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Bismuth ferrite (BiFeO3) nanocomposites were synthesized using a novel nano-agitator bead milling method followed by calcination. Bismuth oxide and iron oxide nanoparticles were mixed in a stoichiometric ratio and milled for 3 h and calcined at 650 °C in air. X-ray diffraction with Rietveld refinement, scanning electron microscopy, and transmission electron microscopy techniques were used to elucidate the structure of BiFeO3. The particle diameter was found to be ∼17 nm. Magnetic and electrical measurements were performed, and these results were compared with those of similar methods. Mostly, BiFeO3 was obtained with minor secondary phase formation. The resulting powder was weakly ferromagnetic with a remnant magnetization of 0.078 emu/g. This can be attributed to residual strain and defects introduced during the milling process. Electrical testing revealed a high leakage current density that is typical of undoped bismuth ferrite.