The XRD analysis (Figure 2 ) explains the presence of Cr3C2 [13, 15, 20, 27, 29], and Cr7C3 in the micrometric powder. The intensity of the peaks decreases, while they expand as a function of milling time. The increase in the width of the XRD peaks with the grinding time is attributed to the decrease in the carbide structure that forms small grains. Moreover, the peaks of the Cr3C2 persist after 12 hours of HEM, indicating preservation of some extent of the crystalline structure. The Cr7C3 content decreases with the HEM time, which can be explained by the atom’s rearrangement due the high strain energy. Furthermore, the Cr2O3peak emerges with the HEM time increase, which could be explained by the increased amount of the Cr2O3 protective film surrounding the increased amount of nanoparticle free surfaces, as the particle’s diameter decrease. Ni XRD analysis was not performed because the major concern was with carbide, as it is harder and has a higher melting point, which makes it more difficult to deform when HEM process is performed.