phosphosilicate (80 P2O5: 20 SiO2) nanoparticles modified with three different concentrations of Al2O3 ions (10, 15, 20 mol %) and doped with Ni2O3 in the formula (59 P2O5: 20 SiO2: 20Al2O3: 1 Ni2O3) were prepared by sol-gel method at room temperature using triethylphosphate, tetraethylorthosilicate, aluminum and nickel nitrates as a sources for P2O5, SiO 2, Al2O3 and Ni2O3. Monolithic, transparent gels were formed with both prepared samples and calcined at 900 C for 3h in air. The effect of Al2O3 contents on the morphological properties of pure and doped phosphosilicate were investigated. The prepared monolithic samples were characterized by X-ray diffraction (XRD), transmission and scanning electron microscopy (TEM/SEM), Fourier transform infrared spectroscopy (FTIR). X-ray diffraction and FT-IR showed that the addition of Al2O3 caused the formation of phosphosilicate network as P–O–Si, and formation of aluminophosphosilicate network as P–O–Si–O–Al. The magnetite measurement is formed for the aluminophosphosilicate system doped with 1 mol% Ni2O3 ions,using the vibrating sample magnetometer (VSM) at room temperature.