Abstract
The electrochemical activation of CuInS2/MoS x for photoelectrochemical (PEC) H2 production was revealed for the first time through in operando Raman spectroscopy. During the activation process, the initial metallic MoS x phase was transformed to semiconducting MoS x , which facilitates charge carrier transfer between CuInS2 and MoS x . 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.
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