LCMCP, UMR7574 CNRS/UPMC, Collège de France, 11 place Marcellin Berthelot, 75231 Paris Cedex 05, France.
Chemphyschem. 2010 Jun 21;11(9):1971-7. doi: 10.1002/cphc.200900929.
A sol-gel strategy is developed to fabricate highly regular Au nanoelectrode arrays (NEAs) consisting of a nanoperforated ultrathin membrane of ZrO(2), which exhibits a well-ordered array of pores (65+/-5) nm in diameter with a mean center-to-center distance of (110+/-10) nm, on a polycrystalline gold surface. The structural properties are investigated by field-emission scanning electron microscopy (FE-SEM), while grazing incidence small-angle X-ray scattering (GISAXS) is used to assess the thickness homogeneity and the period of the array of electrodes. In addition, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) are carried out to describe quantitatively the accessibility, electrochemical behavior, and diffusion processes of the gold NEA. A model applying parameters obtained from FE-SEM, CV, and EIS analyses is proposed to simulate the experimental results. A fairly good agreement between the experimental and the simulated data is obtained, thus allowing the deconvolution of the different diffusion regimes at the NEA.
采用溶胶-凝胶策略制备了由 ZrO(2) 纳米穿孔超薄膜组成的高度规则的 Au 纳米电极阵列 (NEA)，该超薄膜具有直径为 (65+/-5)nm 的规则排列的孔，平均中心到中心距离为 (110+/-10)nm，位于多晶金表面上。通过场发射扫描电子显微镜 (FE-SEM) 研究了结构特性，而掠入射小角 X 射线散射 (GISAXS) 用于评估电极阵列的厚度均匀性和周期。此外，进行了循环伏安法 (CV) 和电化学阻抗谱 (EIS) 以定量描述 Au NEA 的可及性、电化学行为和扩散过程。提出了一个应用从 FE-SEM、CV 和 EIS 分析中获得的参数的模型来模拟实验结果。实验数据和模拟数据之间得到了相当好的一致性，从而允许对 NEA 中的不同扩散区域进行解卷积。
