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。     

芳亚甲基丙二腈、芳亚甲基氰乙酰胺的固相合成

芳醛和丙二腈、氰乙酰胺在NH4Ac催化下经固相反应高产率的得到芳亚甲基丙 二腈和芳亚甲基氰乙酰胺。     

Facile cyclic ammonium salt with the smallest size for high performance electric double layer capacitors

A novel cyclic ammonium salt, N,N-dimethylpyrrolidinium tetrafluoroborate (P₁₁-BF₄), was successfully synthesized for the first time. The smallest cyclic structure of P₁₁-BF₄ induced high solubility and conductivity in PC, which can easier enter the micropores of activated carbon and occupy more surface area during charge/discharge process.     

Properties and Photoelectrocatalytic Behaviour of Sol-Gel Derived TiO2 Thin Films

Titanium dioxide (TiO₂) thin films have been prepared on indium doped tin oxide (ITO) glass by sol-gel dip-coating method. Properties of the films were determined as a function of heat-treatment by X-ray diffraction, scanning electron microscopy and photoelectrochemical tests. The films heat-treated at higher temperatures show better crystallinity and photoresponse. The microscopic structure on the film after heat-treatment is attributed to the incorporation of organic polymer into the precursor solution. The performance of the electrodes treated at different temperature on photoelectrocatalytic degradation of methyl orange was investigated. The effect of applied potential and the ability of the electrode to be repeatedly used in photoelectrocatalytic degradation were also evaluated.     

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.     

脉冲激光光声量热装置的研制及用之对香豆素激光染料无辐射跃迁过程的研究

本文报道了一套适用于液相体系的高灵敏度脉冲激光光声量热装置的建立。用此仪器对香豆素激光染料C428, C47和C120的无辐射过程进行了研究, 测得它们在无水乙醇中的无辐射跃迁量子产额分别为0.50, 0.47和0.38。     

The effect of lanthanide on the degradation of RB in nanocrystalline Ln/TiO2 aqueous solution

A series of Nd³⁺, Pr³⁺, Er³⁺, and Dy³⁺ (0.25–5 at.%) homogeneously doped nanocrystalline titanium dioxides (Ln/TiO₂) were prepared by an easy sol–gel technique, and the roles of lanthanide doping on the photocatalytic activity in the degradation of rhodamine B (RB) in aqueous solution were studied. Both the concentration of the lanthanide dopant and calcination temperature showed significant effect to the photodegradation of RB. The photocatalytic activity of pure titania was drastically decreased when calcination temperature was at 700 °C, while the high photocatalytic activity was still maintained for lanthanide-doped samples. HPLC-MS method was used to study the degradation process, and it is demonstrated that the degradation of RB catalyzed by Ln/TiO₂ was principally go through with a stepwise de-ethylation photochemical process.     

Ab initio study of the complexes of halogen-containing molecules RX (X=Cl, Br, and I) and NH3: towards understanding the nature of halogen bonding and the electron-accepting propensities of covalently bonded halogen atoms

Ab initio calculations have been performed on a series of complexes formed between halogen-containing molecules and ammonia to gain a deeper insight into the nature of halogen bonding. It appears that the dihalogen molecules form the strongest halogen-bonded complexes with ammonia, followed by HOX; the charge-transfer-type contribution has been demonstrated to dominate the halogen bonding in these complexes. For the complexes involving carbon-bound halogen molecules, our calculations clearly indicate that electrostatic interactions are mainly responsible for their binding energies. Whereas the halogen-bond strength is significantly enhanced by progressive fluorine substitution, the substitution of a hydrogen atom by a methyl group in the CH(3)X...NH(3) complex weakened the halogen bonding. Moreover, remote substituent effects have also been noted in the complexes of halobenzenes with different para substituents. The influence of the hybridization state of the carbon atom bonded to the halogen atom has also been examined and the results reveal that halogen-bond strengths decrease in the order HC triple bond CX > H(2)C=CHX approximately O=CHX approximately C(6)H(5)X > CH(3)X. In addition, several excellent linear correlations have been established between the interaction energies and both the amount of charge transfer and the electrostatic potentials corresponding to an electron density of 0.002 au along the R-X axis; these correlations provide good models with which to evaluate the electron-accepting abilities of the covalently bonded halogen atoms. Finally, some positively charged halogen-bonded systems have been investigated and the effect of the charge has been discussed.     

A New Efficient Synthesis of p-Nitrocalix[4]arene

A new efficient synthesis of p-nitrocalix[4]arene from calix[4]arene by using nitrogen dioxide is described.The compound is an useful intermediates for the introduction of other functional groups to obtain N containing substituted calix[4]arene.The reaction mechanism is briefly discussed.     

Diastereoselective Three Component Reaction of N‐Glyoxyloyl Camphorpyrazolidinone,Amine and Allyltributylstannane: Facile Synthesis of Homoallylic Amines

Diastereoselective allylation of imine derived from N‐glyoxyloyl camphorpyrazolidinone and amines was treated with allyltributylstannane in the presence of triflic acid. The corresponding optically enriched homoallylic amines were obtained in reasonable to high material yields and with practical levels of stereoselectivity in 10 min at ambient temperature.