Varying glycine to nitrate ratio in the initial solution the powders based on nanocrystalline LaFeO 3 were synthesized by solution combustion synthesis. The powders were studied by X-ray diffractometry, scanning electron microscopy, adsorption analysis and helium pycnometry. The average crystallite size of the synthesized LaFeO 3 nanocrystals ranged from 18±2 to 85±9 nm, and the specific surface area of the nanopowders based on them ranged from 8 to 33 m 2 /g. Based on the results, the influence of redox composition of the reaction solution on the nature of the combustion processes, as well as the composition, structure and properties of LaFeO 3 nanocrystals were analyzed. Here, it wasshown, that the nanopowders have specific microstructure in terms of monocrystalline nanoscale layers of lanthanum orthoferrite, therefore it is allowed to consider them as a promising base for catalytically and magnetically functional materials.