Group of Electrochemistry and Conducting Polymers, Leibniz-Institute of Solid State and Materials Research, Helmholtzstrasse 20, D-01069 Dresden, Germany.
Anal Chem. 2009 Mar 1;81(5):2017-21. doi: 10.1021/ac802336y.
A recently developed rotating spectroelectrochemical cell for in situ Raman spectroscopic studies of photoreactive compounds without marked decomposition of the sample is presented. Photochemically and thermally sensitive redox systems are difficult to be studied under stationary conditions by in situ spectroelectrochemistry using laser excitation as in Raman spectroscopy. A rotating spectroelectrochemical cell can circumvent these difficulties. It can be used for any type of a planar electrode and for all electrode materials in contact with aqueous or nonaqueous solutions as well as with ionic liquids. The innovative technical solution consists of the precession movement of the spectroelectrochemical cell using an eccentric drive. This precession movement allows a fixed electrical connection to be applied for interfacing the electrochemical cell to a potentiostat. Hence, any electrical imperfections and noise, which would be produced by sliding contacts, are removed. A further advantage of the rotating cell is a dramatic decrease of the thermal load of the electrochemical system. The size of the spectroelectrochemical cell is variable and dependent on the thickness of the cuvettes used ranging up to approximately 10 mm. The larger measuring area causes a higher sensitivity in the spectroscopic studies. The as constructed spectroelectrochemical cell is easy to handle. The performance of the cell is demonstrated for ordered fullerene C(60) layers and the spectroelectrochemical behavior of nanostructured fullerenes. Here the charge transfer at highly ordered fullerene C(60) films was studied by in situ Raman spectroelectrochemistry under appropriate laser power and accumulation time without marked photodecomposition of the sample.
一种新开发的旋转光谱电化学池，用于原位喇曼光谱研究光反应性化合物，而不会导致样品明显分解。用光激发的原位光谱电化学在研究光化学和热敏感氧化还原体系时，由于样品的显著分解而变得困难。旋转光谱电化学池可以避免这些困难。它可以用于任何类型的平面电极，以及与水相或非水相溶液以及离子液体接触的所有电极材料。这项创新的技术解决方案是使用偏心驱动器实现光谱电化学池的进动运动。这种进动运动允许固定的电连接应用于将电化学池与电位计接口。因此，任何由滑动接触产生的电气缺陷和噪声都被消除了。旋转池的另一个优点是电化学系统的热负荷显著降低。光谱电化学池的尺寸是可变的，取决于使用的比色皿的厚度，最大可达约 10 毫米。较大的测量面积导致光谱研究的灵敏度更高。所构建的光谱电化学池易于操作。该电池的性能已通过有序富勒烯 C(60)层和纳米结构富勒烯的光谱电化学行为得到证明。在这里，通过原位喇曼光谱电化学在适当的激光功率和积累时间下研究了高度有序的富勒烯 C(60)薄膜的电荷转移，而不会导致样品明显的光分解。
