Nickel nanoparticle-poly(N-vinyl-2-pyrrolidone)/TiO 2 -ZrO 2 composite (Ni-PVP/TiO 2 -ZrO 2 ) was prepared by in situ polymerization method. The physical and chemical properties of Ni-PVP/TiO 2 -ZrO 2 were investigated by XRD, FT-IR, BET, TGA, SEM and TEM techniques. The catalytic performance of this novel heterogeneous catalyst was determined for the Suzuki-Miyaura cross-coupling reaction between aryl halides and phenylboronic acid in the presence of methanol-water mixture as solvent. The effects of reaction temperature, the amount of catalyst, amount of support, solvent, and amount of metal for the synthesis of Ni-PVP/TiO 2 -ZrO 2 , were investigated as well as recyclability of the heterogeneous composite. The catalyst used for this synthetically useful transformation showed considerable level of reusability besides very good activity.