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Supercritical hydrothermal synthesis method of nanometer zirconium oxide powder

A nano-zirconia, supercritical water technology, applied in zirconia, nanotechnology, nanotechnology and other directions, can solve the problems of abnormal growth of powder particles, unavoidable grain growth, long reaction time, etc., to achieve narrow particle size distribution, Good stability and high purity

Active Publication Date: 2013-04-24
SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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Problems solved by technology

[0003] At present, there are many methods for preparing nano-zirconia powder, such as precipitation method, sol-gel method, metal alkoxide hydrolysis method, microemulsion method, conventional hydrothermal method, etc., among which precipitation method, sol-gel method, hydrolysis method, micro Generally, the emulsion method needs to be calcined at high temperature, which leads to very serious agglomeration and abnormal growth of powder particles. Although this phenomenon can be effectively alleviated by lowering the calcination temperature, it will lead to the problem of low crystallinity.
The conventional hydrothermal method requires a long reaction time, and it is difficult to avoid the problem of grain growth.

Method used

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  • Supercritical hydrothermal synthesis method of nanometer zirconium oxide powder

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[0022] A nano-zirconia powder supercritical hydrothermal synthesis method, the synthesis steps are:

[0023] 1) Dissolving the oxalic acid and the soluble zirconium compound in water respectively at a temperature of 60-80°C to obtain an oxalic acid solution with a molar concentration of 0.4-2.5 mol / L and a zirconium compound solution with a molar concentration of 0.1-2.0 mol / L;

[0024] 2) Under stirring, add the zirconium compound solution into the oxalic acid solution for precipitation reaction to obtain white zirconium oxalate precipitate, the molar ratio of oxalic acid to zirconium ions is ≥2.0;

[0025] 3) The obtained zirconium oxalate precipitate is washed and then dried, and then thermally decomposed after drying. The thermal decomposition reaction temperature is 360°C-470°C, and the thermal decomposition reaction time is 0.5-1h;

[0026] 4) The product after the thermal decomposition reaction is subjected to wet pulverization to obtain nano-scale dispersion slurry;

...

Embodiment

[0038] Weigh 322 g of zirconium oxychloride octahydrate and 270 g of oxalic acid, dissolve them in 600 ml and 1000 ml of pure water respectively at 70°C, add the zirconium oxychloride solution into the oxalic acid solution under stirring to form a white precipitate; Wash until the chloride ion content is less than 100ppm, then dry, heat at 400°C for 40 minutes after drying, then transfer to a planetary mill, control the material-water ratio = 1:2, and grind at 300 rpm for 7 hours; grind the Slurry transfer adopts continuous supercritical hydrothermal synthesis equipment for reaction (reaction temperature = 420°C, reaction pressure = 30Mpa, reaction time = 30 seconds), the product obtained by the reaction is washed several times with pure water and dried to measure the specific surface area and XRD, specific surface area=117.45m2 / g, XRD measurement shows that the crystal phase of the product is a monoclinic phase.

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Abstract

The invention relates to a supercritical hydrothermal synthesis method of nanometer zirconium oxide powder. The method comprises the following steps of: respectively dissolving oxalic acid and a soluble zirconium compound in water, adding the zirconium oxide solution into the oxalic acid solution under a stirring condition, performing precipitation reaction to obtain white zirconium oxalate precipitate; washing and drying the zirconium oxalate precipitate and then performing thermal decomposition reaction, and performing wet-type grinding on the thermally decomposed product to obtain nanometer-grade dispersed slurry; and performing supercritical hydrothermal reaction on the nanometer slurry to obtain the nanometer zirconium oxide powder. The nanometer zirconium oxide powder prepared by using the method has the advantages of fine grain, narrow granularity distribution, good stability and high purity.

Description

technical field [0001] The invention relates to a method for synthesizing inorganic materials, in particular to a method for synthesizing nanoscale zirconia powder. Background technique [0002] Zirconia is used in fine ceramics, refractory materials, catalyst raw materials, piezoelectric components, optical fiber connectors, gas sensors, solid fuel cells and thermal barrier coatings, etc., and has excellent physical, chemical and material process characteristics. Nano zirconia powder has the characteristics of small particle size and large specific surface, which improves its application performance. [0003] At present, there are many methods for preparing nano-zirconia powder, such as precipitation method, sol-gel method, metal alkoxide hydrolysis method, microemulsion method, conventional hydrothermal method, etc., among which precipitation method, sol-gel method, hydrolysis method, micro Generally, the emulsion method needs to be calcined at high temperature, which lea...

Claims

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Application Information

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IPC IPC(8): C01G25/02B82Y30/00
CPCY02P20/54
Inventor 莫雪魁宋锡滨张兵张曦
Owner SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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