In situ synchrotron investigation of MoSi2 formation mechanisms during current-activated SHS sintering

The development and control of the mechanically activated spark plasma sintering (MASPS) process is the main objective to be achieved in producing bulk nano-organized materials with perfectly controlled composition and microstructure. Consequently, it was essential to develop original experiments, such as time resolved X-ray diffraction with the X-ray synchrotron beam (D2AM-BM2, ESRF Grenoble) coupled to IR thermography to monitor in situ structural and thermal evolution during the current-activated SHS sintering process in the Mo–Si system. A new sample holder was designed in order to reproduce the synthesis conditions of the MASPS process, obviously without the consolidation step. The versatility of the set-up and the new possibilities offered by the design of new sample holders allow a new interpretation of MoSi2 formation mechanisms during current-activated SHS sintering.