Nanophase gamma-Gd2S3 polycrystalline thin films were deposited by a so-called asynchronous pulse ultrasonic spray pyrolysis method on glass substrates at relatively low temperature without any complexing agent. The films were characterized by X-ray diffraction, scanning electron microscopy and Raman spectrum. The technical conditions leading to optimal performance were identified. An appropriate ratio of pulse time thin films. to interval time between pulses is found to be necessary for obtaining homogeneous and uniform nanostructural gamma-Gd2S3 (c) 2005 Elsevier B.V. All rights reserved.