Preparation method of nano zirconium oxide powder

A nano-zirconia, powder technology, applied in nanotechnology and other directions, can solve the problems of inability to mix the binder uniformly, difficult flexible molding, and decreased sintering performance.

Active Publication Date: 2020-10-30
上海大学浙江嘉兴新兴产业研究院
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Problems solved by technology

These two requirements are often contradictory, that is, if the sintering performance is good, the zirconia powder particles are required to be fine, but they are prone to agglomeration, resulting in the inability to mix uniformly with the binder, which makes the material formability poor; on the contrary, increasing the oxidation Although the particle size of zirconium will make the material more formable, it will inevitably lead to a decrease in sintering performance
For example, patent CN99124041.3 relates to a low-temperature sintered zirconia powder, which has good sintering activity, but its specific surface area reaches 110m2 / g, making it difficult to perform flexible molding; another example is patent CN02115615 .8 It involves a zirconia powder with controllable specific surface area. Although it can achieve a low specific surface area, the sintering activity of the powder is poor

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  • Preparation method of nano zirconium oxide powder

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preparation example Construction

[0025] The invention provides a preparation method of nano zirconia powder, comprising the following steps:

[0026] (1) mixing inorganic zirconium salt, inorganic yttrium salt with water to obtain a mixed solution;

[0027] (2) adding the mixed solution obtained in the step (1) dropwise into an aqueous ammonia solution to carry out a precipitation reaction to obtain a precipitation solution;

[0028] (3) mixing the precipitation solution obtained in the step (2) with an organic solvent to obtain a precursor precipitation solution;

[0029] (4) filtering part of the precursor precipitation solution obtained in the step (3) to obtain a precursor;

[0030] (5) The precursor obtained in the step (4) is mixed with the remaining precursor precipitation solution obtained in the step (3) and then filtered to obtain a powder;

[0031] (6) Calcining the powder obtained in the step (5) to obtain nano zirconia powder.

[0032] The invention mixes inorganic zirconium salt, inorganic yt...

Embodiment 1

[0047] (1) Weigh 161.00g ZrOCl of medicine 2 ·8H 2 O and 4.55 g YCl 3 ·6H 2 O is placed in the container (inorganic zirconium salt ZrOCl 2 ·8H 2 O and inorganic yttrium salt YCl 3 ·6H 2 The ratio of the amount of O to the substance is 100:3), add deionized water to 1 liter, and stir evenly at a speed of 200r / min until a clear solution is obtained to obtain a mixed solution, wherein the concentration of zirconium ions in the mixed solution is 0.5mol / L ;

[0048] (2) Prepare an ammonia solution first, wherein the pH value is 12, and the temperature is 30°C; then the mixed solution is added dropwise to the ammonia solution at a rate of 5 mL / min, and mechanically stirred at a speed of 350 r / min to obtain a precipitate liquid; where zirconium ions in the mixed solution and NH in the ammonia solution 3 ·H 2 The ratio of the amount of O to the substance is 1:2.5;

[0049] (3) Keep the temperature of the precipitation solution at 30°C, add ethanol to it, the volume ratio of ...

Embodiment 2

[0055] (1) Weigh 85.80g Zr(NO 3 ) 4 ·5H 2 O and 3.06g Y (NO 3 ) 3 ·6H 2 O is placed in the container (inorganic zirconium salt Zr(NO 3 ) 4 ·5H 2 O and inorganic yttrium salt Y(NO 3 ) 3 ·6H 2 The ratio of the amount of O to the substance is 100:4), add deionized water, and stir evenly at a speed of 200r / min until a clear solution is obtained to obtain a mixed solution, wherein the concentration of zirconium ions in the mixed solution is 0.2mol / L;

[0056] (2) Prepare an ammonia solution first, wherein the pH value is 12, and the temperature is 50°C; then add the mixed solution dropwise to the ammonia solution at a rate of 5mL / min, and perform mechanical stirring at a speed of 400r / min to obtain a precipitate liquid; where zirconium ions in the mixed solution and NH in the ammonia solution 3 ·H 2 The ratio of the amount of O to the substance is 1:3;

[0057] (3) Keep the temperature of the precipitation solution at 50°C, add isopropanol to it, the volume ratio of th...

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Abstract

The invention provides a preparation method of nano zirconium oxide powder, comprising the following steps of: mixing inorganic zirconium salt, inorganic yttrium salt and water to obtain a mixed solution; dropwise adding the mixed solution into an ammonia water solution, and carrying out a precipitation reaction to obtain a precipitation solution; mixing the precipitation solution with an organicsolvent to obtain a precursor precipitation solution; filtering part of the precursor precipitation solution to obtain a precursor; mixing the precursor with the residual precursor precipitation solution, and filtering to obtain powder; and calcining the powder to obtain the nano zirconium oxide powder. By adding the organic solvent, the dielectric constant of the medium is effectively reduced, and the electrostatic repulsion between ions is reduced, so that the monodisperse spherical zirconium oxide powder is obtained; before calcination, the powder and the precursor precipitation solution are mixed, so that the particle surface defects and the surface activity are further reduced, the nano zirconium oxide powder with a low specific surface area is prepared, and the low specific surface area and high sintering activity of the zirconium oxide powder are realized.

Description

technical field [0001] The invention belongs to the technical field of ceramic powder preparation, and in particular relates to a preparation method of nano zirconia powder. Background technique [0002] Due to its excellent physical and chemical properties, zirconia ceramics are widely used in many fields such as catalysis, oxygen sensitive sensors, high-temperature solid-state fuel cells, chemically inert surface materials for refractories, decorative materials, and biological materials, and have become one of the hot spots of research and development today. . [0003] High-performance zirconia powder must meet two conditions: first, it has good sintering performance, and the sintering density must reach more than 99%, so the particle size of zirconia powder is required to be as small as possible; second, in order to be beneficial to molding, The zirconia powder must be able to mix well with various binders, and the binder needs to be evenly bonded to the zirconia powder,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/48C04B35/626B82Y40/00
CPCC04B35/48C04B35/62605B82Y40/00C04B2235/444C04B2235/443C04B2235/95C04B2235/96Y02E60/50
Inventor 施利毅袁帅王漪
Owner 上海大学浙江嘉兴新兴产业研究院
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