Two single crystals with compositions Fe-Ni-Co-Al-Ta and Fe-Ni-Co-Al-Ta-B were selected and fabricated by Bridgman method. Subsequently, ingots were homogenized, oriented and subjected to a two-step heat treatment process in order to obtain fine and coherent γ' precipitates. Subsequently, superelastic cycling experiments were performed at 77 K. The next step included detailed microstructural characterization using transmission electron microscopy and high-energy synchrotron X-ray diffraction measurements together with Rietveld refinement. The results show that the number of fully reversible superelastic strains is very sensitive to the size of γ' precipitates. The smaller (3 nm) γ' precipitates ensured more superelastic response compared to material with larger γ' particles size (5 nm), in which the material did not receive its original shape after 10 cycles even after being heated.