Post Annealing Effects on Iron Oxide Nanoparticles Synthesized by Novel Hydrothermal Process

We have investigated the effects of post annealing on iron oxide nanoparticles synthesized by the novel hydrothermal synthesis method with the $FeSO_4{\cdot}7H_2O$. To investigate the post annealing effect, the as-synthesized iron oxide nanoparticles were annealed at different temperatures in a vacuum chamber. The morphological, structural and magnetic properties of the iron oxide nanoparticles were investigated with high resolution X-ray powder diffraction (XRD), high resolution transmission electron microscopy (HRTEM), Mossbauer spectroscopy, and vibrating sample magnetometer analysis. According to the XRD and HRTEM analysis results, as-synthesized iron oxide nanoparticles were only magnetite ($Fe_3O_4$) phase with face-centered cubic structure but post annealed iron oxide nanoparticles at $700^\circC$ were mainly magnetite phase with trivial maghemite ($\gamma-Fe_2O_3$) phase which was induced in the post annealing treatment. The crystallinity of the iron oxide nanoparticles is enhanced by the post annealing treatment. The particle size of the as-synthesized iron oxide nanoparticles was about 5 nm and the particle shape was almost spherical. But the particle size of the post annealed iron oxide nanoparticles at $700^\circC$ was around 25 nm and the particle shape was spherical and irregular. The as-synthesized iron oxide nanoparticles showed superparamagnetic behavior, but post annealed iron oxide nanoparticles at $700^\circC$ did not show superparamagnetic behavior due to the increase of particle size by post annealing treatment. The saturation of magnetization of the as-synthesized nanoparticles, post annealed nanoparticles at $500^\circC$, and post annealed nanoparticles at $700^\circC$ was found to be 3.7 emu/g, 6.1 emu/g, and 7.5 emu/g, respectively. The much smaller saturation magnetization value than one of bulk magnetite can be attributed to spin disorder and/or spin canting, spin pinning at the nanoparticle surface.