Department of Chemistry and Biochemistry, Queens College-CUNY, Flushing, NY 11367, USA.
Chemphyschem. 2010 Sep 10;11(13):3011-7. doi: 10.1002/cphc.201000321.
Most nanometer-sized electrodes reported to date are made from either Pt or Au. For technical reasons, it is difficult to make nanoelectrodes from many other metals (e.g. Hg) by heat-sealing microwires into glass capillaries or by other established techniques. Such nanoelectrodes can be useful for a wide range of analytical and physicochemical applications from high sensitivity stripping analysis (Hg) to pH nano-sensors to studies of electrocatalysis. In this paper, nanometer-sized metal electrodes are prepared by electrodeposition of Hg or Pt on disk-type, polished or recessed nanoelectrodes. The deposition of Hg is monitored chronoamperometrically to produce near-hemispherical electrodes, which are characterized by voltammetry and scanning electrochemical microscopy (SECM). The well-shaped deposits of a solid metal (Pt) at Au nanoelectrodes are prepared and imaged by scanning electron microscopy (SEM). Catalytic metal clusters can also be prepared using this methodology. Electrodes with the metal surface flush with glass insulator, most suitable for quantitative voltammetric and SECM experiments are fabricated by electrodeposition of a metal inside an etched nanocavity.
迄今为止，大多数纳米尺寸的电极都是由 Pt 或 Au 制成的。出于技术原因，很难通过将微丝热封到玻璃毛细管中或通过其他成熟技术，由许多其他金属（例如 Hg）来制造纳米电极。此类纳米电极可用于广泛的分析和物理化学应用，从高灵敏度的剥离分析（Hg）到 pH 纳米传感器再到电催化研究。在本文中，通过在盘状、抛光或凹陷纳米电极上电化学沉积 Hg 或 Pt 来制备纳米尺寸的金属电极。通过计时安培法监测 Hg 的沉积以产生近半球形电极，并用伏安法和扫描电化学显微镜（SECM）对其进行表征。通过扫描电子显微镜（SEM）对 Au 纳米电极上 Pt 的固态金属的良好成型沉积物进行制备和成像。也可以使用这种方法制备催化金属簇。通过在蚀刻纳米腔体内电化学沉积金属来制造金属表面与玻璃绝缘体齐平的电极，这是最适合定量伏安法和 SECM 实验的电极。
