Electrochemically deposited manganese oxides for OER: approaches to in-situ measurements

Frederic Sulzmann^a, Marc Willinger^a, Axel Knop-Gericke ^a, Katarzyna Skorupska^a^,^b, Robert Schlögl^a^,^b, Juan-Jesus Velasco-Vélez^a^,^b, Michael Hävecker^a^,^b, Sebastian Fiechter^c, Cheng-Hao Chuang^d

^aFritz-Haber-Institut der Max-Planck-Gesellschaft, Faradayweg 4-6, Berlin, 14195

^bDepartment of Heterogeneous Reactions, Max-Planck-Institut für Chemische En- ergiekonversion, Stiftstraße 34-36, 45470 Mülheim an der Ruhr, Germany, Germany

^cDepartment of Physics, Tamkang University, No.151, Yingzhuan Rd., Tamsui Dist., New Taipei City, 25137, Taiwan, Republic of China

Materials for Sustainable Development Conference (MATSUS)
Proceedings of September Meeting 2016 (NFM16)

Berlin, Germany, 2016 September 5th - 13th

Organizers: Marin Alexe, Enrique Cánovas, Celso de Mello Donega, Ivan Infante, Thomas Kirchartz, Maksym Kovalenko, Federico Rosei, Lukas Schmidt-Mende, Laurens Siebbeles, Peter Strasser, Teodor K Todorov, Roel van de Krol and Ulrike Woggon

Poster, Katarzyna Skorupska, 070
Publication date: 14th June 2016

The process of (photo)electrochemical water splitting and hydrogen production is one of the milestones in search for alternative sources of renewable energy.The very complex mechanism of the oxygen evolution reaction (OER) where the loss of four electrons and four protons from two water molecules have to be accompanied by the formation of oxygen – oxygen bonds is a bottleneck in the water splitting process. Understanding the role of catalytic centers and their limitations it is very important in order to find stable catalyst materials with reduced overpotential for OER. The optimal but also very challenging way to achieve this goal is to perform studies under realistic reaction conditions.Here we will report on the development of manganese oxide based electrodes for the oxygen evolution reaction designed for in-situ measurements. Near edge X-ray absorption fine structure (NEXAFS) with soft x-rays were used to obtain Mn L-edge spectra. The method is suitable for the study of 3d metals where due to the probing of unoccupied 3d orbitals the oxidation state of manganese in manganese oxides can be obtained.The deposition and electrochemical characterization of manganese oxides were performed using an in-situ electrochemical flow cell with a silicon nitride membrane, both designed for the in-situ NEXAFS measurements.Influence of a calcination process in different gas environments on the performance of prepared electrodes based on in-situ NEXAFS, environmental SEM (ESEM) and TEM studied will be discussed.We will report on a first approach of in-situ electrochemical deposition of manganese oxides on SiNx membranes followed by their characterization under OER conditions. All the results will be correlated to those obtained for manganese oxides deposited on FTO.

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