Zirconium → Zirconyl nitrate

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This example describes a low temperature method for the bulk synthesis of fine particle, crystalline ZrW2O8. 0.5M solutions of zirconium oxynitrate and ammonium metatungstate were prepared. 200ml of ammonium metatungstate solution were heated to 60° C. in a 2.0 L beaker. 100 ml of the zirconium salt solution were added to the breaker with a burette, and the mixture was stirred using mechanical stirring. The addition took approximately 1.5 hours. The addition was drop wise with very good stirring and simultaneous heating (60° C.). After the addition was complete, stirring was continued magnetically until the solution was concentrated (for one more hour). Then 250 ml of 6M HCl were added and the heating and stirring were continued until the solution was concentrated once again into a slurry (for about three hours). The slurry was transferred to a Parr bomb and was heated at 180° C. over night (for about fifteen hours) for a fast setting of gel under hydrothermal pressures. The hydrate gel was then filtered, washed with deionized water and dried in the oven (ZWO-HT-1) for three hours. This gel was then fired at 650° C. for 2.5 hours. The product obtained (ZWO-HT-2) was analyzed by XRD. The gel also was sintered at 1473K (ZWO-HT-3) for thirty minutes and was analyzed for its phase purity and bulk density. The X-ray diffractograms of the samples prior to and subsequent to sintering are presented in FIGS. 12-13.

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