Chemistry of an InSb(111)A surface treated with ammonium sulfide solution followed by annealing at various temperatures has been studied by x-ray photoelectron spectroscopy (XPS). It is found that indium sulfide is formed and the intensity ratio of indium sulfide to indium antimonide on the as-treated surface is almost unity at the detection angles of the normal (0 • ) and 80• off the normal to the surface. Upon annealing the sample at 250• C, the ratio significantly increased and slightly decreased at 80• and 0 • , respectively. It decreased upon further annealing and finally indium sulfide disappeared at 390• C, where the 2 × 2 low energy electron diffraction (LEED) patters were observed. The Sb-S/O component is detected for the as-treated surface and it disappeared upon annealing at 250• C. Three components of sulfur are found: the main one at 161.6 eV, and the other weak ones at 163.1 and 160.2 eV. The 161.6-and 163.1-eV peaks can be ascribed to sulfur bonded to indium and antimony, respectively. The latter component disappeared upon annealing at 250• C. The behavior of the sulfides upon annealing the sample at various temperatures is discussed in terms of dissociation of Sb-S and diffusion of sulfur in the surface region.