聚苯胺的电荷传输特性及其分子量依赖性

研究了樟脑磺酸掺杂的聚苯胺 (PAn CSA)膜的导电性对温度的依赖性 ,发现有一个临界温度 (Tc) ,当测试温度高于Tc 时 ,PAn CSA显示金属的导电特性 ,反之则显示半导体导电特性 .Tc 和聚苯胺的分子量有关 ,分子量越高 ,Tc 越低 .单向拉伸后 ,PAn CSA膜的电导率大大提高 ,拉伸 6 0 %时 ,室温电导率可达 75 0S/cm ,但Tc 不随拉伸而变化

Synthesis and thermo-decomposition mechanism of rare earth complexes with phenylacetic acid

Rare earth complexes with phenylacetic acid (LnL(3) . nH(2)O, Ln is Ce, Nd, Pr, Ho, Er, Yb and Y, L is phenylacetate, n = 1-2) were prepared and characterized by elemental analysis, IR spectroscopy, chemical analysis, and X-ray crystal structure. The mechanism of thermal decomposition of the complexes was studied by means of TG-DTG, DTA and DSC. The activation energy and enthalpy change for the dehydration and melting processes were determined.

Studies on preparation, characterization of cobalt(II) phenanthroline and 8-hydroxyquinoline complexes/Y zeolite, and catalytic hydroxylation of phenol

Cobalt(II) phenanthroline and 8-hydroxyquinoline complexes/Y zeolite, denoted as CoPhen/Y and CoOx/Y respectively, were prepared, The formation of the metal complexes mentioned above within the cages of Y zeolite and their crystal structures were determined by elementary analyses, TG-DTA, diffuse reflectance UV-Vis, SEM, BET and XRD methods. The influence of experimental parameters upon phenol conversion and product selectivities was investigated as well.

Synthesis, characterization and catalytic activity for H2O2 decomposition of tetrabasic tungstovanadophosphate heteropoly rare earth element complexes with Dawson structure

Nine tetrabasic tungstovanadophosphate heteropoly rare earth element complexes with Dawson structure were synthesized. Their general molecular formulas are K15H4[Ln . (P2W16VO61)(2)] . xH(2)O(Ln = La3+, Pr3+, Nd3+, Sm3+, Eu3+, Gd3+, Dy3+, Yb3+). Their structures and properties were investigated by IR, UV, NMR, ESR, XRD, TG-DTA. The results showed that the series of complexes have the same structure as K-16[Ce(P2W17O61)(2)] . 50H(2)O. At the same time, the catalytic activity of the complexes for H2O2-decomposition was also investigated.

Synthesis of N-(n-octyl)-N'-(10-mercaptodecyl)-4,4'-bipyridinium dibromide and electrochemical behaviour of its monolayers on a gold electrode

A new viologen derivative of N-(n-octyl)-N'-(10-mercaptodecyl)-4,4'-bipyridinium dibromide has been prepared and characterized by elemental analysis, IR, H-1 NMR, MS and TG-DTA. X-Ray photoelectron spectroscopy, cyclic voltammetry and chronoamperometry have been used to characterize the monolayers formed by this compound on the bulk gold electrodes by self-assembly.

3,4－聚异成二烯的合成及所得聚合物结构与性能表征

近二十多年来，在异成二烯的络合催化聚合中，由Ni、Co、Ti及稀土等过渡金属元素络合物组成的催化体系，研究报道得很多，有些已投入工业生产。但由最常见的过渡金属元素铁络合物组成的催化体系，对异成二烯聚的聚合却不多见。本工作研究了三乙酰基丙酮铁为主催化剂，烷基铝为助催化剂，添加含氮类给电子试剂组成三元体系，对异成二烯聚合的催化作用。Fe(a cac)_3 - Al(i-Bu)_3二元体系不能引起异成二烯聚合，而加入少量的含氮类给电子试剂如邻菲啰啉、α,α'－联吡啶等，催化活性显著提高。聚合活性与含氮类给电子试剂的性质有关，并随着下列顺序依次递减：邻菲啰啉、α,α'－联吡啶、对苯二胺、邻苯二胺，对硝基苯胺、邻硝基苯胺；吡啶和已二胺对催化活性的提高几乎没有贡献。烷基铝的不同对催化活性也有明显的影响。其活性顺序为：Al(i-Bu)_3 approx Al Eτ_3 > Al(i-Bu)_2H。首次合成了结晶的3,4－聚异成二烯，3,4－链节含量为70％左右时，Tm为121 ℃左右， Tc为65 ℃左右，透射电镜下观察到结晶的3,4－聚异成二烯具有球晶状结构。初步研究了铁系三元催化体系的反应机理，设想铁化合物和烷基铝生成的烷基铁必须与含氮类给电子试剂作用才能形成活性中心；可见光谱和催化活性实验数据证实了含氮类给电子试剂参与活性中心的形成，并起着稳定活性中心的作用。本文详细地研究了Fe(a cac)_3 - phen - Al(i-Bu)_3催化体系对异成二烯的聚合，考察了起始单体浓度、聚合温度，催化剂总用量以及催化剂各组分配比对聚合速率、聚合物的特性粘数和链节结构的影响，从实验结果讨论了Fe(a cac)_3 - phen - Al(i-Bu)_3体系催化异成二烯的聚合机理，并进行了一些动力学的基本计算，得到了与实验结果基本相符的结果，解释了一些实验现象。铁系聚异成二烯橡胶的表征工作未见诸文献，本工作对铁系聚异成二烯生胶的结晶、力学、流变及阻尼性能作了较系统的研究，并对硫化胶的物理机械性能，弹性及阻尼性能作了初步的表征。铁系聚异成二烯橡胶在室温具有较好的阻尼性能，并且生热值和冲击弹性均较低，可作为室温阻尼材料使用。

铁邻菲咯啉、8-羟基喹啉配合物/Y型分子筛的制备、表征及催化苯酚羟化的研究

制备了铁邻菲咯啉、8-羟基喹啉配合物/Y型分子筛(简记为FePhen/Y,FeO_x/Y).用元素分析,TG-DTA,UV-Vis,IR,SEM,BET,及XRD等方法确定了分子筛笼中金属配合物的生成及其晶体结构,考察了实验参数对苯酚转化率及产物选择性的影响.

THERMAL-ANALYSIS OF Y1-XCAXBA2CU3O7-Y

TG and DTA analysis of Y1-xCaxBa2Cu3O7-y suggests that the stability of the 123 phase increases with increasing Ca contents. The O(1) in the Cu(1)-O chain is unstable but O(2) and O(3) in Cu(2)-O planes are very stable. There are hardly any oxygen vacanci

间硝基苯甲酸稀土配合物的热分解

用TG-DTA,高温X-射线衍射研究了稀土间硝基苯甲酸配合物LnL_3·nH_2O(n=2,Ln=La→Lu+Y;n=0,Ln=Sc,HL=间硝基苯甲酸)的热分解行为,DSC测定其脱水相变过程中的热力学函数,同时用透射电镜观察了热分解产物的超微性。

CRYSTAL STRUCTURE AND THERMAL ANALYSIS OF ERBIUM COMPLEX WITH BENZENE ACETIC ACID

The crystal structure of erbium (III) complex of benzene acetic acid is reported. The complex crystallizes in the monoclinic space group P2(1)/a with a = 0,9008(3)nm, b=1.4242(5) nm, c=1.8437(7) nm, beta=98.80(3)degrees, V = 2.337(1) nm(3), Z = 4. The mechanism of thermal decomposition of complex has been studied by TG-DTG-DTA. The activation energy for dehydration reaction has been calculated by Freeman Carroll method. The enthalpy change for dehydration and phase change process has been determined.

SERRS OF PHTHALOCYANINE DERIVATIVES LB MONOLAYER

SERRS of copper tetrakis(2,4-ditert-penthyl phenoxy) Phthalocyanine LB monolayer on Ag island film and RRS of the compound in solid state have been obtained. On comparison between the spectra, it is proposed that the macrocycle of the molecule on the Ag substrate is oriented parallel to the surface.

对-(二乙氨基)苯基锗倍半氧化物的合成及对体外培养癌细胞的作用

β-羧乙基锗倍半氧化物(Ge-132)的无毒广谱抗癌作用以及潜在的治疗艾滋病的功能~[1～3]促进了Ge-132及其衍生物合成及生物活性研究~[4～6],而对锗原子直接与苯环及其衍生物连接的有机锗倍半氧化物的研究则相对较少.我们曾报道了~[7]p-(二甲氨基)苯基锗倍半氧化物的合成、结构及对癌细胞的作用,p-(二乙氨基)苯基锗倍半氧化物的研究尚未见报道.本文采用改进的方法合成了p-(二乙氨基)苯基锗倍半氧化物(Ge-164).通过元素分析、IP、XPS和TG-DTA确定了组成和结构,观察了它对体外培养人乳腺癌细胞有丝分裂的影响.

Er_2((PhCH_2COO)_6)·4H_2O的结构及热分析

用X-射线四圆衍射仪测定了Er_2(PhCH_2COO)_6·4H_2O的晶体结构。配合物属于单斜晶系,空间群为P2_1/α,晶胞参数:α=0.9008(3)nm,b=1.4243(5)nm,c=1.8437(7)nm,β=98.80(3)°,V=2.337(1)nm~3,Z=4.采用TG-DTG-DTA研究了配合物的热分解过程,确定了热分解机理。采用Freeman-Carroll方法计算了配合物脱水过程的活化能和反应级数。用DSC测定了配合物脱水,熔化过程的焓变。

Bi系中2212相的超导电性研究

已知在Bi系高Tc超导体中存在三个超导相:2223相的Tc～110k,c～37(?);2212相的Tc～85k,c～30.6(?);2201相的Tc～10k。在实验过程中,我们注意到还可能有另外的超导相存在,通过改变元素名义配比和制备工艺观察到一个具有2212相结构,但Tc却表现为～105k的新现象存在。 实验部分 样品制备采用固相反应方法将Bi_2O_3、PbO、Sb_2O_3、SrCO_3、CaCO_3、CuO(均为A.R.级)混匀、碾磨,于～810℃在刚玉坩埚中预烧20h;再碾,压片后于～870℃在磁舟中烧结60-240h,然后作测试分析。

铽芳香族羧酸配合物的热分解机理及动力学研究

本文采用TG-DTA-DTG等技术研究了铽羧酸配合物的热分解过程,通过对中间产物进行红外光谱、元素分析、确定了热分解机理。采用三种方法尝试求得了希土羧酸配合物热分解过程的活化能和焓变,发现并总结了其相变过程。