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Mono-dispersed particle-size-controllable nanometer yttrium stabilized zirconia powder, preparation method and applications thereof

A zirconia powder and yttrium stabilization technology, applied in the field of zirconia powder and its preparation, can solve the problems of product morphology, crystal phase and particle size being difficult to control, complex precursor preparation system, etc., achieving a wide range of concentrations and mild conditions. , the effect of low cost

Pending Publication Date: 2019-05-07
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] Based on this, the purpose of the present invention is to provide a method for preparing monodisperse nano-yttrium-stabilized zirconia powder with controllable crystal phase and particle size, which solves the problem of complex precursor preparation system and product appearance in the existing technology for preparing nano-yttrium-stabilized zirconia powder. , The technical problem that the crystal phase and particle size are not easy to control

Method used

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  • Mono-dispersed particle-size-controllable nanometer yttrium stabilized zirconia powder, preparation method and applications thereof
  • Mono-dispersed particle-size-controllable nanometer yttrium stabilized zirconia powder, preparation method and applications thereof
  • Mono-dispersed particle-size-controllable nanometer yttrium stabilized zirconia powder, preparation method and applications thereof

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preparation example Construction

[0044] A preparation method of nano-yttrium stabilized zirconia powder with controllable monodisperse particle size, the preparation method comprises the following steps:

[0045] (1) Reaction solution preparation method: prepare zirconium oxychloride, yttrium chloride, dispersant raw material solution, Zr 4+ with Y 3+ The molar concentration ratio is 99:2~90:20;

[0046] (2) Hydrothermal hydrolysis process: Transfer the reaction solution obtained in step (1) to a polytetrafluoroethylene-lined stainless steel homogeneous reaction kettle, heat up to 120-300°C for 3-20 hours of hydrothermal reaction, during the reaction process , under the condition of high-speed stirring 300-10000r / min, the concentration of 0.5-6mol / L ammonia solution or 0.1-3mol / L acid solution is added through the atomizer at 1-10000mL / min to adjust the raw material solution H + Concentration, so that Zr in the solution 4+ Partial hydrolysis to generate crystal nuclei, adjust the solution H + The concentr...

Embodiment 1

[0051] (1) Preparation of ZrOCl 2 , YCl 3 , dispersant mixed solution, wherein, hydroxypropyl methyl cellulose, hydroxypropyl cellulose, sodium tripolyphosphate are composed in equal proportions, Zr 4+ :Y 3+ The molar ratio is 97:6;

[0052] (2) Transfer the solution obtained in step (1) to a polytetrafluoroethylene-lined stainless steel reactor, heat it to 180°C for hydrothermal hydrolysis, and during the hydrothermal hydrolysis process, stir at 500r / min, by adding 3.85mol / L dilute ammonia solution to adjust the H of the final reaction solution + concentration, so that the solution final C Zr 4+ =0.6mol / L, H + The concentration is 0.1mol / L, the concentration of the dispersant is 1g / L, after 12 hours of reaction, cool to obtain a hydrated zirconia suspension;

[0053] (3) Add 10% ammonia water to the hydrated zirconia suspension at 60°C and 500r / min at 10mL / min to make Y 3+ Uniformly precipitate on the surface of hydrated zirconia particles, stop adding ammonia water w...

Embodiment 2

[0056] (1) Preparation of ZrOCl 2 , YCl 3 , hydroxypropyl cellulose mixed solution, wherein Zr 4+ :Y 3+ The molar ratio is 97:6;

[0057] (2) Transfer the solution obtained in step (1) to a polytetrafluoroethylene-lined stainless steel reactor, heat it to 180°C for hydrothermal hydrolysis, and during the hydrothermal hydrolysis process, stir at 500r / min, by adding 3.15mol / L dilute ammonia solution to adjust the H of the final reaction solution + concentration, so that the solution final C Zr 4+ =0.6mol / L, H + Concentration is 0.3mol / L, hydroxypropyl cellulose concentration is 1g / L, cools after reacting for 12h to obtain hydrated zirconia suspension;

[0058] (3) Add 10% ammonia water to the hydrated zirconia suspension at 60°C and 500r / min at 10mL / min to make Y 3+ Precipitate uniformly on the surface of hydrated zirconia particles, stop adding ammonia water when the pH of the suspension is > 9, obtain the suspension after yttrium precipitation, statically age for 12 ho...

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Abstract

The invention relates to mono-dispersed particle-size-controllable nanometer yttrium stabilized zirconia powder, a preparation method and applications thereof. The preparation method comprises: mixingand dissolving a zirconium salt, an yttrium salt and a dispersing agent according to a certain ratio to obtain a mixed solution; heating the mixed solution, carrying out a hydrothermal reaction, adjusting the H<+> concentration of the solution by adding ammonia water or an acid solution during the hydrothermal process, and cooling to a temperature of less than 90 DEG C after the reaction is completely performed to obtain a hydrated zirconia suspension; adding ammonia water to the zirconia suspension to adjust the pH value to achieve an alkaline state, carrying out standing aging, and carryingout centrifugal separation to obtain zirconia precipitate; and carrying out a series of post-treatment processes on the zirconia precipitate to obtain the nanometer yttrium stabilized zirconia powder. According to the present invention, the method easily controls the shape, the particle size and crystal phase of the product, has simple and convenient operation, and is suitable for factory production.

Description

technical field [0001] The invention relates to the technical field of material science, and more particularly relates to a nanometer yttrium-stabilized zirconia powder with controllable monodisperse particle size and its preparation method and application. Background technique [0002] Zirconia ceramics are known as the second largest metal oxide ceramics after alumina ceramics, and the main raw material for its production is zirconia powder. Composite zirconia powder is a non-toxic, odorless white powder with fine powder, good chemical uniformity, easy molding, and sintering. It is mainly used in various structural ceramics, electronic ceramics, sensitive ceramics, bioceramics, advanced refractory materials, In industries such as mechanical parts, cutting tools, watch cases, optical fiber connectors, and solid oxygen fuel cells, it has the characteristics of high strength, high fracture toughness, corrosion resistance, wear resistance, and pollution prevention. [0003] I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/48C04B35/626C04B35/622
Inventor 刘智勇朱银刘志宏李启厚洪明浩
Owner CENT SOUTH UNIV
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