The synthesis of bismuth ferrite by solid-state reaction of Bi 2 O 3 and Fe 2 O 3 results in the formation of multiphase products. Even coprecipitation followed by calcination leads to the formation of impurity phases. Here, we report the synthesis of magnetoelectric bismuth ferrite by a ferrioxalate precursor method. In this process, bismuth ferrite, synthesized through solutions of some specific salts led to the formation of phase pure (perovskite) nanocrystalline powder (11–22nm as evident from X-ray diffraction analysis) at a temperature of 600°C. The synthesized powders were characterized by X-ray diffractometry, thermogravimetry and differential thermal analysis, Fourier transformation infrared spectroscopy and scanning electron microscopy. The synthesis route is simple, energy saving and cost-effective. Such nanosized bismuth ferrite powder may have a potential application in making lead free piezoelectric materials for actuators as well as magnetoelectric sensors.