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A Bi–W–Mo–O thin-film materials library was fabricated by combinatorial reactive magnetron sputtering. The composition spread was investigated using high-throughput methods to determine crystalline phases, composition, morphology, optical properties, and photoelectrochemical performance. The aurivillius phase (Bi 2 O 2 ) 2+  (Bi M (W 1−N Mo N ) M−1 O 3M+1 ) 2−  is the predominantly observed crystal structure, indicating that the thin films in the library are solid solutions. With increasing amounts of Mo ≙ 7–22% the diffraction peak at 2θ = 28° ≙ [131] shifts due to lattice distortion, the photoelectrochemical activity is increasing up to a wavelength of 460 nm with an incident photon to current efficiency (IPCE) of 4.5%, and the bandgap decreases. A maximum photocurrent density of 31 μA/cm 2  was measured for Bi 31 W 62 Mo 7 O z  at a bias potential of 1.23 V vs. RHE (0.1 M Na 2 SO 4 ).

High-Throughput Characterization of Structural and Photoelectrochemical Properties of a Bi–Mo–W–O Thin-Film Materials Library