In the present work, Al2O3doped (80 P 2O5: 20 SiO2 ) nanostructures were successfully prepared using a sol–gel process using triethyphosphate and tetraethylorthosilicate. We investigated the phase structure, microstructure and spectroscopic properties. Three different solutions were prepared by changing Al/P molar ratios such as 0, 10 and 15 in acidic condition. The obtained gel were aged at room temperature and dried at 100°C forming xerogel and subsequently calcined at different temperatures from 100 up to 700 o C for 3h in air. The obtained oxides were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). The micro-structural observations demonstrated that Al 2O3 content improved surface morphology of the nanostructure phosphosilicate. X-ray diffraction and FT-IR showed that the addition of Al 2O3 caused the formation of phosphosilicate network as P–O–Si, and formation of mixed phases based on P–O–Si–O–Al and P–O–Al separated from the phosphate matrix