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ZnO nanosheet thin films were obtained by the ultrasonic spray pyrolysis technique (USP) on tourmaline and glass substrates at different deposition temperature. Structural studies suggested that ZnO crystals were polycrystalline with hexagonal wurtzite structure. The intensity of the characteristic Raman peak, and the (002) preferential orientation, the degree of crystallinity, the grain size achieved by the XRD results were significantly increased with the elevation of the substrate temperature. SEM images showed that the ZnO nanoplates laminated in parallel to the substrate and assembled to the flower-like column morphology, ZnO nano crystals had larger lamellae sizes and wider crystalline columns at higher temperature. UV-Vis measurement confirmed the maximum absorption peak of the ZnO films on the tourmalines had more red shifts and stronger intensities than that on the glass substrates, and relatively greater wavelength shifts under higher substrate temperature were also observed.