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Abstract  

Thermogravimetric analysis was used in order to study the reduction in air of submicronic powders of Co3−xMnxO4 spinels, with 0 ≤ x ≤ 1. For x = 0 (i.e. Co3O4), cation reduction occurred in a single step. It involved the CoIII ions at the octahedral sites, which were reduced to Co2+ on producing CoO. For 0 < x ≤ 1, the reduction occurred in two stages at increasing temperature with increasing amounts of manganese. The first step corresponded to the reduction of octahedral CoIII ions and the second was attributed to the reduction of octahedral Mn4+ ions to Mn3+. From the individual weight losses and the electrical neutrality of the lattice, the CoIII and Mn4+ ion concentrations were calculated. The distribution of cobalt and manganese ions present on each crystallographic site of the spinel was determined. In contrast to most previous studies that took into account either CoIII and Mn3+ or Co2+, CoIII and Mn4+ only, our thermal analysis study showed that Co2+/CoIII and Mn3+/Mn4+ pairs occupy the octahedral sites. These results were used to explain the resistivity measurements carried out on dense ceramics prepared from our powders sintered at low temperature (700–750 °C) in a Spark Plasma Sintering apparatus.

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A series of samples of the system Ni0.65Zn0.35CuxFe2−xO4 (x=0, 0.1, 0.2, 0.3, 0.4, 0.5 and 0.6) are prepared by the usual ceramic technique. X-ray analysis shows that they are cubic spinel (single phase). The lattice parameter, theoretical density (D x), bulk density (D) and the porosity (P) are measured for the samples. The vacancy concentration of oxygen is an important parameter in the sintering process of spinel ferrites. The decrease in the population of Fe3+ ion in the octahedral sites with the introduction of Cu2+ results in the decrease of lattice parameter. The DTA tracing shows a strong exothermic peak at 90°C.

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Abstract  

Synthesis of the green spinel pigment Co0.46Zn0.55(Ti0.064Cr0.91)2O4 by a novel two-step method of preparation have been investigated. Inorganic pigments are almost always prepared by a solid state reaction. It is classical ceramic method which used oxides, hydroxides or carbonates as precursors. The reaction is performed at temperature higher than 1300C and an agent of mineralization is usually present. The presented novel method of preparation decreases the calcining temperature necessary for reaching of bright and clear hue of the pigments prepared. Main attention was focused on the influence of two types of titanium raw materials on the temperature region of the spinel structure formation and on the colour properties of the pigments. The mixture of precursors with TiO2 gives a one-phase system when calcining at 1100C but the colour properties are more interesting at 1150C. Thermal stability of this pigment is limited by temperature 1300C. This temperature is connected with partial oxidation of Cr(III) to Cr(VI). Thermal analysis provided the first information about the temperature region of the pigment formation and determined the thermal stability of pigment.

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Nanoscale spinel ferrites prepared by mechanochemical route

Thermal stability and size dependent magnetic properties

Journal of Thermal Analysis and Calorimetry
Authors: V. Šepelák, P. Heitjans, and K. Becker

Abstract  

Among the many types of preparation and processing techniques, the nonconventional mechanochemical route has been recognized as a powerful method for the production of novel, high-performance, and low-cost nanomaterials. Because of their small constituent sizes and disordered structural state, nanoscale materials prepared by mechanochemical route are inherently unstable with respect to structural changes at elevated temperatures. Taking into account the considerable relevance of the thermal stability of nanoscale complex oxides to nanoscience and nanotechnology, in the present work, results on the response of mechanochemically prepared MgFe2O4 and NiFe2O4 to changes in temperature will be presented. Several interesting features are involved in the work, e.g., a relaxation of the mechanically induced cation distribution towards its equilibrium configuration, a disappearance of the superparamagnetism on heating, an increase of both the saturation magnetization and the Néel temperature with increasing particle size, and a core-shell structure of nanoparticles.

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The newly discovered crustal xenoliths from Miocene andesites in the Mátra Mts (Northeast Hungary) were classified into three petrographic types. Type 1 is a garnetiferous, plagioclase-rich cumulate rock, presumed to originate from the felsic portion of the nearby Szarvaskõ-Darnó mafic igneous complex. The almandine-rich garnet has been inferred to be of granulite facies origin. Garnet - orthopyroxene geothermobarometry on the orthopyroxene - plagioclase corona structure around it indicates a later high temperature (800-950 °C) low pressure (3-4 kbar) retrogression event. Type 2 is also plagioclase-rich cumulate rock with contact metamorphic assemblage containing spinel, corundum and andalusite, which crystallized in the course of dehydration reactions of biotite and/or smectite in hornblende hornfels to sanidinite facies conditions. Type 3 is microsyenite, which contains abundant anorthoclase and minor amount of Na- and K-rich kaersutitic-barkevikitic amphibole.

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Journal of Thermal Analysis and Calorimetry
Authors: V. Ramírez-Valle, M. Jiménez de Haro, M. Avilés, L. Pérez-Maqueda, A. Durán, J. Pascual, and J. Pérez-Rodríguez

Abstract  

Static and dynamic heating of vermiculite samples from Santa Olalla, Huelva, Spain, saturated with different cations, i.e. Na+, Cs+, NH4 +, Mg2+, Ca2+, Ba2+ and Al3+, have been studied. The characterization of the phases formed during heating has been carried out by X-ray diffraction. The phases formed depend on the cation present in the interlamellar position and the heating process. The phases identified in the vermiculite samples saturated with different cations and heated at different temperatures are the following: enstatite, forsterite, spinel, cordierite, anorthite, pollucite, nepheline, coesite, celsian and others various mixed silicates; also some dehydrated and amorphous phases have been observed. On static heating, at the maximum temperature reached in this work, the phases formed appear mixed with a glassy phase.

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Journal of Thermal Analysis and Calorimetry
Authors: M. R. S. Silva, S. C. Souza, I. M. G. Santos, M. R. Cassia-Santos, L. E. B. Soledade, A. G. Souza, S. J. G. Lima, and E. Longo
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Journal of Thermal Analysis and Calorimetry
Authors: S. C. Souza, M. A. F. Souza, S. J. G. Lima, M. R. Cassia-Santos, V. J. Fernandes Jr., L. E. B. Soledade, E. Longo, A. G. Souza, and I. M. G. Santos
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