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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

Inactive Publication Date: 2005-01-05
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there are no reports on the preparation of zirconia nanopowders by coupling ultrasonic technology and sol-gel method at home and abroad.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention discloses a method of preparing ZrO2 nano powder by ultrasonic sol-gel method, including the following steps: adding a certain amount of ammonia water to a reactor, and during continuously stirring, dropping in zirconium oxychloride solution at a proper speed; making ultrasonic action; ageing; washing zirconium oxychloride colloid by distilled water until no residual ions exist, and in washing, applying ultrasonic action; drying the prepared wet gel by anhydrous alcohol and grinding, burning at temperature 500-750 deg.C for 2 h and obtaining ZrO2 nano powder. It combines the ultrasonic technique with the sol-gel method to prepare ZrO2 nano powder, achieving remarkable effect and able to produce obvious social and economical benefits.

Description

technical field [0001] The invention relates to a preparation method of zirconia nano-powder, in particular, the coupling of ultrasonic technology and sol-gel preparation technology is used for the preparation of zirconia nano-powder. Background technique [0002] There are many methods for preparing zirconia nanopowders, including gas-phase method and liquid-phase method. The liquid-phase chemical method has a stronger competitive advantage, because the industrial process control and equipment amplification technology related to this method have already been developed. More mature and less expensive. Liquid-phase methods include sol-gel method, alcohol salt hydrolysis method, hydrothermal method, emulsion method and co-precipitation method, etc. Among them, sol-gel method is a method that is particularly valued in liquid-phase wet chemical method. The advantages of low temperature, simple process and easy control are an effective method for industrial production. However,...

Claims

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Application Information

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IPC IPC(8): C01G25/02
Inventor 陈玲李晓玺叶建东李琳胡松青李冰
Owner SOUTH CHINA UNIV OF TECH
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