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Journal of Structural Chemistry

2014 year, number 3

A NOVEL PROCESS FOR MAKING ALKALINE IRON OXIDE NANOPARTICLES BY A SOLVO THERMAL APPROACH

D. Mishra, R. Arora, S. Lahiri, S.S. Amritphale, N. Chandra
Council of Scientific and Industrial Research, Advanced Materials and Processes Research Institute, Bhopal, India
Keywords: alkaline iron oxide, nanoparticles, solvo thermal

Abstract

In the present work alkaline iron oxide nanoparticles are synthesized by a novel solvo thermal approach and characterized exhaustively by various complementary techniques. Field emission scanning electron microscopy (FESEM) studies reveal that the size of nanoparticles is in the range of 31.5 nm to 96.9 nm. Energy-dispersive X-ray spectroscopy spectral analysis reveals the presence of oxygen, carbon, iron, and sodium. The X-ray diffraction studies confirm the formation of tetragonal NaFeO 2 as the major phase along with orthorhombic NaFeO 2×H 2O and rhombohedral FeCO 3 (siderite) as the minor phases. Fourier transform infrared spectroscopy exhibits peaks due to the stretching and bending vibrations of O-H, C=O, CH 3-N, CH 3, C-H, C-N, and Fe-O groups. Differential scanning calorimetry (DSC) results display an endothermic peak at 100.85 °C and a very small endothermic peak at 791.56 °C with 819.73 mJ and 349.28 mJ energies respectively. These DSC peaks can be correlated with thermal gravimetric analysis (TGA) peaks representing 31.04 % weight loss and 7.70 % weight loss respectively in the sample at around 160 °C and 980 °C respectively.