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变温扫描电化学显微镜。

Scanning electrochemical microscopy at variable temperatures.

机构信息

Analytische Chemie-Elektroanalytik & Sensorik, Ruhr-Universität Bochum, Bochum, Germany.

出版信息

Phys Chem Chem Phys. 2013 Apr 14;15(14):5215-23. doi: 10.1039/c3cp43520b.

DOI:10.1039/c3cp43520b
PMID:23348196
Abstract

All chemical reactions are influenced by temperature, however, temperature is usually not considered an important parameter which has to be varied or at least controlled in SECM measurements. A precise temperature-control unit was designed and integrated into a SECM setup which allows setting the temperature of the sample and the adjacent electrolyte in a range between 0 and 100 °C without causing convection. Data acquisition was synchronized with the current pulses through the Peltier element to decrease the noise and keep the tip-to-sample distance constant during imaging. SECM images in the feedback mode, generator collector mode and the redox competition mode for model samples such as an enzyme entrapped within a polymer spot or oxygen reduction catalysts demonstrate the importance of controlling temperature as well as performing SECM experiments at predefined and constant increased temperature.

摘要

所有化学反应都受到温度的影响,然而,在 SECM 测量中,温度通常不被认为是一个需要改变或至少控制的重要参数。设计了一个精确的温度控制单元,并将其集成到 SECM 设置中,允许在 0 到 100°C 的范围内设置样品和相邻电解质的温度,而不会引起对流。通过珀耳帖元件使数据采集与电流脉冲同步,以降低噪声并在成像过程中保持针尖到样品的距离恒定。对于模型样品(例如聚合物斑点内包埋的酶或氧还原催化剂)的反馈模式、发生器-收集器模式和氧化还原竞争模式的 SECM 图像表明了控制温度的重要性,以及在预设和恒定升高的温度下进行 SECM 实验的重要性。

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1
Scanning electrochemical microscopy at variable temperatures.变温扫描电化学显微镜。
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Integration of thermocouple microelectrode in the scanning electrochemical microscope at variable temperatures: simultaneous temperature and electrochemical imaging and its kinetic studies.
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Constant-distance mode SECM as a tool to visualize local electrocatalytic activity of oxygen reduction catalysts.恒距模式 SECM 作为一种可视化氧还原催化剂局部电催化活性的工具。
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