The aim of the present paper was to compare the evolution of Ni–Ti intermetallics in two non-conventional production techniques for the synthesis of NiTi shape memory alloy. Short term ultrahigh energy mechanical alloying is proposed to be able to describe the early stages of the milling process, which was not described in the literature previously, and to obtain intermetallics in shorter process durations. The reactive sintering using high heating rate (>300°C min− 1) is a process designed to suppress the formation of secondary intermetallics and to reduce the porosity of the product. The same phases’ formation sequence was determined for both processes. The detrimental Ti2Ni phase forms preferentially, and therefore, its presence cannot be avoided in any of the investigated techniques.
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