An optimised Cell for in situ XAS of Gas Diffusion Electrocatalyst Electrodes

IF 3.8 3区 化学 Q2 CHEMISTRY, PHYSICAL
ChemCatChem Pub Date : 2024-06-15 DOI:10.1002/cctc.202400221
Connor Sherwin, Dr. Veronica Celorrio, Dr. Ursa Podbevsek, Katie Rigg, Toby Hodges, Armando Ibraliu, Abbey J. Telfer, Dr. Lucy McLeod, Alessandro Difilippo, Dr. Elena C. Corbos, Dr. Chris Zalitis, Prof. Andrea E. Russell
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Abstract

The quality of in situ XAS of electrochemical systems is highly sensitive to electrode disturbances, such as gas evolution and gas consumption at an electrolyte/catalyst interface. A novel in situ spectro-electrochemical X-ray absorption spectroscopy (SPEC-XAS) cell is presented as a new tool for the characterisation of gas evolving and consuming electrocatalysts at high overpotentials. By utilising a thin, porous membrane with efficient electrolyte and gas circulating loops, an improved three phase interface is established that enabled efficient gas supply and minimised the interference from bubble formation. X-ray absorption spectroscopy (XAS) measurements were conducted in fluorescence mode with three experiments selected to demonstrate the cell's performance. The first two reactions; an in-situ study of a highly active amorphous iridium oxide catalyst during the oxygen evolution reaction (OER) and an in-situ study of copper oxide during the carbon dioxide reduction reaction (CO2RR) are used to exemplify the XAS data quality achieved under operational conditions. Thirdly, a detailed XAS investigation of a highly dispersed platinum catalyst during the oxygen reduction reaction (ORR) is presented, along with comparative data in nitrogen. These measurements show the retention of oxygen on the surface of the platinum metal particles down to 0.48 V (vs. RHE), well below the platinum oxide reduction peak.

Abstract Image

用于气体扩散电催化剂电极原位 XAS 的优化电池
电化学系统原位 XAS 的质量对电极干扰非常敏感,例如电解质/催化剂界面上的气体演化和气体消耗。本文介绍了一种新型原位光谱电化学 X 射线吸收光谱池,它是表征高过电位下气体演化和消耗电催化剂的一种新工具。通过利用具有高效电解质和气体循环回路的薄多孔膜,改进的三相界面实现了高效气体供应,并最大限度地减少了气泡形成的干扰。X 射线吸收光谱测量是在荧光模式下进行的,选择了三个实验来展示电池的性能。前两个反应:氧进化反应过程中对高活性无定形氧化铱催化剂的原位研究,以及二氧化碳还原反应过程中对氧化铜的原位研究,都是在运行条件下实现 XAS 数据质量的例证。第三,介绍了氧还原反应中高度分散铂催化剂的详细 XAS 研究,以及氮气中的比较数据。这些测量结果表明,氧气在铂金属颗粒表面的保留电压低至 0.48 V(相对于 RHE),远低于氧化铂还原峰值。
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来源期刊
ChemCatChem
ChemCatChem 化学-物理化学
CiteScore
8.10
自引率
4.40%
发文量
511
审稿时长
1.3 months
期刊介绍: With an impact factor of 4.495 (2018), ChemCatChem is one of the premier journals in the field of catalysis. The journal provides primary research papers and critical secondary information on heterogeneous, homogeneous and bio- and nanocatalysis. The journal is well placed to strengthen cross-communication within between these communities. Its authors and readers come from academia, the chemical industry, and government laboratories across the world. It is published on behalf of Chemistry Europe, an association of 16 European chemical societies, and is supported by the German Catalysis Society.
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