, Atlanta, GA, USA; School of Chemical & 

Biomolecular Engineering, Georgia Institute of Technology, 

Atlanta, GA, USA 

Resume: Natural gas is cleaner and safer than traditionally 

used energy sources including coal, oil, and nuclear power 

and is considered an important transition energy source 

until renewable energy becomes more affordable and 

efficient. Natural gas often includes acid gases such as CO2 

that need to be removed prior to use and improvements in 

the efficiency of this separation would expand the type of 

natural gas reserves that can be treated and lower the 

overall processing costs. Zeolites are of interest for natural 

gas separations because their angstrom-scale pores can be 

chosen or tuned to provide excellent selectivity between 

gases of different kinetic diameters. Nanocomposite 

membranes consisting of a bulk polymer phase and a 

dispersed selective zeolite phase are gaining attention for 

improving the membrane gas separation capabilities of 

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traditional polymer membranes while eliminating the extra 

expense and fragility of purely inorganic membranes. 

Unfortunately, during processing the nanocomposite 

membranes form a gap between the polymer and zeolite 

phase providing a nonselective pathway for gases around 

the more selective zeolite. Functionalization of the zeolite 

with Mg-based inorganic surface nanostructures has been 

shown to improve compatibility between phases in these 

membranes and eliminate or minimize the gap. In this 

work, four unique methods of surface roughening are 

presented on the aluminosilicate zeolite LTA and the 

functionalized nanoparticles are characterized using high 

resolution transmission electron microscopy, nitrogen 

adsorption characterization of surface area and pore 

volume, X-ray diffraction, and elemental analysis. 

Additionally, we show how these nanostructures impact the 

various properties of polyimide nanocomposite membranes 

including gas selectivity, mechanical properties, and phase 

compatibility using CO2/CH4 gas permeation, 

nanoindentation, and TEM imaging of membrane cross 

sections. We will show that one method, ion exchange 

induced surface deposition, shows significantly improved 

interfacial compatibility with the glassy polymer while 

maintaining the intrinsic structure and gas selectivity 

characteristics of the zeolite. 

09:55 SiOC/ZrO2 Ceramic Nanocomposites – Candidate Materials 

for Applications in Harsh Environments 

Authors : Christoph Linck, Emanuel Ionescu, Hans-Joachim 

Kleebe, Ralf Riedel 

Affiliations : Fachbereich Material- und Geowissenschaften, 

Technische Universität Darmstadt, Darmstadt, D-64287, 

Germany 

Resume: Dense polymer-derived SiOC/ZrO2 ceramic 

nanocomposites were prepared via chemical modification of 

a commercially available polysiloxane with Zr(OnPr)4 as 

zirconia precursor. The prepared materials were cross 

linked, pyrolyzed at 900 °C and subsequently hot-pressed 

in argon atmosphere to provide SiOC/ZrO2 ceramic 

nanocomposites as monoliths. The obtained SiOC/ZrO2 

materials were characterized via XRD, elemental analysis, 

Raman spectroscopy, solid state NMR as well as electron 

microscopy (SEM, TEM). The oxidation behavior and the 

hydrothermal corrosion resistance of the prepared ceramic 

nanocomposites were investigated. The oxidation 

experiments were performed at temperatures from 1300° 

to 1500°C in air atmosphere up to 100h. The oxidized 

samples were investigated with respect to microstructure 

evolution and their crystalline phase composition. The 

oxidation rates were determined by recording their specific 

mass change upon oxidation. The corrosion experiments 

were performed at three temperatures (150, 200 and 250 

°C) and three different corrosion times (25, 50 and 100 h) 

to determine the rate and the activation energy of the 

hydrothermal corrosion process. The obtained results 

emphasize that SiOC/ZrO2 should be considered mass 

stable in oxidative atmosphere at temperatures up to 1500 

°C. They exhibit promising behavior at moderate 

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temperatures in hydrothermal environments, showing 

corrosion rates which are lower by several orders of 

magnitude than that of e.g. silicon carbide. 

10:10 ON THE INFLUENCE OF SILICA TYPE ON THE STRUCTURAL 

INTEGRITY OF DENSE La9.33Si2Ge4O26 ELECTROLYTES 

FOR SOFCs 

Authors : C. Alves, T. Marcelo, F.A.C. Oliveira, L. C. Alves, 

J. Mascarenhas, B. Trindade 

Affiliations : C. Alves;T. Marcelo; F.A.C. Oliveira; J. 

Mascarenhas- Laboratório Nacional de Energia e Geologia 

I.P., Estrada do Paço do Lumiar, 1649-038 Lisboa, Portugal 

L. C. Alves-IST/ITN Instituto Superior Técnico, Technical 

University of Lisbon, Estrada Nacional 10, 2686-953 

Sacavém, Portugal B. Trindade-CEMUC, Mechanical 

Engineering Department, University of Coimbra, Rua Luís 

Reis Santos, 3030-788 Coimbra, Portugal 

Resume: Apatite-type rare earth based oxides, such as Rdoped 

lanthanum oxides of general formula 

La9.33(RO4)6O2 with R = Ge, Si, exhibit high ionic 

conductivity and low activation energy at moderate 

temperatures, when compared to the yttria-stabilized 

zirconia electrolyte making them potential materials to be 

used in the range 500–700ºC, for intermediate temperature 

solid oxide fuel cells (IT-SOFCs). In this study, dense 

oxyapatite-based La9.33Si2Ge4O26 electrolytes have been 

successfully prepared either by electrical sintering at 

1400ºC or microwave hybrid sintering at 1350ºC for 1 h 

from La2O3, SiO2 and GeO2 powders dry milled at 350 rpm 

for 15 h in a planetary ball mill. The densification behavior 

of the apatite-type phase synthesized by mechanical 

alloying was found to be dependent on the grade of SiO2 

used: either pre-milled quartz powder or amorphous 

nanosized fumed silica. The influence of the silica type on 

the La9.33Si2Ge4O26 integrity was assessed by dynamic 

Young modulus, microhardness and indentation fracture 

toughness measurements. A good correlation between the 

degree of densification (as observed by SEM/EDS) and the 

resulting mechanical properties could be established. Premilling 

of quartz powder has favored higher densification 

rates to be attained suggesting that both Fe content, 

resulting from the ball pre-milling (as determined by PIXE 

analyses) and crystallinity of SiO2 do promote densification 

of these electrolytes thereby improving their structural 

integrity. 

10:40 Towards a practical rechargeable 5 V Li ion battery 

Authors : R. I. Eglitis 

Affiliations : Institute of Solid State Physics, University of 

Latvia, 8 Kengaraga Str., Riga LV1063, Latvia 

Resume: Current lithium-ion batteries are the state-of-theart 

power sources for consumer electronics operating 

mainly in the 4 V regime. One frequently discussed 

direction to improve the performance of such batteries is 

the development of a family of 5 V cathode materials. I 

report here a Full Potential Linearized Augmented Plane 

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5

12:30 Lunch 

Wave (FP-LAPW) calculation for Li2Co1Mn3O8 in the Fd3m 

spinel structure. My calculated battery voltage for this 

material is around 5 V. This result is stable against 

interchange of positions of Mn and Co atoms as well as 

choice of the position of the Li vacancy [1]. Recently by 

Kawai et al. [2,3] was reported the first experimental 

single-cell lithium battery system to operate over 5 V for a 

significant period of discharge, by incorporation of a new 

cathode material Li2Co1Mn3O8. Discharge performance was 

limited to 40 mAhg-1 at 5 V, but nevertheless this indicates 

the possibilities for developing practical 5 V batteries [2,3]. 

References: 1. R. I. Eglitis and G. Borstel, phys. stat. sol. 

(a) 202, R13 (2005). 2. H. Kawai, M. Nagata, H. Tukamato, 

and A. R. West, Electrochem. Solid-State Lett. 1, 212 

(1998). 3. H. Kawai, M. Nagata, H. Tukamato, and A. R. 

West, J. Mater. Chem. 8, 837 (1998).

Symposium F Nanoceramics and Ceramic based ... - EMRS

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