用新显色剂1,1′-[2,2′-(4,4′-双噻唑基)-双偶氮]-2,2′-双萘酚与TritonX-100体系析相光度法测定微量铀

将新显色剂1,1′-[2,2′-(4,4′-双噻唑基)-双偶氮]-2,2′-双萘酚(简称4,4′-bi-TAN),用作为测定铀的高选择性的试剂。析相体系为UO_2~(2+)-4,4′-bi-TAN-TritonX-100,在580nm波长下测定UO_2~(2+),许多共存离子不干扰测定,用此法测定了铀矿废水中UO_2~(2+)的含量,结果令人满意。     

新型4,4′-双取代-2,2′-二吡啶衍生物的合成及其光学性能

以4,4′-二甲基-2,2′-二联吡啶为原料,经酸化、酰氯化,酯化和缩合反应合成了两个新型的4,4′-双取代-2,2′-二吡啶衍生物—4,4′双(4,5-二苯基嗯唑-2-基)-2,2′-二吡啶(6a)和4,4′-双(4,5-二对甲氧基苯嗯唑-2-基)-2,2′-二毗啶(6b),其结构经1H NMR,IR和MS表征.用UV-Vis和荧光激发光谱测定了6a和6b的光学性能,结果表明,6a和6b的λmax分别为229 nm和238 nm;最大发射波长均为432 nm.     

固相研磨合成4,4′-联吡啶季铵盐

采用室温固相研磨的方法,4,4′-联吡啶与连有阻塞基的乙氧乙醇磺酸酯(或苄溴)反应,得到单取代的4,4′-联吡啶六氟磷酸盐(2),2再与α,α′-二(溴甲基)-2,2′-联吡啶反应,得到哑铃型化合物——2,2′-联吡啶桥连的双-4,4′-联吡啶六氟磷酸盐(3),收率约90%。2和3的结构经1HNMR,13CNMR和MS表征。     

铜三氟柳配合物的合成,结构和仿生催化溴化（英文）

合成了一系列2-羟基-4-三氟甲基苯甲酸(h2tba)-铜配合物:[Cu(htba)2(pz)2](1),[Cu(htba)(2,2′-bipy)](htba)(2)和[Cu(htba)2(4,4′-bipy)](3)(h2tba=2-羟基-4-三氟甲基苯甲酸,pz=吡唑,2,2′-bipy=2,2′-联吡啶,4,4′-bipy=4,4′-联吡啶),并且通过元素分析、红外光谱、紫外光谱、粉末X射线衍射、单晶X射线衍射和热重分析方法对配合物结构进行了表征。这些配合物能够在过氧化氢和溴化物存在的条件下催化苯酚红溴化,并且展示出了较高的催化溴化活性。     

两种N-2-嘧啶基-4-氨基苯磺酰Co(Ⅱ)配合物的合成、晶体结构及电催化性能研究(英文)

水热法合成两种新的Co(Ⅱ)化合物[Co(SD)2(2,2′-bpy)](1)和{[Co(SD)2(4,4′-bpy)]·4H2O}n(2)(SD=N-2-嘧啶基-4-氨基苯磺酰,2,2′-bpy=2,2′-联吡啶,4,4′-bpy=4,4′-联吡啶),并通过元素分析、红外光谱、X射线粉末衍射、热重分析、循环伏安法进行结构和性能表征。单晶X-ray衍射分析表明化合物1是三斜晶系,空间群为P1;化合物2是单斜晶系,空间群为C2/c。电催化实验发现化合物1和2对H2O2、HCHO都具有良好的电催化活性。     

原位一步法制备BTDA/4,4′-ODA/4,4′-SDA聚酰亚胺表面银化薄膜

采用原位一步自金属化的方法制备了具有反射性和导电性的表面银(Ag)化的聚酰亚胺(PI)薄膜,PI是由一种二酐(3,3′,4,4′-四羧基二苯酮酐,BTDA)和两种二胺(4,4′-二氨基二苯醚,4,4′-ODA与4,4′-二氨基二苯硫醚,4,4′-SDA)三元共聚而得,系统研究了4,4′-SDA的引入对薄膜性能及相态结构的影响.结果表明,4,4′-SDA的加入有助于银的还原和迁移,并利于薄膜导电性的提高,薄膜的反射率在两种二胺单体4,4′-ODA与4,4′-SDA的摩尔比为1比1时达到最佳.     

原位一步法制备BTDA/4,4′-ODA/4,4′-SDA 聚酰亚胺表面银化薄膜

采用原位一步自金属化的方法制备了具有反射性和导电性的表面银(Ag)化的聚酰亚胺(PI)薄膜,PI是由一种二酐(3,3′,4,4′-四羧基二苯酮酐,BTDA)和两种二胺(4,4′-二氨基二苯醚,4,4′-ODA与4,4′-二氨基二苯硫醚,4,4′-SDA)三元共聚而得,系统研究了4,4′-SDA的引入对薄膜性能及相态结构的影响.结果表明,4,4′-SDA的加入有助于银的还原和迁移,并利于薄膜导电性的提高,薄膜的反射率在两种二胺单体4,4′-ODA与4,4′-SDA的摩尔比为1比1时达到最佳.     

A Novel Three-dimensional Ni Coordination Polymer Based on Flexible Di-carboxylate Ligand and 4,4-Pyridine： Synthesis, Characterization and Topological Analysis

A novel Ni(II) coordination polymer [Ni(dtba)(4,4′-bpy)] (1, H2dtba = 2,2′-dithio- bisbenzoic acid, 4,4′-bpy = 4,4′-bipyridine) has been synthesized by H2dtba and Ni(CH3COO)2·4H2O with exo-bidentate rigid ligand 4,4′-bpy by using hydrothermal method, and its structure was determined by single-crystal X-ray diffraction. X-ray crystal structure analysis reveals that complex 1 crystallizes in monoclinic, space group Cc with a = 11.7624(9), b = 18.7933(19), c = 10.3071(11), β = 97.6510(10)°, V = 2258.2(4)3, Z = 4, C24H16N2NiO4S2, Mr = 519.22, Dc = 1.527 g/cm3, μ = 1.079 mm-1 and F(000) = 1064. The structure was solved by direct methods and refined to R = 0.0434 and wR = 0.1000 for 3281 observed reflections (I > 2σ(I)). The coordination environment of Ni(II) is a distorted octahedron, and a three-dimensional structure was formed with the coordination effect of dtba2- and 4,4′-bpy ligands. The topological analysis reveals that the whole framework of 1 is a 2-nodal net of (52.6)(53.64.72.8) topology. The thermal stability and XRD pattern of 1 were also investigated.     

两亲型多吡啶钌(II)染料的合成及其在染料敏化太阳电池中的应用

合成了两亲型多吡啶钌(II)配合物：顺式-二异硫氰根(4,4'-二叔丁基-2,2’-联吡啶)(4,4’-二羧酸-2,2’-联吡啶)合钌(II)(K005)，并用循环伏安法、核磁共振氢谱、紫外－可见吸收光谱、傅立叶变换红外光谱等对其进行了表征。该配合物在537和418 nm处有强的金属－配体电荷转移吸收带，可以在很宽带光谱范围内对纳米二氧化钛薄膜进行敏化。对K005染料的光物理和光化学性能和著名的N3染料和两亲型染料Z907进行了对比。通过循环伏安测试，观察到了一对可逆氧化还原电对，其阳极峰电位和阴极峰电位差0.08 V，半波电位为0.725 V(相对于饱和甘汞电极)，这个电对归属于RuII/III的氧化还原。这个配合物成功用作染料敏化太阳电池的敏化剂，在未对二氧化钛薄膜和电解质进行优化时，在AM 1.5，100 mW cm-2的太阳辐照下，获得了3.72%的光电转换效率。     

两种联苯酚类化合物的太赫兹时域光谱研究

利用太赫兹时域光谱技术获得了295 K时2,2′-二羟基联苯(2,2′-biphenol, 2BP)和4,4′-二羟基联苯(4,4′-biphenol, 4BP)在0.1~1.6 THz波段的光谱. 实验结果显示, 两种同分异构体在太赫兹频率范围内的吸收谱有显著的差异. 结合量子化学计算, 2BP中的两个羟基间能够形成分子内氢键, 在1.45 THz的运动模式初步判断为包含氢键在内的两个苯环的低频摆动.     

染料敏化TiO2/WO3薄膜电池的光电变色

The light-to-electricity conversion process of the TiO2 nanostructured electrode sensitized by a dye was investigated using the photoelectrochemical method in this paper. At the same time, the WO3 thin film was electrodeposited on conducting glass. The results showed that the dye-sensitized nanoporous TiO2 film has the properties of energy conversion, along with good electrochromic properties of electrodeposited MoO3 thin film. A self-powered smart window was achieved by combining a dye-sensitized nanoporous TiO2 film as the photovoltaic layer and an electrodeposited WO3 film as the electrochromic layer. This window changed from being almost transparent to blue spontaneously under illumination, and thus could modulate light transmittance.     

In Situ Electrodeposition of an Asymmetric Sol–Gel Membrane Based on an Octadecyltrimethoxysilane Langmuir Film

The unique properties of Langmuir film formation were utilized in assembling a thin skin of an asymmetric membrane. An octadecyltrimethoxysilane (ODTMS) Langmuir monolayer was formed at the air–water interface and served as the substrate for growing a bulky sol–gel polymer in situ. The latter was based on the electrochemical deposition of tetramethoxysilane dissolved in the water subphase by means of horizontal touch electrochemistry. The resultant asymmetric layer that consisted of a thin hydrophobic ODTMS Langmuir film connected to a bulk hydrophilic sol–gel network was studied in situ and ex situ by using various techniques, such as cyclic voltammetry, electrochemical impedance spectroscopy (EIS), scanning electron microscopy, transmission electron microscopy (TEM), and goniometry. We found that a porous hydrophilic film grew on top of a hydrophobic layer as was evident from TEM, contact angle, and EIS analyses. The film thickness and film permeability could be controlled by changing the deposition conditions such as the potential window applied and its duration. Hence, this method offers an alternative approach for assembling asymmetric films for various applications     

Electrochemical Properties of Poly (ethyl acrylate-co-lithium methacrylate) Latex Film Solid Electrolyte

Muchattentionhasbeenpaidtothedevelopmentofnewpolymerelectrolytewithspecialmorphology,soastoimprovetheirelectrochemicalpropertiestomeettheneedsoflithium(ion)battery.Inthiswork,PEMlatexwassynthesizedbyemulsion-fi-eepolymerization.ThemicrophotoofPEMlate...     

硫化镉纳米膜的生物还原-化学沉淀耦合制备及其性能表征

本文应用生物还原-化学沉淀耦合反应(CRBRCP-EDTA)制备出硫化镉纳米薄膜,并借助XRD和SEM对合成材料的物相、结构、形貌进行了表征。研究表明,以铝片为基底时CdS难以沉积,CdS纳米薄膜不能形成;以导电玻璃和单晶硅片为基底时CdS纳米薄膜方可生成。导电玻璃和单晶硅片薄膜都是双层结构,导电玻璃薄膜下层厚度大约40~50 nm,上层厚度大约450~500 nm,整体厚度大约500~550 nm;硅片薄膜的上下两层厚度基本相等,均为300 nm左右,而整体厚度达到600~650 nm。Cd²⁺浓度增加和分散剂PAM加入显著改善了导电玻璃薄膜质量,膜的致密性、均匀性和光催化活性都有所提高。     

不锈钢上黑色钼盐转化膜的研究

用阴极电沉积法从钼酸盐和磷酸盐温和溶液中获得了黑色的不锈钢转化膜,该膜具有良好的热稳定性。电子能谱（ＸＰＳ和ＡＥＳ）分析表明,膜厚约为８２０ｎｍ,膜的表面铝以Ｍｏ（Ⅵ）存在,而在膜内则以Ｍｏ（Ⅵ）与Ｍｏ（Ⅳ）共存。从ＡＥＳ深度剥蚀曲线的组成恒定区求得膜的组成为：Ｏ５０．９％,Ｍｏ２９．４％,Ｐ１２．６％和Ｆｅ７．１％。循环伏安的氧化峰也证明膜内存在Ｍｏ（Ⅳ）。     

馆库温湿度对醋酸纤维素酯胶片物理性能影响的研究

醋酸纤维素酯胶片档案保存环境的温湿度是影响胶片长期保存的关键因素之一。由于技术及理念等方面原因,使得我国大部分档案馆的保存环境均未达到国际标准组织所推荐的条件,致使这些宝贵的胶片档案正在遭受醋酸综合症的危害。本文选取20世纪80年代国产的醋酸纤维素酯胶片作为研究对象,研究了接近实际馆藏温度和湿度对胶片片基层和乳剂层的影响。结果表明:当胶片档案保存的实际温度高于20℃、湿度高于60%RH时,均会对胶片的乳剂层和片基层造成不同程度的损伤,特别是高湿条件会严重损毁胶片乳剂层所载信息。本研究对胶片档案的保存具有一定的参考意义。     

聚乙烯醇缩甲酰苯基-乙烯基吡啶鎓盐的自组装膜及图案化

1991年发展起来的层层自组装(SA)是一种继Langmuir-Blodgett(LB)制膜技术之后的又一种以分子级控制的制备超薄膜的方法。虽然SA方法比LB膜技术晚了半个多世纪,但由于方法简单,不需专用设备;通常在水溶液中进行,对环境友好;对承受膜的物件形状和基材无严格限制等优点,十多年来一直受到关注,SA膜虽比LB膜稳定,但其层层间的离子键或氢键,仍不足以经受极性溶剂等的浸蚀,使其应用受到很大限制。     

联苯胺盐酸盐和聚阴离子有机超薄膜的制备和表征

有机薄膜具有良好的机械和化学稳定性、组成和厚度可控等优点 ,近年来被广泛接受[1 ,2 ] 。用自组装形成的多层复合膜已在渗透膜、导电膜、生物传感器、表面修饰改性、抗静电涂层、非线形光学器件等领域获得了广泛的研究[3,4] 。本文制备了以聚对磺酸钠苯乙烯和联苯胺盐酸盐的分子沉积膜。1　实验部分1 1　试剂与仪器聚对磺酸钠苯乙烯 (ＰＳＳ ,ＭＷ =70 0 0 0 ) ,4,4′—二氨基联苯胺盐酸盐 ,3 氨基丙基三乙氧基硅烷 (ＡＰＳ) ,未进一步处理。ＨＰ845 3型紫外可见光谱分析仪 ,日本协和科学株式会社产ＣＡ -Ａ型接触角测量仪 ,Ｌ1 1 6-Ｅ型…     

MEL分子筛膜不同取向生长的控制

采用晶种涂层的方法在单晶硅表面上制备了不同取向的MEL分子筛膜, 详细研究了膜的择优生长条件及其取向控制. 水含量和反应时间对膜的取向有较大影响. 在水含量较低的反应体系中, 缩短反应时间有利于得到(101)取向的分子筛膜. 水含量提高导致膜的取向发生变化, 由(101)取向变为(101)/(200)混合取向. 晶种层对膜的取向没有直接影响, 晶种层连续生长形成单层分子筛膜.     

Study on the Structure and Properties of Ordered Conductive Polymer Ultrathin Film

A Langmuir-Blodgett (LB) inducing method was firstly used to prepare single layer and multilayer conducting composite PEDOT-PSS film. The film-forming ability of ionization ODA and ODA-SA monolayer spread on PEDOT-PSS nanoparticle sub-phase and the behavior of ODA/PEDOT-PSS assembly particles on pure water were firstly investigated. The results indicated that nanoparticles in the suphase are packed in the ionization monolayer and stable complex Langmuir film is formed at the air/water interface. It has been found that the best film-forming conditions for composite film are as follows:distinct interface was formed between ODA and PEDOT-PSS layer and single layer thickness of PEDOT-PSS was about 23 nm,well accordant to the size of PEDOT-PSS nanoparticles. Different structures were designed to test the conductive ability of these composite films and a variable range hopping (VRH) model was used to explain the film conductive mechanism. The results indicated that a 3D-VRH model explained well the transferring of charge carrier in the multilayer film.