A facile approach for the synthesis of porous hematite and magnetite nanoparticles through sol-gel self-combustion.

ABSTRACT

Porous magnetite (Fe3O4) and hematite (α-Fe2O3) nanoparticles were prepared via the sol-gel auto-combustion method. The gels were prepared by reacting ferric nitrates (as oxidants) with starch (as fuel) at an elevated temperature of 200 °C. Different ratios (Φ) of ferric nitrates to starch were used for the synthesis (Φ = fuel/oxidant). The synthesized iron oxides were characterized by Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy, X-ray diffraction (XRD) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer-Emmet-Teller (BET) and vibrating sample magnetometer (VSM) analysis techniques. The crystal structure, morphology, and specific surface area of the iron oxide nanoparticles (Fe3O4 and α-Fe2O3) were found to be dependent on the starch content. The FT-IR, XRD and VSM analysis of the iron oxides for Φ = 0.3 and 0.7 confirmed the formation of the α-Fe2O3 core, whereas at Φ = 1, 1.7, and 2 showed that Fe3O4 cores were formed with the highest saturation magnetization of 60.36 emu/g at Φ = 1. The morphology of the Fe3O4 nanoparticles exhibited a quasi-spherical shape, while α-Fe2O3 nanoparticles appeared polygonal and formed clusters. The highest specific surface area was found to be 48 m2 g-1 for Φ = 1.7 owing to the rapid thermal decomposition process. Type II and type III isotherms indicated mesoporous structures.