Abstract—: Nanocrystalline BiFeO₃-based powder materials with an average crystallite size near 40 nm have been prepared by solution combustion synthesis from bismuth and iron nitrates using sucrose and tartaric acid as fuel. The materials have been characterized by X-ray diffraction, helium pycnometry, scanning electron microscopy, energy dispersive X-ray microanalysis, and Mössbauer spectroscopy. Magnetometry results demonstrate that the magnetic response of the materials varies over several orders of magnitude, depending on the synthesis procedure.