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A Ni-based alloy was heat treated by changing the temperature and ambient atmosphere of the heat treatment. Morphology, crystal structure, and physical performance of the Ni-based alloy were characterized via SEM, XRD, TEM, and PPMS. Results show that due to the heat treatment process, the grain growth of the Ni-based alloy and the removal of impurities and defects are promoted. Both the orientation and stress caused by rolling are reduced. The permeability and saturation magnetization of the alloy are improved. The hysteresis loss and coercivity are decreased. Higher heat treatment temperature leads to increased improvement of permeability and saturation magnetization. Heat treatment in hydrogen is more conducive to the removal of impurities. At the same temperature, the magnetic performance of the heat-treated alloy in hydrogen is better than that of an alloy with heat treatment in vacuum. The Ni-based alloy shows an excellent magnetic performance on 1,373 K heat treatment in hydrogen atmosphere. In this process, the µ , B , P , and H of the obtained alloy are 427 mHm , 509 mT, 0.866 Jm , and 0.514 Am , respectively. At the same time, the resistivity of alloy decreases and its thermal conductivity increases in response to heat treatment.