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A variety of synthesis parameters for the preparation of Zirconia nanoparticles in water-cylcohexane-hexanol-Triton X-100 microemulsion have been investigated. The results show that reaction temperatures and the molar ratio of water to surfactant( r(0)) were the predominant factors to control the specific surface area as well as particle sizes of ZrO2. The particle size first decreased with a decrease in the value of r(0), then increased after reaching a critical particle size upon further decreasing the r(0) value; on the other hand, an increase in the reaction temperature led to smaller ZrO2 particles, but the ZrO2 particle size became larger at a temperature close to the cloud point of the reverse micelles, where a small temperature disturbance would easily lead the system out of the microemulsion phase. XRD, TEM and N-2 adsorption experiments were used to characterize the ZrO2 sample. XRD results showed that the …