Surfactant-free synthesis and magnetic property evaluation of air-stable cobalt oxide nanostructures

Abstract We report the synthesis of metastable cobalt oxide (CoO) nanostructures via the low-temperature microwave-assisted solvothermal (MAS) process. An alcoholic solution of cobalt (II) acetylacetonate in a sealed vessel was irradiated with microwaves at a temperature <150 °C and a pressure below 100 psi. As-synthesized powder material was characterized in terms of its structure and morphology. X-ray diffractometry (XRD) indicates the formation of well-crystallized CoO nanoparticles without the need for post-synthesis annealing. The mean crystallite size of the nanoparticles was estimated to be 41 nm. The morphology of the as-prepared powder sample was evaluated by field-emission scanning electron microscopy (FESEM), which revealed the formation of densely packed nanospheres of diameter <100 nm. The CoO nanospheres were obtained without the need for any surfactants or capping agents; they were found to be quite resistant to oxidation in ambient air over several months. We attribute the stability of CoO nanospheres to their dense packing, the driving force being the minimization of surface energy and surface area. Fourier-transform infrared (FT-IR) spectroscopy and Raman spectroscopy confirm the formation of phase-pure CoO nanostructures. The deconvolution of the active modes in Raman spectra obtained at room temperature reveals the Oh symmetry in rock-salt CoO produced by the MAS route. We have analyzed its effect on the magnetic characteristics of the CoO nanostructures. Isothermal field-dependent magnetization (MH) and inverse magnetic susceptibility measurements show a phase transition from antiferromagnetic to ferromagnetic interactions in the CoO nanostructures at around 10 K. The results indicate that the phenomenon of magnetic phase transition as a function of temperature is unique to CoO nanoparticles. This finding reveals the magnetic behavior of CoO nanostructures and presents opportunities for its possible application as an anisotropy source for magnetic recording.