Nanocrystalline NiSb and NiSb2 have been prepared through a solvothermal co-reduction route at low temperatures (120 - 180 degrees C). The features of this method include: (1) the reactants are simple inorganic salts (NiCl2 center dot 6H(2)O and SbCl3); (2) two types of nickel antimonides (NiSb and NiSb2) can be obtained respectively by changing the reducing agents and temperatures. The as-prepared samples were characterized by XRD and TEM. A possible formation mechanism has been presented. The thermoelectric properties of as-prepared NiSb, and the magnetic properties of NiSb2 were investigated. (c) 2008 Elsevier B.V. All rights reserved.