The paper presents a comparative study of two methods for the fabrication of Ni/Al-based metal-intermetallic laminate (MIL) composites within a steel matrix: shock wave loading (SWL) and a combined SWL/heat treatment (HT) method. Initiating the reaction in self-propagating high-temperature synthesis (SHS) mode under shock wave loading resulted in the formation of an intermetallic layer (IL) with an average microhardness of 500 HV. This IL exhibited both non-uniform thickness and cracking. The reaction initiated at the sample's end, where conditions conducive to SHS were established, and then propagated towards the top. At the top of the sample, the reaction products were quenched because heat removal exceeded heat generation. The two-step SWL/HT method ensured the formation of a multiphase IL (NiAl, Ni2Al3, Ni3Al) without cracks, but it was accompanied by gas evolution, causing deformation and delamination. The microhardness varied from 370 to 850 HV, with an average of 530 HV. Optimizing the process by removing gases maintained the interface's integrity but resulted in localized transverse cracks. The average microhardness of the IL was 590 HV, with a range of 450–900 HV. The heating rate during HT significantly affected the completeness of the transformation: slow heating (11.5 °C/min) promoted more complete NiAl formation compared to rapid heating (23 °C/min). Recommendations for minimizing defects in each method were developed. The results obtained are of interest for fabricating composites with improved mechanical and thermal properties, which are in demand in the aerospace and energy industries.
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