For the development of ceramic thermal barrier coatings, spray-grade yttria-stabilized zirconia microspheres were prepared by the sol-gel technique. Oxide microspheres were obtained by calcination of the corresponding gel spheres at 1000 °C. Scanning electron microscopic and optical microscopic observations revealed the material thus obtained to have a predominantly spherical morphology and the requisite size distribution (5-50 μm). The dense, calcined microspheres showed good flowability. X-ray diffraction studies indicated the presence of the tetragonal polymorph of ZrO2 as the major phase, in addition to about 14% monoclinic ZrO2. The plasma-sprayed YSZ coatings made from the sol-gel-derived microspheres showed a further decrease in the monoclinic ZrO2 content (6%). The coatings survived 40-50 thermal cycles (30 min at 1200 °C followed by a water quench), indicating good thermal shock resistance. © 1993 Chapman & Hall.