Process of preparing zirconium oxide nano powder by supersonic sol-gel process
A technology of nano-powder and gel method, which is applied in the direction of zirconia to achieve the effect of promoting the preparation reaction, inhibiting the formation of agglomeration, and overcoming the agglomeration phenomenon
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Embodiment 1
[0020] 100ml of ammonia water (pH=10) was added into the reactor, and then 150ml of zirconium oxychloride solution with a concentration of 0.25mol / L was added dropwise at a rate of 7ml / min under constant stirring to adjust the pH value of the reaction system to 9. During this process, the sound field is added at uniform time intervals, the ultrasonic power is 500W, and the action time is 60 seconds each time. The obtained zirconium hydroxide colloid was aged at 30°C for 10 hours, washed with distilled water until chloride ions could not be detected with silver nitrate solution, no ultrasound was added during the washing stage, and the wet gel was dried at 80°C for 2 hours and ground, then dried at 600°C Calcined to obtain white zirconia powder. According to TEM and X-ray diffraction analysis, the zirconium hydroxide wet gel is finer, denser and more uniform. The obtained zirconia particles have the smallest particle size and narrow distribution, with a grain size of 15.2 nm. ...
Embodiment 2
[0022] Add 800ml of ammonia water with pH=11 in the reactor, then drip 100ml of zirconium oxychloride solution with a concentration of 1.0mol / L under constant stirring at a rate of 10ml / min, and adjust the pH value of the reaction system at 9 with ammonia water. The obtained zirconium hydroxide colloid was aged at 30°C for 8 hours, washed 8 times with distilled water using a probe-type ultrasonic generator under the condition of an ultrasonic field of 600W, and finally ultrasonically washed once with absolute ethanol, and each ultrasonic action time was 60 Second. The wet gel was dried at 80°C for 2 hours and ground, then calcined at 600°C for 2 hours to obtain white zirconia powder. According to TEM and X-ray diffraction analysis, the grain size of the obtained zirconia nanopowder is 15.3nm.
Embodiment 3
[0024] Add 400ml of ammonia water with pH=10 in the reactor, then drop 200ml of zirconium oxychloride solution with a concentration of 0.5mol / L at a rate of 5ml / min under constant stirring, and adjust the pH value of the reaction system between 9.3 with ammonia water between. After each instillation, it was subjected to an ultrasonic action with a power of 520W, and each ultrasonic action time was 60s. The obtained zirconium hydroxide colloid was aged at 30°C for 8 hours, washed 8 times with distilled water using a probe-type ultrasonic generator under the condition of an ultrasonic field of 600W, and finally ultrasonically washed once with absolute ethanol, and each ultrasonic action time was 60 Second. The wet gel was dried at 80°C for 2 hours and ground, then calcined at 600°C for 2 hours to obtain white zirconia powder. According to TEM and X-diffraction analysis, the grain size of the obtained zirconia nanopowder is 14.7nm.
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