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The oxidation behavior of zirconium diboride containing 30 vol% silicon carbide particulates was investigated under reducing conditions. A gas mixture of CO and ∼350 ppm CO2 was used to produce an oxygen partial pressure of ∼10−10 Pa at 1500°C. The kinetics of the growth of the reaction layer were examined for reaction times of up to 8 h. Microstructures and chemistries of reaction layers were characterized using scanning electron microscopy and X-ray diffraction analysis. The kinetic measurements, the microstructure analysis, and a thermodynamic model indicate that oxidation in CO–CO2 produced a non-protective oxide surface scale.