In this study we present an effect of glycine and urea fuels on the phase formation and morphology of the α-Al2O3 and NiO nanomaterials. Materials were synthesized using facile solution combustion method at temperature 500 °C ± 10 °C. The synthesized products were characterized by various analytical techniques. PXRD results of α-Al2O3 confirm that the hexagonal phase is best represented using urea as a fuel compared to glycine. FE-SEM micrographs observed with urea are like flake like structure whereas with glycine net like porous structure is observed. TEM micrographs show the well crystalline nature of the nanomaterials. Large mismatching was observed in the FTIR spectra of synthesized materials using urea and glycine fuels with respect to the OH and metal to oxygen vibrational frequencies. PXRD results of NiO confirm that the cubic structure is obtained with urea fuel without any secondary phases, whereas with glycine a small peak of Ni was observed at 2θ = 44.5°. FE-SEM micrographs NiO with urea represents spherical like structure whereas large number of voids with porous structure was observed with glycine. The results of the study show that the fuels used for the synthesis of nanomaterials have a great effect on phase formation and morphology.