ZnO micro-whiskers were successfully prepared by oxidizing of sublimated zinc acetylacetonate (Zn(C5H7O2)(2)) products. Crystallinity of ZnO whiskers was considerably improved by increasing thermal oxidation temperature. Full width at half maximum (FWHM) of ZnO (10 (1) over bar1) plane peak observed in the X-ray diffraction was 0.186degrees. SEM images of the whiskers oxidized at 1000 degreesC were a bundle of very fine whiskers and almost uniform for surface morphology. Room temperature photoluminescence (PL) spectrum of the whiskers oxidized over 400 degreesC shows a blue emission at wavelength of 420 nm. In the low temperature (4.2 K) PL spectrum of the ZnO whiskers oxidized over 800 degreesC, the emission from exciton bound to natural donor and that from free-exciton recombination were observed at 3.361 and at 3.376 eV, respectively. (C) 2003 Elsevier Science B.V. All rights reserved.