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peaks do not appear in the diffractograms. Trace amounts of spinel and cristobalite are obtained from thermal recrystallization. Quartz is present as an impurity in the Wyoming bentonite and after the amorphization of MONT its X-ray peak becomes very

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Abstract  

The chemistry, structure, and properties of spinel ferrites are largely governed by the method of preparation. The metal carboxylato-hydrazinate precursors are known to yield nanosized oxides at a comparatively lower temperature. In this study, we are reporting the synthesis of one such precursor, cobalt nickel ferrous fumarato-hydrazinate which decomposes autocatalytically to give cobalt nickel ferrite nanoparticles. The XRD study of this decomposed product confirms the formation of single-phase spinel, i.e., Co0.5Ni0.5Fe2O4. The thermal decomposition of the precursor has been studied by isothermal, thermogravimetric (TG), and differential scanning calorimetric (DSC) analysis. The precursor has also been characterized by FTIR, EDX, and chemical analysis, and its chemical composition has been determined as Co0.5Ni0.5Fe2(C4H2O4)3·6N2H4.

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In this study, thermogravimetric analysis (TG) testing is used to measure the mass loss of polished Al–6Zn–XMg (X = 0 and 2 mass%) alloy samples heated at 773 K for 6 h in dry air or nitrogen gas. The progressive development of thermally formed oxides on an Al–6Zn–XMg (X = 0 and 2 mass%) alloy as shown by X-ray diffractometer analyses is discussed. Zn-spinel and Mg-spinel are detected on the Al–6Zn and Al–6Zn–2Mg alloy samples, respectively, and then heated in the dry air atmosphere; AlN and Mg3N2 are detected in alloy samples heated in nitrogen gas. The chain reactions that cause the serrated change in the mass loss curve are proposed and discussed.

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Journal of Thermal Analysis and Calorimetry
Authors: F. Kovanda, V. Balek, V. Dorničák, P. Martinec, M. Mašláň, L. Bílková, D. Koloušek, and I. Bountseva

Abstract  

Thermal behaviour of synthetic pyroaurite-like anionic clay with molar ratio Mg/Fe=2 was studied in the range of 60-1100C during heating in air. TG/DTA coupled with evolved gas analysis, emanation thermal analysis (ETA), surface area measurements, XRD, IR and Mssbauer spectroscopy were used. Microstructure changes characterized by ETA were in a good agreement with the results of surface area measurements and other methods. After the thermal decomposition of the pyroaurite-like anionic clay, which took place mainly up to 400C, a predominantly amorphous mixture of oxides is formed. A gradual crystallization of MgO (periclase) and Fe2O3 (maghemite) was observed at 400-700C by XRD. The MgFe2O4 spinel and periclase were detected at 800-1100C. The spinel formation was also confirmed by Mssbauer spectroscopy.

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Abstract  

Spinel iron oxide (Fe3O4-γ-Fe2O3) particles were supported on microbeads of silica gel by the calcination of the silica gel base adsorbing citric acid and Fe3+ ions. The X-ray diffraction patterns and the57Fe Mössbauer spectra measured for the spinel iron oxide indicated that the particle size of the oxide was regulated by the mean pore diameter (4–82 nm) of the silica gel support employed. In the case of α-Fe2O3 particles prepared by using the same silica gel beads, it was revealed by the Mössbauer spectra and the electron micrographs that there were relatively large particles of the oxide on the surface of the beads, in addition to the particles in the silica gel micropores.

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Abstract  

The paper deals with the possible application of various methods to follow the course of reaction between zinc oxide and Fe(III) oxide with respect to various kinds of Fe(III) oxides used (Fe(III) pigments - red, yellow and black). Differential thermal analysis and chemical analysis can be recommended as the most suitable methods for following reactions leading to spinel formation. The possibilities of determining the activation energy of the studied processes are discussed. When Fe(III) red pigment is used as a reactant and therefore no reaction occurs except spinel formation, conductometric thermal analysis was found to be suitable and more sensitive for the evaluation of differences in reactivities. It has also been observed that the kind of Fe(III) pigment, due to its individual reactivity significantly affects the colouring properties of the final product (e.g., of the ceramic stain).

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Abstract  

DTA study of an Indian Kaolinite has been performed by varying packing density and rate of heating. Both these two parameters influence the intensities of both endothermic and exothermic peaks related to the dehydration, dehydroxylation and then crystallizations of Al-Si spinel, mullite and cristobalite phases. Significantly, the study reveals that mullitization takes place by two separate reactions as indicated by two exotherms in the 1200-1400C range of DTA trace.

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Abstract  

The mechanism of the thermal decomposition of Fe2(SO4)3 in air has been studied at different temperatures (520-700 °C) using mainly 57Fe Mössbauer spectroscopy. Iron(III) oxides with corundum (), bixbyite (), spinel () and orthorhombic () structures were identified as solid products of this conversion. A significant influence of the heating temperature on the decomposition mechanism and on the phase composition of reaction products was found.

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Abstract  

The thermal decomposition kinetics of nickel ferrite (NiFe2O4) precursor prepared using egg white solution route in dynamical air atmosphere was studied by means of TG with different heating rates. The activation energy (E α) values of one reaction process were estimated using the methods of Flynn–Wall–Ozawa (FWO) and Kissinger–Akahira–Sunose (KAS), which were found to be consistent. The dependent activation energies on extent of conversions of the decomposition reaction indicate “multi-step” processes. XRD, SEM and FTIR showed that the synthesized NiFe2O4 precursor after calcination at 773 K has a pure spinel phase, having particle sizes of ~54 ± 29 nm.

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Abstract  

The thermal decompositions of hydrotalcites with hexacyanoferrate(II) and hexacyanoferrate(III) in the interlayer have been studied using thermogravimetry combined with mass spectrometry. X-ray diffraction shows the hydrotalcites have a d(003) spacing of 11.1 and 10.9 which compares with a d-spacing of 7.9 and 7.98 for the hydrotalcite with carbonate or sulphate in the interlayer. XRD was also used to determine the products of the thermal decomposition. For the hydrotalcite decomposition the products were MgO, Fe2O3 and a spinel MgAl2O4. Dehydration and dehydroxylation take place in three steps each and the loss of cyanide ions in two steps.

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