Zhang Bo, Galusha Jeremy, Shiozawa Peter G, Wang Gangli, Bergren Adam Johan, Jones Ronald M, White Ryan J, Ervin Eric N, Cauley Chris C, White Henry S
Department of Chemistry, University of Utah, 315 S, 1400 E, Salt Lake City, Utah 84112, USA.
Anal Chem. 2007 Jul 1;79(13):4778-87. doi: 10.1021/ac070609j. Epub 2007 Jun 6.
A simple benchtop method of fabricating glass-sealed nanometer-sized Au and Pt disk electrodes, glass nanopore electrodes, and glass nanopore membranes is reported. The synthesis of all three structures is initiated by sealing the tips of electrochemically sharpened Au and Pt microwires into glass membranes at the end of a soda lime or lead glass capillary. Pt and Au nanodisk electrodes are obtained by hand polishing using a high-input impedance metal oxide semiconductor field effect transistor (MOSFET)-based circuit to monitor the radius of the metal disk. Proper biasing of the MOSFET circuit, based on a numerical analysis of the polishing circuit impedance, allows for the reproducible fabrication of Pt disk electrodes of radii as small as 10 nm. Significantly smaller background currents in voltammetric measurements are obtained using lead glass capillaries, a consequence of the lower mobility of Pb(2+) (relative to Na(+)) in the glass matrix. Glass nanopore electrodes and glass nanopore membranes are fabricated, respectively, by removal of part or all of the metal sealed in the glass membranes. The nanostructures are characterized by atomic force microscopy, steady-state voltammetry, and ion conductivity measurements.
报道了一种在实验台上制备玻璃密封纳米尺寸金和铂圆盘电极、玻璃纳米孔电极及玻璃纳米孔膜的简单方法。所有这三种结构的合成均始于将电化学锐化的金和铂微丝尖端密封到钠钙玻璃或铅玻璃毛细管末端的玻璃膜中。通过使用基于高输入阻抗金属氧化物半导体场效应晶体管(MOSFET)的电路进行手工抛光来获得铂和金纳米圆盘电极,该电路用于监测金属圆盘的半径。基于对抛光电路阻抗的数值分析,对MOSFET电路进行适当偏置,可实现半径小至10nm的铂圆盘电极的可重复制备。使用铅玻璃毛细管在伏安测量中可获得显著更小的背景电流,这是玻璃基质中Pb(2+)(相对于Na(+))迁移率较低的结果。分别通过去除密封在玻璃膜中的部分或全部金属来制备玻璃纳米孔电极和玻璃纳米孔膜。通过原子力显微镜、稳态伏安法和离子电导率测量对这些纳米结构进行表征。