水滑石有序组装超薄膜及其电化学性能

发布时间：2018-01-03 10:25

本文关键词：水滑石有序组装超薄膜及其电化学性能　出处：《湘潭大学》2015年硕士论文　论文类型：学位论文

【摘要】：水滑石类化合物包括水滑石和类水滑石,其主体一般由两种金属的氢氧化物构成,因此又称为层状双羟基复合金属化合物(Layered Double Hydroxide,LDH),由这些化合物插层组装的一系列超分子材料称为水滑石类插层材料(LDHs)。其特有的层状结构使其具有更强的兼容性,水滑石类层状化合物自发现以来已有一个世纪,历代研究者通过对其结构改造进而在催化化学、吸附、离子交换、电化学、光化学等领域进行广泛应用,近代水滑石研究领域有了更广阔的拓展,如环保、化妆品、功能高分子材料、纳米复合材料、医药学、生物-无机材料等。本文研究Mg/Fe-NO3水滑石合成、剥层、自组装以及电极修饰,阐述镁铁水滑石修饰电极(Mg/Fe/[Fe(CN)6]/GCE)的电荷传输机理,为今后水滑石剥层和电极修饰的进一步研究提供理论依据。本论文通过制备Mg/Fe-CO3型水滑石,通过酸碱法处理Mg/Fe-CO3型水滑石制备Mg/Fe-NO3型水滑石,并通过XRD、FT-IR、SEM和EDS进行表征分析。在甲酰胺溶液中通过回流法对Mg/Fe-NO3水滑石进行剥层,制得淡黄色透明的Mg/Fe水滑石纳米单片胶体溶液,其表现出胶体特有的丁达尔现象,并且有很好的稳定性,根据实验结果可知剥离后的纳米片胶体溶液可在氮气保护下稳定存在一周。考察不同Mg/Fe摩尔比、剥层温度、剥层时间、水滑石起始量下Mg/Fe-NO3水滑石剥层率,从热力学角度讨论水滑石剥层过程和机理,结合热力学和动力学为剥层反应提供理论基础。对Mg/Fe水滑石纳米单片和K3[Fe(CN)6]进行自组装研究,制备Mg/Fe/[Fe(CN)6]多层薄膜材料,通过XRD、FT-IR、EDS进行样品结构分析,结果表明通过层层自组装制备的样品Mg/Fe/[Fe(CN)6]具备水滑石层板结构。通过层层自组装法在玻碳电极表面进行Mg/Fe/[Fe(CN)6]膜组装,对玻碳电极进行电化学反应条件进行优化,得出Mg/Fe/[Fe(CN)6]/GCE在K3[Fe(CN)6]中进行电化学测试的最优条件为:组装层数为10层、电解质K3[Fe(CN)6]浓度为0.5 mol/L、电解体系pH为9.0,扫描速率为100mV/s。对Mg/Fe/[Fe(CN)6]/GCE的测量稳定性和存储稳定性进行考察,通过循环伏安法(CV)和交流阻抗分析(EIS)对不同Mg/Fe摩尔比Mg/Fe/[Fe(CN)6]/GCE的电化学行为进行分析,研究电荷传输过程机理,并进行等效电路模拟,计算等效阻抗和容抗。
[Abstract]:Hydrotalcite compounds include hydrotalcite and hydrotalcite, the main body of which is generally composed of two kinds of metal hydroxides. Therefore, it is also called layered Double Hydroxide (LDH). A series of supramolecular materials assembled by the intercalation of these compounds are called hydrotalcite intercalation materials, and their unique layered structure makes them more compatible. It has been a century since the discovery of layered hydrotalcite compounds. Researchers have been widely used in the fields of catalytic chemistry, adsorption, ion exchange, electrochemistry, photochemistry and so on. The research field of modern hydrotalcite has been expanded, such as environmental protection, cosmetics, functional polymer materials, nanocomposites, medicine. In this paper, the synthesis, stripping, self-assembly and electrode modification of Mg/Fe-NO3 hydrotalcite were studied. The mg / Fe / mg / Fe / mg / Fe modified electrode was described. [The charge transport mechanism of Fe(CN)6] / GCE provides a theoretical basis for further research on the delamination and electrode modification of hydrotalcite. In this paper, Mg/Fe-CO3 hydrotalcite is prepared. Mg/Fe-NO3 hydrotalcite was prepared by treating Mg/Fe-CO3 hydrotalcite with acid-base method and FT-IR was used to prepare Mg/Fe-NO3 hydrotalcite. SEM and EDS were used to characterize Mg/Fe-NO3 hydrotalcite in formamide solution. Mg/Fe hydrotalcite nano-colloidal solution was prepared by stripping Mg/Fe-NO3 hydrotalcite in formamide solution. It shows the unique phenomenon of Dindall colloid and has good stability. According to the experimental results, it can be found that the colloidal solution can exist steadily for one week under the protection of nitrogen. The different Mg/Fe molar ratio, stripping temperature and stripping time are investigated. The process and mechanism of Mg/Fe-NO3 hydrotalcite stripping are discussed from the point of view of thermodynamics under the initial value of hydrotalcite. The combination of thermodynamics and kinetics provides a theoretical basis for the stripping reaction. Study on Mg/Fe Hydrotalcite Nano-monoliths and K3. [Fe(CN)6] self-assembly to prepare mg / Fe /. [The structure of multilayer thin films was analyzed by XRDX FT-IRDS. The results showed that the samples were prepared by layer by layer self-assembly. [Fe(CN)6] has a hydrotalcite laminate structure. Mg / Fe / Al _ 2O _ 3 was prepared on the surface of glassy carbon electrode by layer-by-layer self-assembly method. [Fe(CN)6 film was assembled, and the electrochemical reaction conditions of glassy carbon electrode were optimized. [Fe(CN)6] / GCE in K3. [The optimal conditions for electrochemical measurement in Fe(CN)6 are as follows: the number of assembled layers is 10 and electrolyte K3 is obtained. [The concentration of Fe(CN)6 is 0.5 mol / L, the pH of electrolytic system is 9.0, and the scanning rate is 100mV / s. [The measured stability and storage stability of Fe(CN)6 / Mg/Fe were investigated by cyclic voltammetry (CV) and AC impedance analysis (EIS). [The electrochemical behavior of Fe(CN)6 / / GCE was analyzed, the mechanism of charge transport was studied, and the equivalent circuit was simulated to calculate the equivalent impedance and capacitance reactance.
【学位授予单位】：湘潭大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB383.2

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