电化学现场X-射线衍射电解池及电极调节装置

设计了一种能在常规粉末衍射仪上通用的电化学现场X-射线衍射测定的电解池及其电极调节装置,实现了电极表面与窗片之间液层厚度的连续可调,精度达±2μm。理论计算与实测结果均表明液层厚与衍射峰强度和峰位之间存在定量关系。     

一类含多氟烷基侧链的螺环化合物的合成及结构表征

A series of spiro compounds have been synthesized via several steps.The structure of these compounds wereconfirmed by ~1H NMR,~(13)C NMR,IR,MS spectra and X-ray diffraction analysis.The possible mechanism to formthese products was also proposed.     

聚乳酸/壳聚糖季铵盐皂石纳米复合材料的原位插层聚合及性能表征

通过两步法将2,3-环氧丙基三甲基氯化铵接枝壳聚糖合成了水溶性壳聚糖季铵盐(HTCC),以其为插层剂对稀有的新疆皂石(Saponite)黏土矿物进行有机改性,制备了壳聚糖季铵盐皂石(HTCC-saponite),并以其为助剂,以丙交酯为单体,通过原位插层聚合法制备了聚乳酸(PLA)/HTCC-saponite纳米复合材料.最优化合成条件:聚合反应温度150℃,辛酸亚锡加量2%(质量分数),HTCC-saponite加量1%(质量分数)、聚合反应时间16 h.微观结构分析表明HTCC-saponite具有插层与剥离共存的结构.采用X射线衍射(XRD)、透射电子显微镜(TEM)、热重分析(TG-DTG)和差示扫描量热仪(DSC)等对PLA/HTCC-saponite纳米复合材料的微观结构、形貌及热稳定性进行了表征和分析.结果表明,HTCC-saponite有效改善了PLA的结晶性能,提高PLA的热稳定性.抗菌测试结果表明,HTCC-saponite具有良好的抗菌性,并赋予PLA/HTCC-saponite复合材料较强的抑菌能力.     

基于阴离子-石墨嵌层化合物的电化学电容器

石墨可以在高电势下电化学可逆存储阴离子,有望在高电压储能器件中担当正极材料.本文介绍了基于阴离子-石墨嵌层化合物型正极材料的高比能电容器的研究进展,剖析了影响电容器性能的各方面因素,探讨了一系列表征相关电极材料储能机制的方法和手段,揭示了溶剂化效应对阴离子插嵌石墨正极电化学行为的关键性作用.并进一步概述了该种正极材料近年来在新型储能器件-双离子电池中的发展态势,展望了其应用前景和即将面临的潜在问题.     

三种长链季铵盐在低共熔溶剂中胶束结构的小角X-射线研究

通过小角X-射线散射技术,研究了十二烷基三甲基溴化铵（DTAB）、十四烷基三甲基溴化铵（TTAB）、十六烷基三甲基溴化铵（CTAB）三种阳离子季铵盐表面活性剂在Ch G和ChEG低共熔溶剂中的胶束行为并表征胶束的结构。研究结果表明,表面活性剂烷基链长及低共熔溶剂类型对胶束结构影响较大,而温度对其影响较小。所得结果为低共熔溶剂中有序分子聚集体的构建提供参考。     

喹啉季铵盐和1,3-茚满二酮及2-芳亚甲基1,3-茚满二酮的环加成反应合成茚满酮类含氮杂环化合物（英文）

在三乙胺存在下, N-苯甲酰基甲基喹啉溴化物和1,3-茚满二酮在乙醇中于室温反应,主要产物为多取代二氢吡咯[1,2-a]喹啉,次要产物为2-(1-苯甲酰基甲基)喹啉-4-亚基)-1,3-茚满二酮.在相同条件下,N-苄基喹啉溴化物和1,3-茚满二酮在乙醇中于室温反应,主要产物则为2-(1-苯甲酰基甲基)喹啉-4-亚基)-1,3-茚满二酮.另一方面, N-苯甲酰基甲基和N-乙氧羰基甲基以及N-(对硝基苄基)喹啉溴化物和芳香醛,1,3-茚满二酮的三组分反应,在三乙胺存在下在乙醇中高效地生成螺[茚满-2,3’-吡咯[1,2-a]喹啉]衍生物,反应具有很好的非对映选择性.     

在石墨电极上脱氧核糖核酸与米托蒽醌嵌入作用的电化学研究

本文研究了单链ＤＮＡ分子在石墨电上的固定方法，采用核酸分子杂交技术，使具有电化学活性的米托蒽酯嵌入ＤＮＡ分子双螺旋结构的碱基对中，在电极上形成ｄｓＤＮＡ－ＭＳ层，通过伏安法研究ＤＮＡ分子和ＭＸ相互作用的电化学行为。     

壳聚糖季铵盐改性石墨烯的制备及电化学性能研究

采用2-羟丙基三甲基氯化铵壳聚糖(HACC)通过非共价作用修饰氧化石墨烯,然后通过水合肼还原得到HACC改性的石墨烯(HACC-RGO).采用红外光谱、X射线衍射和场发射扫描电子显微镜对改性石墨烯进行结构和形貌的表征.通过热重测试分析HACC在改性石墨烯中的实际含量.分析对比不同改性石墨烯的zeta电位值,并通过动态光散射粒径仪研究HACC-RGO在不同p H值溶剂中的分散性及粒径大小.结果表明,HACC成功结合到石墨烯表面上并插入石墨烯片层间,得到的HACC-RGO在p H为2~9的水溶液中均能稳定分散,在水溶液p H值为7时分散粒径最小.随着HACC用量的增大,HACC在HACC-RGO中的含量增加,HACC-RGO在水中的zeta电位值也相应增加,而HACC-RGO的平均粒径却减小.通过循环伏安法研究HACCRGO的电化学性能,结果表明HACC-RGO具有较好的导电性,铁氰化钾在HACC-RGO/GCE上的还原峰电流随着HACC用量的增加而增大,氧化还原峰电流随着还原剂水合肼用量的减少而降低.     

Intercalation of Sodium and Lithium into Graphite as a First Stage in an Electrochemical Method for Producing Carbon Nanotubes

A cyclic voltammetry method is used to show that the process of reduction of sodium (and, possibly, lithium) out of melts of corresponding chlorides on the molybdenum, glassy-carbon, and graphite electrodes is complicated by the process of dissolution of the corresponding alkali metal in the melt. A notion called “reversibility of material balance” is introduced. The notion reflects the ratio of the amount of substance that undergoes oxidation in the anodic half-cycle of a voltammetric curve to the amount of substance that is deposited in the cathodic half-cycle of the curve. The adsorption of sodium and lithium on glassy carbon and graphite plays an important role in the process of reduction, leading to an increase in the reversibility of the process. This is pronounced especially strongly at potential scan rates below 1 V s^?1. The sodium intercalation into graphite leads to a decrease in the reversibility of the process of reduction, the more so at potential scan rates below 0.03 V s^?1. However, the intercalation of lithium (probably because of its small atomic radius) does not exert practically any influence on the reversibility of process at the above potential scan rates.     

Preparation,Characterization and Electrochemical Behavior of Pd‐Au Alloy Incorporated into Zeolites/Graphite Electrodes

The present article reports the preparation of Pd‐Au alloy incorporated into NaY zeolites layer via simple immersion technique. Pd‐Au particles were incorporated into zeolites cages via Co‐impregnation or alternate impregnation of metal ions. Cyclic voltammetry was used to evaluate the state of the modified electrodes in alkaline media. Surface morphology as well as elemental composition of the modified layer were examined using Scanning electron microscopy (SEM) and energy dispersive X‐ray (EDX).     

Study on the Texture of Zinc Electrodeposits by X-ray Diffraction

The texture of zinc electrodeposits obtained under potentiostatic and galvanostatic conditions was studied by X-ray diffraction.It is found that the crystal orientation of zinc electrodeposits depends strongly upon the potentials and duration of deposition,the results are discussed in terms of the geometric selection theory and the "outward" growth mode,crystallographic and electrochemical factors are considered together.     

X射线衍射及散射方法研究Al-Li合金回火相变

A l-Li合金是一种低密度、高比模、高比强的新型铝合金,其在航空、航天、汽车、船舶和兵器等工业中具有广泛的应用前景。由于A l-Li合金回火析出相δ(′A l3Li)的相变过程比较复杂,人们一直在从事这方面的理论研究工作。然而关于δ′相的形成长大机理,至今仍存在形核长大与调幅     

Electrochemical Preconcentration of Arsenic(III) in Its Determination by Stripping Voltammetry at Graphite Electrodes Modified with Gold and Copper

The effect of some factors (potential and time of electrolysis, nature and concentration of supporting electrolyte) on the electrochemical preconcentration of arsenic at graphite electrodes modified with copper and gold adatoms was studied. The data obtained were used for the determination of 10^–7to 10^–6M arsenic(III) by stripping voltammetry. The detection limits for arsenic using graphite electrodes modified with copper and gold were 6.3 × 10^–7and 2.3 × 10^–7M, respectively.     

X射线粉末衍射技术在酞菁同质多晶异构体研究中的应用

综述了无金属酞菁的晶体结构的研究状况、晶体类型的划分,并对晶型存在的合理性进行了初步探讨。     

共沉淀法制备Fe3O4超微粉的X射线衍射研究

进行了用化学共沉淀法制备Fe3O4超微粉的研究,讨论了反应液浓度相同而Fe2 和Fe3 的比例不同以及Fe2 和Fe3 的比例相同而反应液浓度不同时对粉体的影响,并通过X射线衍射和透射电镜对超微粉样品进行了表征.当Fe2 /Fe3 的比值为1.125时得到较好的Fe304超微粉.     

Effect of the Nature of a Quaternary Ammonium Salt and the Addition of a Neutral Carrier on Analytical Characteristics of Sulfate-Selective Electrodes

A film polyvinyl chloride sulfate-selective electrode based on the sterically accessible higher quaternary ammonium salt, 3,4,5-tris(dodecyloxy)benzyl(oxyethyl)3trimethylammonium chloride, using 1-bromonapthalene as a plasticizer and heptyl p-trifluoroacetylbenzoate as a solvating agent was developed. The limit of detection of the electrode was 6.7 × 10^?7 M, lifetime was 1 month, and the slope of the electrode function was 27 mV/decade. The electrode is selective in the presence of interfering Cl^?, C₂O₄^?, Br^?, and NO₃^?ions. The interference of carbonate ions was eliminated by maintaining pH at 3.2 ± 0.1. Based on IR spectroscopic and potentiometric studies, it is most likely that the solvation of sulfate ions with heptyl p-trifluoroacetylbenzoate occurs through interaction with the trifluoroacetyl carbonyl carbon atom rather than with hydroxyl groups of the hydrate form.