铁氰化铜/Nafion/g-C_3N_4复合修饰电极的制备及电催化检测水合肼

Fabrication of Electrocatalytic Sensor Based on Cu HCF/Nafion/g-C_3N_4 Nanocomposite Modified Glassy Carbon Electrode for Detection of Hydrazine Hydrate

利用铁氰化钾和硝酸铜为原料沉淀法制备铁氰化铜(copper hexacyanoferrate,CuHCF),三聚氰胺高温热解和超声剥离法合成类石墨相氮化碳(g-C_3N_4)纳米片。将所制备的CuHCF和g-C_3N_4超声分散到含Nafion的乙醇溶液中,得到了CuHCF/Nafion/g-C_3N_4纳米复合物。利用扫描电子显微镜、X射线衍射仪和比表面积检测仪对所制备的样品进行结构表征。采用滴涂法将该纳米复合物修饰到玻碳电极表面,得到CuHCF/Nafion/g-C_3N_4/GCE。研究发现:该修饰电极对水合肼具有良好的电催化氧化作用。在优化实验条件下,当水合肼的浓度介于10~1 100μmol/L时,其催化氧化峰电流与浓度具有良好的线性关系,水合肼检测限低至1μmol/L。该传感器具有良好的选择性、重复性和稳定性。

A novel sensor based on CuHCF/Nafion/g-C3N4 nano-sheet nanocomposite has been developed for rapid and selective sensing of hydrazine hydrate. The nanocomposite was prepared by ultrasonic dispersion of the mixture of copper hexacyanoferrate（CuHCF）, prepared from the reaction between potassium ferricyanide and copper nitrate, and C3N4 nanosheet, obtained by high temperature pyrolysis of melamine followed by ultrasonic treatment of the g-C3N4 suspension, in aqueous ethanol containing Nafion. The morphology and structure of the materials were characterized by scanning electron microscope（SEM）, X-ray diffractometer（XRD） and Brunauer-Emmett-Teller（BET） specific surface area analyzer. The as-prepared CuHCF/Nafion/g-C3N4 nanocomposite modified glassy carbon electrode showed excellent electrochemical performance towards the oxidation of hydrazine by means of cyclic voltammetry and chronoamperometry. Under optimized experimental conditions, the anodic current was linearly proportional to the hydrazine hydrate concentration in the range of 10 to 1 100 μmol/L. The detection limit of the method was as low as 1 μmol/L. Furthermore, results also showed that the sensor had good selectivity, stability and reproducibility.