纳米碳酸锌的制备和热分解动力学参数的测定

Nanosized zinc carbonate was prepared in the droplet of nano-reactor based on microemusion. The influences of the concentration of the surfactant and reactant on the diameter of nanoparticles were studied and the kinetic pa-rameters of thermal decomposition reaction were determined. It can be shown from experimental results， the di-ameter of the droplet in the microemulsion which have dissolved reactant zinc nitrate and sal volatile is between 4.9nm and 7.7nm， 6.2nm and 12.4nm， respectively. Nanosized zinc carbonate prepared by the method of mi-croemusion has shown good dispersion， narrow distribution and light agglomeration. The particle size of nanosized zinc carbonate is between 5nm and 40nm， and its kinetic parameters of thermal decomposition reaction-activation energy E and reaction order n are 110kJ·mol^-1 and 0.9， respectively.     

WS2 超细粉体的固相法合成

WS2 超细粉体的固相法合成;WS2;固相反应;过硫系数;高能球磨;粒度     

纳米PbSnO3的制备及其燃烧催化性能的研究

Nanocomposite PbSnO₃was synthesized by coprecipitation method , and its phase evolution process was investigated. The particle size, crystal form, and phase of samples were determined with XRD, TEM and EDS. The catalytic actiyity of sample on the thermal decomposition of RDX was investigated by DSC. The results show that nanocomposite PbSnO₃with the diameter of 9 nm can be obtained by calcining at 600 ℃ for 2 h, which crystal is cubic (pyrochlore type). The catalytic actiyity of nanocomposite PbSnO₃on the thermal decomposition of RDX is much higher than that of normal PbSnO₃. The nanocomposite PbSnO₃can decrease the peak temperature of thermal decomposition of RDX from 240.1 ℃ to 236.5 ℃, and the decomposition enthalpy ΔH of RDX increases 722 J·g^-1 （about 70%）.     

铁基超细粒子催化剂结构与还原行为的Mssbauer谱研究

铁基超细粒子催化剂具有优良的F-T反应性能。本工作利用原位Mssbauer谱辅以XRD技术研究了含有钾助剂的F-T合成铁基超细粒子催化剂的结构与还原行为,考察了催化剂组成和第二金属组分(Mn,Zn,Mg)的影响。“纯”铁超细粒子催化剂在氢气中很容易经Fe_3O_4还原为零价铁。第二金属组分的引入,一方面阻碍了催化剂的还原,另一方面稳定了Fe~(2+)的存在而使其成为还原的主要中间相,这有利于反应条件下形成类尖晶石结构的活性相。对于Fe-Mn催化剂,上述效应随锰含量的增加而更趋显著。铁基超细粒子催化剂在氢气中的还原能力依“纯”Fe>Fe-Zn>Fe-Mn>Fe-Mg的顺序递减,这在一定程度上反映了铁与第二金属组分之间相互作用的强弱。     

Electrical Potential Distribution around a Charged Colloidal Particle: Nonlinear Integral Equation

多电解质溶液中带电胶体粒子的电势分布由球形Ｐｏｉｓｓｏｎ－Ｂｏｌｔｚｍａｎｎ方程（ＰＢＥ）描述．ＰＢＥ是一个非线性的微分方程，且难以求得其解析解．本文采用非线性Ｐ－Ｂ积分方程，计算电势分布的数值解．首先，根据静电场和热力学系统中的物理定理，导出描述电势分布的Ｐ－Ｂ积分方程（ＰＢＩＥ）；其次，用迭代方法求ＰＢＩＥ的数值解．最后，计算了在３－１型电解液中无量纲半径κａ分别为０．１２和０．２２，无量纲表面电势ξ分别为１，２，４，６时球形胶体粒子外部的电势值．为了检验数值解的精度，计算了表面电荷密度，并与Ｌｏｅｂ（１９６１）和Ｏｓｈｉｍａ（１９９５）等人的结果比较，本文结果的相对误差小于１％，优于Ｏｓｈｉｍａ的结果．     

溶胶-凝胶法制备铁酸盐超微粒子催化剂

采用溶胶－凝胶法制备了含Zn,Ni,Co的铁酸盐超微粒子催化剂，运用DTA－TG、IR、XRD以及BET比表面测试等手段对所制备的样品进行了表征。同时，考察了铁酸盐对二氧化碳选择性氧化乙苯制苯乙烯的催化性能。结果表明：制备的铁酸盐均为尖晶石型晶体，粒子的比表面积为31．9－36．3m^2/g，晶粒大小约为30－35nm，在由二氧化碳选择性氧化乙苯制苯乙烯的反应中表现出较好的催化活性。     

碳酸氢铵沉淀法制备氧化钇粉体时反应条件对产物粒度的影响

研究了碳酸氢铵沉淀法的反应条件对氧化钇粒度的影响,探讨了粒度变化规律。发现在沉淀反应中,晶型碳酸钇铵的形成与否是影响氧化钇粒度的关键因素。在较低的反应温度下,当碳酸氢铵和氯化钇的浓度大于0.25mol·L-1,摩尔比大于5,陈化时间大于60min时得到碳酸钇铵沉淀,经煅烧可获得粒度(D50)大于1μm的氧化钇。当反应物浓度较低、摩尔比小,陈化时间较短时得到无定型碳酸钇沉淀,煅烧沉淀可获得粒度(D50)小于0.5μm的氧化钇。实验证明选择适当的沉淀反应条件,可制备D50在0.3～10μm范围内的不同粒度级别的氧化钇粉体。     

Voltammetric sizing of a sphere.

The size of a glass sphere positioned in the center of a microdisk electrode is determined by using a simple electrochemical procedure and is confirmed, additionally, by a microscopical measurement of the sphere at the time of the electrochemical measurement. The cyclic voltammetric response of the naked electrode and of the electrode with the sphere positioned in its center is recorded over a wide range of scan rates (0.002-1.5 V s(-1)). The size of the sphere is then determined by comparison of the experimental voltammogram with simulations for each individual scan rate.     

Pore size distributions in low‐k dielectric thin films from X‐ray porosimetry

X‐ray reflectivity has been used to determine the mass uptake of probe molecules in porous thin films supported on thick silicon wafers. The adsorption occurs by capillary condensation when the films are exposed to probe vapor at controlled partial vapor pressures. The probe solvent partial pressure was varied by mixing saturated air and dry air at constant temperature or by changing sample temperature at a constant vapor concentration. Pore size distribution in the films can be calculated from the probe uptake with typical porosimetric approaches such as the application of the Kelvin equation to convert partial pressure into pore size. For illustration, the pore size distribution of three different nanoporous thin films, the primary candidate of ultra‐low‐k interlevel dielectrics in the next generation of integrated circuit chips, was determined with this technique. These samples represent different generations of low‐k dielectrics developed by industry. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 40: 2170–2177, 2002     

负载型无铬超细铁基变换催化剂的制备和催化性能

 以镁铝尖晶石为载体，以过渡金属氧化物为助剂，用吸附γ－Fe2O3胶体法制备了负载型无铬铁基变换催化剂．TEM，XRD，BET和活性测试结果表明，采用胶体负载法制备的变换催化剂，其活性组分Fe3O4以分立的超细微颗粒分布在镁铝尖晶石载体表面上，颗粒之间存在一定的间隔．过渡金属氧化物NiO或V2O5能够进入Fe3O4晶格形成固溶体，起到代替氧化铬的作用，提高催化活性．负载型催化剂FeNi／MgAl2O4（m（NiO）／m（Fe2O3）＝3％）在汽／气比为1和空速为2000h－1的反应条件下，CO转化率在400和350℃时分别为95％和80％；在高空速和低汽／气比条件下也具有很好的催化性能．稳定性实验结果表明，该催化剂 具有良好的热稳定性和一定的抗硫能力．与非负载型催化剂相比，负载型催化剂具有更为优越的催化性能．