In this work, the comparison between nitrogen and air synthesis environments in obtaining In0.6Ga0.4N powders is presented, and the effect of how the air environment can reduce the pyrolysis temperature of In0.6Ga0.4N powders to 271 °C using the thermal gravimetric analysis, and derivative thermogravimetry methods. X‐ray diffraction patterns demonstrate the presence of a cubic phase in nanocrystallites, in addition to less presence of the hexagonal phase. In contrast, scanning electron microscopy micrographs show a surface morphology of irregular agglomerates with a porous appearance and the presence of nonuniform plates. Energy‐dispersive spectroscopy and X‐ray photoelectron spectroscopy spectra demonstrate the presence of elemental contributions of gallium, indium, and nitrogen. At the same time, transmission electron microscopy shows the cubic structure and an interplanar distance of 2.7 Å for the (200) plane. Raman scattering shows the presence of E2(high) vibration mode for the hexagonal phase with a value of 560 cm−1. Finally, the photoluminescence spectrum shows an energy emission at 1.39 eV (886 nm), which is associated with the emission of the In0.6Ga0.4N powders.