Design and application of a high-temperature microfurnace for an in situ X-ray diffraction study of phase transformation.

Thermal treatment of mineral ores such as ilmenite can initiate phase transformations that could affect their activation or deactivation, subsequently influencing their ability to dissolve in a leaching agent. Most laboratory-based X-ray diffraction (XRD) studies were carried out ex situ in which realistic diffraction patterns could not be obtained simultaneously with occurring reactions and were time-consuming. The availability of synchrotron-radiation-based XRD not only allows in situ analysis, but significantly shortens the data recording time. The present study details the design of a robust high-temperature microfurnace which allows thermal processing of mineral ore samples and the simultaneous collection of high-resolution synchrotron XRD data. In addition, the application of the manufactured microfurnace for in situ study of phase transformations of ilmenite ore under reducing conditions is demonstrated.