CN111233443A - High-solid-content 3D printing ceramic core slurry and preparation method thereof - Google Patents

High-solid-content 3D printing ceramic core slurry and preparation method thereof Download PDF

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CN111233443A
CN111233443A CN202010110023.3A CN202010110023A CN111233443A CN 111233443 A CN111233443 A CN 111233443A CN 202010110023 A CN202010110023 A CN 202010110023A CN 111233443 A CN111233443 A CN 111233443A
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ceramic core
slurry
mixture
printing
inorganic powder
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刘永胜
李鹤
刘岩松
曾庆丰
董宁
王晶
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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Abstract

The invention relates to high solid content 3D printing ceramic core slurry and a preparation method thereof. Preparation of slurry: adding a coupling agent into acrylic photosensitive resin, uniformly stirring, adding the mixture of inorganic powder, placing the mixture in an ultrasonic oscillator for ultrasonic treatment, ball-milling the mixture on a ball mill, placing the ball mill in a vacuum drying oven, and carrying out vacuum treatment at normal temperature to obtain the 3D printing ceramic core slurry with high solid content. The invention improves the solid phase content of the ceramic slurry by introducing the coupling agent and the graded inorganic powder, has simple and efficient preparation method, accelerates the production period of the ceramic core and reduces the manufacturing cost of the ceramic core. Can be applied to the production field of alumina-based ceramic cores.

Description

High-solid-content 3D printing ceramic core slurry and preparation method thereof
Technical Field
The invention belongs to the technical field of additive manufacturing, and relates to high-solid-phase-content 3D printing ceramic core slurry and a preparation method thereof.
Background
The alumina-based ceramic core is an important structural part for forming the inner cavity of the hollow turbine blade for the novel engine due to the reasons of excellent high-temperature resistance, low thermal expansion rate, no crystal form transformation, good metallurgical chemical stability, excellent creep resistance, stable structure, good high temperature resistance and the like.
The traditional method for preparing the alumina-based ceramic core by using an investment casting technology has the problems of complex process flow, long production period, high manufacturing cost and the like (Chinese patent, patent number CN 109574636A). The photocuring 3D printing technology has the characteristics of short flow, high precision, low cost and the like, and is suitable for forming ceramic cores with complex structures.
The university of qinghua (chinese patent, patent No. CN109251022A) proposed the use of selective laser sintering 3D printing technology to prepare porous ceramic cores, shortening the production cycle of ceramic cores and reducing production costs. Shandong industrial ceramic research design institute Co., Ltd (Chinese patent, patent No. CN108083777A) provides a photocuring 3D printing ceramic slurry and a method for preparing a ceramic core, and the problem of poor fluidity of the ceramic slurry is solved. The university of Xian traffic (Chinese patent, patent No. CN101306950) proposes a manufacturing method for manufacturing a hollow blade ceramic casting mold by a light curing process, and shortens the preparation period of a ceramic core. However, the problems of low solid content and the like still exist in the photocuring 3D printing alumina-based ceramic core slurry, and the difficulty in printing parts with complex structures is still high.
How to facilitate the photocuring 3D printing technology to prepare the alumina-based ceramic core quickly, simply and cheaply still has a plurality of technical problems.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides high-solid-content 3D printing ceramic core slurry and a preparation method thereof, relates to high-solid-content photocuring 3D printing ceramic core slurry and a preparation method thereof, and can realize the molding of photocuring 3D printing alumina ceramic core biscuit. The production flow of the ceramic core is accelerated. Is suitable for the forming process of the alumina-based ceramic core.
Technical scheme
The high solid content 3D printing ceramic core slurry is characterized by comprising 1-30% of coupling agent, 50-90% of mixture inorganic powder and 9-20% of acrylic photosensitive resin in balance by mass; the mixture inorganic powder comprises two or more of alumina, silica, zirconia, titania, calcium oxide, magnesia and yttria; wherein the mass percentage content of the alumina powder is not less than 50 percent and not more than 90 percent.
The coupling agent is one or more of 3-aminopropyltriethoxysilane, N- (β -aminoethyl-gamma-aminopropyl) methyldimethoxysilane and 3- (methacryloyloxy) propyl trimethoxysilane.
A preparation method of high solid content 3D printing ceramic core slurry is characterized by comprising the following steps:
step 1: adding a coupling agent into acrylic photosensitive resin to obtain a solution; the mass percentage of the coupling agent is 1-30%;
step 2: adding mixture inorganic powder consisting of two or more of alumina, silica, zirconia, titania, calcium oxide, magnesia and yttria into the solution; the mass percentage of the mixture inorganic powder is 50-90%, wherein the mass percentage of the alumina powder is not less than 50% and not more than 90%;
and step 3: then placing the mixture in an ultrasonic oscillator for ultrasonic treatment for 0.2 to 12 hours; then ball milling is carried out on the ball mill for 0.2 to 12 hours;
and 4, step 4: and then placing the ceramic core slurry in a vacuum drying oven, and carrying out vacuum treatment for 0.2-12 hours at normal temperature to obtain the high-solid-phase-content 3D printing ceramic core slurry.
The mixture inorganic powder is formed by mixing particles with different particle diameters, wherein the mass percentage of the powder with the particle diameter of 5-20 mu m is not less than 40%, and the mass percentage of the powder with the particle diameter of 10-200 nm is not less than 10%.
Advantageous effects
The invention provides high solid content 3D printing ceramic core slurry and a preparation method thereof. Preparation of slurry: adding a coupling agent into acrylic photosensitive resin, uniformly stirring, adding the mixture of inorganic powder, placing the mixture in an ultrasonic oscillator for ultrasonic treatment, ball-milling the mixture on a ball mill, placing the ball mill in a vacuum drying oven, and carrying out vacuum treatment at normal temperature to obtain the 3D printing ceramic core slurry with high solid content. The invention improves the solid phase content of the ceramic slurry by introducing the coupling agent and the graded inorganic powder, has simple and efficient preparation method, accelerates the production period of the ceramic core and reduces the manufacturing cost of the ceramic core. Can be applied to the production field of alumina-based ceramic cores.
The invention has the following beneficial effects:
(1) according to the invention, the coupling agent with the mass percentage content of 1-30%, and the inorganic powder with the size of micrometer (5-20 μm) and nanometer (10-200 nm) are graded, so that the slurry for the 3D printing ceramic core with high solid content is prepared, the slurry preparation method is simple and efficient, the production period of the ceramic core is accelerated, and the manufacturing cost of the ceramic core is reduced.
(2) According to the invention, by increasing the content of inorganic powder in the 3D printing ceramic core slurry, the content of volatile resin in a formed biscuit is reduced, the problem that the ceramic core is easy to deform in the degreasing process of the photocuring 3D printing ceramic core is solved, the phenomena of deformation and cracking of the ceramic core are reduced, and the dimensional accuracy of the ceramic core is improved.
(3) According to the invention, the photocuring 3D printing alumina ceramic core biscuit with high solid content is prepared, so that the forming of the photocuring 3D printing alumina ceramic core biscuit can be realized. The invention provides a preparation method of high solid content 3D printing ceramic core slurry, which is suitable for a forming process of an alumina-based ceramic core.
(4) Changes in the photocurable 3D printing ceramic core slurry formulation were not attainable with limited experimentation because: the experimental material photosensitive resin is expensive, the experiment cost of the photocuring 3D printing ceramic core is high, the core model is complex, and the experiment difficulty is high; since limited trials cannot be performed, the composition and content of the photocurable 3D printing ceramic core paste is limited. Due to the diversity of the formulation of the photocurable 3D printing ceramic core slurry, the process varied by the present invention is not simple to determine.
Drawings
FIG. 1 is a flow chart of a method for photocuring 3D printing of alumina-based ceramic cores
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the method for preparing the high solid content 3D printing ceramic core slurry is described in detail below.
Adding a coupling agent into the acrylic photosensitive resin and uniformly stirring, wherein the coupling agent accounts for 1-30% by mass, and obtaining a solution A.
And adding mixture inorganic powder consisting of two or more of alumina, silicon oxide, zirconia, titanium oxide, calcium oxide, magnesium oxide and yttrium oxide into the solution A and uniformly stirring, wherein the mass percentage of the mixture inorganic powder is 50-90%, and the mixture inorganic powder is formed by mixing particles with different particle diameters to obtain the solution B.
And placing the B in an ultrasonic oscillator for ultrasonic treatment for 0.2-12 hours to obtain C.
And ball-milling the obtained C on a ball mill for 0.2-12 hours to obtain D.
And (5) placing the D in a vacuum drying oven, and carrying out vacuum treatment for 0.2-12 hours at normal temperature to obtain the high-solid-phase-content 3D printing ceramic core slurry.
The preparation method of the high solid content 3D printing ceramic core slurry according to claim 1, wherein the mixture inorganic powder is formed by mixing particles with different particle sizes, wherein the mass percentage of the powder with the particle size of 5-20 μm is not less than 40%, and the mass percentage of the powder with the particle size of 10-200 nm is not less than 10%.
The preparation method of the high-solid-content 3D printing ceramic core slurry is characterized in that the mass percentage of alumina powder in the ceramic slurry is not lower than 50% and not higher than 90%.
The method for preparing the high solid content 3D printing ceramic core slurry as claimed in claim 1, wherein the coupling agent is one or more of 3-aminopropyltriethoxysilane, N- (β -aminoethyl-gamma-aminopropyl) methyldimethoxysilane and 3- (methacryloyloxy) propyltrimethoxysilane.
Example 1
(1) Adding 8g N- (β -aminoethyl-gamma-aminopropyl) methyldimethoxysilane into 32g of acrylic photosensitive resin, and uniformly stirring to obtain a solution A, (2) adding a mixture inorganic powder consisting of 120g of alumina, 20g of silicon oxide, 10g of zirconium oxide and 10g of magnesium oxide into the solution A, and uniformly stirring to obtain a solution B, (3) placing the solution B into an ultrasonic oscillator, performing ultrasonic treatment for 3 hours to obtain a solution C, (4) ball-milling the obtained solution C on a ball mill for 3 hours to obtain a solution D, and (5) placing the solution D in a vacuum drying oven, and performing vacuum treatment for 5 hours at normal temperature to obtain the 3D printing ceramic core slurry with high solid content.
Example 2
(1) Adding 1.5g of 3- (methacryloyloxy) propyl trimethoxy silane into 28.5g of acrylic photosensitive resin, and uniformly stirring to obtain a solution A; (2) adding a mixture of 150g of alumina, 10g of silicon oxide and 10g of zirconium oxide into the solution A, and uniformly stirring to obtain B, wherein the mass percentage of powder with the particle size of 5-20 mu m in the powder is 60%, and the mass percentage of powder with the particle size of 10-200 nm in the powder is 40%; (3) placing the B in an ultrasonic oscillator for ultrasonic treatment for 6 hours to obtain C; (4) ball-milling the obtained C on a ball mill for 6 hours to obtain D; (5) and (5) placing the D in a vacuum drying oven, and carrying out vacuum treatment for 6 hours at normal temperature to obtain the 3D printing ceramic core slurry with high solid content.
Example 3
(1) Adding 3.4g of 3-aminopropyltriethoxysilane into 30.6g of acrylic photosensitive resin, and uniformly stirring to obtain a solution A; (2) adding a mixture of 149.4g of alumina and 16.6g of silicon oxide into the solution A, and uniformly stirring to obtain B, wherein the mass percentage of powder with the particle size of 5-20 mu m in the powder is 55%, and the mass percentage of powder with the particle size of 10-200 nm in the powder is 45%; (3) placing the B in an ultrasonic oscillator for ultrasonic treatment for 2 hours to obtain C; (4) ball-milling the obtained C on a ball mill for 2 hours to obtain D; (5) and (5) placing the D in a vacuum drying oven, and carrying out vacuum treatment for 2 hours at normal temperature to obtain the 3D printing ceramic core slurry with high solid content.

Claims (4)

1. The high solid content 3D printing ceramic core slurry is characterized by comprising 1-30% of coupling agent, 50-90% of mixture inorganic powder and 9-20% of acrylic photosensitive resin in balance by mass; the mixture inorganic powder comprises two or more of alumina, silica, zirconia, titania, calcium oxide, magnesia and yttria.
2. The high solid content 3D printing ceramic core slurry as claimed in claim 1, wherein the coupling agent is one or more of 3-aminopropyltriethoxysilane, N- (β -aminoethyl-gamma-aminopropyl) methyldimethoxysilane, and 3- (methacryloyloxy) propyltrimethoxysilane.
3. A method of preparing a high solids content 3D printing ceramic core paste according to claim 1 or 2, characterized by the steps of:
step 1: adding a coupling agent into acrylic photosensitive resin to obtain a solution; the mass percentage of the coupling agent is 1-30%;
step 2: adding mixture inorganic powder consisting of two or more of alumina, silica, zirconia, titania, calcium oxide, magnesia and yttria into the solution; the mass percentage of the mixture inorganic powder is 50-90%, wherein the mass percentage of the alumina powder is not less than 50% and not more than 90%;
and step 3: then placing the mixture in an ultrasonic oscillator for ultrasonic treatment for 0.2 to 12 hours; then ball milling is carried out on the ball mill for 0.2 to 12 hours;
and 4, step 4: and then placing the ceramic core slurry in a vacuum drying oven, and carrying out vacuum treatment for 0.2-12 hours at normal temperature to obtain the high-solid-phase-content 3D printing ceramic core slurry.
4. The method for preparing a high solid content 3D printing ceramic core paste according to claim 1 or 2, wherein: the mixture inorganic powder is formed by mixing particles with different particle diameters, wherein the mass percentage of the powder with the particle diameter of 5-20 mu m is not less than 40%, and the mass percentage of the powder with the particle diameter of 10-200 nm is not less than 10%.
CN202010110023.3A 2020-02-23 2020-02-23 High-solid-content 3D printing ceramic core slurry and preparation method thereof Pending CN111233443A (en)

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Cited By (9)

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CN112608136A (en) * 2020-12-19 2021-04-06 西北工业大学 Photocuring 3D printing manufacturing method of high-porosity ceramic core
CN113105240A (en) * 2021-03-31 2021-07-13 上海联泰科技股份有限公司 Photocuring 3D printing yttrium oxide ceramic core and preparation method thereof
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CN114075069A (en) * 2020-08-13 2022-02-22 航天特种材料及工艺技术研究所 Alumina ceramic slurry for photocuring 3D printing, preparation method and alumina ceramic
CN112537948A (en) * 2020-12-19 2021-03-23 西北工业大学 Photocuring 3D printing manufacturing method of alumina-based ceramic core
CN112608136A (en) * 2020-12-19 2021-04-06 西北工业大学 Photocuring 3D printing manufacturing method of high-porosity ceramic core
CN113105240A (en) * 2021-03-31 2021-07-13 上海联泰科技股份有限公司 Photocuring 3D printing yttrium oxide ceramic core and preparation method thereof
CN113511901A (en) * 2021-04-21 2021-10-19 广东工业大学 Photocuring-formed silicon nitride ceramic with high solid content and preparation method and application thereof
CN113511901B (en) * 2021-04-21 2022-12-02 广东工业大学 Photocuring-formed silicon nitride ceramic with high solid content and preparation method and application thereof
CN115838288A (en) * 2021-09-18 2023-03-24 中国科学院上海硅酸盐研究所 SiC ceramic photosensitive slurry for photocuring 3D printing and preparation method thereof
CN115838288B (en) * 2021-09-18 2023-12-26 中国科学院上海硅酸盐研究所 SiC ceramic photosensitive slurry for photo-curing 3D printing and preparation method thereof
CN115043658A (en) * 2022-04-12 2022-09-13 山东大学 Preparation method of photocuring ceramic slurry
CN114853450A (en) * 2022-05-23 2022-08-05 西北工业大学 Photocuring 3D printing alumina-based ceramic core and preparation method thereof
CN114750411A (en) * 2022-06-16 2022-07-15 季华实验室 Material extrusion type 3D printing method

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