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Transition metal dichalcogenides (TMDs) have garnered attention as potential catalysts for water splitting owing to their unique structures, diverse electronic properties, and composition from earth‐abundant elements. While certain TMD catalysts, notably MoS2, have shown promising activity for hydrogen evolution reactions (HER), achieving performance comparable to traditional platinum catalysts remains a challenge. While significant effort has been invested into understanding the effect of TMD's structural properties, such as defectiveness and crystalline phases, recent work has emphasized the role of extrinsic factors on HER. This review summarizes the current understanding of the impact of commonly overlooked electrocatalytic effects that exhibit an enhanced importance in TMD‐based HER. By combining recent advances in theoretical modeling and experimental work, we review the dominating effects of extrinsic factors including electronic resistance, interfacial barriers, surface roughness, oxidation, and valence impurities. Our work aims to provide insights into optimizing TMDs as highly efficient catalysts for HER, facilitating future advancements in hydrogen generation technology. [ABSTRACT FROM AUTHOR]

Local laser‐induced oxidation is an extremely valuable technique to perform high‐throughput optimization across multidimensional parameter sets. In this work, a versatile method is presented for the synthesis of titanium dioxide (TiO2) thin‐films with varying crystalline structures through the use of localized, visible, continuous‐wave laser‐processing. By controlling the laser intensity and the exposure time, the conversion of amorphous titanium disulfide (a‐TiS2) precursor films into distinct phases of TiO2 is achieved and a laser‐induced oxidation phase diagram is constructed with the resulting material phases, including anatase, rutile, and black TiO2. By utilizing the dependence of phase formation on the rate and duration of laser energy input, mixtures of anatase and rutile phases are fabricated with controlled spatial arrangements. Photocatalytic properties of the synthesized films are evaluated using the degradation of nitrogen oxide (NOx) gas under UV illumination and an organic dye under white‐light illumination, revealing that mixtures of anatase and rutile phases demonstrate superior photocatalytic activity. The laser‐induced oxidation method highlighted showcases a strategy for precisely tailored phase composition for directly tunable properties, paving the way for in‐depth studies into structure‐property relationships in photocatalysis and other applications of metal oxide films. [ABSTRACT FROM AUTHOR]