We have been developing the selective deposition method onto TiO 2 nanoparticles, named as the liquid-phase selective-deposition method, where TiO2 plays a role of formation center of Ni nanoparticles as well as protection from the aggregative growth of the particles. The concept of this method is to well disperse and stabilize Ni nanoparticles on TiO2 surface by specific adsorption of Ni precursory complexes and then heterogeneous nucleation on the adsorption sites. The particle size was decreased with increasing the amount of Zn added, thus the catalytically active Ni surface area was increased. The selective deposition onto TiO2 surface and addition of Zn to the nanoparticle promoted the catalytic activity of Ni-Zn nanoparticle, e.g. the catalytic activity of Ni-Zn/TiO2 was ca. 10 times higher than that of the unsupported Ni nanoparticles. Ni in the nanocomposite was assigned as metallic, although their surface was oxidized under the atmospheric condition, but Zn and B were deposited as their oxide.