High-temperature X-ray diffraction studies of the formation of V?Mo?O catalyst

High-temperature X-ray diffraction analysis in the temperature range of 553–823 K was used to study the formation and the region of thermal stability of VMo₃O₁₁ being an active component of the V–Mo–O catalyst for acrolein oxidation to acrylic acid.

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553–823 K VMo₃O₁₁, V-Mo-O .

     

Solid-state reactions in Y2O3:3Al2O3:4B2O3 system studied by FTIR spectroscopy and X-ray diffraction

In the Y₂O₃:3Al₂O₃:4B₂O₃ system infrared absorption spectroscopy and X-ray diffraction have been used to study the solid-state reactions in the 600–1300°C temperature range. The expected YAl₃(BO₃)₄ formation (whose optimum temperature is at about 1150°C) was proceeded and accompanied by the appearance of YBO₃ and Al₄B₂O₉ intermediate phases. At higher temperatures the Al₁₈B₄O₃₃ phase was also identified with both methods. Based on these results, some chemical reactions were suggested.     

Structural characterization of glassy phases in the system Na2O-Ga2O3-P2O5 by MAS-NMR, EXAFS and vibrational spectroscopy. I. Cations coordination

The cationic coordinations of phosphate based gallium sodium glasses in the system Na2O-Ga2O3-P2O5 have been studied by several techniques (71Ga and 23Na MAS-NMR, EXAFS and vibrational spectroscopies) in order to study the relationship between the structure and the chemical composition. We found that three different environments are available for the gallium ions while it is very difficult to get accurate information on the sodium coordinations. Our data show that in orthophosphate glasses, gallium is mainly tetrahedral but when the mean phosphate chain length increases, its coordination becomes more and more octahedral. In these glassy structure, it becomes then possible to dissolve large amounts of typically octahedral cations like Fe3+ or Cr3+.     

X-ray spectral study on valency-electron distributions in compounds in the V2O5-MoO3 system

Measurements have been made on Mo L_{2, 15} and V K_"5 x-ray emission spectra for V₂O₅-MoO₃ compounds. There is a relationship between the Mo L_2,15 characteristics and the population in the 4d-like molybdenum band. That 4d band for molybdenum in V₂O₅-MoO₃ has an appreciable electron density, which decreases as the molybdenum concentration increases. A model has been proposed for the electronic structures in these compounds, in which the valency d electrons are delocalized between the molybdenum and vanadium atoms.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 24, No. 3, pp. 305–311, May–June, 1988.     

Phase equilibria and solid solution relationships in the La2O3-TiO2-ZrO2 system

In the ternary La₂O₃-TiO₂-ZrO₂ system the subsolidus phase relations at 1350 °C were determined using X-ray diffraction, scanning electron microscopy end energy dispersive X-ray analysis. The collected results are presented in the form of a phase diagram. In the equilibrium state there are 7 ternary and 5 binary compatible subsystems. In the system TiO₂ss, ZrO₂ss, ZrTiO₄ss, La₂Zr₂O₇ss and La₂O₃ss solid solutions were confirmed and La₄Ti₉O₂ss and La₂Ti₂O₇ss solid solutions were identified. The addition of ZrO₂ does not stabilize the La_2/3TiO₃ perovskite compound, nor the addition of TiO₂ a highly temperature stable compound La_2/3ZrO₃.     

Time-resolved X-ray diffraction microprobe studies of the conversion of cellulose I to ethylenediamine-cellulose I

Structural changes during the treatment of films of highly crystalline microfibers of Cladophora cellulose with ethylenediamine (EDA) have been studied by time-resolved X-ray microprobe diffraction methods. As EDA penetrates the sample and converts cellulose I to EDA-cellulose I, the measured profile widths of reflections reveal changes in the shapes and average dimensions of cellulose I and EDA-cellulose I crystals. The (200) direction of cellulose I is most resistant to EDA penetration, with EDA penetrating most effectively at the hydrophilic edges of the hydrogen bonded sheets of cellulose chains. Most of the cellulose chains in the initial crystals of cellulose I are incorporated into crystals of EDA-cellulose I. The size of the emerging EDA-cellulose I crystals is limited to about half of their size in cellulose I, most likely due to strains introduced by the penetration of EDA molecules. There is no evidence of any gradual structural transition from cellulose I to EDA-cellulose I involving a continuously changing intermediate phase. Rather, the results point to a rapid transition to EDA-cellulose I in regions of the microfibrils that have been penetrated by EDA.     

X-ray powder diffraction and electron microscopic studies of the ZnTe-CdSe system

Substitutional solid solutions in the ZnTe-CdSe system were synthesized by isothermal diffusion. Within the composition range 100-68 mol % ZnTe, they crystallize in the cubic sphalerite structure; and at ZnTe contents below 26 mol %, in the wurtzite hexagonal structure. The cubic-to-hexagonal structure transition occurs within the composition range 26–68 mol % ZnTe. The atomic concentrations of chemical elements on the oxidized surface of grains of the solid solutions and in their bulk differ. X-ray powder diffraction and electron microscopic studies showed that, with decreasing specific geometric surface area of grains, the average sizes of coherent scattering regions increase.     

Structural studies coupling X-ray diffraction and high-energy X-ray scattering in the UO2(2+)-HBr(aq) system

The structural chemistry of uranium(VI) in concentrated aqueous hydrobromic acid solutions was investigated using both single crystal X-ray diffraction and synchrotron-based high-energy X-ray scattering (HEXS) to reveal the structure of the uranium(VI) complexes in solution prior to crystallization. The crystal structures of a series of uranyl tetrabromide salts are reported, including Cs(2)UO(2)Br(4), Rb(2)UO(2)Br(4)·2H(2)O, K(2)UO(2)Br(4)·2H(2)O, and (NH(4))(2)UO(2)Br(4)·2H(2)O, as well as a molecular dimer of uranium(VI), (UO(2))(2)(OH)(2)Br(2)(H(2)O)(4). Limited correspondence exists between the structures observed in the solid state and those in solution. Quantitative analysis of the HEXS data show an average U-Br coordination number of 1.9(2) in solution, in contrast to the U-Br coordination number of 4 in the solid salts.     

Synthesis and X-ray diffraction study of Tm M 3 II Fe5O12 (MII = Ca, Sr, Ba) compounds

Double ferrites were synthesized by solid-phase annealing from thulium and iron oxides and alkaline-earth carbonates for the first time. Their symmetry systems and unit cell parameters were determined by X-ray diffraction analysis.     

The effects of La2O3 on the early stages of crystallization for MgO-Al2O3-SiO2-TiO2-La2O3 glass-ceramics

The early stages of crystallization for MgO-Al₂O₃-SiO₂-TiO₂-La₂O₃ glasses with different La₂O₃ concentrations were studied by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The glass transition temperature (Tg) of the glass decreases at first and then increases again with increasing La₂O₃ concentration. This indicates that the structure of the glass becomes weaker at first and then stronger again. Lanthanum acts in glasses as network modifier and will usually decrease the network connectivity of the glass structure. Nevertheless, if the La₂O₃ concentration is high enough, the oxygen and other ions start to agglomerate around La, resulting in a more closely packed structure. Heat-treatment of the sample with x = 0.1 at 770–810 °C results in the precipitation of a droplet phase with higher mean atomic weight embedded in a matrix with lower mean atomic weight. The initial crystalline phase magnesium aluminum titanate (MAT) precipitates from the droplet phase. Nevertheless, for the sample with x = 0.4, dendrite-like structure could be observed after heat-treatment of the glass at 810 °C. Furthermore, the crystalline phase first precipitated is the lanthanum containing perrierite, which could be attributed to the rearrangement of the glass structure as an effect of La³⁺ incorporation.     

Fe2O3—TiO2—K2O复合氧化物体系结构与湿敏性能

Ｆｅ２Ｏ３┐ＴｉＯ２┐Ｋ２Ｏ复合氧化物体系结构与湿敏性能储向峰刘杏芹＊王弘（中国科学技术大学材料科学与工程系合肥２３００２６）关键词Ｆｅ２Ｏ３－ＴｉＯ２－Ｋ２Ｏ，复合氧化物，湿度传感器１９９７－０４－３０收稿，１９９７－０９－２９修回Ｆｅ２Ｏ３是一种...     

The effect of calcination on the surface properties of the systems Al2O3-TiO2, SiO2-Al2O3, and SiO2-TiO2 prepared from metal alkoxides

Summary The effect of calcining temperature on the surface properties of the systems Al₂O₃-TiO₂, SiO₂-Al₂O₃, and SiO₂-TiO₂ prepared by co-hydrolysis of the corresponding metal alkoxide mixtures was studied from the crystal structure, the specific surface area, the heat of immersion in water and the surface acidity.Generally, the crystal growth of the systems accelerates with the rise of temperature of calcination. The specific surface area diminishes markedly with the rise of temperature of calcination, while the surface acidity remains almost constant. But the heat of immersion depends on the composition of the systems.

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Zusammenfassung Die Systeme Al₂O₃-TiO₂, SiO₂-Al₂O₃ und SiO₂-TiO₂ wurden durch die Hydrolyse der korrespondierenden Metallalkoxyde hergestellt. Von den Systemen wurden die spezifische Oberfläche, die Kristallstruktur, die Benetzungswärme in Wasser und das Oberflächen-p_H in Abhängigkeit von der Glühtemperatur gemessen.Im allgemeinen wird das Kristallwachstum mit der Erhöhung der Glühtemperatur beschleunigt und die spezifische Oberfläche vermindert. Hingegen ist der Oberflächen-p_H-Wert mit der Erhöhung der Glühtemperatur fast unveränderlich. Aber die Benetzungswärme hängt von der Komposition der Systeme ab.