Heat treatment of ␥-Ni(Al)/␥Ј-Ni 3 Al multilayer thin films demonstrates that multilayer hardness correlates with the magnitude of biaxial stress in alternating layers. Films with a columnar grain morphology and (001) texture were fabricated over a range of volume fraction and bilayer thickness via direct current magnetron sputtering onto NaCl (001) substrates at 623 K. The films were removed from substrates, heat-treated at either 673 K or 1073 K in argon, and then mounted for nanoindentation and x-ray diffraction. The biaxial stress state in each phase was furnished from x-ray diffraction measurement of (002) interplanar spacings. The 673 K treatment increases the magnitude of alternating biaxial stress state by 70 to 100% and increases hardness by 25 to 100%, depending on bilayer thickness. In contrast, the 1073 K heat treatment decreases the stress magnitude by 70% and decreases hardness by 50%. The results suggest that the yield strength of these thin films is controlled, in part, by the magnitude of internal stress. Further, thermal treatments are demonstrated to be an effective means to manipulate internal stress.