聚邻苯二胺负载纳米铜氧化物修饰玻碳电极的制备及表征  

Preparation of Nano-copper Oxide Loaded Poly-o-phenylenediamine Modified Glassy Carbon Electrode and Its Characterization

作　　者：刘有芹[1] 乐文志[1] 薛峰峰[2] 颜芸[1] 徐莉[1] 

机构地区：[1]华南农业大学理学院应用化学系,广州510642 [2]河北工程技术高等专科学校,沧州061001

出　　处：《材料导报》2010年第8期103-108,共6页Materials Reports

基　　金：广东省自然科学基金博士科研启动基金(5300842)

摘　　要：在磷酸盐缓冲溶液中于玻碳电极表面聚合邻苯二胺,再负载纳米铜氧化物,成功制备了邻苯二胺负载纳米铜氧化物修饰玻碳电极(CuO/P-oPD/GC)。探讨了聚合和负载机理,用电化学交流阻抗谱表征了修饰电极界面的阻抗变化,用扫描电镜表征了聚邻苯二胺膜和负载铜氧化物后的表面形态,发现CuO/P-oPD/GC电极对H2O2有显著的电催化氧化、还原双重活性,并呈现"协同增敏"效应。考察了制备条件对CuO/P-oPD/GC电极电催化活性的影响,最佳CuO负载扫描次数为20,Cu2+的质量浓度为1.67mmol/L。对H2O2电催化氧化的线性方程为Δipa(μA)=0.08+5.64c(mmol/L)(R=0.9982),线性范围为2.4×10-2～48mmol/L,检测限为2.8×10-3mmol/L(3S/k);电催化还原的线性方程为Δipc(μA)=0.11-2.45c(mmol/L)(R=0.9820),线性范围为2.4×10-3～38.4mmol/L,检测限为2.0×10-4mmol/L(3S/k)。该复合材料修饰电极的灵敏度高、稳定性好,用于实际水样中H2O2测定结果满意。A nano-copper oxide loaded poly-o-phenylenediamine film modified glassy carbon electrode （CuO/P- oPD/GC） is successfully prepared. First, the poly-o-phenylenediamine film is polymerized on GC electrode surface in phosphate buffer solution by cyclic voltammetry, and then the nano-copper oxide is loaded in P-oPD film. The mecha- nism of polymerization and loading is discussed. The impedance changes of GC electrode surface during the modifica- tion process are characterized by electrochemical AC impedance spectroscopy, and the surface morphology of poly-o- phenylenediamine film and nano-CuO loaded poly-o-phenylenediamine film are characterized by scanning electron mi- croscope. The results show that the CuO/P-oPD/GC electrode has significant dual activity toward the electrocatalytic oxidation and reduction of H2O2, finding that CuO and P-oPD show synergistic effect. The factors influencing the electro-catalytic activity of CuO/P-oPD/GC electrode are investigated, showing that the optimal scanning number is 20 and Cu2＋ concentration is 1.67mmol/L. The linear regression equation for H2O2 oxidation is △ipa （μA）=0. 08＋5.64c （mmol/L） （R=0. 9982）, and the linear range is 2.4× 10-2 48mmol/L with a detection limit of 2.8× 10-3mmol/L （3S/k）. The linear regression equation for H2O2 reduction was △ipc （μA）=0. 11-2. 45c（mmol/L） （R=0. 9820） and the linear range is 2. 4×10-3 -38. 4mmol/L with a detection limit of 2. 0× 10-4mmol/L （3S/k）. The CuO/P-oPD/ GC composite electrode has high sensitivity and good stability, which is used for H2O2 determination in actual water sample with satisfactory results.

关 键 词：邻苯二胺 铜氧化物 玻碳电极 过氧化氢电催化 

分 类 号：O631.1[理学—高分子化学] O657.1[理学—化学]