碳微球的溶剂热法制备及其在修饰电极上的应用

发布时间：2018-05-22 17:18

本文选题：碳微球 + 溶剂热法　；参考：《湖北民族学院》2010年硕士论文

【摘要】：碳微球是碳材料的一个分支,具有许多优良的特性,因此很多学者对其进行了研究,包括性质、合成方法、应用等。溶剂热法制备碳微球是近几年来兴起的一种制备碳微球的有效方法,因其操作简单和对环境友好而备受青睐。本论文以葡萄糖为碳源,利用溶剂热的方法对碳微球的合成进行了探讨,制得了球形和橄榄球形碳球,并对影响碳微球形貌和直径的条件进行了探索。实验数据表明,溶剂和升温速率分别是影响碳微球形貌和直径大小的关键因素。长期以来,碳微球的应用主要集中在复合材料模板、催化剂载体和锂离子电池材料等方面,碳微球在修饰电极上的应用几乎没有报道。本论文通过对碳微球性质的深入分析,提出了将碳微球修饰于玻碳电极表面,制得碳微球修饰玻碳电极的构想,实验证明这种构想是可行的,在碳微球修饰玻碳电极对镉离子的测定中修饰电极表现出的良好的选择性、稳定性、和低检测限充分说明了这一点。从而拓展了碳微球的应用领域。论文主要包括以下几个方面的内容: 1.碳微球的溶剂热法制备。利用溶剂热法制备碳微球,并对碳微球进行了表征。通过改变反应的升温速率和溶剂,使得碳微球的大小和形貌都分别发生了改变,实验表明,碳微球的直径受反应升温速率的影响,而形貌则受溶剂的影响。为研究碳微球的形成机理研究提供了依据。 2.碳微球修饰玻碳电极的制备。通过对不同分散剂分散效果的对比,选择环己醇作为分散剂,制备了碳微球修饰玻碳电极,并对修饰电极进行了表征,扫描电镜表面碳微球能较好地分散并修饰于玻碳电极上,碳微球的修饰对玻碳电极的性能产生了影响。碳微球修饰玻碳电极对镉离子具有响应。 3.碳微球修饰玻碳电极对镉离子的测定及其条件的优化。详细研究了利用碳微球修饰玻碳电极测量镉离子浓度的条件,采用循环伏安法研究了镉离子在修饰电极上的伏安行为和最佳检测条件。在所选最优化实验条件下,峰电流与镉离子浓度在5×10~(-9)-1.34×10~(-7) mol/L和1.34×10~(-7)-1×10~(-6) mol/L范围内呈现良好的线性关系,线性相关系数分别为0.9989和0.9998,检测限为10~(-10)mol/L。该法用于模拟水样中镉离子的测定,结果令人满意。
[Abstract]:Carbon microspheres are a branch of carbon materials with many excellent properties, so many scholars have studied them, including their properties, synthesis methods, applications and so on. Solvothermal preparation of carbon microspheres is an effective method for the preparation of carbon microspheres in recent years. In this paper, the synthesis of carbon microspheres using glucose as carbon source was investigated by solvothermal method. Spherical and rugby carbon spheres were prepared, and the conditions affecting the morphology and diameter of carbon microspheres were explored. Experimental data show that solvent and heating rate are the key factors affecting the morphology and diameter of carbon microspheres, respectively. For a long time, the application of carbon microspheres has been mainly focused on composite template, catalyst carrier and lithium ion battery materials, etc. The application of carbon microspheres in modified electrodes has not been reported. Based on the analysis of the properties of carbon microspheres, the idea of preparing carbon microspheres to modify glassy carbon electrodes by modifying carbon microspheres on the surface of glassy carbon electrodes is proposed in this paper, which is proved to be feasible by experiments. The good selectivity, stability and low detection limit of the modified electrode for the determination of cadmium ion at the glassy carbon electrode modified with carbon microspheres fully demonstrate this point. Thus the application field of carbon microspheres is expanded. This paper mainly includes the following aspects: 1. Preparation of carbon microspheres by solvothermal method. Carbon microspheres were prepared by solvothermal method and characterized. The size and morphology of the carbon microspheres were changed by changing the heating rate and solvent. The experimental results showed that the diameter of the carbon microspheres was affected by the reaction heating rate and the morphology was influenced by the solvent. It provides a basis for the study of the formation mechanism of carbon microspheres. 2. Preparation of glassy carbon electrode modified with carbon microspheres. By comparing the dispersion effects of different dispersants, the carbon microspheres modified glassy carbon electrodes were prepared by using cyclohexanol as dispersant, and the modified electrodes were characterized. The carbon microspheres on the surface of scanning electron microscope can be dispersed and modified onto the glassy carbon electrodes. The modification of carbon microspheres affected the performance of glassy carbon electrode. Carbon microspheres modified glassy carbon electrode are responsive to cadmium ion. 3. Determination of cadmium ion at glassy carbon electrode modified by carbon microspheres and optimization of its conditions. The conditions for the determination of cadmium ion concentration at glassy carbon electrode modified by carbon microspheres were studied in detail. The voltammetric behavior of cadmium ion on the modified electrode and the optimum detection conditions were studied by cyclic voltammetry. Under the optimized experimental conditions, the linear relationship between the peak current and the concentration of cadmium ion in the range of 5 脳 10 ~ (-9) -1.34 脳 10 ~ (-7) mol/L and 1.34 脳 10 ~ (10) ~ (-7) ~ (-1) mol/L was obtained. The linear correlation coefficients were 0.9989 and 0.9998, respectively, and the detection limit was 10 ~ (-10) mol 路L ~ (-1). The method has been applied to the determination of cadmium ion in simulated water with satisfactory results.
【学位授予单位】：湖北民族学院
【学位级别】：硕士
【学位授予年份】：2010
【分类号】：O646.54

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