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Technical Paper 

Reference : TP-GB-RE-LAF-097 

Page : 1/13 

New Calcium Aluminates with Improved Corrosion 

Resistance for the Next Generation of Refractory 

Monolithics 

C. Parr, G. Assis, C. Wöhrmeyer, H. Fryda, G. Bhattacharya 

Kerneos SA, Paris, France 

Presented at the 9th Indian International Refractories Congress, Kolkata, 2 nd - 4 th February 2012 

Kerneos 

8, Rue des Graviers - 92521 Neuilly sur Seine Cedex, France 

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Page : 2/13 

ABSTRACT 

By changing the microstructure of a monolithic castable it is possible to enhance the in-situ lining 

performance and ultimately, to increase the service life of the refractory. To achieve this, novel 

calcium aluminates (CA) have recently been developed, namely a 50% alumina (Al 2 

O 3 

) containing 

CA aggregate and a calcium magnesium aluminate (CMA) binder. Calcium aluminates can not only 

provide the binder function but can also add to and enhance the final performance as measured by 

corrosion resistance. 

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1 Introduction 

The first part of this study looks at the influence 

of a calcium aluminate aggregate, namely R50, 

on the properties of a refractory castable in 

comparison to bauxite and fireclay aggregates. 

R50 aggregate contains hydraulic phases like 

calcium mono-aluminate that allow the surface 

of this aggregate to react chemically during 

hydration and de-hydration with the calcium 

aluminate cement in the binder phase, unlike 

other aggregates consisting of CA 6 

, corundum 

or mullite. The chemical bonds between the R50 

aggregate and the matrix enhance the physical 

properties of the castable. 

In contact with aluminium, traditional bauxite- based 

mixtures require anti-wetting agents to reduce metal 

infiltration. However, these can negatively influence 

the refractoriness of the castable if the temperature 

of the aluminium furnace is raised above normal 

operating conditions. If temperatures reach 

unexpectedly high levels (>1200 °C), traditional 

anti-wetting additives like barium sulphate or 

calcium fluoride can destroy a bauxite-based 

castable. Castables made from R50, however, 

show superior infiltration resistance against 

aluminium alloys in aluminium contact areas 

with significantly lower (or no) anti-wetting agent 

additions. Minimising the use of the antiwetting 

agent and using R50 enhances the refractoriness 

of the castable up to 1400°C. This makes R50 

interesting for many applications where good 

heat containment, abrasion resistance and low 

liquid penetration / low accretion build-up are 

required. 

In the second part of this paper we will discuss 

the new CMA binder that brings microcrystalline 

spinel phases into areas of the castable 

microstructure which are normally occupied 

by calcium aluminate phases only. The basis 

of this new calcium magnesium aluminate 

cement is a novel multiphase clinker with a 

microstructure of CA phases embedded in a 

matrix of microcrystalline magnesium aluminate 

spinel crystals. Using this novel CMA as a 

binder in different types of ladle castables has 

shown significant improvements in corrosion 

and penetration resistance with a wide range of 

ladle slag compositions. 

2 Experimental Procedure 

2.1 Material Details : CA aggregate 

R50 is a low iron oxide, fused calcium aluminate 

aggregate with a very low C 12 

A 7 

content (



Page : 4/13 

Table 1 : Chemistry and mineralogy of aggregates. 

R50 

Bauxite 

Fused 

Sintered 

Chemistry (mass %) 

Al 2 

O 3 

52.5 89.5 

SiO 2 

5.5 4 

CaO 37 0.1 

Fe 2 

O 3 

2 1.5 

TiO 2 

2 3.7 

Mineralogy (A= Al 2 

O 3 

, S=SiO 2 

, C=CaO, F=Fe 2 

O 3 

) 

A - XXX 

A 3 

S 2 

- X 

S - X 

CA 2 

- - 

CA XXX - 

C 12 

A 7 

- - 

C 3 

A - - 

C 2 

S - - 

C 2 

AS XX - 

C 4 

AF - - 

XXX= primary phase, XX=secondary phase, X= minor phase (< = 1%) 

2.2 Test methods : Aggregate Testing 

Classical monolithic refractory test methods such 

as vibration flow, porosity by water immersion 

and strength measurements have been used to 

study the basic castable properties. Quantitative 

chemical and mineralogical analyses have 

been conducted using the XRF and XRD 

methods. The aggregates have been tested in a 

deflocculated medium cement castable (MCC) 

formulation (Tab. 2). 

3 Experimental Results & Discussion 

3.1 Aggregate testing 

Previous work has shown [1] that R50 provides 

a very similar castable rheology in conventional 

formulations. This is because R50 is a fused 

and almost pore free aggregate, minimising the 

casting water required and ensuring that there 

is no flow decay during placing. In addition, the 

mineralogy of the R50 (with its high calcium 

monoaluminate and low C 12 

A 7 

content) ensures 

that early stiffening is prevented and working 

time maintained. 

For this work, microsilica-free MCC formulations 

(Tab. 2) were chosen in order to minimise the 

chemical reactions between the aluminium melt 

and the castable matrix. Different contents of 

barium sulphate (BaSO 4 

) were used as an antiwetting 

agent. The corrosion and penetration 

resistance was tested in contact with liquid 

aluminium. The BaSO 4 

addition is absolutely 

necessary for the bauxite based castables to 

minimise metal infiltration of the castable, but 

the results below will show that the addition can 

be reduced or even completely eliminated when 

R50 is used [1, 2] . 

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Table 2 : Model MCC recipes with bauxite 

(B1-B3) and R50 (R1-R3) with different 

barium sulphate contents. 

Bauxite R50 

B1 B2 B3 R1 R2 R3 

R50 3-5 mm % - 33 

R50 1-3 mm % - 12 

R50 0-1 mm % - 20 

SECAR ® 51 % - - 5 5 

Bauxite 3-6 mm % 21 - 



Bauxite 0-0.09 mm % - 5 5 - 

Calc. Alumina % - - 5 - - 5 

BaSO 4 

% 10 5 - 10 5 - 

React. Alumina % 10 10 

SECAR ® 71 % 15 15 

Polyprop fibres % 0.05 0.05 

Peramin® AL200 % 0.15 0.12 

H 2 

O % 5 4.5 

A polycarboxylate ether (Peramin ® AL200) 

deflocculates and fluidifies these castables very 

efficiently with 5% water in case of bauxite and 

only 4.5% in case of R50. Despite the lower 

water addition and a lower deflocculant level, 

better flow properties were achieved for all R50 

containing MCC’s (R1-R3) (Fig. 3). The open 

porosity after firing to 800 & 1200°C, the critical 

temperature range for aluminium applications, 

is, in all cases, significantly lower with R50 

despite these castables also having lower bulk 

densities (Fig. 4, 5). The cold crushing strength 

of the R50 formulations (irrespective of the 

BaSO 4 

content) is higher than formulation B1 

(10% BaSO 4 

) which could be considered as the 

reference formulation for this application (Fig. 

6). 

Vibration flow (mm) 

230 

220 

210 

200 

190 

180 

170 

160 

150 

0 30 60 

Time (min) 

Fig. 3 : Vibration flow for R50 (R1-R3) and 

bauxite (B1-B3). 

App. Porosity (Vol.%) 

21 

19 

17 

15 

13 

11 

9 

7 

5 

800°C 1200°C 

R1 

R3 

R2 

B1 

B3 

B2 

B1 B2 B3 R1 R2 R3 

Castable 

Fig. 4 : Apparent porosity for R50 (R1-R3) 

and bauxite (B1-B3). 

Bulk density (Vol.%) 

3 

2,95 

2,9 

2,85 

2,8 

2,75 

2,7 

2,65 

2,6 

2,55 

2,5 

800°C 1200°C 

B1 B2 B3 R1 R2 R3 

Castable 

Fig. 5 : Bulk density for R50 (R1-R3) and 


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800°C 1200°C 

250 

200 

CCS (MPa) 

150 

100 

Penetration 

B1: Bauxite (10% BaSO 4 

) B3: Bauxite (0% BaSO 4 

) 

50 

0 

B1 B2 B3 R1 R2 R3 

Castable 

Fig. 6 : Cold crushing strength of MCC with 

R50 (R1-R3) and bauxite (B1-B3). 

To simulate the in situ performance of these 

castable formulations given in Tab. 2, static 

corrosion tests in ‘Alcoa cups’ cast from each 

formulation were performed . The cups were 

filled with aluminium alloy 7075, heated to 

800°C and held at this temperature for 72 hours. 

Thereafter, the cups were emptied, cooled and 

sectioned. 

Fig. 8 shows photos of the sectioned cups for 

formulations B1 & R1 both with 10% BaSO 4 

, and 

B3 & R3 without BaSO 4 

additions. There is very 

little adherence of aluminium to the samples 

made with R50, and where it does exist, only very 

thin layers can be seen. More significantly, whilst 

sample B3 clearly shows areas of aluminium 

metal penetration into the refractory, there is no 

recognisable infiltration into the microstructure 

of sample R3. This correlates with the lower 

apparent porosity results of all the R50 samples 

as shown in Fig. 4. The chemical bonding of the 

R50 aggregate to the matrix, and the reduced 

casting water demand due to the fused nature 

of the R50 aggregate ensure the low porosity 

of the R50-based formulations. This, in turn, 

significantly enhances the penetration and 

corrosion resistance. 

R1: R50 (10% BaSO 4 

) R3: R50 (0% BaSO 4 

) 

Fig. 7 : Alcoa cup tests after heating to 800°C 

for 72 hours. 

A final, but significant, consideration is that 

BaSO 4 

starts to decompose at 1200°C which 

leads to a massive volume expansion around 

1400°C, as seen in Fig. 8 for the bauxite-based 

formulations (B1 & B2). In the case of R50, however, 

since significantly less BaSO 4 

needs to 

be added to maintain the infiltration resistance 

of the castable, the associated advantages of 

a higher service temperature can be realised. 

Consequently, using R50 as the aggregate 

gives supplementary security even if unexpectedly 

high temperatures occur during aluminium 

production. 

App. Porosity (Vol. %) 

35 

30 

25 

20 

15 

10 

5 

B3 

R3 

R2 

B2 

R1 

0 

-2,00 -1,00 0,00 1,00 2,00 3,00 4,00 5,00 

Permanent linear change 110°C --> 1400°C (%) 

Fig. 8 : Permanent linear change after firing at 

1400°C vs open porosity for R50 (R1-R3) and 


B1 

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4 Experimental Procedure 

4.1 Material Details : Calcuim Magnesium 

Aluminate (CMA) binder 

Castable developments for steel ladles during 

the last three decades have shown aluminaspinel 

and alumina-magnesia systems to 

be most effective [3-5] . More recently, hybrid 

systems which combine both materials have 

been developed [6] . Kantani and Imaiida [7] 

found that the best compromise between slag 

penetration and corrosion resistance could be 

achieved when the castable contains 20 - 40% 

magnesium aluminate spinel after firing. It has 

also been shown that the slag penetration can 

be minimized by reducing the spinel grain size [8] . 

Very fine spinel can be created by adding 

magnesia to the castable, which reacts during 

firing with the alumina fillers to form spinel insitu. 

However, the magnesia addition often has 

negative side effects, creating problems during 

dry-out due to the magnesia hydration and 

volume expansion at firing temperatures due 

to the spinel formation. To improve the volume 

stability of the castable, small amounts of 

microsilica are often added to the dry-mix which 

creates a small amount of liquid phase during 

firing. Although this counteracts the expansion 

caused by the spinel formation [5, 9, 10] . 

Development work on a composite hydraulic 

binder (calcium-magnesium-aluminate cement) 

which would combine micro-crystalline spinel 

(MA) with calcium aluminate phases (CA, CA 2 

) 

has been the centre of numerous patents and 

publications since 1969 (Patent no 1575633, 

Romania) [11] . Numerous publications were 

lodged in the late 1990’s by predominantly 

Japanese (1996) [12] , Spanish (1999) [13] , and 

Chinese [14] authors. Kerneos lodged a unique 

patent in 1999 [15] to produce a commercially and 

industrially viable calcium magnesium aluminate 

(CMA) binder for steel ladle applications. This 

new CMA 72 has been successfully produced 

on an industrial scale. The raw material mix is 

sintered in a rotary kiln to simultaneously form 

a micro-crystalline spinel together with calcium 

aluminate phases within the same clinker. This 

can be achieved below the sintering temperature 

of pure spinel and with crystal sizes as small as 

spinel that is generated in-situ inside the matrix 

of an alumina-magnesia castable. 

CA 

CA2 

CA 

CAC grain 

CA2 

MA 

MA 

MA 

MA 

CA 

MA 

CA 

CMA grain 

Fig. 9 : Schematic microstructure of a CAC 

and a CMA grain (average grain diameter ca. 

15µm). 

The exact chemical and mineralogical 

comparison between SECAR ® 71 and CMA can 

be found in Tab. 10. Both products contain 70% 

Al 2 

O 3 

but CMA contains only 10% CaO and 

20% MgO, the latter facilitating the presence 

of the MA phase in the CMA. CMA clinker 

displays a unique microstructure resulting from 

the intergrowth of the hydraulic phases calcium 

mono-aluminate (CA) and calcium di-aluminate 

(CA 2 

) with MA phases during clinker formation in 

the rotary kiln (Fig. 9). The hydraulic properties 

of this new CMA cement are described by Assis 

et al. [16] . Both binders have been ground to a 

specific surface area of approx. 4000cm 2 /g 

(Blaine) with a median grain size d50 for both 

cements of about 15µm. 

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Table 10 : Chemical and mineralogical 

compositions. 

Chemistry Al 2 

O 3 

CaO MgO SiO 2 

SECAR ® 71 68.7-70.5 28.5-30.5



Page : 9/13 

The corrosion and penetration resistance 

against different slag compositions was tested 

in a laboratory scale rotary kiln according to 

ASTM C874-99. Here, the test specimens were 

prepared using a bigger mixer than those for 

the physical property tests. The higher mixing 

energy of the larger mixer allowed a further 

reduction of water. The water was reduced to 

3.9% for the alumina-spinel castables (MA) and 

to 4.0% for the alumina-magnesia formulations 

(M). The vibrated samples were cured at 20°C 

for 24h, dried at 110°C, and then pre-fired to 

1550°C for 5h. The specimens were installed in 

the pilot rotary kiln where they were heated up 

to 1550°C again and kept at this temperature for 

30 minutes prior to the first addition of 900g of 

slag. 1.7kg/h of fresh slag was introduced into 

the kiln during the following 5h at 1550°C. 

The furnace rotated at a constant speed of 2½ 

rpm. The furnace was tilted 3º axially towards 

an oxy-acetylene flame burner at the lower end 

of the kiln. The slag pellets were charged into 

the upper end of the tilted rotary kiln. In this way, 

the molten slag washed over the lining, finally 

dripping off at the lower end of the kiln. Two 

different slag compositions were used (Tab. 12). 

The dimensions of the castable specimens were 

measured before and after the test to quantify 

the degree of wear. 

Table 12 : Slag compositions (Slag A: Al-killed 

steel slag, Slag B: BOF-slag). 

Corrosion tests were also conducted in a 

laboratory induction furnace. Samples of the 

test formulations lined the wall of the induction 

furnace which was charged with steel and 

covered with one of the slags (composition in 

Tab. 12). The test temperature was 1600°C. The 

steel contained 0.08% C, 1.9% Si, 0.3% Mn, 

0.01% S, and 0.02% P. The wear was quantified 

by determining the ratio between the original 

cross sectional area of the specimens and the 

cross sectional area remaining after the test. The 

areas were measured using image analyzing 

software. Furthermore, SEM techniques were 

used to study the microstructure of the castables 

and to quantify the depth of penetration of the 

slag. 

5 Experimental Results & Discussion 

5.1 Thermo-physical castable properties 

The difference between the castables with preformed 

spinel (MA1, MA2) and those with in-situ 

spinel formation (M1, M2) can easily be seen in 

Fig. 13. 

While both MA1 and MA2 keep high volume 

stability, those with free MgO (namely M1 & 

M2) show a significant permanent linear change 

after firing to 1550°C due to the in-situ spinel 

formation. However, mix M2, which contains 

less free MgO than M1, shows lower expansion. 

Mass % Al 2 

O 3 

SiO 2 

FeO MnO CaO MgO 

Slag A 30 5 0.8 0.2 57 7 

Slag B 2 15 19 6 53 5 

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Fig. 13 : Permanent linear change of castables. 

The measurement of the thermo-physical 

properties (Fig. 14) also indicates that the 

permanent expansion with M2 is lower than with 

M1 when a load of only 0.05 MPa is applied on 

the sample during the first heat-up and during 

1h soaking at 1550°C followed by cooling to 

1000°C. 

After this pre-firing procedure, the application 

of a load of 0.2 MPa results in an excellent 

refractoriness under load with a T 2 

of 1680°C 

for the CMA containing M2. While the silica 

free castables MA1 and MA2 show very high 

hot modulus of rupture (HMOR), the values are 

quite low in the case of M1 and M2 at 1350°C 

and 1550°C respectively (Fig. 15) due to the 

silica content. However, the lower permanent 

expansion of M2 and the presence of the 

microcrystalline spinel in CMA indicate that an 

optimization step of this formulation with respect 

to silica and periclase content could improve the 

hot properties of this formulation. 

Fig. 14 : Thermo-physical properties of model 

castable M1 (SECAR ® 71) and M2 (CMA 72). 

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5.2 Castable microstructure 

SEM micrographs of polished matrix samples 

fired at 1550°C are shown in Fig. 16. These 

matrix samples were derived from the castable 

formulations given in Tab. 11 after the removal 

of any aggregate coarser than 300µm. The 

micrographs clearly show that the pores in 

the CAC containing matrices are significantly 

larger than the pores in the CMA 72 containing 

matrices. 

HMOR (MPa) 

30 

25 

20 

15 

10 

5 

0 

MA1 (CAC) MA2 (CMA) M1 (CAC) M2 (CMA) 

1000 1350 1550 

Temperature (°C) 

Fig. 15 : Hot modulus of rupture of model 

castables. 

Furthermore, in the latter case, the microcrystalline 

phases of spinel and calcium 

aluminate are more homogeneously distributed. 

For the CAC matrices, a certain area in the 

microstructure is occupied by calcium aluminates 

alone, but the corresponding area is occupied by 

ultra-fine spinel and calcium aluminate phases 

in the CMA 72 containing matrices. 

5.3 Thermo-chemical castable properties 

The following results show quite clearly that 

the CMA 72 containing castables achieve both 

better corrosion and penetration resistance to 

the slag chemistries tested. In the induction 

furnace, the corrosion of the CMA containing 

mixes was around 50% lower than the CAC 

containing reference mixes. The castables 

based on CMA 72 resisted both of the slags tested 

better than the CAC containing formulations (Fig. 

17). A similar trend can be seen in the results from 

the rotary kiln tests where an improvement in the 

range of 20% was measured between the MA1 

and MA2 samples, and again between the M1 and 

M2 formulation samples (Fig. 18). In all cases, the 

iron oxide rich slag B caused more corrosion 

than slag A. CMA-based castable M2 showed 

the highest resistance to wear and the lowest 

corrosion with the typical ladle slag A. Slag 

penetration was lowest in the MA2 castable, 

even with the iron rich slag B (Fig. 19). 

This improved resistance to slag penetration 

could be significant for functional pre-cast 

products where adhering slag and steel is 

often cleaned from the working surface by 

oxygen lance. This cleaning method creates 

very aggressive iron-rich slags which could be 

resisted more effectively by CMA containing 

formulations. 

100 µm 

MA1 ((Secarr 71)) 

MA2 ((CMA 72)) 

Fig. 16 : Matrix microstructure of model castables 

with Secar 71 and CMA 72 (1550°C, 3h). 

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Corroded cross section area (%) 

16 

14 

12 

10 

8 

6 

4 

2 

0 

Slag B 

Slag A 


Fig. 17 : Corrosion of the model castables in 

a laboratory scale induction furnace with the 

two slag compositions. 

Wear (mm) 

16 

14 

12 

10 

8 

6 

4 

2 

0 

Slag B 

Slag A 


Fig. 18 : Corrosion of the model castables in 

laboratory scale rotary kiln with the two slag 

compositions. 

Penetration (µm) 

1000 

800 

600 

400 

200 

Slag B 

Slag A 

6 Conclusions 

Novel calcium aluminate containing products can 

not only provide the binder function but also add 

to and enhance the final refractory performance 

as measured by corrosion resistance. 

The fused calcium aluminate aggregate, R50, 

displays enhanced bonding properties due 

to the physical and chemical bonds formed 

between the refractory matrix and the reactive 

surface of the R50 aggregate. When applied 

in microsilica-free medium cement castables 

for aluminium applications, R50 facilitates new 

formulation options to improve the operating 

temperature resistance. Compared with the 

traditional bauxite-based MCC containing barium 

sulphate, the R50-based formulation without the 

anti-wetting agent displays equivalent infiltration 

and corrosion resistance but provides increased 

thermal stability and lining integrity up to 1350°C. 

CMA, the new calcium magnesium aluminate 

cement significantly improves the corrosion and 

penetration resistance of monolithics for steel 

ladle applications. This is based on the innovative 

microstructure of CMA which provides microcrystalline 

spinel within the matrix, minimising 

the pore size and improving penetration 

resistance. Homogeneous distribution of the 

microcrystalline spinel within the castable 

matrix enhances the in-situ life of both spinel 

containing and spinel-forming castables. 

0 


Fig. 19 : Slag penetration of model castables 

in laboratory rotary kiln. 

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Page : 13/13 

7 Acknowledgements 

We would like to thank the Kerneos laboratories 

in France and China, the Wuhan University 

of Science and Technology, China, the ITMA 

institute, Spain, the ICAR institute, France, and 

the BCMC institute, Belgium, for the support of 

this study. 

8 References 

[1] C. Wöhrmeyer, C. Parr, H. Fryda, E. Frier: 

Stronger bonds for monolithic castables 

through surface reactive calcium aluminate 

aggregates. Aachen congress, Germany, 

(2010). 

[2] C. Wöhrmeyer, N. Kreuels, C. Parr, T. Bier: 

The use of calcium aluminate solutions in 

the aluminium industry. Unitecr congress, 

Berlin, (1999). 

[3] T. Yamamura et al.: Development of 

alumina-spinel castables for steel ladles. 

Taikabutsu 42, 8 pp 427-434 (1990). 

[4] S. Asano et al.: Mechanism of slag 

penetration in alumina-spinel castable for 

steel ladle: Taikabutsu 43, 4, pp 193-199 

(1991). 

[5] H. Naaby, O. Abbildgaard, G. Stallmann, C. 

Wöhrmeyer and J. Meidell: Refractory wear 

mechanisms and influence on metallurgy, 

37 th Int. Colloquium on Refractories, 

Aachen, Germany, pp. 198-204 (1994). 

[6] K.H. Dott: Monolithic ladle lining at SSAB 

Tunnplåt in Luleå, Sweden. RHI Bulletin, 1, 

pp 34-37 (2008). 

[7] T. Kanatani, Y. Imaiida : Application of an 

alumina-spinel castable to the teeming ladle 

for stainless steelmaking. UNITECR’93, pp 

1255-1266, (1993). 

[8] M. Nakashima, T. Isobe, S. Itose: 

Improvement in corrosion of alumina-spinel 

castable by adding ultra fine spinel powder. 

Taikabutsu, 52,2, pp 65-72, (2000). 

[9] T. Bier, C. Parr, C. Revais, M. Vialle : Spinel 

forming castables : Physical and chemical 

mechanisms during drying. Refractories 

Application 4, pp 3-4, (2000). 

[10] Y.C. Ko: Development and production of 

Al2O3-MgO and AlsO3-spinel castables for 

steel ladles. Mining and Metallurgy, Taipei, 47, 

1, pp 132-140. 

[11] A. Braniski, T. Jonescu, N. Deica, Patent 

(PV no. 145.441, No 1575633), Romania. 

[12] Y. Koya, Y. Sasagawa, Denki Kagaku 

Kôgyô Ltd., Patent (HEI 8-198649), Japan. 

[13] A.H. De Aza, P. Pena, S. De Aza: Ternary 

system Al2O3-MgO-CaO: Paper I, J. Am 

Ceram Soc., Vol 82 [8], (1999). 

[14] D. Feng, et al.: Preparation & application of 

aluminate cements containing magnesiaalumina 

spinel, J. Naihuo Cailiao 41(1), 

(2007). 

[15] J.P. Falaschi et al. : Liant du type clinker, 

utilisation et procede de fabrication d’un 

tel liant. Demand de brevet d’invention, 

FR2788762A1, (1999). 

[16] G. Assis et al.: Castables with improved 

corrosion resistance for steel making 

applications, Unitecr’11, (2011). 

[17] C. Wörhmeyer et al.: New spinel containing 

calcium aluminate cement for corrosion 

resistant castables, Unitecr’11, (2011). 

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