Abstract: Zr(IV) was extracted by tri-n-butyl phosphate in kerosene from concentrated nitric acid solutions and the formation of the third phase during extraction was experimentally investigated. Zirconia powders were prepared by using the loaded organic phase as the bulk solution precipitated with aqueous ammonia or NaOH solution. The powder prepared was characterized with TEM, XRD,EDAX and TG-DTA. Effects of some conditions on powder preparation were studied and it was shown that nanosized particles could be obtained from this extraction system but conditions should be carefully controlled for powder purity and particle size.