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扫描凝胶电化学显微镜(SGECM):电流和切向力反馈的横向物理分辨率。

Scanning Gel Electrochemical Microscopy (SGECM): Lateral Physical Resolution by Current and Shear Force Feedback.

机构信息

Université de Lorraine, CNRS, Laboratoire de Chimie Physique et Microbiologie pour les Matériaux et l'Environnement (LCPME), F-54000 Nancy, France.

出版信息

Anal Chem. 2020 May 5;92(9):6415-6422. doi: 10.1021/acs.analchem.9b05538. Epub 2020 Apr 16.

Abstract

Scanning gel electrochemical microscopy (SGECM) is a novel technique measuring local electrochemistry based on a gel probe. The gel probe, which is fabricated by electrodeposition of hydrogel on a microdisk electrode, immobilizes the electrolyte, and constitutes a two-electrode system upon contact with the sample. The contact area determines the lateral physical resolution of the measurement, and considering the soft nature of the gel it is essential to be well analyzed. In this work, the lateral physical resolution of SGECM is quantitatively studied from two aspects: (1) marking single sampling points by locally oxidizing Ag to AgCl and measuring their size; (2) line scan over reference samples with periodic topography and composition. The gel probe is approached to the sample by either current or shear force feedback, and the physical resolution of them is compared. For the optimal gel probe based on 25 μm diameter Pt disk electrode of ≈ 2, the lateral physical resolution of SGECM at contact position is ca. 50 μm for current feedback and ca. 63 μm for shear force feedback. More importantly, the lateral physical resolution of SGECM can be flexibly tuned in the range of 14-78 μm by pulling or pressing the gel probe after touching the sample. In general, current feedback is more sensitive to gel-sample contact than shear force feedback. But the latter is more versatile, which is also applicable to nonconductive samples.

摘要

扫描凝胶电化学显微镜(SGECM)是一种基于凝胶探针测量局部电化学的新技术。凝胶探针通过在微盘电极上电沉积水凝胶制成,固定电解质,并在与样品接触时构成两电极系统。接触面积决定了测量的横向物理分辨率,并且由于凝胶的柔软性质,必须对其进行很好的分析。在这项工作中,从两个方面定量研究了 SGECM 的横向物理分辨率:(1)通过局部氧化 Ag 到 AgCl 来标记单个采样点,并测量它们的大小;(2)在具有周期性形貌和组成的参考样品上进行线扫描。通过电流或剪切力反馈将凝胶探针接近样品,并比较它们的物理分辨率。对于基于直径为 25μm 的 Pt 圆盘电极的最佳凝胶探针,在接触位置,SGECM 的横向物理分辨率约为 50μm(电流反馈)和约 63μm(剪切力反馈)。更重要的是,在接触样品后拉动或按压凝胶探针,可以将 SGECM 的横向物理分辨率在 14-78μm 的范围内灵活调节。一般来说,电流反馈比剪切力反馈对凝胶-样品接触更敏感。但后者更通用,也适用于非导电样品。

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