Effect of Aging on Superelastic Response in [001]-Oriented Single Crystals of FeNiCoAlTiNb Shape-Memory Alloys.

In this study, the effect of aging heat treatment on the superelastic properties and microstructure of [001]-oriented FeNiCoAlTiNb (at.%) single crystals was investigated using the cyclic superelastic strain test and a transmission electron microscope (TEM). The TEM results reveal that the average precipitate size is around 3-5 nm in the 600 °C/24 h samples, 6-8 nm in the 600 °C/48 h samples, and 10-12 nm in the 600 °C/72 h samples. The results indicate that precipitate size increases as aging time increases from 24 to 72 h. EDS analysis results show decreased Fe and increased Ni when the analyzed line crosses the precipitate region. The diffraction pattern results show that the precipitate has an L1 crystal structure. The thermo-magnetization curves of single crystals under the three aging conditions (600 °C/24 h, 600 °C/48 h, and 600 °C/72 h) show that the values of the transformation temperatures increased from 24 to 72 h. Magnetization was saturated at 140 emu/g under the magnetic field of 7 Tesla. When increasing the magnetic field from 0.05 to 7 Tesla, the transformation temperatures rose. The results indicate that magnetic fields can activate martensitic transformation. From the results of the superelasticity test at room temperature, [001]-oriented FeNiCoAlTiNb single crystals aged at 600 °C for 24, 48, and 72 h presented recoverable strains of 3%, 5.1%, and 2.6%, respectively. Digital image correlation (DIC) results of the aged samples show that two martensite variants were activated during the superelasticity test. The two variants form corresponding variant pairs (CVPs) and improve the recoverable strain of superelasticity. Although maximum recoverable strain was obtained for the 600 °C/48 h samples, the samples show poor cyclic stability at room temperature after applying the 6% strain. According to the DIC results, the retained martensite, which is pinned by dislocations, was observed after the test. The irrecoverable strain was attributed to the residual martensite. For the 600 °C/72 h samples, the large size of the precipitates poses an obstacle to dislocation transformation and formation. The dislocations increase the stress hysteresis width and stabilize the martensite, causing poor recoverability.