Precise Electrodeposition of Mo 6 ‐Cluster Thin Films: Mechanistic Pathways to Ambipolar Photoelectrodes With Tailored Microstructure

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Photoelectrodes based on transition metal clusters (MCs) are critical for advancing solar energy conversion, where precise control over film morphology and electronic properties is essential. While electrophoretic deposition (EPD) has been widely used for the design of MCs‐based photoelectrodes, its intrinsic limitations—such as poor film homogeneity, crack formation, and limited microstructural control—compromise device performance. In this study, we demonstrate that electrodeposition (ED) of [{Mo 6 I i 8 }I a 6 ] 2− clusters produces homogeneous, crack‐free films with the composition [{Mo 6 I i 8 }I a 4 (H 2 O) a 2 }]· x H 2 O. The ED process, driven by a two‐step oxidation mechanism (1.1 and 1.6 V vs. Ag/AgCl), enables unprecedented control over film thickness (60–600 nm) and microstructure, resulting in increased photoconductivity (photocurrent 2–3 times higher and lower charge transfer resistance, R tc ∼ 500 Ω). The films exhibit ambipolar conductivity and a quasi‐pinned mid‐gap Fermi level, confirming their potential for high‐performance solar energy applications . Compared to EPD‐derived films, ED films show enhanced charge extraction efficiency and minimized recombination losses, which are attributed to their defect‐free microstructure and stable electronic properties . This work establishes ED as a superior method for fabricating high‐quality MC‐based photoelectrodes, addressing key limitations of traditional deposition techniques.

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