The synthesis of ultrafine zirconia powders by mechanochemical reactio
n of ZrCl4 with CaO has been investigated using x-ray diffraction, TEM
and DSC measurements. Mechanical milling resulted in a nanoscale mixt
ure of CaO and amorphous ZrCl4, with no evidence of any reaction havin
g occurred. Subsequent heat treatment at temperatures above 300 degree
s C resulted in the formation of separated particles of cubic ZrO2, 5-
10 nm in diameter, within an CaCl2 matrix. Measurements of the effect
of particle size on the crystal structure of ZrO2 are also reported.