Methods for Electrochemical Synthesis and Photoelectrochemical Characterization for Photoelectrodes

Electrodeposition is a widely used technique for electrode synthesis in various applications. Because of its low synthesis cost and easy scalability, electrodeposition is particularly attractive for the production of semiconductor and catalyst electrodes for use in solar fuel production. For researchers who are interested in learning about or utilizing electrodeposition, the current paper describes detailed methods for electrodeposition, which include procedures for preparing electrodes and plating solutions, determining deposition conditions, and performing electrodeposition. Postdeposition treatments that can be used to prepare electrodes of more diverse compositions and photodeposition procedures that can be used to place catalyst layers on semiconductor electrodes are also provided. The methods are described using the synthesis and modification of photoelectrodes as an example, but most principles and procedures explained in this paper are general and can be applied to electrodeposition of various electrodes. In addition to methods for electrochemically preparing photoelectrodes, methods for photoelectrochemical characterization, which include light setup and calibration, photo electrochemical characterization, and efficiency calculations, are described along with rationale for each setup and procedure. This will improve understanding and performance of various experimental procedures used for photoelectrode evaluation.