Multiferroic BiFeO3 (BFO) has shown ferroelectric and ferromagnetism behavior at room temperature. This material is commonly used in memory devices, telecommunication, and sensors. Currently, it could be applied as a candidate for microwave absorbing material due to its magnetoelectric coupling. This paper describes the efficient synthesis of BFO nanoparticles using a sol-gel method. This method has advantages: cheap, homogenous product, minimal particle size, and low synthesize temperature. The crystal structure of BFO obtained by X-Ray Diffraction (XRD) and exhibited the rhombohedral symmetry and space group R3c when indexed to ICSD 98-006-6143. Vector Network Analyzer investigated the microwave absorption properties of BFO nanoparticles in the range 8 GHz to 12 GHz, which shows high reflection loss at -36,78 dB under measurement frequency at 10.78 GHz, shows 99,74% for its EM absorption value for as annealed sample at 900 BFO at thickness about 2 mm. The reflection loss of BFO nanoparticles is more than 20 dB, which indicated that the BFO nanoparticles have proper absorption to electromagnetic (EM) waves in X-band. These excellent EM absorption properties of BFO nanoparticles could be due to the good electromagnetic match due to the size effect and coexistence of ferroelectricity, and a weak ferromagnetic order in BFO nanoparticles was verified through dielectric and magnetic measurement.