Synthesis of magnetite nanoparticles by high energy ball milling

We report on the preparation of magnetite nanoparticles, with size ranging from 12 nm to 20 nm, by high energy ball milling. The synthesis is made using stoichiometric amounts of distilled water and metallic iron powder. The milled powder samples were analyzed by Mossbauer spectroscopy (MS), X-ray diffraction (XRD) and vibrating sample magnetometry (VSM). Our results indicate that the milling time is a key parameter of the synthesis. By increasing the milling time one achieves high purity magnetite samples. Also, the particle size decreases with the milling time. The sample milled during 10 h contained a fraction of 56 nm metallic Fe particles and 20 nm magnetite particles. By increasing the milling time to 96 h we have obtained a sample that is mainly composed of 12 nm magnetite particles. MS performed at room temperature showed a spectrum consisting of two sextets with hyperfine parameters related to iron ions occupying octahedral (A) and tetrahedral (B) sites. We have used a self-consistent method to investigate the impact of the dipolar interaction to drive the system to a magnetically blocked regime.