A Germanate Compound Constructed from Dissymmetric Ge7 Chains and Metal Complexes

Abstract. A novel germanate compound, |[Ni(dien)₂]₃(H₂O)₃|[Ge₇O₁₃F₅]₂(designated JU‐85, dien = diethylenetriamine), was solvothermally synthesized. The structure of JU‐85 was determined by single‐crystal X‐ray diffraction and further characterized by powder X‐ray diffraction, inductively coupled plasma, infrared spectroscopy, elemental analysis, and thermogravimetric analysis. JU‐85 has dissymmetric chains constructed from diagonally linked Ge₇ building units and various Ni(dien)₂²⁺ complexes formed in situ during the synthesis. Compared with its structural analogue, FJ‐6, JU‐85 contains less complex cations and different host‐guest assembly. Besides the diagonal linkage in JU‐85, other dissymmetric linkages of Ge₇ building units were enumerated, which could be used as the stereogenic centers for the design of novel chiral germanate compounds.     

UPLC-ELSD Determination of 1-Octacosanol in Raw Material and Health Products

Determination of the levels of 1-octacosanol is important in food stuff for the study of its pharmacological activities and health benefits. In this study, a novel, simple and fast internal standard method for the non-derivatization ultra-performance liquid chromatographic determination of 1-octacosanol in raw materials and health products was developed and validated based on evaporative light scattering detection. The linearity (r ² > 0.998), recovery (99.1–100.2%, RSD <2.7%), intra- and inter-day precision (RSD <3.8%), limit of detection (1.0 mg/L), limit of quantification (2.2 mg/L) of the 1-octacosanol were determined. The method was successfully applied to nine real 1-octacosanol products. The results of analyses had close agreement with the labeled claims of 1-octacosanol content in these products. Compared with the classical gas chromatography method, the developed method was simpler, faster and more environmentally friendly due to avoiding any derivatization step. This protocol represents a rapid and feasible method for quality control of 1-octacosanol products.

     

Synthesis of mikto‐topology star polymer containing one cyclic arm

Well‐defined mikto‐topology star polystyrene composed of one cyclic arm and four linear arms was synthesized by a combination of atom transfer radical polymerization (ATRP) and Cu‐catalyzed azide‐alkyne cycloaddition (CuAAC) click reaction. First, the bromine‐alkyne α,ω‐linear polystyrenes containing four hydroxyl groups protected with acetone‐based ketal groups were synthesized by ATRP of styrene using a designed initiator. Then, the bromine end‐group was converted to the azide and the linear polystyrene was cyclized intra‐molecularly by the CuAAC reaction. The four hydroxyl groups were released by deprotection and then esterified with 2‐bromoisobutyryl bromide to produce a cyclic polymer bearing four ATRP initiating units. By subsequent ATRP of styrene to grow linear polymers with the cyclic polystyrene as a macroinitiator, the mikto‐topology star polymers were prepared. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012     

低温生长Cu(InGa)Se2薄膜吸收层的掺钠工艺研究

在柔性聚酰亚胺衬底上低温制备Cu(In,Ga)Se₂薄膜太阳能电池, Na的掺入会改善电池特性, 但不同的掺Na工艺对Cu(In,Ga)Se₂薄膜和器件特性的改善机理不同. 本实验通过对比前掺NaF和后掺NaF工艺发现, 在前掺Na工艺下, 由于Na始终存在于Cu(In,Ga)Se₂薄膜生长过程中, Na存在于多晶 Cu(In,Ga)Se₂ 薄膜晶界处, 起到了扩散势垒的作用, 导致晶粒细碎、加剧两相分离, 同时减小了施主缺陷的形成概率; 而在后掺Na工艺下, 掺入的Na对薄膜的结构及生长不产生影响, 仅仅起到了钝化施主缺陷、改善薄膜缺陷态的作用. 同时, 研究表明, 后掺Na工艺中, NaF必须依靠外界能量辅助才能扩散进Cu(In,Ga)Se₂内部, 实验结果证实, 只有衬底温度达到350 ℃以上时, 掺入的NaF才能较好地改善薄膜特性. 最终经掺Na工艺的优化, 得到低温工艺制备的柔性聚酰亚胺衬底器件效率达10.4%.     

ELLIPSOMETRIC SPECTRA OF CONDUCTING POLYANILINE

We report the ellipsometric spectrum studies on a new kind of conducting polymers, polyaniline. In the UV-visible range (1.4-4.8eV photon energy region) the absorption coef-ficient, the complex dielectric function and the refractive index of polyaniline as functions of photon energy are obtained. The spectra of nonconducting and fully conducting polyaniline have been analyzed and discussed. The experimental results show that the emeraldine base form of polyaniline has a large energy gap (E_g～3.6eV) and its absorption spectrum shows a broad exciton absorption peak centered at 2 eV. The absorption spectrum of emeraldine salt after protonation have four absorption peaks centered at 1.5, 1.83, 3.0 and 3.88eV. We also investigated the spectrum evolution of the samples from nonconducting (σ<10^-9Ω^-1·cm^-1) to conducting (σ≈10⁺¹Ω^-1·cm^-1) states, and give the dielectric function and the refractive index of the samples.     

超软X射线流气式正比计数管

介绍了一种用于测量183～933eV超软X射线的圆柱形、侧窗式、流气式正比计数管,工作气体是0.11MPa的P-10气体或氦气-丙烷混合气体。计数管内径为φ25mm,直径为φ0.3mm的入射窗是由厚度80～90μgcm~2聚乙烯甲醛制成的。该计数管的特点:(1)薄窗,对软X射线透过率高。(2)流气式,工作寿命长。(3)能量分辨率好。(4)计数率高(1×10~(14)个/s)。(5)可测能区宽(0.183～10keV)。(6)可以方便更换窗膜材料、厚度及窗口直径。近几年来该计数管已经为高强度低能X光源提供较好监测。