Origins of nanoscale damage to glass-sealed platinum electrodes with submicrometer and nanometer size.
Origins of nanoscale damage to glass-sealed platinum electrodes with submicrometer and nanometer size.
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DOI：
10.1021/ac401316n
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发表时间：
2013-07-02
影响因子：
7.4
通讯作者：
Amemiya, Shigeru
中科院分区：
文献类型：
--
作者：
Nioradze, Nikoloz;Chen, Ran;Kim, Jiyeon;Shen, Mei;Santhosh, Padmanabhan;Amemiya, Shigeru
亚微米和纳米尺寸的玻璃密封铂电极已成功开发并应用于纳米级电化学测量，例如扫描电化学显微镜（SECM）。然而，这些小电极很难使用，因为它们经常会失去电流响应或在电流-距离曲线中给出较低的 SECM 反馈。在这里，我们报告说，这些问题可能是由于静电放电在空气中或通过电化学蚀刻在电解质溶液中容易且不知不觉地对小尖端造成纳米级损坏造成的。损坏的铂电极凹陷并被去除的电极材料污染，以降低其电流响应。扫描电子显微镜和 X 射线能量色散光谱证实了受损 Pt UME 的衰退和污染。凹陷的几何形状在 SECM 中也很明显，但在循环伏安图中并不明显。仅通过循环伏安法表征具有凹进几何形状的受损 Pt 电极可能会由于镶嵌圆盘几何形状的无效假设而从较低的极限电流低估电极尺寸。值得注意的是，通过将铂电极和附近的物体（最重要的是作为静电电荷源的操作员）接地，可以避免静电损坏。通过维持 Pt 电极的恒电位控制，无需在伏安测量之间从内部断开电极与恒电位仪的连接，可以避免电化学损坏。亚微米和纳米尺寸的无损伤铂电极对于可靠和定量的纳米电化学测量至关重要。
Glass-sealed Pt electrodes with submicrometer and nanometer size have been successfully developed and applied for nanoscale electrochemical measurements such as scanning electrochemical microscopy (SECM). These small electrodes, however, are difficult to work with because they often lose a current response or give a low SECM feedback in current–distance curves. Here we report that these problems can be due to the nanometer-scale damage that is readily and unknowingly made to the small tips in air by electrostatic discharge or in electrolyte solution by electrochemical etching. The damaged Pt electrodes are recessed and contaminated with removed electrode materials to lower their current responses. The recession and contamination of damaged Pt UMEs are demonstrated by scanning electron microscopy and X-ray energy dispersive spectroscopy. The recessed geometry is noticeable also by SECM, but is not obvious from a cyclic voltammogram. Characterization of a damaged Pt electrode with recessed geometry only by cyclic voltammetry may underestimate electrode size from a lower limiting current owing to invalid assumption of inlaid disk geometry. Significantly, electrostatic damage can be avoided by grounding a Pt electrode and nearby objects, most importantly, an operator as a source of electrostatic charge. Electrochemical damage can be avoided by maintaining potentiostatic control of a Pt electrode without internally disconnecting the electrode from a potentiostat between voltammetric measurements. Damage-free Pt electrodes with submicrometer and nanometer size are pivotal for reliable and quantitative nanoelectrochemical measurements.
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影响因子：
7.4
作者：
Nioradze, Nikoloz;Kim, Jiyeon;Amemiya, Shigeru
通讯作者：
Amemiya, Shigeru
影响因子：
7.4
作者：
Chang, Jinho;Leonard, Kevin C.;Bard, Allen J.
通讯作者：
Bard, Allen J.
影响因子：
7.4
作者：
Li, Yongxin;Bergman, David;Zhang, Bo
通讯作者：
Zhang, Bo
影响因子：
7.4
作者：
Liu, CY;Bard, AJ
通讯作者：
Bard, AJ
影响因子：
4.5
作者：
BOND, AM;LUSCOMBE, D;ZOSKI, CG
通讯作者：
ZOSKI, CG