Structural and mechanical stability of the nano-crystalline Ni–Ti (50.9 at.% Ni) shape memory alloy during short-term heat treatments

• Change in microstructure of cold deformed NiTi wire by short term annealing.
• Recrystallization of nano-NiTi above 450 °C.
• Best properties obtained for NiTi wire annealed at 450 °C/15 min.

In this study, the nano-crystalline Nitinol (50.9 at.% Ni) was prepared by 40% cold deformation. Subsequently it was subjected to 15-min-heat treatments at 300–550 °C. Changes of the structure and mechanical properties were studied by transmission electron microscopy, micro X-ray diffraction, differential scanning calorimetry, Vickers hardness measurements, tensile and bend-type fatigue testing. It was shown that the cold drawn material contains textured nano-crystalline B2 grains of 50 nm in thickness and a high concentration of lattice defects. Its tensile strength, hardness and fatigue life were 1521 MPa, 421 HV0.05 and 2435 bending cycles to fracture, respectively. After heat-treatment up to 450 °C/15 min the material underwent Ni4Ti3 precipitation and partial recovery processes. Heat-treatments at above 450 °C induced recrystallization, grain and precipitate growth. Hardness and fatigue lives showed maxima of 692 HV0.05 and 5883 cycles, respectively, after heat-treatments at 450 °C/15 min. In contrast, both tensile strength and B2 → B19′ transformation stress decreased with increasing heat-treatment temperature, but a decrease of the tensile strength after heat-treatments at 300–450 °C was slow (tensile strength after heat-treatment at 450 °C/15 min was 1486 MPa). The observed variations of mechanical characteristics were discussed in relation to structural changes observed.

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