In order to solve the problems of low light utilization efficiency and difficult recovery and reuse of powder Bi2O3 photocatalyst,Bi2O3/NiF electrode was prepared with impregnation-microwave radiation hybrid technology,and its characterizations such as SEM,XRD,XPS and electrochemical properties were used to analyze the morphology,chemical structure and photoelectrocatalytic performance.Experimental results displayed that the flower-shaped Bi2O3 was successfully loaded on the surface of three-dimensional framework NiF,and it exhibited excellent photoelectric conversion efficiency.Photoelectrocatalytic degradation efficiency was about 95.35%when the photocurrent density was 15μA/cm2,initial voltage was 2V,RhB concentration was 8mg/L and pH value was 3.Bi2O3/NiF photoelectrocatalytic degradation of RhB fitted well with the first-order reaction kinetics.Furthermore,the free radical trapping test confirmed that h+played a major role in the process of Bi2O3/NiF photoelectrocatalytic degradation of RhB.