Аннотация
This study investigates the control of the phase-structural state in Ni–45Ti–xCu (x = 5, 7 at.%) shape memory alloys fabricated via a shortened powder metallurgy route: mechanical activation → spark plasma sintering (SPS) → heat treatment. Compact samples were produced from mechanically alloyed powders (650–750 rpm, up to 5 h) and sintered at 900 °C. The structure and microstructure were characterized using X-ray diffraction (to identify B2/B19′/Ni4Ti3 phases and assess ordering) and SEM–BSE/EDS (to analyze morphology, porosity, and Ni-rich precipitates). Two post-processing treatments were applied: single-stage annealing (500 °C, 2 h) and a three-stage treatment (900 °C/30 min → water quenching → 300 °C/20 min). Mechanical alloying transformed the initial elemental powder mixture (fcc-Ni, hcp-Ti, fcc-Cu) into a supersaturated fcc-(Ni, Cu, Ti) solid solution with emerging NiTi phases, with a minimum particle size achieved after ~300 min at 750 rpm. SPS compaction yielded a high-density matrix consisting predominantly of the B2 phase. Single-stage annealing preserved B19′ martensite and Ni4Ti3 precipitates, particularly in the 5 at.% Cu alloy. In contrast, the three-stage treatment dissolved the Ni4Ti3 precipitates, suppressed the formation of B19′ and R phases, and stabilized a highly ordered B2 matrix. Increasing the Cu content from 5 to 7 at.% significantly enhanced the B2 phase fraction, reduced secondary nickel-rich phases, and improved structural homogeneity, evidenced by a continuous neck network and closed porosity. The optimized condition—7 at.% Cu combined with the three-stage annealing—produced a microstructure with >95% B2 phase, <1% Ni4Ti3, and ~98% relative density. This forms the prerequisite microstructural state for a narrow transformation hysteresis and high functional cyclic stability.