Department of Chemistry, Indiana University, 800 East Kirkwood Avenue, Bloomington, Indiana 47405, United States.
Langmuir. 2011 Nov 15;27(22):13925-30. doi: 10.1021/la203032u. Epub 2011 Oct 24.
Scanning electrochemical-atomic force microscopy (SECM-AFM) is a powerful technique that can be used to obtain in situ information related to electrochemical phenomena at interfaces. Fabrication of probes to perform SECM-AFM experiments remains a challenge. Herein, we describe a method for formation of microelectrodes at the tip of commercial conductive AFM probes and demonstrate application of these probes to SECM-AFM. Probes were first insulated with a thin parylene layer, followed by subsequent exposure of active electrodes at the probe tips by mechanical abrasion of the insulating layer. Characterization of probes was performed by electron microscopy and cyclic voltammetry. In situ measurement of localized electrochemical activity with parylene-coated probes was demonstrated through measurement of the diffusion of Ru(NH)(6)(3+) across a porous membrane.
扫描电化学原子力显微镜（SECM-AFM）是一种强大的技术，可以用于获得与界面处电化学现象相关的原位信息。用于进行 SECM-AFM 实验的探针的制造仍然是一个挑战。在此，我们描述了一种在商用导电 AFM 探针的尖端形成微电极的方法，并展示了这些探针在 SECM-AFM 中的应用。首先，探针用一层薄的聚对二甲苯层进行绝缘，然后通过机械磨损绝缘层来暴露探针尖端的活性电极。通过电子显微镜和循环伏安法对探针进行了表征。通过测量 Ru(NH)(6)(3+)穿过多孔膜的扩散，证明了用聚对二甲苯涂层探针进行原位局部电化学活性测量的可行性。
