Measurement of Phase Transformation Rates During the Reduction of Iron Oxides Using High-Temperature X-Ray Diffraction

Recent advances in X-ray diffraction (XRD) technology have made it possible to conduct powder XRD measurements on samples at high temperatures during reaction. State-of-the-art detectors are now capable of rapidly acquiring diffraction patterns across a wide angular range (typically 120"20) enabling phase transformation rates to be measured directly during sample reaction. In this study, the phase transformations during the reduction of hematite to metallic iron by five per cent hydro ºen in nitrogen gas mixtures, were measured in situ between 500 - 700 C. Complete X-ray diffraction patterns were acquired within 15 seconds every one minute, enabling direct measurement of the transient phase abundances during the reaction. The data were quantitatively analysed by the Rietveld method to yield the abundances of hematite, magnetite, wustite and metallic iron, as functions of time during the reduction process. A first-order reactions-in-series model was proposed, and the reaction rate constants and activation energy were determined from the time-dependent phase abundance data.