Kim Jiyeon, Renault Christophe, Nioradze Nikoloz, Arroyo-Currás Netzahualcóyotl, Leonard Kevin C, Bard Allen J
Department of Chemistry, The University of Rhode Island , Kingston, Rhode Island 02881, United States.
Laboratoire de Physique de la Matière Condensée, Ecole Polytechnique Palaiseau , 91128 Palaiseau, France.
Anal Chem. 2016 Oct 18;88(20):10284-10289. doi: 10.1021/acs.analchem.6b03024. Epub 2016 Oct 3.
We report the crucial components required to perform scanning electrochemical microscopy (SECM) with nanometer-scale resolution. The construction and modification of the software and hardware instrumentation for nanoscale SECM are explicitly explained including (1) the LabVIEW code that synchronizes the SECM tip movement with the electrochemical response, (2) the construction of an isothermal chamber to stabilize the nanometer scale gap between the tip and substrate, (3) the modification of a commercial bipotentiostat to avoid electrochemical tip damage during SECM experiments, and (4) the construction of an SECM stage to avoid artifacts in SECM images. These findings enabled us to successfully build a nanoscale SECM, which can be utilized to map the electrocatalytic activity of individual nanoparticles in a typical ensemble sample and study the structure/reactivity relationship of single nanostructures.
我们报告了实现具有纳米级分辨率的扫描电化学显微镜（SECM）所需的关键组件。详细解释了用于纳米级SECM的软件和硬件仪器的构建与修改，包括：（1）使SECM尖端移动与电化学响应同步的LabVIEW代码；（2）构建等温腔以稳定尖端与基底之间的纳米级间隙；（3）对商用双恒电位仪进行修改以避免在SECM实验期间电化学尖端受损；（4）构建SECM平台以避免SECM图像中出现伪像。这些发现使我们能够成功构建纳米级SECM，可用于绘制典型集合样品中单个纳米颗粒的电催化活性图谱，并研究单个纳米结构的结构/反应性关系。
