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A series of samples in the system Ni0.65Zn0.35CuxFe2−xO4 (x=0.0, 0.1, 0.2, 0.3, 0.4 and 0.5) were prepared by the usual ceramic technique. X-ray analysis showed that they were cubic spinel (single phase). Young's modulus, the dielectric loss and the change in capacitance under mechanical stress were measured for the samples. Young's modulus decreased with increasing Cu content. This is due to the fact that Cu2+ ions entered the lattice substitutionally for Fe3+ ions at the octahedral sites, creating lattice vacancies gave rise to lattice strain.

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Journal of Thermal Analysis and Calorimetry
Authors: M. Jiménez de Haro, L. Pérez Maqueda, E. Stepkowska, J. Ma Martínez, and J. Pérez-Rodríguez

Abstract  

Grinding and contact with water or salt solution increased the specific surface (ssa) but lowered the first dehydration effect (escaping up to 150C) and increased the second dehydration effect (150 to 500C). The dehydroxylation was moved to lower temperatures and was only ΔM(500-1100C)=3.70.3 % as compared to 5.5% in the parent vermiculite (V). Except ΔM(20-150C), the mass losses measured at the remaining T ranges, were consistent in the ground samples, thus the grinding for 2 min caused the homogenization of the crystal structure of vermiculite [ΔM(150-500C)=7.60.7%]. DTA curves after grinding and cation exchange indicate an important exothermal peak at 795-870C, its temperature depending on exchangeable cation. It indicates the formation of high temperature phases (enstatite, forsterite, spinel). The lowest temperature of the peak (795C) was observed in V-gr-Li, here lithium silicate was formed. The highest peak temperature (870C) was found in V-gr-K, where almost only forsterite developed. These exothermal peaks were very weak in unground V with various exchangeable cations.

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The high-temperature (950–1500°) changes in synthetic montmorillonite of relatively simple chemical composition, studied by X-ray diffraction analysis, infrared spectroscopy and electron microscopy, are described. It was found that this montmorillonite belongs to the Wyoming type and the high-temperature phases involve cristobalite, mullite, anorthite and spinel. Only mullite crystallized from this sample on heating for two hours at 1500°.

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Abstract  

The CO2 absorption properties and the microstructure of (Ba,Ca)(Fe,Mg)O3 - have been studied by TGA, XRD, and Mössbauer spectrometry. Paramagnetic doublets of FeIV and FeIII appeared in the Mössbauer spectra of cubic (Ba0.5Ca0.5)(Fe0.5Mg0.5)O3 - heated in CO2 up to 600 °C, and a pair of sextets of tetrahedral FeIII (Hin = 43 T) and octahedral FeIII (Hin = 51 T) were produced above 800 °C, and an additional sextet characteristic of FeIII in a spinel structure (Hin = 48 T) was observed at 1000 °C. On the other hand, a pair of sextets of tetrahedral and octahedral FeIII of the orthorhombic (Ca0.95Ba0.05)(Fe0.5Mg0.5)O3 - showed hardly any change after absorption of CO2. It is concluded that only a small portion of Mg entered the orthorhombic phase of (Ca0.95Ba0.05)(Fe,Mg)O3 - and Mg preferred the octahedral B site of the perovskite lattice. The excess Mg formed separate CaO-MgO mixed oxide, and the primary mechanism of CO2-trapping is the formation of CaMg(CO3)2.

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Abstract  

Perovskite oxides of composition (Sr1-xCax)(Fe0.5Co0.5)O3- were investigated for CO2 absorption properties and were proved to be useful as materials for CO2 absorption in the temperature range from 550 to 850 °C. The absorption rate of CO2 increased with Ca doping. The mechanical treatment of perovskite oxides for several minutes, especially for the oxides containing a small amount of Ca, was found to be effective for activating the oxides for CO2 absorption and for reducing the starting temperature of CO2 absorption by about 80 °C. However, it was not less effective to treat the oxides for a long time. The site distortion due to Sr and Ca ions at site A and the mixed valence states at site B were confirmed to be effective for CO2 absorption at high temperatures. During the absorption of CO2, a spinel compound was formed according to the following reaction: 2(Sr,Ca)(Fe,Co)O2.5 + CO2 (Sr,Ca)CO3 + (Sr,Ca)(Fe,Co)2O4.

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Abstract  

The purified bentonite parent clay, fraction ≤; 2 mm of montmorillonite type, has been pillared by various polyhydroxy cations, Al, AlFe and AlCu, using conventional pillaring methods. The thermal behavior of PILCs was investigated by combination of X-ray diffraction (XRD), thermal analysis (DTA, TG) and low temperature N2 adsorption/desorption (LTNA). Thermal stability of Al-, AlFe- and AlCu-PILC samples was estimated after isothermal pretreatment in static air on the temperatures 300, 500, 600 and 900C. Crucial structural changes were not registered up to 600C, but the fine changes in interlayer surrounding and porous/microporous structure being obvious at lower temperatures, depending on the nature of the second pillaring ion. AlFe-PILC showed higher thermal stability of the texture, the AlCu-PILC having lower values and lower thermal stability concerning both overall texture and micropore surface and volume. Poorer thermal stability of AlCu-PILC sample at higher temperatures was confirmed, the presence of Cu in the system contributing to complete destruction of aluminum silicate structure, by 'extracting' aluminum in stabile spinel form.

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Journal of Thermal Analysis and Calorimetry
Authors: D. Bhosale, N. Choudhari, S. Sawant, V. Patil, P. Kulkarni, and V. Kelkar

Abstract  

Homogeneous solid solution oxalates of Fe2+, Cu2+, Mg2+ and Zn2+ metals were prepared by co-precipitation from respective metal acetate solutions with oxalic acid solution. The thermogravimetric (TG) analysis of co-precipitated oxalate complexes with general formula MgxCu(0.50-x)Zn0.50Fe2(C2O4)3nH2O (x=0.00, 0.05, 0.10, 0.15, 0.20, 0.25, 0.30, 0.35, 0.40, 0.45, 0.50) were carried out by manual method in static air atmosphere. The total mass loss % and stepwise mass loss % values are in good agreement with theoretically calculated mass loss % values. The thermal decomposition of oxalate complexes occur at relatively lower temperatures (561 to 698 K). The lowering of decomposition temperatures may be attributed to earlier initiation of Fe2+ oxalate in oxalate complexes. At temperatures between 598–698 K the thermal decomposition of Cu-Mg-Zn-Fe solid solution oxalate complexes leads to formation of ferrites of spinel structure. After tampering at 873 and 1273 K, homogeneous ferrites arise, which is revealed from XRD studies.

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Abstract  

Thermal analysis complimented with evolved gas mass spectrometry has been applied to hydrotalcites containing carbonate prepared by coprecipitation and with varying divalent/trivalent cation ratios. The resulting materials were characterised by XRD, and TG/DTG to determine the stability of the hydrotalcites synthesised. Hydrotalcites of formula Mg4(Fe,Al)2(OH)12(CO3)·4H2O, Mg6(Fe,Al)2(OH)16(CO3)·5H2O, and Mg8(Fe,Al)2(OH)20(CO3)·8H2O were formed by intercalation with the carbonate anion as a function of the divalent/trivalent cationic ratio. XRD showed slight variations in the d-spacing between the hydrotalcites. The thermal decomposition of carbonate hydrotalcites consists of two decomposition steps between 300 and 400°C, attributed to the simultaneous dehydroxylation and decarbonation of the hydrotalcite lattice. Water loss ascribed to dehydroxylation occurs in two decomposition steps, where the first step is due to the partial dehydroxylation of the lattice, while the second step is due to the loss of water interacting with the interlayer anions. Dehydroxylation results in the collapse of the hydrotalcite structure to that of its corresponding metal oxides and spinels, including MgO, MgAl2O4, and MgFeAlO4.

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Abstract  

Kinetics of oxidation of Fe-Cr steel containing 25 wt.-percent Cr was studied as a function of temperature (1023–1173 K) for up to 480 h in flowing air, which corresponds to SOFC cathode environment operating conditions. The oxidation process was found to be a parabolic, suggesting that the diffusion of ionic defects in the scale is the slowest, rate determining step and it occurs predominantly by short-circuit diffusion paths. Comparison of the determined activation energy of oxidation of the studied steel with literature data indicates that at 1098–1173 K the chromia scale grows by the outward solid-state diffusion of chromium interstitials, whereas at 1023–1098 K — through a significant contribution of counter-current oxygen/chromium diffusion along Cr2O3 grain boundaries. The oxide scales were composed mainly of Cr2O3 with a continuous thin Mn1.5Cr1.5O4 spinel layer on top of the chromia scale. The oxidation test results on Fe-25Cr steel demonstrate the applicability of the commercial type DIN 50049 stainless steel as interconnect for SOFC.

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Comparative thermogravimetric and heat-flux DSC investigations of phase formations by heating of sinteractive powders, which were prepared by thermal decomposition of a NiCO3∶ MnCO3=1∶2 mixture and thermal decomposition of oxalate mixed crystals NiMn2(C2O4)3.6H2O, show the metastability of the defect spinel from the oxalate precursor and its high reactivity.

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