Nanocrystalline dinickel phosphide was synthesized via a solvo-thermal route using PCl3 and NiCl2 as precursors, and Na as reductant. The crystals were characterized by X-ray powder diffraction and transmission electronic microscopy. It was shown that the product is pure Ni2P which crystallizes very well with an average size of about 80 nm. (C) 2003 Elsevier B.V. All rights reserved.