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Slurry for photocuring 3D printing and preparation method thereof, and silicon nitride ceramic

A silicon nitride ceramic, 3D printing technology, applied in the direction of additive processing, can solve the problems of harsh preparation conditions, low curing thickness, affecting molding accuracy, etc., to improve electrodynamic and colloidal properties, reduce scattering phenomenon, mechanical Excellent performance

Inactive Publication Date: 2019-10-22
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Application Information

AI Technical Summary

Problems solved by technology

[0004] When adopting photocuring molding technology to prepare silicon nitride ceramics at present, its used raw material is silicon nitride ceramic material usually, but present this type of silicon nitride ceramic slurry and its preparation process (CN, 106699191A) have the following problems: (1 ) The affinity between silicon nitride powder and resin is poor, resulting in low solid content of ceramic slurry (about 30vol%); (2) The difference in refractive index between silicon nitride powder and resin is large, which affects the molding accuracy (3) Silicon nitride powder has light absorption, and the obtained cured thickness is low, and the molding process requires high exposure power and exposure time, which affects the life of the equipment and printing efficiency; these three main problems limit the light curing molding. Development of Technology and Applications of Silicon Nitride Ceramics
Although there are also patents that try to solve the above problems by thermal oxidation treatment of silicon nitride powder, thermal oxidation requires higher temperature (not lower than 1000°C), consumes more energy, has harsh preparation conditions and needs to add a large amount of sintering aids, especially It is unable to solve the affinity between powder and resin

Method used

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  • Slurry for photocuring 3D printing and preparation method thereof, and silicon nitride ceramic

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preparation example Construction

[0027] In order to solve the above problems, according to an embodiment of the present invention, a method for preparing a photocurable 3D printing slurry is provided, wherein the method includes the following steps:

[0028] Step 1, silicon nitride powder pretreatment, including:

[0029] Disperse the silicon nitride powder in an appropriate amount of alkaline solution to obtain an alkaline suspension;

[0030] Add appropriate amount of Y to the alkaline suspension 3+ and Mg 2+ The mixed salt solution, after the reaction is completed, the silicon nitride powder containing the coating is obtained;

[0031] Post-treating the silicon nitride powder containing the coating, and then calcining at a temperature of 600° C. or less to obtain a pretreated silicon nitride powder;

[0032] Step 2, slurry preparation, including:

[0033] The pretreated silicon nitride powder is mixed with a resin monomer, a dispersant and a photoinitiator to obtain a silicon nitride ceramic slurry.

...

Embodiment 1

[0056] Step 1: Pretreatment of silicon nitride powder. First, ultrasonically disperse the silicon nitride powder in an aqueous solution of TEAOH to obtain a suspension (pH=9.8). Under magnetic stirring, add dropwise to the suspension at a molar ratio of 2.7: 1.1 Y(NO 3 ) 3 with Mg(NO 3 ) 2 mixed salt solution and ammonia water (20-25wt%), after the reaction is completed (the pH of the solution remains unchanged during this process), the coating is washed twice with deionized water and alcohol respectively, dried at 80°C for 24h, and passed A 60-mesh sieve can be calcined for 1 hour at 600° C. under a nitrogen atmosphere, wherein the coating is 6 wt % of the mass of the silicon nitride powder.

[0057] Step 2: Slurry preparation, the silicon nitride powder pretreated in step 1, 1,6-hexanediol diacrylate, sodium polyacrylate and (2,4,6-trimethylbenzoyl)diphenyl The mass ratio of phosphine oxide is 470:100:2.4:0.8, mixed with ball mill and vacuum pumped for 0.5h to obtain sil...

Embodiment 2

[0059] Step 1: Pretreatment of silicon nitride powder. First, ultrasonically disperse the silicon nitride powder in an aqueous solution of TEAOH to obtain a suspension (pH=9.8). Under magnetic stirring, add dropwise to the suspension at a molar ratio of 2.7: 1.1 Y(NO 3 ) 3 with Mg(NO 3 ) 2 mixed salt solution and ammonia water (20-25wt%), after the reaction is completed (the pH of the solution remains unchanged during this process), the coating is washed three times with deionized water and alcohol respectively, dried at 80°C for 24h, and then 60-mesh sieve, calcined at 600° C. for 1.5 h in a nitrogen atmosphere, wherein the coating is 8 wt % of the mass of the silicon nitride powder.

[0060] Step 2: slurry preparation, the silicon nitride powder pretreated in step 1, 1,6-hexanediol diacrylate and propoxylated neopentyl glycol diacrylate resin with a mass ratio of 2:1 Body, sodium polyacrylate and (2,4,6-trimethylbenzoyl) diphenylphosphine oxide in a mass ratio of 460:100...

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Abstract

The invention provides a slurry for photocuring 3D printing and a preparation method thereof, and a silicon nitride ceramic to overcome problems in conventional silicon nitride ceramic slurry for photocuring 3D printing and preparation processes thereof. The preparation method comprises the following steps: pretreatment of silicon nitride powder: dispersing the silicon nitride powder in an appropriate amount of an alkaline solution to obtain an alkaline suspension, adding an appropriate amount of a mixed salt solution containing Y<3+> and Mg<2+> into the alkaline suspension, carrying out a reaction to obtain coated silicon nitride powder, subjecting the coated silicon nitride powder to post-treatment, and then carrying out calcination at a temperature of 500-600 DEG C to obtain pretreatedsilicon nitride powder; and preparation of the slurry: mixing the pretreated silicon nitride powder with a resin monomer, a dispersant and a photoinitiator to obtain the silicon nitride ceramic slurry.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional ceramics, and in particular relates to a slurry for photocuring 3D printing, a preparation method and silicon nitride ceramics. Background technique [0002] Silicon nitride ceramics have excellent high temperature strength, corrosion resistance and thermal shock resistance, and have low density and low expansion coefficient. At present, they have been widely used in aviation, aerospace, engine, metallurgy, chemical industry, etc. In the working environment of corrosive medium. The preparation methods mainly include: extrusion molding, dry pressing molding, injection molding, isostatic pressing molding, tape casting molding, grouting molding, gel injection molding and the like. When preparing components by these processes, it is necessary to prepare a mold with a corresponding shape according to the shape of the component. If the structure of the component changes slightly, it i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/626C04B35/628C04B35/584B33Y70/00
CPCB33Y70/00C04B35/584C04B35/62605C04B35/6281C04B35/62815C04B2235/5427C04B2235/6026C04B2235/96
Inventor 董衡韩耀肖振兴李淑琴张剑吕毅张天翔张昊
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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