真空蒸镀法制备锡薄膜及其嵌锂电化学性能

采用真空蒸镀法在铜片基底上沉积锡薄膜作为锂离子电池负极材料,对所制备的锡薄膜采用扫描电子显微镜、X射线衍射表征,研究了其表面形貌和组成。 将制备的薄膜在手套箱中组装成CR2032型钮扣式电池,进行电化学测试,研究其电化学性能。 实验结果表明,在相同蒸发时间和基底温度的条件下,随着蒸发功率的增加,沉积的锡颗粒逐渐增大,相应的电化学性能降低。 以蒸发功率200 W、基底温度150 ℃制得的样品粒径为100~200 nm,含有Cu6Sn5合金相,以0.2C倍率充放电循环20周后放电容量达527 mA·h/g。     

Y2O2S∶Er3+，Yb3+的制备及Er3+离子在晶场中的能级分裂

采用沉淀法制备前驱体,通过不同温度合成了上转换发光材料Y2O2S∶Er3+,Yb3+,运用XRD,SEM和上转换发射光谱对其进行表征。结果表明,所合成的Y2O2S∶Er3+Yb3+属于六方晶系晶体,随着合成温度的升高,产物的粒径不断增大,上转换发射光强度逐渐增加。研究Y2O2S∶Er3+Yb3+的上转换发光过程,红光发射和绿光发射分别源于Er3+离子的4F9/2→4I15/2以及2H11/2→4I15/2,4S3/2→4I15/2能级跃迁。利用群论计算了晶场中Er3+离子的能级分裂数目。     

固体酸催化二氟二苯甲酮和苯胺缩合合成N-(双(4-氟苯基)亚甲基)苯胺

以固体酸为催化剂,4,4’-二氟二苯甲酮与苯胺脱水缩合,合成了N-(双(4-氟苯基)亚甲基)苯胺.比较了不同固体酸催化剂H型ZSM-5、Na型ZSM-5、介孔分子筛MCM-41(Al)及强酸型离子交换树脂Amberlyst 15的催化效果.使用比表面、NH3-TPD对催化剂进行了表征,并与催化效果关联.考察了催化剂用量、原料摩尔比、浓度及溶剂等反应条件对产物收率的影响.产物通过熔点、核磁共振谱进行了表征.结果表明,HZSM-5固体酸催化剂具有优异的催化作用.在优化条件下,以对二甲苯为反应溶剂和脱水剂,4,4’-二氟二苯甲酮0.1 mol,苯胺0.2 mol,催化剂用量2.0 g,反应24 h,产物收率达91%.此外,催化剂易于分离,能够重复使用多次.     

半夹芯16电子化合物CpCo(S_2C_2B_(10)H_(10))与乙炔基二茂铁在甲醇中的反应性

半夹芯16电子化合物CpCo(S2C2B10H10)(1)(Cp:cyclopentadienyl)与过量乙炔基二茂铁(FcC≡CH)(Fc:ferrocenyl)在甲醇中反应,分离得到了化合物(CHCFc)(CH=CFc)(S2C2B9H10)(8)和2个乙炔基二茂铁环三聚产物1,2,4-三二茂铁基苯和1,3,5-三二茂铁基苯。在8中,2个乙炔基二茂铁分子以"头对头"方式聚合连接到CpCo(S2C2B10H10)分子中的2个S原子上,导致CpCo结构单元的丢失。碳硼烷笼体B(3)位上的BH键发生活化,该B原子与1个乙炔基二茂铁分子的乙炔基末端C原子连接生成C-B键;同时,B(6)位的BH碎片在甲醇作用下失去,从而closo-C2B10闭式结构转变成nido-C2B9巢式结构。化合物8用单晶X-射线衍射分析方法进行了表征。     

ELECTROCHROMETIC STUDIES ON POLAR MULTILAYERS OF LIQUID CRYSTALLINE POLYMERS

Electrochrometic measurements were carried on the Z-type Langmuir-Blodgett films oftwo liquid crystalline polymers: mono-{6-[4-(phenylazo) naphthyloxy] hexyl} (1a) andmono-{6-[4-(anthraquinone-1-azo) naphthyloxy] hexyl} (2a) ester of polymaleic acid. Itwas found that for both polymers, poling fields parallel and antiparalle1 to dipole momentsof the polymer side chains induce red and blue shift in absorption bands, respectively. Forpolymer la blue shift is accompanied by absorbance increase, while red shift by absorbancedecrease;but for polymer 2a only decrease in absorbance is observed. A simple model wasproposed to analyze the results.     

A Study of Spectroscopy on TCAQ Microcrystal

UV-visible absorption spectra of 11,11,12,12-tetracyano-9,10-anthraquinodimethane (TCAQ) solution, crystal and evaporated film were, measured. The absorption spectrum of TCAQ solution in DMF had three bands at 287 nm(4.45), 310 nm(4.23) and 350 nm(4.38) respectively; that of evaporated films had one band at 370 nm and that of crystalline powder had four bands at 243 nm, 275 nm, 320 nm and 430 nm respectively. Surface photovoltage spectra of TCAQ microcrystal gave two bands at P₁ (320 nm) and P₂ (430 nm) respectively. The absorption bands were assigned and the energy levels of frontier orbitals were tentatively determined. In addition,the mechanism of hole, production and transportation in crystalline TCAQ was discussed.     

A Novel Amphiphilic Push-pull Ferrocene Derivative: Langmuir-Blodgett Films and Second-order Optical Nonlinearity

We investigated Langmuir-Blodgett(LB) films built from the mixture of an amphiphilic push-pull ferrocene derivative(P) and behenic acid. Langmuir films of P diluted by behenic acid exhibit a very good cohesion, and the mixed films can easily be transferred onto solid substrates. Linear dichroism UV-visible and IR spectroscopy measurements of the mixed LB multilayers confirm that the molecules(P) are oriented to the substrate. The nonlinear optical experiments on the mixed monolayer deposited on the CaF₂ slide showed that P displays efficient optical second harmonic generation(SHG) with a molecular hyperpolarizability (β)h, high as 6.0×10^-29e. s. u..     

Crystallization of Ammonium Nitrate Under Organised Monolayers at Air-Aqueous Interface

The crystallization of NH₄NO₃ under compressed Langmuir monolayers of carboxybe-taine(C₂₂N₃COO^-),C₂₂H₁₅N(CH₂)₃(CH₂)₃COO^--[C₂₂N₃COO^-] and dioleoyl-L-a-lecithin(DOPC) was studied by means of π-A. ΔV-A and fluorescence microscopy (FM). The surface pressure, surface potential and molecular area of C₂₂N₃COO^- were decreased on the NH₄NO₃ solution subphase. The surface pressure and molecular area of DOPC was increased. The surface potential of DOPC was decreased. We can directly observe the surface crystallization of NH₄NO₃ by FM. The results revaled that C₂₂N₃COO^- monolayer was the promoter of NH₄NO₃ surface crystallization. In contrast,DOPC monolayer was the inhibitor of the surface crystallization of NH₄NO₃.     

超高效液相色谱-串联质谱联用法同步检测抗生素生产废水中螺旋霉素与新螺旋霉素残留

采用超高效液相色谱-串联质谱法同步测定了抗生素生产废水中残留的螺旋霉素(SPM-Ⅰ)和新螺旋霉素(NSPM-Ⅰ)。考察了萃取溶剂种类、水样pH值、萃取次数、水样与萃取溶剂的体积比等因素对目标物回收率的影响。以ACQUITY UPLC BEH C18(100 mm×2.1 mm i.d.,1.7 μm)为分析柱,0.1%甲酸水溶液和乙腈为流动相梯度淋洗,流速0.2 mL/min,电喷雾正离子多重反应监测模式检测。标准曲线在0.02~1.00 mg/L范围内线性关系良好,r2均大于0.999。方法回收率为70% ~ 88%,相对标准偏差小于10%,检出限(S/N=3)分别为0.03 μg/L(SPM-Ⅰ)和0.06 μg/L(NSPM-Ⅰ)。该方法应用于无锡市某制药厂抗生素生产废水中SPM-Ⅰ和NSPM-Ⅰ的检测,检出质量浓度分别为（115.6±2.7） mg/L和（5.3±0.4） mg/L。     

PPV-PDMeOPV共聚物发光性质的实验和理论研究

具有优良电致发光性能的有机聚合物材料的研制及其发光性能和应用的研究是９０年代新兴的高科技领域．聚对苯乙炔［Ｐｏｌｙ（ｐ－ｐｈｅｎｙｌｅｎｅｖｉｎｙｌｅｎｅ）,缩写为ＰＰＶ,又称聚苯撑乙烯］是这一领域最先研制出来的具有代表性的材料［１,２］．为改变ＰＰ...