Synthesis of TiO2-Al2O3-SiO2nanopowder composite, as well as composite coating on soda lime glass and Si (100) by sol-gel method is reported.The morphology and the crystal structure of composite are characterized by the use of field emission scanning electron microscopy (FE-SEM), Energy dispersive X-ray (EDAX), atomic force microscopy (AFM) and X-ray diffraction (XRD) techniques. The effects of chemical compositions and Calcination temperature on surface topography and the crystallization of phases are studied. In addition, the lattice strain and coating roughness parameters are calculated during thermal treatment.Figure 1. XRD patterns of TiO2-Al2O3-SiO2 for molar ratio (MR = 1) obtained from: without hydrothermal treatment (as-prepared), calcined at 300 °C, calcined at 600 °C and calcined at 900 °C.