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The stability of microstructure and the microhardness of a NiCoCrAlY alloy was studied after thermal treatment at high temperatures and subsequent quenching into ice water. The alloy revealed mainly two ordered phases, a gamma' phase with L12 lattice structure and a beta phase with B2 structure. The gamma' phase is shown to become unstable in the temperature range between 1073 K and 1373 K where it undergoes an order-disorder phase transformation. The low transformation temperature compared to pure Ni3Al is ascribed to deviations from the Ni3Al stoichiometry and to the additional alloying elements Co and Cr. The gamma'-gamma order-disorder transformation is shown to be attended by a decrease in microhardness of about 30 %.