铟锡氧化物纳米网的微波法制备及其光催化特性研究

By using ultrasonic and chemical liquid coprecipitation, the precursor was prepared with high purity In, SnCl₄·5H₂O and urea. The In₂O₃·SnO₂ nanonets were obtained from precursor by heating in microwave oven. The powders were characterized by XRD, TEM. The analyzed results show the sample is In₂O₃·SnO₂, and In₂O₃is rhombohedral system while SnO₂ is tetragonal system. The sample is in spherical grain shape, with average granularity of 35 nm, and the mesh diameter of 10～80 nm. The sample was with fluorescence and good photocatalytic performance for degradation of organic dyestuff.     

单分散超细ZnO粉体的制备与表征

Monodispersed superfine ZnO powders with particle size of about 200～400nm were successfully prepared by the decompressed distillation process with n-butyl alcohol as the solvent. The starting materials were Zn(NO₃)2·6H₂O and NH₃·H₂O. TG-DSC， XRD， TEM and BET surface areas techniques were used to characterize the precursor and as-prepared superfine ZnO powders. In the preparation process of superfine ZnO powders， two techniques including the decompressed distillation with n-butyl alcohol and washing with absolute ethanol were used to avoid agglomeration. It is showed that the decompressed distillation process has a better effect in avoiding ag-glomeration than washing with absolute ethanol. The precursor obtained by the decompressed distillation technique has a lower calcination temperature than the one obtained by washing with absolute ethanol. Zincite phase of ZnO with some impurities was obtained when the precursor was calcined at 200℃ for 2h. After it was calcined at 300℃ for 2h， pure superfine ZnO powder was obtained.     

纳米SnO2的非水溶剂溶胶-凝胶法制备与表征

Nanometer SnO₂ powders were successfully prepared by non-hydrolytic sol-gel approach combined with heat treatments using tin tetrachloride as starting material and ethylene glycol as solvent. The reaction mechanism of the sol-gel process is proposed. Results indicate that the -OHCH₂CH₂OH- prevent Cl^- ion from accessing to tin Sn⁴⁺ due to steric effect, and hence increaseing the stability of the sol solution. Ethylene glycol functions not only as a complextion agent to form a polymer network but also as a “spacer” to modulate the distance between metal ions, preventing metal oxide particles from aggregation during desiccation of the sol. The effects of heat treatments on the evolution of structure and morphology of nanosized SnO₂ powders were studied. The powders with narrow size distribution around 15～20 nm could be obtained at 500 ℃ for 4 h.     

锂离子电池正极材料LiMn2O4的合成与晶体结构（英）

Spinel LiMn₂O₄ powders were prepared using two-step synthesis method consisting of solid-state reaction method and citrate modified sol-gel method. The effects of the calcination temperature and the Li/Mn ratio of raw materials were studied on the physicochemical and electrochemical properties of the spinel LiMn₂O₄ powders, such as crystallinity, lattice constant and density. The title compound was characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Polycrystalline LiMn₂O₄ powers calcined at 750 ℃ were found to be composed of very uniformly-sized microcrystal with an average particle size of 300 nm. The improvement in electrochemical properties was mainly attributed to the process of re-grinding by absolute alcohol.     

无氨湿法制备纳米晶In2O3及表征

Preparation of In₂O₃nano-scale powders by ultrasonic and homogeneous precipitation, using metal In and urea as raw materials, was reported for the first time, while the effects of reaction temperature, the ratio of the materials and the pH etc. on the preparation was dicussed. This method can be operated and industrialized easily with very low cost． The structural properties of precursor and In₂O₃were characterized by TG-DTA, XRD, ESCA and TEM. The results show that In₂O₃produced are very pure, monophase and spherical nano-scale powders with average size of 25 nm.     

电镀烧结法制备Ti/SnO2-Sb2O4电极的研究

The Ti/SnO₂-Sb₂O₄ electrode has been prepared by the electroplate-sinter method. The effect of SbCl₃ adding amount and sintering temperature on its electrode lifetime and oxygen evolution potential were investigated by means of EDX, SEM and XRD analysis. The results indicated that the electrode appeared the best performance when the SbCl₃ adding amounts was 0.2g and the sintering temperature was 550℃. In optimized conditions Ti substrate was entirely covered by SnO₂-Sb₂O₄ and the combinations among them were tight. Due to the use of electroplate method, the electrical conductivity, the oxygen evolution potential and the electrode lifetime were increased, so the elec-tro-catalytic activity and the electrochemical stability of the prepared electrode were found to be superior.     

柠檬酸溶解-热解法合成纳米晶SnO2粉体

The SnO₂ nanocrystaline powders were synthesized by citric acid dissolution-pyrolysis method. The medium products were analyzed by FTIR. The products were characterized by TG-DTA, XRD, TEM, SEM etc. The results showed that the Sn was coordinated with aconitase acid during the dissolution. The SnO₂ particles prepared by this method were with a mean size of 5～10 nm. The calcined products presented lacunose micro-arc structure, thus favoring the application as gas-sensitive materials.     

草酸盐共沉淀法制备Y1.84La0.16O3纳米粉体

Nanopowder of Y_1.84La_0.16O₃ was prepared by oxalate co-precipitation method. The powder was characterized by TG-DTA, XRD and TEM. The results show that the precursor is Re₂(NO₃)₂(C₂O₄)₂·2H₂O (Re=Y, La), and the Y_1.84La_0.16O₃ nanopowders produced by calcining the precursor at 1 000 ℃ for 4 h are 20～40 nm spherical particles and well dispersed. The powders were with high sintering activity and could be fabricated to transparent ceramic without additive at 1 450～1 550 ℃ in H₂ atmosphere for 3 hours. The total transmission of the transparent ceramic could reach 80%.     

有机体系中电合成纳米PbTiO3粉体及表征

The precursor PbTi(OCH₂CH₃)_6-y(acac)_y for the mixed oxide PbTiO₃was synthesized by electrochemical dissolution of Lead and Titanium with a 1∶2 electricity quality in ethanol and acetyl-acetone solution. Nano-sized PbTiO₃powder was prepared by drying and calcining the xerogel from a direct sol-gel hydrolyzation of the precursor solution under pH of 8.5. The FTIR, TG-DTA, XRD and TEM were employed to characterize the structure of the precursor and nano-sized PbTiO₃. The results showed that the optimized conditions for the preparation of nano-sized PbTiO₃ were the electrolysis of the Lead plate and Titanium plate at 50 ℃ and 40 ℃ respectively under 0.03mol·dm^-3Bu₄NBr solution. The nano-sized PbTiO₃prepared by electrolysis exhibited a dispersive structure with an average diameter of 10 to 15 nm.     

LiAlO2细粉料的制备及反应机理研究

As a functional inorganic material, LiAlO₂ was focused on widely, especially in the field of tritium breeder of fusion reactor. In this article, the proper reaction conditions and mechanism to synthesis the γ-LiAlO₂ by solid state method are considered. In the experiments, it has been found that the phase of β- and γ-LiAlO₂ are only produced by the reaction of LiOH and Al₂O₃, while the α- and γ-LiAlO₂ can be obtained by the reaction of Li₂CO₃ and Al₂O₃. As compared with Li₂CO₃ and Al₂O₃ reacted at 900～1000℃ for the preparation of γ-LiAlO₂, the γ-LiAlO₂ can also be made by the reaction of LiOH and Al₂O₃ at some more lower temperatures that is due to the bulk diffuse mech-anism. But the former can get better crystal and have smaller particles for the mechanism of surface fast reaction. As a result, the sub-micron γ-LiAlO₂ powders with the diameter less than 0.3μm are obtained.     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。