The electrochemical activation of CuInS2/MoSx for photoelectrochemical (PEC) H2 production was revealed for the first time through in operando Raman spectroscopy. During the activation process, the initial metallic MoSx phase was transformed to semiconducting MoSx, which facilitates charge carrier transfer between CuInS2 and MoSx. Ex situ X-ray photoelectron spectroscopy and Raman spectroscopy suggest the existence of MoO3 after the activation process. However, apart from contradicting these results, in operando Raman spectroscopy revealed some of the intermediate steps of the activation process.
This study was supported by the institutional program of the Korea Institute of Science and Technology (KIST\u20102E31831), the C1 Gas Refinery Program through the National Research Foundation of Korea (NRF), funded by the Ministry of Science, ICT, and Future Planning (2015M3D3A1A01064899), and the Basic Science Research Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Education (2020R1I1A1A01073326).