Selective Propargylation of Carbonyl Compounds and Imines with Barium Reagents

A Barbier‐type regioselective propargylation of aldehydes and ketones with (3‐bromobut‐1‐ynyl)trimethylsilane has been achieved using reactive barium as a low‐valent metal in THF. Especially in the case of ketones, the corresponding homopropargylic alcohols form almost exclusively. In the reaction of α,β‐unsaturated carbonyl compounds, only 1,2‐adducts have been observed. This method is also applicable to propargylation of imines, and the corresponding homopropargylic amines are obtained regiospecifically in good yields with diastereomeric ratios of up to 87:13.     

Bi12TiO20纳米粉体的制备及其光吸收特性研究

以钛酸四丁酯和硝酸铋为原料 ,利用化学溶液分解法制备了Bi12 TiO2 0 纳米多晶粉体 .采用XRD和TEM对其结构和形貌进行了表征 .结合热重 差热 (TG DTA)分析 ,探讨了Bi12 TiO2 0 晶相的形成机理 .通过UV Vis漫反射谱的测定 ,研究了Bi12 TiO2 0 纳米晶粉体的光吸收特性 .结果显示 ,从组成为化学计量比的前驱液中可以很容易制得纯Bi12 TiO2 0 纳米晶粉体 ,该Bi12 TiO2 0 纳米晶粉体呈现了在很宽的波长范围内 (5 6 0～ 385nm )对光的吸收的特性 .     

Effect of post-metallization annealing on the ferroelectric properties of sol-gel derived PZT thin films

A series of monolithic Pt-PZT-Pt capacitors was prepared based on sol-gel derived PZT 53/47 films fired to 700 C. After deposition of top Pt electrodes, the capacitors were subjected to post-metallization annealing (PMA) temperatures of 100 C to 700 C. Dielectric and ferroelectric (FE) characterizations were performed. Increasing the PMA temperature produced lower values of spontaneous and remanent polarizations, dielectric constant and leakage currents. The observations are correlated with a proposed FE capacitor model.     

Inorganic Sol-Gel Preparation of Medium Sized Microparticles of Li2TiO3 from TiCl4 as Tritium Breeding Material for Fusion Reactors

Microspheres of Li₂TiO₃ were fabricated by a classical, inorganic sol-gel process from commercially available TiCl₄. Elaborated process consists of the following main steps: (1) dissolving of TiCl₄ in concentrated aqueous HCl and addition of LiOH; (2) formation of sol emulsion in 2-ethylhexanol-1 containing the surfactant SPAN-80 (EH); (3) gelation of emulsion drops by extraction of water with partially dehydrated EH; (4) impregnation of gel to Li:Ti molar ratio MR = 2; (5) thermal treatment at 1200°C in order to receive chloride free product. This temperature can be significantly lowered (to 750°C) by dechlorination starting solution TiCl₄ by chemical treatment of the with nitric acid to form of nitrate-stabilized titania sols. Tritium release from sol-gel made Li₂TiO₃ microspheres were found very close to that observed for other traditional materials, however for the first sample process starts slightly earlier.     

掺杂SrTiO3体系上甲烷氧化偶联反应的研究—活性氧物种的作用

本文采用循环氧化还原法,脉冲反应及TPD等实验手段对钙钛矿型氧化物掺杂SrTiO_3体系上甲烷氧化偶联反应中的活性氧物种的作用进行了研究.结果表明,催化剂由于掺杂产生的未被充分还原的氧物种(O~(α-)(0<α<2)是活化甲烷并促使其发生偶联反应的主要的活性中心,而表面晶格氧(O_L~(2-))则主要使甲烷深度氧化;消耗掉的未被充分还原的氧或晶格氧可以在高温下氧气氛中氧化复原.对于掺杂的SrTiO_3样品,体相中的氧在惰性气氛或还原气氛中可以向表面扩散.吸附氧可能不直接与甲烷作用而主要通过催化剂表面活性氧物种(O~(α-)或O_L~(2-))而起作用.     

棒状钡铁氧体的反相微乳法制备

A rodlike barium ferrite precursor with an average size of 0.72～19.6 μm and aspect ratio of 2.6～8.3 has been successfully prepared in an inverse microemulsion consisting of isooctane, cetanyl trimethyl ammonium bromide (CTAB), n-C₄H₉OH and water with ammonia and ammonium oxalate as precipitants. On sintering at 780(C, the rodlike precursor particles could be transformed into rodlike particles of barium ferrite(BaFe₁₂O₁₉) with the average size and aspect ratio of 0.69～18.2 μm and 2.3～5.8, respectively. The effect of volume ratio of aqueous phase to oleic phase, the starting concentrations of metal ions and the starting concentration ratios of metal ions to precipitants were investigated.     

Darstellung und Kristallstruktur von TICu[CuO2]

Investigations on Electronically Conducting Oxide Systems. XVI. Solid Solutions and Conductivity in the System MgTi₂O₅? Ti₃O₅ Solid solution formation is reported for the system Mg_1–xTi_2–x^IVTi_2x^IIIO₅. With increasing x there is at room temperature a transition from the orthorhombic pseudobrookite structure to the monoclinic low-temperature modification of Ti₃O₅. The X-ray diffraction pattern results are supported by DSC measurements, electrical and magnetic investigations. The tendency of Ti? Ti pair formation in the low-temperature Ti₃O₅ structure is accompanied by a drop of the activation energy for electrical conductivity and a decreasing susceptibility at high Ti^III concentrations.     

Thermal and structure analysis of FeSO4·H2O-BaO2 mixtures

Investigations on the thermal decomposition of FeSO₄·H₂O-BaO₂ mixtures were carried out under isothermal conditions by using simultaneously solid electrolyte cell (EMF-method). Evoked interactions producing oxygen in the temperature range 553-673 K were established by means of a solid electrolyte oxygen analyzer. Based on Mössbauer spectroscopy data and X-ray analysis it was proved that these reactions were associated with the release of oxygen from barium peroxide, oxidation of ferrosulphate-monohydrate to FeOHSO₄, and formation of barium ferrites such as BaFe₂O₄ and BaFe₁₂O₁₉.     

螯合型二甘醇钛酸酯的合成及其催化性能研究

报导了两种新的螯合型二甘醇钛酸酯的合成方法，进行了ＩＲ和ＵＶ鉴定，并作为酯化反应催化剂催化合成了邻苯二甲酸二辛酯。研究了酯化反应转化率与反应时间、反应温度及催化剂用量的关系，探讨了催化剂结构与催化性能的关系。     

Heterometallic lead-titanium oxyalkoxide precursors to lead titanate thin films

Two lead titanium oxyalkoxides with composition Pb₂Ti₄O₂(O₂CCH₃)₂(OC₂H₅)₁₄ and Pb₂Ti₂O₂(O₂CCH₃)₂(OCH(CH₃)₂)₈ have been isolated and characterised by elemental analysis, IR, ²⁰⁷Pb NMR and molecular weight measurements. X-ray structural analysis of the 1:2 complex confirmed the presence of two Pb₂Ti₂O units which are linked by a common Pb···Pb edge and are held together by alkoxide and acetate bridges. The acetate groups have migrated from the Pb to the Ti centres during the reaction. Hydrolysis of the 1:1 Pb/Ti complex produced clear gels providing the H₂O/complex ratio was less than 4. Heat treatment of the gel results in loss of residual organics below 400°C. The XRD pattern indicates the presence of the pyrochlore and perovskite phases after heating at 500°C but the sample is poorly crystalline. Complete conversion to the perovskite phase of lead titanate occurs on heating to 600°C for 1 hour. Thin films of lead titanate were deposited by dip-coating a solution of this complex in isopropanol. Analyses of the films, carried out using electron microprobe, Scanning Auger Spectroscopy and Rutherford Backscattering, indicated that they were of excellent quality, crystalline after heating at 600°C and with relatively sharp substrate-coating interface.