The Fabrication and Characterization of a Nickel Nanoparticle Modified Boron Doped Diamond Electrode for Electrocatalysis of Primary Alcohol Oxidation

The Fabrication and Characterization of a Nickel Nanoparticle Modified Boron Doped Diamond Electrode for Electrocatalysis of Primary Alcohol Oxidation
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DOI:
10.1002/elan.200900325
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发表时间:
2009-12
期刊:
影响因子:
3
通讯作者:
N. Stradiotto;Kathryn E. Toghill;Lei Xiao;A. Moshar;R. Compton
N. Stradiotto;Kathryn E. Toghill;Lei Xiao;A. Moshar;R. Compton
中科院分区:
化学4区
文献类型:
--
作者:
N. Stradiotto;Kathryn E. Toghill;Lei Xiao;A. Moshar;R. Compton

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报道了镍纳米粒子修饰BDD电极的制备及其在伯醇电氧化中的应用。采用电沉积方法,以Ni(NO3)2为改性剂,在pH 5的醋酸钠溶液中进行改性。镍改性的BDD(Ni-BDD)的表征进行了非原位原子力显微镜(AFM)和高分辨率扫描电子显微镜(SEM)结合能量色散X射线光谱(EDX)。在BDD表面上观察到大的镍纳米颗粒,高度为5至690 nm,体积为0.18 μ m(-3),平均数密度约为100 μ m。测定了13 × 10(6)纳米颗粒cm(-2)。大范围的尺寸表明渐进的而不是瞬时的成核和生长。在碱性介质中,用未修饰的BDD、Ni-BDD和块体Ni大电极对乙醇和甘油进行电催化。Ni-BDD电极具有较好的电催化性能,对甘油的灵敏度最高。分别在2.8-28.0 mM和23-230 μ M的浓度范围内获得乙醇和甘油添加物的线性校准图。这得到乙醇的检测极限为1.7mM,灵敏度为0.31mA/M,甘油的检测极限为10.3 μ M,灵敏度为35 mA/M。
We report the fabrication of a Ni nanoparticle modified BDD electrode and its application in the electrocatalysis of primary alcohol electrooxidation. Modification was achieved via electrodeposition from Ni(NO3)(2) dissolved in sodium acetate solution (pH 5). Characterization of the Ni-modified BDD (Ni-BDD) was performed using ex situ atomic force microscopy (AFM) and high resolution scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectroscopy (EDX). Large nanoparticles of nickel were observed on the BDD surface ranging 5 to 690 nm in height and 0.18 mu m(-3) in volume, and an average number density of ca. 13 x 10(6) nanoparticles cm(-2) was determined. The large range of sizes suggests progressive rather than instantaneous nucleation and growth. Electrocatalysis of ethanol and glycerol, was conducted in an alkaline medium using an unmodified BDD, Ni-BDD and a bulk Ni macro electrode. The Ni-BDD electrode gave the better electrocatalytic performance, with glycerol showing the greatest sensitivity. Linear calibration plots were obtained for the ethanol and glycerol additions over concentration ranges of 2.8-28.0 mM and 23-230 mu M respectively. This gave an ethanol limit of detection of 1.7 mM and sensitivity of 0.31 mA/M, and the glycerol a limit of detection of 10.3 mu.M with a sensitivity of 35 mA/M.