PbS with nano- and micro-crystals was hydrothermally synthesized from Pb(NO3)2 and thiosemicarbazide using carboxymethyl cellulose (CMC) as a template at 140, 180 and 200 °C for 12 h. CMC, NaOH and hydrothermal temperatures have the influence on the product morphologies characterized using a scanning electron microscope (SEM) and a transmission electron microscope (TEM). PbS (cubic) composing of Pb and S was detected using an X-ray diffractometer (XRD), a selected area electron diffraction (SAED) technique and an energy dispersive X-ray (EDX) analyzer. The interpreted patterns are in accordance with those of the simulations. Raman spectrometer revealed the presence of the vibration modes at 136, 278, 432, 602 and 967 cm-1. Emission spectra of the products were detected at 384-388 nm using a photoluminescence (PL) spectrometer. Copyright © 2010 American Scientific Publishers All rights reserved.