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The microstructure of ZrO 2 fine particles produced by a novel synthesis method at 450°and 950°C has been studied. The fundamentals of the synthesis method, which involves both chemical and diffusion phenomena, are presented. The method is based on mass transport through the gaseous phase between metallic zirconium and Fe 2 O 3 powder. The mass-transporting chemical species are zirconium and iron chlorides. This article focuses on the microstructure and structure of ZrO 2 particles formed by the reaction between gaseous ZrCl 4 and solid Fe 2 O 3 , which is a relevant reaction step that occurs during the synthesis process. The resulting ZrO 2 crystals grown on Fe 2 O 3 particles have been analyzed using transmission electron microscopy. Microstructural characterization has been complemented by X-ray diffractometry analysis. Tetragonal-ZrO 2 is produced at 450°C and monoclinic-ZrO 2 single crystals are produced at 950°C.