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A novel synthesis method is presented for the preparation of nanosized-semiconductor cobalt oxide formed successively from a single-source solid various fuel (starch, urea and glycine). The as obtained samples were characterized by the X-ray diffraction, scanning electron microscopy, transmission electron microscopy; diffuse reflectance spectroscopy (DRS) and photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM). XRD pattern confirmed the formation of cubic phase Co3O4. The materialization of Co3O4 nanoparticles is confirmed by HR-SEM and HR-TEM. The optical absorption and photoluminescence emissions were determined by DRS and PL spectra, respectively. The relatively high saturation magnetization (starch) of Co3O4 shows that it is ferromagnetic and low saturation magnetization (urea and glycine) confirms the super paramagnetic behavior.
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