In situ cleaning and activation of solid electrode surfaces by pulsed laser light
In situ cleaning and activation of solid electrode surfaces by pulsed laser light
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通过脉冲激光原位清洁和活化固体电极表面
DOI：
10.1021/ac00276a064
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发表时间：
1984
影响因子：
7.4
通讯作者：
R. D. Knight
中科院分区：
文献类型：
--
作者：
E. Hershenhart;R. McCreery;R. D. Knight
先生道：无论是用于分析还是用于研究电极过程，固体电极的表面都会随着时间的推移而变化，这是由于溶液中物质的吸附或表面本身的化学变化。这些变化通常会导致灵敏度或可逆性的变化，在极端情况下会导致电荷转移的完全抑制。电分析化学起源于滴汞电极（DME），因为DME表面每隔几秒钟就更新一次，从而确保了清洁、可再现的表面。我们在这里报告了一个类似于DME的固体电极，其中强烈的激光脉冲isused直接在感兴趣的溶液中清洁和活化铂或玻璃碳表面。强脉冲激光辐射对电极的影响包括去除聚合物膜或吸附膜以及电子转移速率的大幅度增加。虽然DME具有表面周期性更新的重要特性，但其潜在范围限于汞的范围，并且其机械性质使其不适合于许多应用。亚当斯开发碳糊的最初动机是希望得到一种适用于汞氧化电位为正的可再生固体电极（1）。已经设计了各种方法用于预处理固体电极，包括抛光、化学预处理、燃烧、电位循环、真空热处理和离子蚀刻（1-11）。这些程序对电荷转移速率产生广泛变化的影响，主要是因为它们在所得的表面清洁度方面变化很大。制备固体电极表面没有公认的标准程序，并且类似程序的结果在不同实验室之间差异很大。这些过程都不能原位去除吸附膜，也不能像DME那样在短时间内重复。电化学的理想表面处理是可以直接在目标溶液中进行的处理，可以产生清洁的、可再现的表面，并且可以在几秒或更短的时间内重复。激光辐射已经被用于通过在溶液外预处理金属以重新分布合金成分来延缓腐蚀（12，13）。激光脉冲也已被用于原位通过去除氧化层（14）和加速电镀（15）来引发腐蚀。在本工作中，将Nd：YAG激光的二次谐波（532 nm）聚焦到
Sir: Whether used for analysis or for studyingelectrode processes, the surface of a solid electrode changes with time due to adsorption of species from solution or chemical changes to the surface itself. These changes often result in variations in sensitivity or reversibility, and in extreme cases lead to complete inhibition of charge transfer. Electroanalytical chemistry originated with the dropping mercury electrode (DME) because the DME surface was renewed every few seconds and a clean, reproducible surface was thereby assured. We report here an analogue to the DME for solid electrodes, where an intense laser pulse isused to clean and activate a platinum or glassy carbon surface directly in the solution of interest. The effects of intense pulsed laser radiation on electrodes include removal of polymeric or adsorbed films and largé increases in electron transfer rate. While the DME has the important property of periodic renewal of the surface, its potential range is constrained to that of mercury, and its mechanical properties make it un-suitable for many applications. The original motivation for the development of carbon paste by Adams was the desire for a renewable Solid electrode suitablefor potentials positive of mercury oxidation (1). A variety of methods have been devised for pretreating solid electrodes, including polishing, chemical pretreatment, flaming; potential cycling, vacuum heat treatments, and ion etching (1-11). These procedures produce widely varying effects on charge transfer rate, mainly because they vary greatly in the resulting degree of surface cleanliness. There is no agreed uponstandard procedure for preparing solid electrode surfaces, and results for similar procedures vary greatly from lab to lab. None of these processes is capable of removing adsorbed films in situ, and none is repeatable on a short time scale, like the DME. An ideal surface treatment for electrochemistry would be one which could be carried out directly in the solution of interest, would generate a clean, reproducible surface, and would be repeatable on a time scale of seconds or less.Laser radiation has been used to retard corrosion by pre-treating a metal outside the solution to redistribute alloy components (12, 13). Laser pulses have also been used in situ to initiate corrosion by removing oxide layers (14) and ac-celerate electroplating (15). In the present work, the second harmonic (532 nm) of a Nd: YAG laser was focused onto