In an effort to prepare thin films of novel semiconductor materials that contain only cost effective, abundant, and relatively less-toxic materials, lead antimony sulfides films have been prepared. Herein, we report the thin film preparation of semseyite (Pb9Sb8S21) via annealing of precursor films under sulfur vapor. Pb/Sb alloy precursor films suffered substantial changes in stoichiometry and produced rough films, whereas precursor films composed of multilayers of PbS and amorphous (Sb,S) produced smooth and compact phase-pure films composed of fine grains. Optical measurements indicated a direct band gap of 1.93 eV and a strong absorption coefficient of 1.0 x 10(5) cm(-1). (C) 2007 Elsevier B.V. All rights reserved.