The aim of the present work is to understand the effect of different parameters such as the molar ratio of metallic ions to fuel in sol-gel solution, pH of the solution, and calcining temperature on the efficiency of the combustion synthesis technique in preparing submicron lanthanum nickel ferrite using metal nitrate-citrate/glycine mixtures. Scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS) was used to evaluate the powder morphology and elemental composition. The crystal structure of the calcined powders was evaluated by X-ray diffraction (XRD) and the thermal characteristics of the LNF precursors were examined by thermo-gravimetric analysis (TGA) in air, to identify suitable processing conditions. It was found that by increasing the molar ratio of fuel to metallic ions in the precursor solution, calcining could take place at lower temperatures. However, by increasing the molar ratio of fuel to metallic ions, the yield of the combustion process was decreased. Furthermore, the pH value of the precursor solution did not have any influence on the process efficiency over the range examined.