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Much effort has been recently directed towards developing new and better solar energy conversion devices, and the interest is to develop new energy sources to supplement and eventually replaces fossil fuels. In 1975, Gerischer succeeded in the direct conversion of solar energy into electricity by Photoelectrochemical solar cells. Since Transition metal dichalcogenides (TMDCs) occupy very favourable position for band gap in the range of 1.1 eV to 2.1 eV author has concentrated on these materials for PEC solar cell investigations. As a part of the program of studying the Photoelectrochemical characterisation of these interesting TMDC layered semiconductors, author has concentrated in this book upon the middle compound of the family i.e. 'MoSSe'. This book entitled " Photoelectrochemical Studies of MoSSe Single Crystals " covers growth, physical properties, transport properties, optical properties, energetic band location and fabrication of PEC solar cell as well as different treatment on the fabricated solar cell to improve their efficiency.