In this paper we report on the formation of nickel silicide by electroless process. The nickel plating solution was composed of a mixture of NiSO(4)center dot 6H(2)O, NaH(2)PO(2)center dot H(2)O, Na(3)C(6)H(5)O(7)- and NH(4)Cl, where NiSO(4)center dot 6H(2)O is the main nickel source and NaH(2)PO(2)center dot H(2)O is the reducing agent. The nickel silicide formation was carried out by heating the deposited samples in vacuum at temperatures from 100 degrees C to 800 degrees C. The evolution of NiSi phase from the nickel film was verified using the X-ray diffraction technique and Raman spectroscopy. The surface morphology was studied using AFM technique. The electroless plating technique can provide a cheap and easy process for forming nickel silicide, and has potentiality of application for the electronic device industries. (C) 2009 Elsevier B.V. All rights reserved.