ZnCo2O4 whiskers 2-5 mu m in diameter and up to 50 mu m in length, retaining their composition and shape up to 800 degrees C, are prepared via decomposition of the mixed oxalate Zn1/3CO2/3C2O4 center dot 2H(2)O in air and are characterized using chemical analysis, x-ray diffraction, IR spectroscopy, and scanning electron microscopy.