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Preparation method of high-density zirconia ceramic material

A technology of zirconia ceramics and zirconia, which is applied in the field of additive manufacturing, can solve the problems of low solid content of slurry, easy cracks, delamination, porosity, and reduction of sintered density of materials, etc., to achieve the effect of good ceramic uniformity

Active Publication Date: 2022-01-25
CHONGQING UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

DLP-3D printing zirconia ceramic slurry contains more resin materials. Since ceramic slurry requires low viscosity, low viscosity reduces cracks and improves the uniformity of microstructure, but ensuring low viscosity will lead to solidification of the prepared slurry. Low content, when the resin material decomposes at high temperature, it will release a large amount of gas, internal chemical water, and some components will volatilize, and the sintering after high temperature degreasing makes the material have a large shrinkage rate and cause great deformation. These factors make the material It is easy to produce cracks, delamination, pores and other defects. These defects will be enlarged during the sintering process, which will reduce the sintering density of the material and affect the performance of the prepared ceramic material.

Method used

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  • Preparation method of high-density zirconia ceramic material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A method of preparing high-density zirconia ceramic material, according to the following steps:

[0039] (1) Preparation of ceramic slurry

[0040] The zirconia powder 1 and the zirconia powder 1 and the particle diameter of 30 nm of the zirconium oxide powder 1 and the particle diameter of 70 nm were mixed according to the mass ratio of 5:95, and the zirconia powder was formed; Sa, PEI was added to anhydrous ethanol, The water bath is 60 ° C, and the zirconia powder is added while stirring, and then the spray dried to obtain a composite modified zirconia powder, the spray drying is under 12 MPa, the air intake temperature is 220 ° C, the air machine is 60 ° C, fan The rotational frequency is 40 Hz, the peristaltic pump is 60 ml / h; the mass ratio of Sa, PEI and anhydrous ethanol is 1: 0.4: 8.5, the zirconia powder and SA, the mass ratio of the ethanol solution of PEI is 1: 4.5;

[0041] Polyurethane acrylate (PUA) and diacrylate 1,6-hexanediol ester (HDDA) are mixed in a ...

Embodiment 2

[0050] A method of preparing high-density zirconia ceramic material, according to the following steps:

[0051] (1) Preparation of ceramic slurry

[0052] The zirconia powder 1 and the zirconia powder 1 and the particle diameter of 40 nm of a cerium have a zirconia powder 1 and a particle diameter of 90 nm were mixed according to the mass ratio of 15:85, and the zirconia powder was formed; Sa, PEI was added to anhydrous ethanol, The water bath is 60 ° C, and the zirconia powder is added while stirring, then spray dried to obtain composite modified zirconia powder, the spray drying is under 10 MPa, the air intake temperature is 230 ° C, the air machine is 80 ° C, fan The rotational frequency is 50 Hz, the peristaltic pump is 70 ml / h; Sa, PEI and anhydrous ethanol have a mass ratio of 1: 0.6: 10, zirconia powder and SA, PEI have a mass ratio of 1: 5;

[0053] Polyurethane acrylate (PUA) and diacrylate 1,6-hexanediol ester (HDDA) are mixed in a mass ratio of 7: 3, and a composite m...

Embodiment 3

[0062] A method of preparing high-density zirconia ceramic material, according to the following steps:

[0063] (1) Preparation of ceramic slurry

[0064] The zirconia powder 1 and the zirconium oxide powder 1 and the particle diameter of 35 nm and the particle diameter of 80 nm were mixed according to the mass ratio of 10:90, and the zirconia powder was formed; Sa, PEI was added to anhydrous ethanol, The water bath to 60 ° C, the zirconia powder is added while stirring, and then spray dried to composite modified zirconia powder, the spray drying is under 12 MPa, the air intake temperature is 225 ° C, the air machine is 70 ° C, fan The rotational frequency is 45 Hz, the peristaltic pump speed is 65 ml / h; the mass ratio of Sa, PEI and anhydrous ethanol is 1: 0.5: 9, the zirconia powder and SA, the mass ratio of the ethanol solution of PEI is 1: 5;

[0065] Polyurethane acrylate (PUA) and diacrylate 1,6-hexanediol ester (HDDA) are mixed in a mass ratio of 7: 3, and a composite mod...

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Abstract

A preparation method of the high-compactness zirconia ceramic material comprises the following steps: carrying out high-temperature and high-pressure spray drying composite modification on zirconia powder by adopting stearic acid (SA) and polyethyleneimine (PEI) to prepare zirconia ceramic slurry; curing under the irradiation of ultraviolet light to obtain a ceramic green body, and then performing five-section degreasing treatment at 180-1000 DEG C under atmospheric pressure; performing high temperature treatment by increasing the temperature to 1000 DEG C under the vacuum degree of 10<-3> Pa for high-temperature treatment, and finally, nitrogen is adopted to adjust the pressure to 1000-3000 Pa, and segmented high-temperature sintering is carried out. The solid content of the prepared zirconium oxide slurry is 90-94%, the viscosity is 1.05-1.39 Pa.s under 30 / s; the prepared zirconium oxide ceramic material has no crack and layering defects, the shrinkage rate after degreasing and sintering is 14-18%, the sintering density reaches 98.9-99.7%, the ceramic uniformity is good, and no crack, layering or other defects exists.

Description

Technical field [0001] The present invention relates to the field of additive manufacturing techniques, and more particularly to a method of preparing highly dense zirconia ceramic materials. Background technique [0002] Zirconia ceramics are widely used in chemical, mechanical, electronics, aerospace and biomedical fields such as physical properties such as mechanical strength, high temperature resistance, corrosion resistance, chemical stability. The conventional ceramic preparation process is usually mixed with ceramic powder and binder or other additives, prepared by injection molding, stamping, casting, gel injection molding, etc., and then dry, high temperature degreasing and Process such as sintering causes dense. However, these conventional preparation methods require a pre-manufacturing mold, resulting in the entire preparation cycle, and unable to prepare a highly complex structure, especially a medium-porous ceramic material parts. With the advancement and development...

Claims

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Application Information

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IPC IPC(8): C04B35/48C04B35/622B33Y70/10
CPCC04B35/48C04B35/622B33Y70/10C04B2235/5454C04B2235/6026C04B2235/656C04B2235/6562C04B2235/6567C04B2235/658C04B2235/77C04B2235/9615Y02P10/25
Inventor 刘兵黄伟九骆嘉琪
Owner CHONGQING UNIV OF ARTS & SCI
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