| Summary: | Investigation of Cu(II) and Se(IV) electrochemical reduction processes in solutions with poly(ethylene glycol) (PEG) provides important theoretical guidance for the preparation of Cu-Se alloy films with stronger thermoelectric properties. The results reveal that PEG adsorbing on the electrode surface does not affect the electrochemical reduction mechanism of Cu(II), Se(IV), and Cu(II)-Se(IV), but inhibits the electrochemical reduction rates. The surface morphology and composition change with a negative shift in the deposition potentials. The Cu-Se alloy film, which was prepared at 0.04 V, was α-Cu<sub>2</sub>Se as-deposited and P-type thermoelectric material after annealing. The highest thermoelectric properties were as follows: Seebeck coefficient (α) was +106 μV·K<sup>−1</sup> and 1.89 times of Cu-Se alloy film electrodeposited in Cu(II)-Se(IV) binary solution without PEG; resistivity (ρ) was 2.12 × 10<sup>−3</sup> Ω·cm, and the calculated power factor (PF) was 5.3 μW·cm<sup>−1</sup>K<sup>−2</sup> and 4.07 times that without PEG.
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