Thermal treatment of natural goethite: Thermal transformation and physical properties

Abstract

XRD (X-ray diffraction), XRF (X-ray fluorescence), TG (thermogravimetry), FT-IES (Fourier transform infrared emission spectroscopy), FESEM (field emission scanning electron microscope), TEM (transmission electron microscope) and nitrogen–adsorption–desorption analysis were used to characterize the composition and thermal evolution of the structure of natural goethite. The in situ FT-IES demonstrated the start temperature (250°C) of the transformation of natural goethite to hematite and the thermodynamic stability of protohematite between 250 and 600°C. The heated products showed a topotactic relationship to the original mineral based on SEM analysis. Finally, the nitrogen–adsorption–desorption isotherm provided the variation of surface area and pore size distribution as a function of temperature. The surface area displayed a remarkable increase up to 350°C, and then decreased above this temperature. The significant increase in surface area was attributed to the formation of regularly arranged slit-shaped micropores running parallel to elongated direction of hematite microcrystal. The main pore size varied from 0.99nm to 3.5nm when heating temperature increases from 300 to 400°C. The hematite derived from heating goethite possesses high surface area and favors the possible application of hematite as an adsorbent as well as catalyst carrier.