High velocity oxy-fuel thermal spraying was used to prepare free-standing CoNiCrAlY (Co–31.7%Ni–20.8%Cr–8.1%Al–0.5%Y, all in wt%) coatings of an approximate thickness of 0.5 mm. Small punch tests under multi-step loading conditions were performed between room temperature and 600 ℃ on these samples to evaluate the ductile-to-brittle transition temperature. The microstructure of the coatings was characterised using a scanning electron microscope with energy-dispersive X-ray analysis. A two-phase structure consisting of fcc γ-Ni and bcc β-NiAl was found to exist. The displacements obtained from small punch multi-step loading tests at each load increment were relatively small and similar at temperatures below 500 ℃ but a significant increase in displacement was noted at 600 ℃. Fractographic investigation showed that the main fracture mode was dominated by extensive γ matrix tearing at elevated temperatures. A distinct stress and strain behaviour was found at 600 ℃, indicating that the ductile-to-brittle transition temperature of this CoNiCrAlY coating occurred between 500 ℃ and 600 ℃.