Simultaneous IR and time-resolved X-ray diffraction measurements for studying self-sustained reactions

Self-propagating high-temperature synthesis provides an attractive practical method for producing advanced materials such as ceramics, composites and intermetallics. This kind of reaction has been investigated in situ using time-resolved X-ray diffraction, with an X-ray synchrotron beam (D43 beamline, LURE, Orsay) coupled to simultaneous IR thermography to study structural transformations and thermal evolution. With short acquisition times (30 ms per pattern) it has been possible to observe several steps before obtaining compounds. Two different compound formations have been described: (i) the different steps of reaction, aluminium melting, subsequent temperature increase and fast reaction between Al and Ni at such temperatures that only Ni and AlNi are solid and all other compositions are liquid and well identified; (ii) the formation of FeAl. Here, a portion of the iron seems to transform into its allotropic phase and this transition stabilizes the reaction temperature at ∼1173 K. In addition, the aluminium melting during the reaction explains why the nanostructure induced by the mechanical activation is maintained in the end product.