Perovskite solid solutions in the BaO-CuO-Y2O3-Nb2O5 system

Freeze dried complex carboxylates are highly reactive precursors for complex perovskite solid solutions in the system BaO-CuO-Y₂O₃-Nb₂O₅ On thermal decomposition of the amorphous precursors the formation of complex crystalline phases begins at 600 °C. In most cases the themodynamically controlled phase composition is reached after a reaction time of two hours at about 900 °C. Beginning from the perovskite compound Ba₂YNbO₆ a partial substitution of Y by Cu or by a combination 2/3 Cu,1/3 Nb leads to extended fields of solid solutions with cubic perovskite structure. Substitution according to Y_0,5xBa₂(Y_1-0,5xCu_xNb)O_6+x is limited to x ≤ 0,4. A compound LBa₂Cu₂NbO₈ (x=2), well characterized for L=La, does not exist for L=Y. The composition of solid solutions depends on the preparation conditions. There are some signs for an inhomogeneous distribution of B-cations in the cubic perovskites.     

Subsolidus phase relations in the Gd2O3-Rh2O3 system

The Gd₂O₃-Rh₂O₃ system is studied using the anneal-and-quench technique, X-ray powder diffraction, thermal analysis, and chemical analysis. A schematic subsolidus phase diagram is designed. One double oxide of composition GdRhO₃ is found to exist. It was characterized using some physicochemical methods.     

Synthesis, composition, and structure of sillenite-type solid solutions in the Bi2O3-SiO2-MnO2 system

Individual compounds and solid solutions are obtained under hydrothermal conditions in the Bi(2)O(3)-SiO(2)-MnO(2) system in the form of faceted crystals and epitaxial films on the Bi(24)Si(2)O(40) substrate. The crystals have the shape of a cube (for the molar ratio of the starting components Na(2)SiO(3)·9H(2)O:Mn(NO(3))(2)·6H(2)O > 1), a tetrahedron (for Na(2)SiO(3)·9H(2)O:Mn(NO(3))(2)·6H(2)O < 1), or a tetrahedron-cube combination (for Na(2)SiO(3)·9H(2)O:Mn(NO(3))(2)·6H(2)O = 1). Crystal-chemical analysis based on the data of single-crystal and powder X-ray diffraction, IR spectra, and the results of calculation of the local balance by the bond-valence method reveals formation of the Bi(24)(Si(4+),Mn(4+))(2)O(40) phases, which probably include Mn(5+) ions (epitaxial films), as well as the Bi(24)(Si(4+),Bi(3+),Mn(4+))(2)O(40) and Bi(24)(Si(4+),Mn(4+))(2)O(40) phases in the (1 - x)Bi(3+)(24)Si(4+)(2)O(40) - x(Bi(3+)(24)Mn(4+)(2)O(40)) system and the Bi(24)(Bi(3+),Mn(4+))(2)O(40) phase in the (1 - x)Bi(3+)(24)Bi(3+)(2)(O(39)?(1)) - x(Bi(3+)(24)Mn(4+)(2)O(40)) system. Precision X-ray diffraction studies of single crystals of the Bi(24)(Bi,Si,Mn)(2)O(40) general composition show that these sillenites crystallize in space group P23 and not I23 as the Bi(24)Si(2)O(40) phase. The dissymmetrization of sillenite phases is observed for the first time. It is explained by a kinetic (growth) phase transition of the order-disorder type due to population of a crystallographic site by atoms with different crystal-chemical properties and quasi-equilibrium conditions of crystal growth in the course of a hydrothermal synthesis below 400 °C at unequal molar amounts of the starting components in the batch.     

High-temperature phases of montmorillonite synthetized from the oxides SiO2-Al2O3-MgO-CaO

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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Zusammenfassung Die durch Röntgendiffraktionsanalyse, Infrarotspektroskopie und Elektronenmikroskopie untersuchten Hochtemperatur (950–1500°) — Änderungen in synthetischem Montmorillonit verhältnismässig einfacher chemischer Zusammensetzung werden beschrieben. Es wurde gefunden, daß dieser Montmorillonit dem Typ Wyoming angehört und, daß die Hochtemperaturphasen Cristobalit, Mullit, Anorthit und Spinell enthalten. Aus dieser Probe kristalliesierte bei zweistündigem Erhitzen auf 1500°C nur Mullit.

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, (950–1500°) . , , , , . 2 1500° .

     

Formation of solid phases in the ZrO2-SO3-KF-H2O system at 20°C

Conclusions Various fluorosulfatozirconates and fluorozirconates were crystallized, some for the first time, from solutions of the ZrO₂-SO₃-H₂O system upon the introduction of KF.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 5, pp. 967–972, May, 1982.     

Synthesis and properties of the TTA/Gd2O3: Eu3+ luminescent system

Journal of Sol-Gel Science and Technology - Hybrid materials based on lanthanide ions or lanthanide-doped nanostructured particles have received a lot of recent attention because organic ligands...     

Kinetics of Ruddlesden-Popper Phase Formation: III. Mechanism of Gd2SrAl2O7 Formation

Studies on phase formation in the system Gd₂O₃-SrO-Al₂O₃ in the range 900-1530°C showed that the synthesis of Gd₂SrAl₂O₇ occur by a mechanism differing from the mechanism of Ln₂SrAl₂O₇ formation (Ln = La, Nd, Sm), and the limiting stage is reaction between Gd₂O₃ and SrAl₂O₄.     

Effective synthesis of novel O-acetylated compounds over ZrO2-Al2O3 solid acid

The solid acids such as ZrO₂, Al₂O₃ and ZrO₂-Al₂O₃ containing different ZrO₂ loadings (10–80 mol%) were prepared by solution combustion method (SCM) and characterized for their total surface acidity by NH₃-TPD/n-butylamine back titration method and crystallinity by powder X-ray diffraction (PXRD) technique. These solid acids were evaluated for their catalytic activity in the synthesis of novel O-acetylated products from substituted phenols, pyridine alcohols and aryl alcohols with acetic anhydride (AA) as an acetylating agent. The reaction conditions were optimized by varying the catalyst, molar ratio of the reactants, reaction temperature and amount of the catalyst. All the solid acids used in this study exhibited good catalytic activity in the reaction. In particular, ZrO₂-Al₂O₃ containing 80 mol% of ZrO₂ was found to be highly active in the acetylation reaction with high yield of acetylated products. Triangular correlation between the surface acidity, crystallinity and catalytic activity of solid acids was observed. These solid acids were found to be reactivable and reusable.     

固体超强酸SO2-4/SnO2-Al2O3的红外光谱研究

以四氯化锡、硫酸铝为原料,氨水为沉淀剂,采用共沉淀法制得新型固体超强酸SO2-4/SnO2-Al2O3.采用FT-IR技术考察了金属元素摩尔比、焙烧温度、浸渍液以及掺杂稀土氧化物对该固体超强酸结构和性能的影响.FT-IR结果表明在该固体超强酸中,锡和硫酸根是以螯合和桥式两种方式配位结合,其中起催化活化作用的主要是和硫酸根以螯合双齿结合的锡;和SO2-4/ZrO2型超强酸相比,SO2-4/SnO2-Al2O3超强酸的硫酸根FT-IR特征吸收峰发生蓝移,显示出更强的酸性.锡铝摩尔比为9∶1、焙烧温度为773K、焙烧时间为3h时,制得的SO2-4/SnO2-Al2O3样品对酯化反应的催化性能最好.     

二乙醇胺-甘油-Na2O-SiO2-Al2O3-H2O系统中沸石的生成

在水热条件下,二乙醇胺(DEA)—甘油(GL)—Na_2O-SiO_2-Al_2O_3—H_2O反应混合物系统中可自发生成大晶粒(>50μm)的丝光沸石,ZSM-5,35,48及新沸石CF-2.。变反应混合物配比或同时使用晶种导向法,可在该系统中合成上述沸石纯相。变更系统中有机物(胺或醇)的种类,可以获得不同的结晶产物。     

Calorimetric Study of Interaction Between Oxygen and β-Al2O3, β-Al2O3+Au and β-Al2O3+Pt

In an attempt to improve the understanding of the electrochemical effects observed on an original potentiometric gas sensor, interactions of oxygen with the device were investigated. These calorimetric measurements have evidenced the existence of a weakly bounded endothermal oxygen species. Moreover these species may be regarded to be responsible for the electrical response developed by the sensor. Such results, which are in agreement with a previously proposed model, validate the underlying hypothesis and shed light on the role of oxygen in the sensor’s responses. This revised version was published online in August 2006 with corrections to the Cover Date.     

Sol-gel derived (LiCl)2-Al2O3-SiO2 thin film solid electrolyte

(LiCl)₂-Al₂O₃-SiO₂ thin film solid electrolyte was prepared by a sol-gel process with a spin coating technique. The thin film was studied by X-ray photoelectron spectroscopy (XPS) and ac impedance. The ionic conductivity of the solid electrolyte film is comparable to that of the bulk xerogel. The highest conductivity measured by ac impedance is 2.5×10^–4 S·cm^–1 at 300°C with E_a=0.75 eV.     

A search for new phases in the system Fe2O3-V2O5-WO3

Studies on the three-component system Fe₂O₃-V₂O₅-WO₃ have shown the occurrence of a new, compound with molecular formula FeVW₂O₁₀. Its X-ray characteristics and its melting temperature, 865±10 °C, have been established.

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Zusammenfassung Einleitende Untersuchungen am Dreikomponentensystem Fe₂O₃-V₂ O₅-WO₃ zeigten das Auftreten einer neuen, noch nicht publizierten Verbindung der Formel FeVW₂O₁₀. Die Verbindung wurde röntgenographisch beschrieben, ihr Schmelzpunkt beträgt 865 ±10°C.

     

γ-Al2O3表面原位合成Ni-Al-CO3LDHs研究

Ni-Al-CO₃LDHs/γ-Al₂O₃have been prepared using an in-situ synthesis technique. NH₃·H₂O was chosen as activation agent of Al on the γ-Al₂O₃surface as well as precipitant. Ni-Al-CO₃LDHs/γ-Al₂O₃was synthesized by controlling the reaction conditions such as temperature, concentration of Ni²⁺ and initial pH. The crystalline structure, chemical composition and porous structure were characterized by means of XRD, FT-IR, TG-DTA, ²⁷Al MAS-NMR and N₂ adsorption-desorption. The resulting sample of Ni-Al-CO₃LDHs/γ-Al₂O₃possesses higher specific area and narrower pore distribution, in which Ni-Al-CO₃LDHs are located on the surface of γ-Al₂O₃and share the same Al-O bonds with the γ-Al₂O₃lattice. Finally a possible structural model was proposed to account for the porous characters of Ni-Al-CO₃LDHs/γ-Al₂O₃.     

固体超强酸SO4^2-／SnO2-Al2O3的红外光谱研究

以四氯化锡、硫酸铝为原料，氨水为沉淀剂，采用共沉淀法制得新型固体超强酸SO4^2-／SnO2-Al2O3。采用FT-IR技术考察了金属元素摩尔比、焙烧温度、浸渍液以及掺杂稀土氧化物对该固体超强酸结构和性能的影响。兀：lR结果表明在该固体超强酸中，锡和硫酸根是以螯合和桥式两种方式配位结合，其中起催化活化作用的主要是和硫酸根以螯合双齿结合的锡；和SO4^2-／SnO2型超强酸相比，SO4^2-／SnO2-Al2O3超强酸的硫酸根FT-IR特征吸收峰发生蓝移，显示出更强的酸性。锡铝摩尔比为9：1、焙烧温度为773K、焙烧时间为3h时。制得的SO4^2-／SnO2-Al2O3样品对酯化反应的催化性能最好。     

Synthesis of ultrafine Gd2O3 nanoparticles inside single-wall carbon nanohorns

The large diameter of single-wall carbon nanohorns (SWNHs) allows various molecules to be easily incorporated in hollow nanospaces. In this report, we prove that the nanospaces of SWNHs even work as the chemical reaction field at high temperature; that is, Gd-acetate clusters inside SWNHs were transformed into ultrafine Gd(2)O(3) nanoparticles with their particle size retained even after heat-treatment at 700 degrees C. This indicates that the confinement of the Gd-acetate clusters in a deep potential well of the SWNH nanospaces prevented a migration to form larger particles, giving rise to ultrafine Gd(2)O(3) nanoparticles of 2.3 nm in average diameter, which is much smaller than the case without SWNHs. The Gd(2)O(3) nanoparticles thus obtained were demonstrated to be actually useful to the magnetic resonance imaging. We believe that the presented effectiveness of the inner hollow spaces of SWNHs, therefore, also those of the carbon nanotubes, for high-temperature chemical reactions should be highlighted, and that the thus produced novel nanomaterials are promising to expand the fields of nanoscience.