ZrS(3) nanocrystallites have been synthesized via a solvothermal route by the reaction between ZrCl(4) and thiourea at relatively low temperature. The product was characterized by X-ray diffraction (XRD), transmission electron microscope, X-ray fluorescence, Raman spectrum, and photoluminescence (PL). X-ray diffraction pattern shows the monoclinic cell of ZrS(3) with the lattice constants a = 5.128 Angstrom, b = 3.611 Angstrom, c = 9.012 Angstrom, beta = 97.13degrees. The result of X-ray fluorescence gives a Zr(Hf):S mole ratio 1:2.97. The Raman spectrum of the ZrS(3) nanocrystallites has a slightly red shift in comparison with that of ZrS3 single crystals. The room temperature photoluminescence of ZrS(3) nanocrystallites is also reported. (C) 2004 Elsevier Ltd. All rights reserved.