阅读说明：本技术 一种光固化氧化铝陶瓷双溶剂浆料的制备方法 (Preparation method of photocuring alumina ceramic double-solvent slurry ) 是由 唐明亮 叶玉秋 郑海 胡增涵 王海华 李峰 于 2020-11-26 设计创作，主要内容包括：本发明公开了一种光固化氧化铝(Al_2O_3)陶瓷双溶剂浆料的制备方法：①称重：按照比例,分别称取己二醇丙烯酸酯、聚氨酯丙稀酸酯和三份的球形Al_2O_3粉、分散剂聚丙烯酸钠、光引发剂和增粘剂；②单溶剂浆料配制：配制己二醇丙烯酸酯与Al_2O_3、聚氨酯丙稀酸酯与Al_2O_3的单溶剂浆料,加入分散剂,调节pH值至碱性,行星球磨搅拌、真空除泡,得到单溶剂浆料；③双溶剂浆料配制：将2种单溶剂浆料混合搅拌,分多次加入余下的Al_2O_3、分散剂、光引发剂和增粘剂,调节pH值至碱性,行星球磨搅拌、真空除泡,得到双溶剂浆料。本发明制备的Al_2O_3陶瓷浆料分散均匀性高,具有优良的流动性和稳定性,保证了光固化打印陶瓷坯体的快速成型,同时在避光条件下可以长期保存。(The invention discloses photocuring alumina (Al) 2 O 3 ) The preparation method of the ceramic double-solvent slurry comprises the following steps: weighing: according to the proportion, respectively weighing hexanediol acrylate, polyurethane acrylate and three parts of spherical Al 2 O 3 Powder, dispersant sodium polyacrylate, photoinitiator and tackifier; preparing single-solvent slurry: preparing hexanediol acrylate and Al 2 O 3 Urethane acrylate and Al 2 O 3 Adding a dispersant into the single-solvent slurry, adjusting the pH value to be alkaline, carrying out planetary ball milling and stirring, carrying out vacuum defoaming,obtaining single solvent slurry; preparing a double-solvent slurry: mixing and stirring 2 kinds of single-solvent slurry, and adding the rest Al for multiple times 2 O 3 The pH value is adjusted to be alkaline, and the double-solvent slurry is obtained through planetary ball milling stirring and vacuum defoaming. Al prepared by the invention 2 O 3 The ceramic slurry has high dispersion uniformity and excellent fluidity and stability, ensures the rapid molding of the photocuring printing ceramic blank, and can be stored for a long time under the condition of keeping out of the sun.)

1. A preparation method of photocuring alumina ceramic double-solvent slurry comprises the following specific steps:

(1) weighing: according to the proportion, respectively weighing hexanediol acrylate, polyurethane acrylate and spherical Al₂O₃Powder, dispersant sodium polyacrylate, photoinitiator and tackifier, and mixing spherical Al₂O₃The powder is A, B, C parts, wherein A part is spherical Al₂O₃B, C portions of spherical Al accounting for 50 percent of the total amount of the powder₂O₃50 percent of the total powder, the proportion of the B part and the C part respectively corresponds to hexanediol acrylate and polyurethane acrylate, the proportion of the sodium polyacrylate is a part, B part and C part, and the proportion corresponds to A, B, C three parts of spherical Al₂O₃Pulverizing;

(2) preparing single-solvent slurry: preparing hexanediol acrylate and B part of spherical Al₂O₃Powder, polyurethane acrylate and C part spherical Al₂O₃Adding corresponding dispersant into the single-solvent slurry of the powder, adjusting the pH value to be alkaline, stirring by planetary ball milling and removing bubbles in vacuum to obtain uniform single-solvent Al₂O₃A ceramic slurry;

(3) preparing a double-solvent slurry: 2 kinds of single-solvent Al to be prepared₂O₃After the ceramic slurry is mixed and stirred for a certain time, A parts of spherical Al are added for multiple times₂O₃Mixing the powder with a dispersant, a photoinitiator and a tackifier, adjusting the pH value to be alkaline, stirring by planetary ball milling, and removing bubbles in vacuum to obtain uniform photocuring Al₂O₃Ceramic two-solvent slurry.

2. The method for preparing the photo-cured alumina ceramic two-solvent slurry according to claim 1, wherein the method comprises the following steps: the double solvents are hexanediol acrylate and polyurethane acrylate, and the mass ratio of the components is 4:1-8: 1.

3. According to the rightThe preparation method of the photocuring alumina ceramic double-solvent slurry according to claim 1, which is characterized by comprising the following steps: al (Al)₂O₃The purity of the powder is more than 99.99 percent, the powder is spherical, and the particle size D50 is between 400 and 500 nm.

4. The method for preparing the photo-cured alumina ceramic two-solvent slurry according to claim 1, wherein the method comprises the following steps: the dispersant is sodium polyacrylate, and the addition amount is 0.4-1.0 wt%.

5. The method for preparing the photo-cured alumina ceramic two-solvent slurry according to claim 1, wherein the method comprises the following steps: the photoinitiator is 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, and the addition amount is 0.6-1.5 wt%.

6. The method for preparing the photo-cured alumina ceramic two-solvent slurry according to claim 1, wherein the method comprises the following steps: the tackifier is organic bentonite, and the addition amount is 1.0-2.0 wt%.

7. The method for preparing the photo-cured alumina ceramic two-solvent slurry according to claim 1, wherein the method comprises the following steps: al in the slurry₂O₃The solid phase content of the powder is 38-45 vol%.

Technical Field

The invention relates to a preparation method of ceramic slurry, in particular to a preparation method of photocuring alumina ceramic slurry.

Background

When the ceramic material is printed by adopting the stereolithography molding (SLA) technology, the preparation of the photocuring ceramic slurry is the most critical step in order to obtain a ceramic blank with certain strength and dimensional accuracy. For ceramic photocuring, the slurry properties should meet both high solids and low viscosity requirements.

(1) If the solid phase content is too low, the printed ceramic blank has low strength and poor mechanical property, and can cause a sample to have larger shrinkage rate, crack or deformation in the subsequent degreasing and sintering processes, so that the mechanical property and the dimensional precision of the ceramic part can be greatly influenced. Generally, the solid content of the currently used photocurable ceramic slurry is about 35-55 vol%.

(2) The low viscosity is generally less than 3000 mPas; if the viscosity of the paste is too high, poor fluidity may result, and a thin layer having a uniform thickness may not be formed during printing, resulting in molding failure.

However, since fluidity and dispersibility are reduced as the amount of the solid phase increases, it is important to prepare a photocurable ceramic slurry having optimum properties while satisfying all the requirements for the properties.

Disclosure of Invention

The invention aims to provide a preparation method of photocuring alumina ceramic slurry, and solve the problem of preparation of the photocuring alumina ceramic slurry.

The technical problem to be solved by the invention is realized by the following technical scheme, and the invention relates to a preparation method of photocuring alumina ceramic double-solvent slurry, which comprises the following steps:

（1）weighing: according to the proportion, respectively weighing hexanediol acrylate, polyurethane acrylate and spherical Al₂O₃Powder, dispersant sodium polyacrylate, photoinitiator and tackifier, and mixing spherical Al₂O₃The powder is A, B, C parts, wherein A part is spherical Al₂O₃B, C portions of spherical Al accounting for 50 percent of the total amount of the powder₂O₃50 percent of the total powder, the proportion of the B part and the C part respectively corresponds to hexanediol acrylate and polyurethane acrylate, the proportion of the sodium polyacrylate is a part, B part and C part, and the proportion corresponds to A, B, C three parts of spherical Al₂O₃Pulverizing;

(2) preparing single-solvent slurry: preparing hexanediol acrylate and B part of spherical Al₂O₃Powder, polyurethane acrylate and C part spherical Al₂O₃Adding corresponding dispersant into the single-solvent slurry of the powder, adjusting the pH value to be alkaline, stirring by planetary ball milling and removing bubbles in vacuum to obtain uniform single-solvent Al₂O₃A ceramic slurry;

(3) preparing a double-solvent slurry: 2 kinds of single-solvent Al to be prepared₂O₃After the ceramic slurry is mixed and stirred for a certain time, A parts of spherical Al are added for multiple times₂O₃Mixing the powder with a dispersant, a photoinitiator and a tackifier, adjusting the pH value to be alkaline, stirring by planetary ball milling, and removing bubbles in vacuum to obtain uniform photocuring Al₂O₃Ceramic two-solvent slurry.

The invention has the beneficial effects that: al (Al)₂O₃The Zeta potential absolute value of the ceramic slurry reaches the maximum in an alkaline region, and the fluidity and the stability of the slurry are the best. Spherical Al₂O₃If the particle size of the powder is too small, the powder is easy to agglomerate, the viscosity and the sedimentation height are increased, the fluidity and the stability of the slurry are influenced, and when the spherical Al is used₂O₃The powder D50 was 400-500 nm, the overall performance was better. The invention selects hexanediol acrylate and polyurethane acrylate as solvents, fully utilizes the activity of active monomers and the rheological property of oligomers, and improves Al₂O₃The curing characteristics of the slurry. The organic bentonite is used as tackifier and has sheet structure with oxygen and hydrogen and oxygenThe groups can also form hydrogen bonds to generate a three-dimensional network structure, so that the thixotropy of the slurry can be enhanced, and the rapid effect of photocuring molding is ensured. The invention uses the method of mixing monomers first and then mixing the monomers into two bodies, thereby improving the spherical Al₂O₃The dispersion uniformity and stability of the powder in the slurry ensure Al₂O₃The isotropy of the ceramic slurry reduces the bubbles in the slurry.

Detailed Description

Specific embodiments of the present invention will now be further described to facilitate further understanding of the present invention by those skilled in the art, and are not to be construed as limiting the claims thereto.

(1) Weighing: respectively weighing hexanediol acrylate, polyurethane acrylate and spherical Al according to the ratio of 5:1₂O₃45 vol% of powder, 500 nm of D50, 0.9 wt% of dispersant sodium polyacrylate, 1.0 wt% of photoinitiator 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, 1.2 wt% of tackifier organobentonite, and mixing spherical Al₂O₃The powder is A, B, C parts, wherein the A part is 22.5 vol%, the B part is 18.75 vol%, the C part is 3.75 vol%, and the sodium polyacrylate is a part, B part and C part, wherein the a part is 0.45 wt%, the B part is 0.375 wt%, and the C part is 0.075 wt%;

(2) preparing single-solvent slurry: preparing hexanediol acrylate and B part of spherical Al₂O₃Powder, polyurethane acrylate and C part spherical Al₂O₃Adding corresponding parts b and c of sodium polyacrylate into the powder single-solvent slurry, adjusting the pH value to 9, stirring for 2 hours by planetary ball milling, standing for 24 hours under the pressure of 0.1 kPa to remove bubbles in the slurry, and obtaining uniform single-solvent Al₂O₃A ceramic slurry;

(3) preparing a double-solvent slurry: 2 kinds of single-solvent Al to be prepared₂O₃After the ceramic slurry is mixed and stirred for 1 hour, A part of 22.5 vol% spherical Al is added in multiple times₂O₃Mixing the powder with a part of sodium polyacrylate, 1.0 wt% of photoinitiator 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 1.2 wt% of tackifier organobentonite, adjusting the pH value to 9, stirring by planetary ball mill for 2 h, and standing under the pressure of 0.1 kPa for 24 h to remove the gas of the slurrySoaking to obtain uniform photocured Al₂O₃Ceramic two-solvent slurry.