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Charge‐selective disordered hetero‐junctions were formed in evaporated In2S3 layers by diffusing at 200 °C CuI from a CuSCN source. The thicknesses of In2S3 layers and diffusion times were varied between 5 and 80 nm and between 2 and 19 min, respectively. In some cases CuSCN layers were etched back with pyridine. Spectral and time‐dependent surface photovoltage measurements were carried out in the capacitor arrangement. It was observed that a competing process of charge separation and relaxation was initiated together with the formation of the charge‐selective In2S3/In2S3:Cu hetero‐junction. Modulated SPV amplitude for different annealing times and thicknesses of the evaporated In2S3 layers.