The present contribution is devoted to the production of the Ni-Bi-Se thin films widely used in the field of electronics, electrotechnology, and computer technology. During the process, at first, the Bi-Se compound has been formed on the nickel electrode by electrochemical method, and then by thermal treatment of this compound at 673K, ternary compound Ni3Bi2Se2 has been obtained. The results show that as the concentration of bismuth is increasing, its amount in deposited films increases regularly. The formation of the Ni3Bi2Se2 compound was also confirmed by XRD results. The photochemical properties of the obtained compounds were investigated in the dark and light, constant current of 100 nA for 0-600 seconds. With the illumination of the dark samples, the potential shifts from a positive side to a negative side, this decrease indicates that obtained thin films are not only photosensitive, also have n-type conductivity.