The Mechanical Activation Self propagating High temperature Synthesis (M.A.S.H.S.) processing is a new way to produce nanocrystalline iron aluminide intermetallic compounds. This process is maily the combination of two steps; in the one hand, a mechanical activation where the Fe-Al powder mixture was milled during a short time at given energy and frequency of shocks and in the other hand, a Self propagating High temperature Synthesis (S.H.S.) reaction, for which the exothermicity of the Fe + Al reaction is used. This fast propagated MASHS reaction has been in situ investigated using the Time Resolved X-Ray Diffraction (TRXRD) using a X-ray synchrotron beam and an infrared thermography camera, allowing the coupling of the materials structure and the temperature field. The effects of the initial mean compositions, of the milling conditions as well as of the-compaction parameters on the MASHS reaction are reported.