Shandite Ni3Pb2S2 was obtained at low temperature under ethylene glycol reflux using PbS and freshly produced nickel as starting, materials. The as-prepared products were characterized with X-ray diffraction pattern, X-ray photoelectron spectroscopy and scanning electron microscopy. Experimental results showed that the diffusion of Ni was the controlling step in the whole process. (c) 2008 Elsevier B.V. All rights reserved.