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Abstract In this paper, a green and simple electrochemical method is developed that can directly deposit thin films of [CuX(pyz)]n and [Cu2X2(pyz)]n (X = Cl, Br, I; pyz = pyrazine) in aqueous solution. This method can overcome the thermodynamical instability of Cu(I) and the poor solubility of hybrid organic–copper(I) halides. By heating in different atmospheres, the single‐crystal transformation between [CuX(pyz)]n and [Cu2X2(pyz)]n can be realized with luminescent switching, which is used for information encryption and encoding. More importantly, the corresponding thin film can be deposited on various substrates leading to flexible light‐emitting and photoelectric devices.