Preparation method of high-dispersion nano-zirconia powder

A nano-zirconia and zirconia powder technology, applied in zirconia and other directions, can solve the problems of colloidal precipitates that are difficult to wash, decrease in purity, material cracking, etc., and achieve the effect of narrow particle size distribution, good dispersibility, and improved purity.

Inactive Publication Date: 2019-04-05
上海上惠纳米科技有限公司
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] Zirconium dioxide (ZrO2) has a special property - martensitic phase transformation. As the temperature changes, the structure of ZrO2 can change. The low temperature is monoclinic ZrO2 (m-ZrO2), and the high temperature reaches 1170 ° C. It is all transformed into tetragonal ZrO2 (t-ZrO2), and then heated to 2370 ° C to transform into cubic ZrO2 (c- ZrO2), and this is a reversible phase transition process, and the transition process is accompanied by shear strain and volume change, so that the zirconia material The thermal shock resistance of the material is greatly reduced and the material cracks, which seriously limits the application of zirconia ceramics.
At present, the methods for preparing zirconia powder include hydrolysis method, precipitation method, microemulsion method, hydrothermal method, high-temperature spray pyrolysis method, spray inductively coupled plasma method and freeze-drying method, among which the coprecipitation method has simple and easy process requirements. Add other oxides as stabilizers, but this method is easy to introduce other impurity elements to cause a decrease in purity, the formed colloidal precipitate is difficult to wash, the filtration speed is slow, and high temperature calcination is required, and block agglomeration is prone to occur during the drying process; and The hydrothermal method can directly obtain crystalline oxides from the solution, avoiding the traditional calcination process of converting hydroxides into oxides, and its particle size and shape can be controlled, reducing the introduction of external impurities and the generation of hard polymers. Possible, but overall process costs are higher and yields are lower

Method used

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Embodiment 1

[0029] A preparation method of high-purity and highly dispersed nano-zirconia powder, the method comprising the following steps:

[0030] A. Weigh 131g of ZrOCl2 8H2O and 3.88g of YCl3 6H2O, put them in a container, add deionized water to 1L, so that the concentration of zirconium ions is 0.4mol / L, and stir evenly until the solution is clear;

[0031] B. Weigh 2g of polyethylene glycol 400, and add it to the clear solution prepared in step A, and stir at room temperature;

[0032] C. control the stirring speed in the step B, slowly drop the NaOH solution of 1mol / L in the solution, until the reaction ends when the pH value of the solution is 10;

[0033] D. At normal temperature, the precipitation solution prepared in step C is aged for 24 hours, then added to the ceramic composite membrane separation equipment, and the precipitation agent is cleaned by ultrafiltration with deionized water to remove impurity ions in the filtrate until the use of 0.1 mol / L silver nitrate soluti...

Embodiment 2

[0038] A preparation method of high-purity and highly dispersed nano-zirconia powder, the method comprising the following steps:

[0039] A. Weigh 131g of ZrOCl2 8H2O and place it in a container, add deionized water to 0.5L to configure the zirconium ion concentration at 0.8mol / L, then weigh 1.5g of yttrium oxide and dissolve it in concentrated nitric acid. After stirring and dissolving Add it to the zirconium solution and stir evenly until the solution becomes clear;

[0040] B. Weigh 2g of polyethylene glycol 400, and add it to the clear solution prepared in step A, and stir at room temperature;

[0041] C. control the stirring speed in the step B, slowly add dropwise the ammonia solution of 25% mass percent concentration in the solution, until the pH value of the solution is at 9 o'clock and the reaction ends;

[0042] D. At normal temperature, the precipitation solution prepared in step C is aged for 18 hours, then added to the ceramic composite membrane separation equipm...

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Abstract

The invention belongs to the technical field of ceramic powder preparation, and particularly relates to a preparation method of high-dispersion nano-zirconia powder. According to the method, doped yttrium metal modification, preparation of a precursor by a co-precipitation method and hydrothermal crystallization are combined to obtain the high-purity and high-dispersion nano-zirconia powder, impurity ions in the precursor are removed by an ultra-filtration composite membrane technique, crystal form control and particle dispersion functions of a mineralizer are more effectively achieved in hydrothermal reaction, the concentration of the nano-zirconia powder in the precursor is improved, and high-purity and high-yield nano-powder is prepared. The nano-zirconia powder with stable yttrium prepared by the method has a spherical particle shape, is narrow in particle size distribution, good in dispersibility, high in purity, free from aggregation and the like and can be widely applied to high-end biological ceramic materials, and the method solves the problem of brittleness of a current zirconia material in the transition process of crystal forms, so that zirconia ceramics are flexibly and widely applied.

Description

technical field [0001] The invention belongs to the technical field of ceramic powder preparation, and in particular relates to a preparation method of high-purity and high-dispersion nano-zirconia. Background technique [0002] Zirconia ceramics have excellent physical and chemical properties, such as anti-corrosion, anti-wear, impact resistance, heat insulation, ceramic insulation, high temperature resistance and electricity insulation, and are widely used in catalysis, oxygen sensitive sensors, and high-temperature solid-state fuel cells. , Refractory materials, chemically inert surface materials, appearance decoration materials and biological materials, etc., have become one of the hot spots of research and development today. [0003] Zirconium dioxide (ZrO2) has a special property - martensitic phase transformation. With the change of temperature, the structure of ZrO2 can change. The low temperature is monoclinic ZrO2 (m-ZrO2), and the high temperature is 1170 ° C. It ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02C04B35/626C04B35/48
CPCC01G25/02C01P2004/64C01P2006/80C04B35/48C04B35/62685C04B2235/3225
Inventor 施利毅王漪袁帅
Owner 上海上惠纳米科技有限公司
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