使用“柔和”X射线常压X射线光电子能谱作为固液界面的直接探测手段。
Using "Tender" X-ray Ambient Pressure X-Ray Photoelectron Spectroscopy as A Direct Probe of Solid-Liquid Interface.
作者信息
Axnanda Stephanus, Crumlin Ethan J, Mao Baohua, Rani Sana, Chang Rui, Karlsson Patrik G, Edwards Mårten O M, Lundqvist Måns, Moberg Robert, Ross Phil, Hussain Zahid, Liu Zhi
机构信息
Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, California, 94720, United States.
1] Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, California, 94720, United States [2] State Key Laboratory of Functional Materials for Informatics, Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences, Shanghai 200050, People's Republic of China.
出版信息
Sci Rep. 2015 May 7;5:9788. doi: 10.1038/srep09788.
We report a new method to probe the solid-liquid interface through the use of a thin liquid layer on a solid surface. An ambient pressure XPS (AP-XPS) endstation that is capable of detecting high kinetic energy photoelectrons (7 keV) at a pressure up to 110 Torr has been constructed and commissioned. Additionally, we have deployed a "dip &pull" method to create a stable nanometers-thick aqueous electrolyte on platinum working electrode surface. Combining the newly constructed AP-XPS system, "dip &pull" approach, with a "tender" X-ray synchrotron source (2 keV-7 keV), we are able to access the interface between liquid and solid dense phases with photoelectrons and directly probe important phenomena occurring at the narrow solid-liquid interface region in an electrochemical system. Using this approach, we have performed electrochemical oxidation of the Pt electrode at an oxygen evolution reaction (OER) potential. Under this potential, we observe the formation of both Pt(2+) and Pt(4+) interfacial species on the Pt working electrode in situ. We believe this thin-film approach and the use of "tender" AP-XPS highlighted in this study is an innovative new approach to probe this key solid-liquid interface region of electrochemistry.
我们报道了一种通过在固体表面使用薄液层来探测固液界面的新方法。我们构建并调试了一个环境压力X射线光电子能谱（AP-XPS）终端站，该终端站能够在高达110托的压力下检测高动能光电子（7 keV）。此外，我们采用了一种“浸拉”方法，在铂工作电极表面制备出稳定的纳米厚水性电解质。将新构建的AP-XPS系统、“浸拉”方法与“柔和”的X射线同步辐射源（2 keV - 7 keV）相结合，我们能够利用光电子进入液固致密相之间的界面，并直接探测电化学系统中狭窄固液界面区域发生的重要现象。使用这种方法，我们在析氧反应（OER）电位下对铂电极进行了电化学氧化。在此电位下，我们原位观察到铂工作电极上形成了Pt(2+)和Pt(4+)界面物种。我们认为，本研究中强调的这种薄膜方法以及“柔和”AP-XPS的使用，是探测电化学这一关键固液界面区域的一种创新新方法。
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