Characterisation and Carbothermal Reduction of a Murray Basin Ilmenite Concentrate

An ilmenite ore from the Murray Basin was initially characterised using combined X-ray Fluorescence Spectroscopy (XRF), X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM) and Electron Probe Microanalysis (EPMA) techniques. XRF analysis showed the ilmenite sample contained 58.7 wt per cent TiO2 and 26.2 wt per cent Fe2O3. Major impurities included: Cr2O3 (4.5 wt per cent), Al2O3 (2.7 wt per cent), SiO2 (1.9 wt per cent), Mn3O4 (1.5 wt per cent) and MgO (1.1 wt per cent). Manganese and magnesium were present as solid solution components within the ilmenite lattice while the elevated Al2O3 and SiO2 levels were due to separate aluminosilicate gangue minerals. Chromium was associated with discrete chrome spinel gangue phases of variable composition, (Fe,Mg)(Cr,Al)2O4. Quantitative XRD analysis of the sample identified rutile (12 per cent), ilmenite (11 per cent), and pseudorutile (67 per cent) as the main titanium-containing phases and chrome-rich spinels (seven per cent) as the major impurity phase. Minor quartz, aluminosilicates, zircon and monazite were also present. The ilmenite was mixed with synthetic graphite, pressed into pellets and reduced carbothermally in nitrogen at 1200 and 1400°C with C/O molar ratio of 1.2. Titanium oxide in the ilmenite was converted to titanium oxycarbonitride. Iron oxides were reduced to metallic iron. The Changes of impurities as a result of reduction was examined by SEM and EPMA analyses. Iron and chromium oxides within Fe-rich chromite were reduced to form a Fe-Cr-C alloy. Mg-rich chrome spinels were partly reduced at 1200°C. Zircon particles were not reduced at 1200°C, but were significantly reduced at 1400°C, with the particles becoming porous and the silicon being removed.