The multilayer Al/Sb thin films were deposited on quartz glass substrates using magnetron sputtering method and annealed at high temperature to obtain AlSb films. The experimental conditions were optimized to obtain the AlSb single phase. XRD measurements indicate that high-temperature annealing is necessary to form AlSb and is helpful to the grain growth of AlSb polycrystalline. The average grain size of AlSb polycrystalline increases obviously with the increase in annealing temperature when higher than 500 degrees C. The electrical measurements show that the prepared AlSb films are p-type semiconductors with the conductivity activation energy of 0.21 and 0.01 eV. The optical band gap for a typical AlSb film is 1.76 eV. The obvious photovoltaic effect has been observed in TCO/CdS/AlSb/ZnTe:Cu/Au devices, which demonstrated the potential of AlSb film as the absorber layer in thin film solar cells. (c) 2010 Elsevier B.V. All rights reserved.