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Chemical reactions, corrosion and electrochemistry at solid-liquid interfaces – routine operando studies with Near Ambient Pressure XPS

  • Gilbère Mannie (SPECS, Germany)
Thursday 2 April 2020
Hotel NH Noordwijk Conference Centre Leeuwenhorst

Gilbère Manniea, Paul Dietricha, Andreas Thissena
aSPECS Surface Nano Analysis GmbH, Voltastraße 5, 13355 Berlin, Germany

Over the last decades XPS under Near Ambient Pressure (NAP) conditions has demonstrated its promising potential in a wide variety of applications. Starting from operando studies of surface reactions in catalysis, the applications soon have been enhanced towards studies of processes at liquid surfaces, mainly using freezing/melting cycles, liquid jets or liquid films on rotation disks or wheels. Since more than 15 years, the need for basic studies of the fundamental chemistry at solid-liquid interfaces has attracted growing interest. Dip-and-pull experiments at synchrotrons finally also demonstrated, that in-situ and operando XPS in electrochemical experiments can be realized, mainly using synchrotron beams, significantly contributing to the basic understanding of modern energy converting or storing devices, like batteries, fuel cells, etc.

The development of pure laboratory NAP-XPS systems with optimized sample environments, like special sample holders, Peltier coolers and operando liquid cells combined with full automation and process control provides possibilities for the preparation and analysis of a multitude of liquid samples or solid-liquid interfaces on a reliable daily base. Interfaces of semiconductors with organic solvents are important for production processes and device operation. The first example presented shows the simplicity of obtaining relevant results on Silicon in different organic solvents without the need of highly sophisticated setups or special excitation sources beyond Al Kα. The next level of complexity is to follow the effects of corrosion in organic or inorganic acids. As an example an operando study of metal corrosion in acetic acid is shown.

Most sophisticated experiments so far have been operando electrochemistry in a classical three-electrode setup. A versatile setup is presented, allowing for studies of solid-electrolyte interfaces for example in Lithium ion batteries as a simple laboratory experiment.

Finally an outlook is given on the future perspective of applications and scientific contributions of routine operando XPS.

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