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L0110 - Iron oxide as an effective sintering aid and a grain boundary scavenger for ceria-based electrolytes
The effect of FeO1.5 addition on the densification behavior and electrical properties of Ce0.8Gd0.2O(2-d) ceramics was examined. The small addition of FeO1.5 (e.g., 0.5 at.%) reduced sintering temperature (by ~200¡C) and promoted densification rate. When sintered at 1300¡C for 5 h, the 0.5 at.% FeO1.5-doped Ce0.8Gd0.2O(2-d) has ~95% relative density, as compared to ~82% relative density for the undoped one. The measurement of lattice parameter indicated that the FeO1.5 addition also promoted the dissolution of Gd2O3 in CeO2 at lower sintering temperatures. On the other hand, the grain boundary (GB) conductivity could be significantly improved by small addition of FeO1.5. The optimum scavenging effect on SiO2 impurity was achieved by adding 0.5 at.% FeO1.5 to Ce0.8Gd0.2O(2-d) ceramics and sintered at 1400-1500¡C.
T.S. Zhang, J. Ma, L.B. Kong, S.H. Chan, P. Hing, J.A. Kilner, Solid State Ionics 167 (2004) 203-207
L0109 - The synthesis mechanism of Ca3Al2O6 from soft mechanochemically activated precursors studied by time-resolved neutron diffraction up to 1000¡C
The reaction pathway for the Ca3Al2O6 formation up to 1300¡C, from mechanochemically treated mixtures of amorphous aluminum hydroxide and CaCO3; was studied in situ by differential thermal analysis, constant heating rate dilatometry and timeresolved neutron powder diffraction. The experiment was carried out, in an open system, on a sample with the nominal Ca3Al2O6 stoichiometry. The results obtained by neutron diffractometry and thermal analysis were in good agreement with the data obtained by scanning electron microscopy and X-ray diffraction on heat-treated and-quenched samples. The synthesis path implied the formation of cryptocrystalline Al2O3; crystalline CaO, CaAl2O4 and Ca12Al14O33 as transitory phases. Finally the nucleation and growth of the single phase Ca3Al2O6 took place at 1300¡C and exhibited porous structure due to CO2 and H2O release.
J.M. Rivas Mercury, A.H. De Aza, X. Turrillas, and P. Pena, Journal of Solid State Chemistry 177 (2004) 866-874
L0108 - Effect of transition metal oxides on densification and electrical properties of Si-containing Ce0.8Gd0.2O(2-d) ceramics
Ce0.8Gd0.2O(2-d) (CGO20) ceramic has been considered as one of the most promising electrolytes for intermediate temperature (IT) fuel cells. It has been reported that some transition metal oxides (TMO), such as MnO2, Fe2O3 and Co3O4, are effective sintering aids for the densification of ceria-based electrolytes. However, very little information is available regarding the effect of TMO addition on the electrical properties of Si-containing CGO20 ceramics. In this study, 0.5 at.% (atomic percent) TMOs have been loaded into the CGO20 with ~30 ppm (pure) and ~200 ppm (impure) SiO2, respectively, and the sintering behavior and ionic conductivity have been investigated. It has been found that Co3O4 is the most effective sintering aid, and the sintering temperature of CGO20 can be reduced by over 200¡C by adding 0.5 at.% CoO4/3. All the TMOs used show a slight effect on the grain-boundary (GB) conductivity of the pure CGO20. However, SiO2 additions, together with MnO2 and Co3O4, have found to be extremely detrimental to the GB conduction of CGO20. As compared to the impure CGO20, the GB resistance has been increased by over six times for the impure one with addition of only 0.5 at.% CoO4/3. On the other hand, in contrast to the Mn or Co doping case, small addition of Fe2O3 has a scavenging effect on SiO2 impurity, and significantly improves the GB conduction of the impure CGO20. Therefore, Fe2O3 could be used as an effective sintering aid, as well as a grain-boundary scavenger for SiO2 contaminated ceria-based electrolytes.
T.S. Zhang, J. Ma, Y.J. Leng, S.H. Chan, P. Hing, J.A. Kilner, Solid State Ionics 168 (2004) 187-195
L0107 - The kinetics of surface area reduction during isothermal sintering of hydroxyapatite adsorbent
The behaviour of non-stoichiometric hydroxyapatite (HA) during the calcination in a solid bed was investigated. The structural properties are described in terms of the specific surface area. Calcination led to a significant decrease of the specific surface area by particle coalescence and densification. Hydroxyapatite begins to shrink near 780¡C and reaches 97% theoretical density at 1100¡C. The specific surface area and density variations are caused both by sintering and chemical reaction. Sintering data from these solids were correlated as a function of time and temperature. The rate of sintering is assumed to obey an Arrhenius equation. These results are compared with a number of literature models describing the mechanism of sintering kinetics using the specific surface area, and a good agreement is observed. The kinetic equation used is based on sintering driven by the curvature gradient in the interparticle neck region associated with initial stage sintering. Then, the decline in specific surface area is accurately described by the empirical equation of the form dS/dt = -B(T)k^b. The changing value of b, also known as the "order" of the reaction, suggests that the diffusion mechanism for loss of surface area may be a function of the temperature.
S. Bailliez, A. Nzihou, Chemical Engineering Journal 98 (2004) 141-152
L0106 - The mechanical behavior of magnesium alloy AZ91 reinforced with fine copper particulates
In this study, a hybrid composite based on magnesium alloy AZ91A reinforced with copper particulateswas fabricated using the disintegrated melt deposition (DMD) processing technique followed by hot extrusion. Microstructural characterization of the as-extruded composite sample revealed a near uniform distribution of the copper particulates and other intermetallic phases through the magnesium alloy metal matrix, good integrity at the copper-magnesium alloy matrix interfaces and evidence of minimal porosity. Mechanical property quantification revealed that addition of copper particulates resulted in a significant increase in elastic modulus, 0.2% offset yield strength and ultimate tensile strength of the composite material. However, ductility of the composite was marginally affected when compared to the unreinforced monolithic counterpart. The overall mechanical properties of AZ91A/Cu composite were found to be higher than the silicon carbide particulate reinforced AZ91 composite, even for higher volume fractions of the particulate reinforcement. Influence of copper in the matrix of magnesium alloy AZ91A is examined in light of intrinsic microstructural features and mechanical properties of the composite.
K.F. Ho, M. Gupta, T.S. Srivatsan, Materials Science and Engineering A369 (2004) 302-308
L0105 - Experimental and numerical analysis of the deformation of ferrite segments during sintering
The thermo-mechanical behaviour of hard ferrite powder compacts at high temperature is investigated with a view to simulating dimensional changes occurring during sintering of industrial components. Emphasis is laid on the anisotropy in both shrinkage and viscosity, which is induced by the prior pressing operation performed under magnetic field. Anisotropic shrinkage and viscosity are described according to an original approach based on an orthotropic thermo-elastic equation, which assumes an analogy between the thermal and elastic terms of this equation and the viscous and free sintering deformations. Finite element calculations using this constitutive equation are then carried out on two industrial parts. The comparison between the obtained numerical results and experimental measurements proves the relevance of the proposed model.
F. Toussaint, D. Bouvard, Ph. Tenaud, E. Di Marcello, Journal of Materials Processing Technology 147 (2004) 72-78
L0104 - Rare earth phosphate powders RePO4 . nH2O (Re=La, Ce or Y) II. Thermal behavior
The thermal behavior, thermostructural and morphological changes, of rare earth phosphate powders RePO4 . nH2O (Re=La, Ce or Y) was investigated up to 1500¡C using high temperature X-ray diffraction, FT-infrared and Raman spectroscopies and thermogravimetry coupled with differential thermal analysis. The hydration water of the compounds was zeolitic (for Re=La or Ce) or coordinated (for Re=Y) and was associated with a divariant or a monovariant equilibrium of dehydration, respectively. The high temperature anhydrous monoclinic phase LaPO4 or CePO4 formed irreversibly at about 750¡C after the total dehydration of the hexagonal hydrated structure while the dehydration of the monoclinic YPO4 . 2H2O phase began from about 190¡C with its simultaneous decomposition into tetragonal YPO4. A polytrioxophosphate secondary minor phase Re(PO3)3 resulting from adsorbed H3PO4 was formed at 950¡C and decomposed at 1350¡C. The particle morphology did not change with the temperature but grain coalescence occurred below 1000¡C.
S. Lucas, E. Champion, D. Bernache-Assollant, and G. Leroy, Journal of Solid State Chemistry 177 (2004) 1312-1320
L0103 - Ce0.8Gd0.2O(2-d) ceramics derived from commercial submicron-sized CeO2 and Gd2O3 powders for use as electrolytes in solid oxide fuel cells
Twenty percentage of Gd2O3-doped ceria solid solution has been prepared as an electrolyte for solid oxide fuel cells via the conventional mixed-oxide method from high-purity commercial CeO2 and Gd2O3. The solubility of Gd2O3 in CeO2 in the temperature range of 1300-1700¡C has been examined based on the measurements of the lattice parameter. It is found that the dissolution of Gd2O3 in CeO2 is completed at 1600¡C for 5 h. The addition of Gd2O3 increases sintering temperature, retards densification, and also depresses grain growth as compared with undoped CeO2. The sample sintered at 1550¡C for 5 h has the highest grain boundary conductivity, while the highest grain interior conductivity is achieved for the sample sintered at 1600¡C for 5 h. It is also observed that below 500¡C, the maximum total conductivity is exhibited by the former sample, but above 500¡C, for the latter one.
J. Ma, T.S. Zhang, L.B. Kong, P. Hing, S.H. Chan, Journal of Power Sources 132 (2004) 71-76
L0102 - Increasing elastic modulus, strength and CTE of AZ91 by reinforcing pure magnesium with elemental copper
Heat-treatable AZ91 and 3.9 vol.% copper particulate reinforced magnesium composite was synthesized using an innovative disintegrated melt deposition (DMD) technique followed by hot extrusion. Microstructural characterization of the composite material revealed retention and uniform distribution of reinforcement with defect free interface with the matrix. Physical properties characterization revealed improved dimensional stability of composite when compared to AZ91. Mechanical properties characterization revealed an increase in average values of modulus, 0.2% yield strength and ultimate tensile strength of un-heat-treated composite when compared to T6 heat-treated AZ91 while the ductility was adversely affected. An attempt is made in the present study to compare the microstructural, physical and mechanical properties of Mg/Cup composite with that of the commercially used AZ91 alloy.
S.F. Hassan, K.F. Ho, M. Gupta, Materials Letters 58 (2004) 2143-2146
L0101 - Mullite phase formation in oxide mixtures in the presence of Y2O3, La2O3 and CeO2
The effect of oxides (Y2O3, La2O3, and CeO2), on phase formation of mullite, reaction sequence and microstructure evolution, in the mixtures of Al2O3 and SiO2, has been investigated. All three dopants showed a positive effect on the mullitization behavior, lowering the mullite formation temperature by about 100¡C. The improved mullitization behavior was attributed to the formation of the low-viscosity liquid phase due to the addition of dopants. The reaction sequence was different in the three doping cases. Two types of yttrium silicate were found in the samples doped with Y2O3, with one being favored at low temperature and another at high temperature. No reaction was observed between CeO2 and Al2O3 or SiO2, while La2O3 was not detected by the X-ray diffraction (XRD) measurement for all doping levels. The samples with La2O3 had the best densification behavior among the three doping cases, while the effect of CeO2 on densification was slightly better than that of Y2O3. The difference in the effects of the three oxides on the mullitization and densification behavior of the doped samples implied the difference in the characteristics of the low-viscosity glass phases formed at high temperatures.
L.B. Kong, T.S. Zhang, J. Ma, F. Boey, R.F. Zhang, Journal of Alloys and Compounds 372 (2004) 290-299
L0100 - Structure, nonstoichiometry and magnetic properties of the perovskites Sr(1-x)CaxMnO(3-d)
The structural, thermal and magnetic properties of the perovskite-type alkaline-earth manganites of the series Sr(1-x)CaxMnO(3-d) (0 < x < 1) were investigated. SrMnO(3-d) forms a hexagonal perovskite lattice and shows a first-order transformation to a highly defective cubic high-temperature modification. By substituting Ca for Sr (x > 0.25) the hexagonal perovskite is suppressed and a cubic (or orthorhombic) lattice becomes stabilized for all temperatures. For x = 0.5 and 0.75 cubic perovskites with a large nonstoichiometry (e.g., d = 0.25 for x = 0.5) are obtained at 1400¡C. The defective perovskites are prepared by either quenching from high temperature or by cooling in an inert atmosphere. The oxygen vacancies are easily filled by subsequent reoxidation at low temperature (400-600¡C) and stoichiometric samples are obtained. Orthorhombic perovskites are formed at T < 1200¡C with the nonstoichiometry d increasing with increasing temperature (e.g., d = 0.06 at 1000¡C and d = 0.14 at 1200¡C for x = 0.5). Slow cooling in air results in almost complete reoxidation (d = 0). CaMnO(3-d) is an orthorhombic perovskite with a large range of nonstoichiometry (0 < d < 0.30). The cubic to hexagonal phase transformation of the Sr-rich samples is accompanied by a large expansion of the lattice that is reduced by Ca substitution. The Ca/Sr-manganites are antiferromagnets with TN of 170 K for x = 0.5 and d = 0.02 and 120 K for x = 1 and d = 0.05.
J. Tpfer, U. Pippardt, I. Voigt, R. Kriegel, Solid State Sciences 6 (2004) 647-654
L0099 - Ductility improvement of Ni-added molybdenum compacts through the addition of Cu and Fe powders
The sintered density of molybdenum can be significantly improved through the addition of a small amount of nickel. However, such addition impairs the ductility due to the formation of a NiMo intermetallic compound at the grain boundaries. This makes the plastic deformation process, such as rolling, drawing, and forging, impossible. This study shows that when copper is added, the sintered density can be further increased, but, not the ductility. This ductility problem of the Mo-Ni-Cu system can be improved when a small amount of iron is added and when the total amount of the alloying Ni, Cu, and Fe is over 6wt%, such as in the Mo-4Ni- 1Cu-1Fe system. Such improvement is attributed to the elimination of the brittle NiMo compounds in the matrix.
K.S. Hwang, H.S. Huang, International Journal of Refractory Metals & Hard Materials 22 (2004) 185-191
L0098 - Correlation between densification rate and microstructural evolution for pure alpha alumina
Correlation between microstructural evolution and macroscopic measurements has been investigated on pure alpha alumina under non-isothermal conditions. The densification of different as-received and milled powders of alumina has been monitored during sintering. Densification rate curves as a function of relative density are sensitive to microstructure, such as initial parameters of microstructure (agglomeration, pore size, heterogeneities), and heating schedule (thermal pre-treatment, heating rate). Densifi- cation rate curves can be correlated with microstructural evolution during overall sintering and are expected to be a good help to choose raw materials.
D. Lance, F. Valdivieso, P. Goeuriot, Journal of the European Ceramic Society 24 (2004) 2749-2761
L0097 - Synthesis of fine La0.8Sr0.2MnO3 powder by different ways
La0.8Sr0.2MnO3 (LSMO) powders were successfully synthesized by three routes (sol-gel, spray dryer and conventional solid state method). The precursors were characterized by particle size analysis, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The sintering stage of all powders was also investigated by dilatometer. Finally, the sintered LSMO ceramics have been investigated magnetically and electrically in view to study the ferromagnetic-paramagnetic and/or metal-insulator transition. The magnetoresistance MR up to 42% above room temperature has been observed.
D. Grossin, J.G. Noudem, Solid State Sciences 6 (2004) 939-944
L0096 - Preparation of spherical zirconia powder in microemulsion system and its densification behavior
The water droplets in the microemulsion system of cyclohexane/water/TritonX-100/hexyl alcohol can act as the nano-reactors which solubilize zirconium oxychloride and ammonia separately. The precipitation reactions will take place in the confined spaces determined by the droplets size. The minute original reactors help us obtain nano-size spherical zirconia amorphous powder with uniform diameter distribution and weak aggregate. Such powder begins to crystallize at the temperature about 475¡C, and its shrinkage of densification will be elementarily finished from 1080 to 1280¡C. The powder is formed by dry pressing process. The 99% relative density and 100% tetragonal phase can be obtained when the green body is sintered at 1400¡C for 2 h.
T. Ma, Y. Huang, J. Yang, J. He, L. Zhao, Materials and Design 25 (2004) 515-519
L0095 - Effect of ZrO2 additions on sintering of SnO2-based ceramics
The effect of zirconia additions on sintering of CoO doped tin dioxide has been investigated in the temperature range 1100- 1250¡C. A first study showed that the substitution of tin by zirconium reduces significantly the volatilisation rate of SnO2 for temperatures greater than 1400¡C. It appeared that the zirconium content increase inhibits the densification kinetics of SnO2-based ceramics. Indeed, the relative density did not exceed 93% for a Zr content lower than 6 mol% in the Sn(1-x)ZrxO2 solid solution. This negative effect can be imputed to the elastic distortions caused by the introduction of Zr in the tin dioxide lattice. So, the diffusion rate of point defects such as oxygen or cobalt ions is lowered.
A. Ma"tre, D. Beyssen, R. Podor, Journal of the European Ceramic Society 24 (2004) 3111--3118
L0094 - Microstructural evolution of Y2O3 and MgAl2O4 ODS EUROFER steels during their elaboration by mechanical milling and hot isostatic pressing
Different ODS EUROFER steels reinforced with Y2O3 and MgAl2O4 were elaborated by mechanical milling and hot isostatic pressing. Good compromise between strength and ductility could be obtained but the impact properties remain low (especially for the Y2O3 ODS steel). The materials were structurally characterized at each step of the elaboration. During milling, the martensite laths of the steel are transformed into nano-metric ferritic grains and the Y2O3 oxides dissolve (but not the MgAl2O4 spinels). After the HIP, all the ODS steels remain ferritic with micrometric grains, surrounded by nano-metric grains for the Y2O3 ODS steels. The mechanisms in the Y2O3 ODS steels are complex: the Y2O3 oxides re-precipitate as nano-Y2O3 particles that impede a complete austenitization during the HIP. The quenchability of the ODS steels is modified by the milling process, the oxide nature and the oxide content. Eventually, the advantages and drawbacks of each oxide type are discussed.
C. Cayron, E. Rath, I. Chu, S. Launois, Journal of Nuclear Materials 335 (2004) 83-102
L0093 - Thermal stability and mechanical properties of a Zr-based bulk amorphous alloy
The thermal and mechanical properties of a Zr-Al-Cu-Ti-Ni bulk metallic glass were investigated. The glass transition and the crystallization were studied by calorimetry and X-ray diffraction. It was found that the crystallization occurred in two steps. The precipitating phases, and the activation energies were determined. It was established that the crystallization was controlled by the diffusion of the alloying Cu and Ni atoms. The creep behavior was investigated by indentation tests. The viscosity and the activation energy of the deformation process determined from indentation were in reasonable agreement with those obtained by compression tests.
D. Fatay, J. Gubicza, P. Szommer, J. Lendvai, M. Bltry, P. Guyot, Materials Science and Engineering A 387-389 (2004) 1001-1004
L0092 - Improvements in sintered density and dimensional stability of powder injection-molded 316L compacts by adjusting the alloying compositions
Powder injection molding is a process that provides advantages when making small parts with high density and complicated shapes. However, dimensional control of powder injection-molded stainless steel parts is difficult due to the presence of the liquid phase and the large amount of shrinkage that occurs during sintering. This study examines whether such a problem can be overcome through adjustments in the alloy composition and by making use of Thermo-Calc analysis. The results show that, with an increase in the molybdenum content up to the maximum limit according to existing specifications, a compact can be sintered to high densities without the presence of the liquid phase, while maintaining it in the dual-phase region of gamma + delta. In addition, dimensional control is improved. A slower heating rate is also found to be beneficial. These results are explained through dilatometric analysis and phase diagrams that are calculated using the Thermo-Calc program.
G.J. Shu, K.S. Hwang, Y.T. Pan, Acta Materialia 54 (2006) 1335-1342
L0091 - Studies of Fe-Co based perovskite cathodes with different A-site cations
Iron-cobalt based perovskite cathodes with different A-site cations ((Ln0.6Sr0.4)0.99Fe0.8Co0.2O(3-d), where Ln is La, Pr, Sm or Gd) have been synthesised, characterised by a powder XRD, dilatometry, 4-point DC conductivity measurements, and electrochemical impedance spectroscopy (EIS) on cone shaped electrodes. In addition to this scanning electron microscopy (SEM) was used to characterise the bars. XRD revealed that only the La-containing perovskite was hexagonal. The Pr and Sm perovskites were orthorhombic. The gadolinium-based perovskite was a two phase system consisting of an orthorhombic and a cubic perovskite phase. The thermal expansion coefficient (TEC) increased systematically with a decrease in the size of the A-site cation until the gadolinium-containing perovskite where the TEC decreases abruptly. The total electric conductivity was the highest for the La-based perovskite and the lowest for the Gd-based perovskite as determined by 4-point DC conductivity measurements on bars. A clear correlation between the size of the A-site cation and the electrochemical performance was revealed, as the area specific resistance (ASR) was the lowest for the compounds with the smallest A-site cation. This might be explained on the background of the creation of a two-phase structure with a unique microstructure when the size of the A-site cation is lowered, or that one of the phases has a high electro-catalytic activity towards the electrochemical reduction of oxygen.
K. Kammer, Solid State Ionics 177 (2006) 1047-1051
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