Composite rare earth modified zirconia ceramic powder and preparation method thereof

A technology of zirconia ceramics and composite rare earth, which is applied in the field of composite rare earth modified zirconia ceramic powder and its preparation, and can solve the problems of difficult treatment and high consumption of organic waste water.

Pending Publication Date: 2019-05-03
CENT SOUTH UNIV
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  • Application Information

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Problems solved by technology

[0004] Based on this, the present invention provides a method for preparing composite rare earth modified zirconia ceramic powder through hydrothermal hydrolysis and surface induced precipitation coating rare earth, which solves the above-mentioned consumption of a large amount of ethylene glycol and polyvinyl alcohol organic matter, and The technical problem that the generated organic waste water is difficult to treat

Method used

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  • Composite rare earth modified zirconia ceramic powder and preparation method thereof
  • Composite rare earth modified zirconia ceramic powder and preparation method thereof
  • Composite rare earth modified zirconia ceramic powder and preparation method thereof

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preparation example Construction

[0040] A method for preparing rare earth-modified zirconia composite powder by means of hydrothermal hydrolysis and surface induction coating rare earth, the preparation method comprising the following steps:

[0041] (1) Reaction solution preparation method: prepare zirconium oxychloride, rare earth salt, dispersant raw material solution, its Zr 4+ Concentration 0.1~2.5mol / L, Zr 4+ with Y 3+ The molar concentration ratio is 99:2~90:20, Zr 4+ The ratio of molar concentration to other rare earth elements is 99:1~92:8, and the concentration of dispersant is 0.5~5g / L; the raw material solution is placed in a reaction kettle, and the temperature is 25~90℃, and the high speed stirring is 300~1000r / min. Next, through an atomizer, add a solution of 0.5-6 mol / L ammonia solution or a 0.1-3 mol / L hydrochloric acid solution at a rate of 1-10000 mL / min to adjust the raw material solution H + Concentration, so that Zr in the solution 4+ Partial hydrolysis to generate crystal nuclei, ad...

Embodiment 1

[0047] (1) Preparation of ZrOCl 2 , YCl 3 , Ce(NO 3 ) 3 , mixed solution of hydroxypropyl cellulose, wherein Zr 4+ :Y 3+ : Ce 3+ The molar ratio is 95.05:1.45:3.5, the raw material solution is placed in the reaction kettle, and the H of the final reaction solution is adjusted by adding 5.95mol / L dilute ammonia solution in a 60°C water bath and stirring at 500r / min. + concentration, so that the solution final C Zr 4+ =1.6mol / L, H + The concentration is 1.5mol / L, the concentration of hydroxypropyl cellulose is 0.5g / L, and the hydrothermal reaction solution is obtained;

[0048] (2) Transfer the solution obtained in step (1) to a polytetrafluoroethylene-lined stainless steel reactor, heat to 180°C for hydrothermal hydrolysis, react for 12 hours and then cool to obtain a hydrated zirconia suspension;

[0049] (3) Add 10% ammonia water to the hydrated zirconia suspension at 60°C and 500r / min at 10mL / min to make Y 3+ / C 3 + Uniformly precipitate on the surface of hydrate...

Embodiment 2

[0052] (1) Preparation of ZrOCl 2 , YCl 3 , Ce(NO 3 ) 3 , mixed solution of hydroxypropyl cellulose, wherein Zr 4+ :Y 3+ : Ce 3+ The molar ratio is 94.57:1.93:3.5, the raw material solution is placed in a reaction kettle, and the H of the final reaction solution is adjusted by adding 5.95mol / L dilute ammonia solution in a 60°C water bath and stirring at 500r / min. + concentration, so that the solution final C Zr 4+ =1.6mol / L, H + The concentration is 1.2mol / L, and the concentration of hydroxypropyl cellulose is 0.5g / L to obtain the hydrothermal reaction solution;

[0053] (2) Transfer the solution obtained in step (1) to a polytetrafluoroethylene-lined stainless steel reactor, heat to 160°C for hydrothermal hydrolysis, and cool after reacting for 12 hours to obtain a hydrated zirconia suspension;

[0054] (3) Put the suspension at 60°C and 500r / min, add 10% ammonia water at 10mL / min to make Y 3+ / C 3+ Uniformly precipitate on the surface of hydrated zirconia particle...

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Abstract

The invention relates to a composite rare earth modified zirconia ceramic powder and a preparation method thereof. The preparation method comprises the following steps: heating a mixed solution of zirconium salt, rare earth salt and a dispersant to 25 DEG C to 90 DEG C, and adding ammonia water or an acid liquid into the mixed solution so as to adjust the concentration of H+ in the mixed solutionto 0.1 to 5 mol / L; heating the H+ concentration adjusted solution, carrying out a hydrothermal reaction, and after the reaction is completed, carrying out cooling to 90 DEG C or below so as to obtaina hydrated zirconia suspension; adding ammonia water into the hydrated zirconia suspension so as to adjust the pH value of the hydrated zirconia suspension to alkaline, and carrying out standing and aging; and centrifuging the mixed solution, carrying out washing, drying and calcining, uniformly mixing a calcined powder with deionized water and a dispersant, carrying out ball milling so as to obtain a slurry, and subjecting the slurry to fine grinding, centrifuging, washing and drying so as to obtain a nanometer composite rare earth modified zirconia ceramic powder. The method provided by theinvention solves the technical problem of consumption of a large amount of ethylene glycol and polyvinyl alcohol organic matters and difficult treatment of organic-matter wastewater generated in a conventional method.

Description

technical field [0001] The invention relates to the technical field of powder material preparation, and more specifically, to a composite rare earth modified zirconia ceramic powder and a preparation method thereof. Background technique [0002] Zirconia is a very important structural material. Rare earth-doped stabilized zirconia, especially yttrium-doped stabilized zirconia, has low thermal conductivity, good strength and toughness, low elastic modulus, high thermal shock resistance, and high operating temperature. Among various metal oxide ceramics, zirconia is second only to alumina ceramics in importance. One of the fatal weaknesses of pure zirconia ceramics is its "brittleness", that is, it has poor fracture toughness due to volume expansion caused by phase transformation. [0003] The Chinese Patent Office discloses a high-performance zirconia ceramic superfine powder raw material and its preparation process (application number: CN02115615.8). Raw material and prepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/48C04B35/626
Inventor 刘智勇刘志宏李启厚洪明浩江道言朱银
Owner CENT SOUTH UNIV
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