Copper-indium-diselenide (CIS) particles were prepared by the electrochemical reduction from the mixture solution of corresponding ion compounds. The prepared CIS was used as an insertion layer or a blending component in the organic photovoltaic bulk heterojunction cells composed of poly(3-octylthiophene) and fullerene. The increase of CIS content resulted in the rapid decrease of the open-circuit voltage as well as short-circuit current. The photovoltaic parameters were analyzed in relation to the structures, composition, and morphology of the photovoltaic blends.