溶胶凝胶法制备纳米二茂铁微粒及其电催化性能研究

采用溶胶凝胶法制备了二茂铁微粒后,将所得二茂铁微粒超声分散于甲基三甲氧基硅烷形成的溶胶结构中,得到了溶胶凝胶固载的二茂铁纳米粒子,并制成化学修饰碳糊电极.采用扫描电镜(SEM)方法对制得粉体微粒进行表征,并通过循环伏安实验与计时安培实验测试修饰电极的电催化活性.结果表明:采用溶胶凝胶法分散的二茂铁纳米粒子,粒径约为300nm,将二茂铁固载于SiO2的凝胶结构中有效地提高了修饰电极的稳定性与二茂铁的分散性.在优化的实验条件下,修饰电极对抗坏血酸(AA)的氧化具有明显的催化作用,安培法检测AA的线性范围为3.0×10-6～2.5×10-3 mol/L,检出限为1.0×10-6 mol/L(3sb,n=10).

Preparation of sol-gel derived ferrocene nano particles and its electrocatalytic activity

The ferrocene nano particles were synthesized from sol-gel technique, and the resulting ferrocene particles were doped into the gel structure derived by methyltrimethoxysilane via associated the sol until result a homogeneous solution, additionally, a chemically modified carbon paste electrode （sol-gel/Fc/CPE） was fabricated. The morphology of ferrocene particles were characterized by scanning electron microscopy （SEM） experiments. The electrocatalytic performance of the sol-gel/Fc/CPE modified electrode was investigated by cyclic voltammetry and chronoamperometry experiments. The results showed that, the size of ferrocene paticles dispersed in sol-gel stucture was about 300 nm with good adherin, and the stability of the resulting modified electrode was improved evidently. Under the optimum conditions, the modified electrode had good electrocatalytic activity toward the oxidation of AA, the catalytic peak current of the modified electrode was proportional to the concentration of AA in the range of 3.0×10^-6～2.5×10^-3 mol/L and the detection limit was 1.0×10^-6mol/L（3sb,n=10）.