In order to produce shape memory rings for constrained-recovery pipe couplings, from Fe-14 Mn-6 Si-9 Cr-5 Ni (mass%) powders, the main technological steps were (i) mechanical alloying, (ii) sintering, (iii) hot rolling, (iv) hot-shape setting, and (v) thermomechanical training. The article generally describes, within its experimental-procedure section, the last four technological steps of this process the primary purpose of which has been to accurately control both chemical composition and the grain size of shape memory rings. Details of the results obtained in the first technological step, on raw powders employed both in an initial commercial state and in a mixture state of commercial and mechanically alloyed (MA) powders, which were subjected to several heating-cooling cycles have been reported and discussed. By means of differential scanning calorimetry (DSC), scanning electron microscopy (SEM), and X-ray diffraction (XRD), the thermal behaviors of the two sample powders have been analyzed. The effects of the heating-cooling cycles, on raw commercial powders and on 50% MA powders, respectively, were argued from the point of view of specific temperatures and heat variations, of elemental diffusion after thermal cycling and of crystallographic parameters, determined by DSC, SEM, and XRD, respectively.