Abstract:This article investigates the effects of electrolyte temperature and pH on the electrochemical crystallization behavior of copper through cyclic voltammetry (CV) and chronoamperometry (CA) experiments. The effects of electrolyte temperature and pH on the phase composition, preferred orientation, microstructure, roughness, and hardness of copper electrodeposited layers were analyzed using X-ray diffraction (XRD), scanning electron microscopy (SEM), three-dimensional ultra depth of field microscopy and microhardness tester. The results indicate that the copper electrocrystallization process is a three-dimensional nucleation and growth mode controlled by diffusion. When the electrolyte temperature is 35 ℃, the electrodeposition efficiency of copper is the highest; When the pH value of the electrolyte is 9, the promotion effect on copper electrodeposition is optimal. The final nucleation mechanism of different electrolyte temperatures and pH values is three-dimensional instantaneous nucleation growth. With the decrease of electrolyte temperature and the increase of pH value, the preferred orientation changes from (111) crystal plane to (220) crystal plane. When the electrolyte temperature is 35 ℃ and pH is 9, a flat, dense, rough and hard electrodeposited copper layer can be obtained.