The formation and decomposition of silico-ferrite of calcium and aluminium (SFCA) and SFCA-I iron ore sinter bonding phases have been investigated using in situ synchrotron and laboratory X-ray diffraction (XRD) and neutron diffraction (ND). An external standard approach for determining absolute phase concentrations via Rietveld refinement-based quantitative phase analysis is discussed. The complementarity of in situ XRD and ND in characterising sinter phase formation and decomposition is also shown, with the volume diffraction afforded by the neutron technique reducing errors in the quantification of magnetite above ~1200 °C. Finally, by collecting 6 s laboratory XRD datasets and using a heating rate of 175 °C min−1, phase formation and decomposition have been monitored under heating rates more closely approximating those encountered in industrial iron ore sintering.

In order to investigate the hydrogenation of intermetallic compounds, a gas pressure cell for in situ neutron powder diffraction based on a sapphire crystal tube was constructed. By proper orientation of the single crystal Bragg peaks of the container material can be avoided, resulting in a very low diffraction background. Using a laser heating and gas pressure controller, the hydrogenation (deuteration) of palladium and palladium rich intermetallics was studied in real time up to 8 MPa gas pressure and 700 K. Crystal structure parameters of palladium deuterides could be obtained under various deuterium gas pressures, corresponding to compositional ranges of 0.04≤x≤0.11 for the α-phase and 0.52≤x≤0.72 for the β-phase at 446 K. In situ neutron powder diffraction of the deuteration of a thallium lead palladium intermetallic Tl1-xPbxPd3 shows two superstructures of the cubic closest packing (ccp) to transform independently into a AuCu3 type structure. This proves a direct reaction to the deuterium filled AuCu3 type structure instead of a reaction cascade involving different ccp superstructures and thus gives new insights into the reaction pathways of palladium rich intermetallic compounds.