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281.
Andrzej Mianowski Izabela Baraniec-Mazurek Rafał Bigda 《Journal of Thermal Analysis and Calorimetry》2012,107(3):1155-1165
For dehydration of CaC2O4·H2O and thermal dissociation of CaCO3 carried out in Mettler Toledo TGA/SDTA-851e/STARe thermobalance similar experimental conditions was applied: 9–10 heating rates, q = 0.2, 0.5, 1, 2, 3, 6, 12, 24, 30, and 36 K min−1, for sample mass 10 mg, in nitrogen atmosphere (100 ml min−1) and in Al2O3 crucibles (70 μl). There were analyzed changes of typical TGA quantities, i.e., T, TG and DTG in the form of the relative rate of reaction/process intended to be analyzed on-line by formula (10). For comparative purposes, the relationship between experimental and equilibrium conversion degrees was used (for P = Pominus P = P^{{ominus}} ). It was found that the solid phase decomposition proceeds in quasi-equilibrium state and enthalpy of reaction is easily “obscured” by activation energy. For small stoichiometric coefficients on gas phase side (here: ν = 1) discussed decomposition processes have typical features of phenomena analyzable by known thermokinetic methods. 相似文献
282.
Cheng-Fang Qiao Qing Wei Zheng-Qiang Xia Chun-Sheng Zhou San-Ping Chen 《Journal of Thermal Analysis and Calorimetry》2012,107(2):527-533
Six lanthanide compounds [Ln(H2O)9](m-BDTH)3·9(H2O) where Ln = La (1), and [Ln(H2O)8](m-BDTH)3·9(H2O) (m-BDTH2 = 1,3-benzeneditetrazol-5-yl) where Ln = Lu (2), Yb (3), Er (4), Ho (5) and Y (6) were hydrothermally synthesized and characterized by elemental analyses, infrared spectra, powder X-ray diffraction (PXRD) and X-ray single crystal diffraction. PXRD indicates that 2–6 are isomorphous. Structural analyses reveal that 1 is coordinated by nine water molecules forming a capped-square antiprism, while 2–6 are coordinated by eight water molecules forming a simple square antiprismatic geometry. Effects of water molecules on thermal stability were also discussed by thermogravimetric (TG), DSC, and PXRD under different temperatures. TG analyses suggest that 1 loses lattice and coordinated water molecules with no diacritical boundary, and 6 removes lattice water molecules first and then coordinated water molecules. DSC and PXRD further confirm the consequence. 相似文献
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Molecular dynamics simulations of solid state recrystallization and grain growth in iron nanoparticles containing 1436 atoms were carried out. During the period of relaxation of supercooled liquid drops and during thermal annealing of the solids they froze to, changes in disorder were followed by monitoring changes in energy and the migration of grain boundaries. All 27 polycrystalline nanoparticles, which were generated with different grain boundaries, were observed to recystallize into single crystals during annealing. Larger grains consumed the smaller ones. In particular, two sets of solid particles, designated as A and B, each with two grains, were treated to generate 18 members of each set with different thermal histories. This provided small ensembles (of 18 members each) from which rates at which the larger grain engulfed the smaller one, could be determined. The rate was higher, the smaller the degree of misorientation between the grains, a result contrary to the general rule based on published experiments, but the reason was clear. Crystal A, which happened to have a somewhat lower angle of misorientation, also had a higher population of defects, as confirmed by its higher energy. Accordingly, its driving force to recrystallize was greater. Although the mechanism of recrystallization is commonly called nucleation, our results, which probe the system on an atomic scale, were not able to identify nuclei unequivocally. By contrast, our technique can and does reveal nuclei in the freezing of liquids and in transformations from one solid phase to another. An alternative rationale for a nucleation-like process in our results is proposed. 相似文献
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