TiO_(2)/CB-NiCo_(2)O_(4)修饰玻碳电极的制备及其对葡萄糖的电化学测定

Preparation of TiO_(2)/CB-NiCo_(2)O_(4)nanocomposites modified glassy carbon electrode and its application for electrochemical determination of glucose

利用低温下的水化学生长法合成了镍钴氧化物(NiCo_(2)O_(4))纳米针,因其自组装而表现出立方晶相,再用二氧化钛/炭黑(TiO_(2)/CB)对NiCo_(2)O_(4)表面进行了改性,合成了TiO_(2)/CB-NiCo_(2)O_(4)复合纳米材料.用X射线光电子能谱仪(XPS)、扫描电子显微镜(SEM)、能量色散X射线光谱仪(EDX)图谱对材料的形貌进行了表征,运用循环伏安法(CV)、时间-电流(i-t)曲线法考察了TiO_(2)/CB-NiCo_(2)O_(4)修饰玻碳电极的电化学行为.实验发现:TiO_(2)/CB-NiCo_(2)O_(4)修饰电极对葡萄糖的氧化有良好的电催化性能,其线性范围为0.001~1.780 mmol·L^(-1),检测限为0.53μmol·L^(-1)(信噪比S/N=3).将该法用于实际样品中葡萄糖的测定,结果令人满意.

Nickel-cobalt oxide(NiCo_(2)O_(4))nanoneedles were synthesized by hydration method at low temperature,which showed cubic crystal phase due to its self-assembly.Then,the surface of NiCo_(2)O_(4) was modified by titanium dioxide/carbon black(TiO_(2)/CB)to synthesize TiO_(2)/CB-NiCo_(2)O_(4) composite nanomaterials.The as-prepared materials were characterized by X-ray photoelectron spectromscanning(XPS),electron microscope(SEM)and energy dispersive X-ray detector(EDX).The electrochemical behavior of TiO_(2)/CB-NiCo_(2)O_(4) modified glassy carbon electrode was investigated by cyclic voltammetry(CV)and current-time curve(i-t).It was found that TiO_(2)/CB-NiCo_(2)O_(4) modified electrode had good electrocatalytic performance for glucose oxidation with a linear range from 0.001 to 1.780 mmol·L^(-1)and a detection limit of 0.53μmol·L^(-1)(signal-to noise ratio S/N=3).The method has been applied to the determination of glucose in real samples with satisfactory results.