纳米硫化铜修饰玻碳电极的原位制备及分析应用  

In Situ Preparation of Nano-CuS Modified Glassy Carbon Electrode and Its Analytical Application

作　　者：刘有芹[1] 肖乔[1] 翟文颖[1] 颜芸[1] 徐悦华[1] 徐莉[1] 

机构地区：[1]华南农业大学理学院生物材料研究所,广州510642

出　　处：《材料导报》2013年第10期26-30,56,共6页Materials Reports

基　　金："211工程"重点学科建设项目(2009B010100001);广东省自然科学基金(5300842)

摘　　要：采用镀膜/循环伏安法原位制备了纳米CuS/GC电极,研究了其制备机理,探讨了具有最大电催化活性的制备及测试条件。通过SEM、EIS对修饰膜进行了表征,表明纳米CuS粒子均匀附着于电极表面,具有较高的导电性。采用电流-时间曲线法研究了CuS/GC电极的分析性能,结果表明,电极对H2O2浓度的响应时间短于0.1s,在0.67～20.5μmol.L-1及0.033～2.93mmol.L-1范围内,电流变化和H2O2浓度的线性方程分别为Δi(μA)=-0.0081+0.0267c(R=0.9998)及Δi(μA)=0.7378+22.17c(R=0.9930),检出限为6.0×10-8 mol.L-1(S/N=3)。该修饰电极具有较高的电化学及贮存稳定性,实际水样测试结果表明回收率为92%～98%,相对标准偏差小于3.6%。A nano-copper sulfide modified glassy carbon electrode （CuS/GC） was successfully prepared by a novel film plating/potential cycling method. The mechanism of nano-copper sulfide formation and factors affecting its electrocatalytic activity were investigated by cyclic voltammetry. The modified electrode surface was characterized by SEM and EIS and results indicate that nano-CuS particles are uniformly fixed on electrode surface with high conducti- vity. The analytical performance of CuS/GC was tested by amperometric detection. The response time to achieve the steady-state current is less than 0. 1 s, and linear equations in the range of 0. 67--20.5μmol . L^-1 and 0. 033--2. 93 mmol . L^-1 are △i（μA）=-0. 0081＋ 0. 0267c （R=0. 9998） and △i （μA） =0. 7378＋22. 17c （R=0. 9930）, respectively. The detection limit was 6. 0X 10-8 mol . L^-1 （S/N=3）. CuS/GC has high electrochemical and storage stabili- ty and is used for the determination of H202 in real water. The recovery is in the range of 92% to 98% with relative standard deviation being less than 3. 6%.

关 键 词：镀膜 循环伏安法 硫化铜 玻碳电极 过氧化氢 电催化 

分 类 号：TB321[一般工业技术—材料科学与工程] O661.1[理学—分析化学]