CN111875394A - Binder for ceramic powder 3DP forming and preparation method thereof - Google Patents
Binder for ceramic powder 3DP forming and preparation method thereof Download PDFInfo
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- CN111875394A CN111875394A CN202010723437.3A CN202010723437A CN111875394A CN 111875394 A CN111875394 A CN 111875394A CN 202010723437 A CN202010723437 A CN 202010723437A CN 111875394 A CN111875394 A CN 111875394A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63424—Polyacrylates; Polymethacrylates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/6303—Inorganic additives
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
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Abstract
The application discloses a binder for ceramic powder 3DP forming, which is characterized by comprising the following components in parts by mass: 90-100 parts of base material, 15-20 parts of water-based styrene-acrylic acid copolymer resin and 0.1-1 part of surfactant, wherein the viscosity of the binder is 2-12mPa.s, and the surface tension is 30-38 mN/m. According to the technical scheme, the water-soluble styrene-acrylic acid copolymer resin is used as a cross-linked polymer, so that the problems of low strength of a blank, difficulty in powder cleaning treatment, low density of a fired ceramic product and high dielectric loss caused by poor surface wettability of the binder and ceramic powder are effectively solved. The adhesive is simple in preparation method, convenient to use and easy to obtain raw materials.
Description
Technical Field
The technology belongs to the technical field of additive manufacturing, and particularly relates to a binder for ceramic powder 3DP forming and a preparation method thereof.
Background
The 3DP technology can realize low-cost and rapid manufacturing of complex special-shaped ceramic parts, and the development of the ceramic 3DP printing technology is limited by the performance of the adhesive. At present, the ceramic powder bonding mode commonly adopted by the 3DP forming process is as follows: the ceramic powder and the adhesive solution are fully mixed to form ceramic coating powder, and then the binder is sprayed and molded. The method has good forming quality and good reliability, but has high cost, different adhesive materials need to be selected according to the types of the ceramic powder, and the density of the ceramic is influenced due to the addition of a large amount of adhesive components, so that the strength after sintering is greatly reduced.
The wetting property of the binder determines the flowing state of a binder fluid on the surface of a solid, and influences the contact area of fluid molecules and powder particles, so that the spreading degree of the binder on the surface of the powder particles is different, and the problems of low precision, poor mechanical property and the like of a formed product are caused.
Experiments have shown that the surface tension and viscosity of the binder are important factors influencing the degree of wetting of the raw powder and the binder and the quality of the finished parts. The surface tension of the binder can adjust the contact angle of the liquid drop and the solid surface so as to influence the wetting property of the binder. The viscosity of the adhesive is too low and too high, which can cause adverse effect on the later molding process of the product, and the viscosity is too high, so that the spray head can not spray smoothly; if the viscosity is too low, the strength of the formed blank is reduced; therefore, the quality of the binder determines the quality of later-stage blank forming, and the binder which can keep the viscosity and the surface tension of the binder in proper ranges so as to strengthen the wettability of the ceramic powder is found, which is a problem to be solved in the application of the 3DP binder.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide the binder for 3DP forming, which has good surface wettability with ceramic powder, less binder addition amount, no residue after binder removal treatment, no influence on ceramic performance and improved ceramic firing density, and the preparation method thereof.
The water-soluble styrene-acrylic resin is used as the raw material of the adhesive, so that the wettability of the raw material powder and the adhesive can be effectively improved.
The wetting properties of a liquid drop are often technically characterized by its contact angle on the surface of the solid. The range of the contact angle represents the wetting property. In order to achieve the purpose, the technical scheme adopts the following technical means:
the binder for 3DP forming of the ceramic powder is characterized by comprising the following components in parts by mass: 90-100 parts of base material, 15-20 parts of water-soluble styrene-acrylic acid copolymer resin and 0.1-1 part of surfactant;
the content of the water-based styrene-acrylic acid copolymer resin in the component is low, on one hand, the bonding and molding of powder can be realized through the low resin content, and the dielectric property of the silicon nitride ceramic is not influenced after binder removal and firing treatment due to the small resin content, so that the dielectric loss of the silicon nitride ceramic is reduced.
Further, the viscosity of the adhesive is 2-12mPa.s, and the surface tension is 30-38 mN/m. The viscosity is controlled to be 2-12mPa.s, so that the spray head can be ensured to be smoothly sprayed out and is not easy to block. The surface tension in the range can reduce the contact angle between the adhesive and the powder to 20-35 degrees, which is beneficial to spreading and penetration of the adhesive on the surface of the powder.
Further, the base stock is distilled water. Distilled water is easy to volatilize at high temperature, which is beneficial to reducing colloid residue after glue discharging and improving the dielectric property of the ceramic material.
Further, the surfactant is one of dodecyl ammonium bromide and absolute ethyl alcohol. The surface tension of the adhesive can be adjusted to 30-38mN/m by the surfactant. Is favorable for improving the wettability of the adhesive and the ceramic powder.
Further, the using temperature of the adhesive is 21-27 ℃. When the temperature is lower than 21 ℃, the ink of the adhesive is not smooth, and when the temperature is higher than 27 ℃, the moisture in the adhesive is volatilized too fast, so that the nozzle is easily blocked.
The preparation method of the binder for 3DP forming of the ceramic powder comprises the following steps:
s01, weighing the raw materials according to the mass parts of the claim 1;
s02, slowly adding the cross-linked polymer weighed in the S01 weight part into the weighed distilled water, and stirring until the cross-linked polymer is fully dissolved. Controlling the viscosity of the solution to be 2-12 mPa.s;
s03, finally adding the surfactant weighed in the S01 in parts by weight, uniformly stirring and fully dissolving, and controlling the surface tension of the solution to be 30-38 mN/m.
The viscosity and the surface tension of the binder are controlled to be in a proper range through the above steps, so that the wettability of the binder with the ceramic powder is enhanced.
The binder for 3DP forming of ceramic powder is applied to bonding of ceramic powder in a 3DP forming process, and the ceramic powder is one of silicon nitride ceramic powder or alumina ceramic powder.
According to the binder, the surfactant is added into the mixed solution of distilled water and water-soluble styrene-acrylic acid copolymer resin, and the viscosity and the surface tension of the solution are adjusted in a proper range, so that the contact angle between the solution and ceramic powder is adjusted, and the wettability of the solution and ceramic powder is improved. In addition, the dosage of the water-soluble styrene-acrylic acid copolymer resin and the surfactant is strictly controlled, and the dosage of the binder only accounts for 13-15% of the mass fraction of the ceramic powder, so that the spreading and permeation uniformity of the binder on the surface of the powder layer can be ensured, the printing quality is improved, and the use cost is greatly reduced. The adhesive takes distilled water as a main solution, so that the problem that the nozzle is blocked due to high viscosity of the adhesive can be solved; the residual rate of the binder in the binder removal process is reduced, the dielectric property of the ceramic product is improved, the use performance of the ceramic product is not affected, and the fired density of the ceramic product reaches 95-99%.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 SEM photograph of silicon nitride ceramic obtained in example 1
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
Example 1
Weighing 90 parts of distilled water, slowly adding 15 parts of water-based styrene-acrylic acid copolymer resin, and stirring until the mixture is fully dissolved. And finally, adding 1 part of surfactant (dodecyl ammonium bromide), uniformly stirring and fully dissolving, wherein the viscosity of the binder is 8.5mPa.s, the surface tension is 32.24mN/m, the contact angle of the binder and the silicon nitride ceramic powder is 32.24 degrees, and the use temperature is 21 ℃.
Adopting 3DP method three-dimensional printing technology, 15% binder consumption, 5.0MPa of molded blank strength, 95% of sintering compactness and 1.2 x 10 of silicon nitride ceramic dielectric loss-3。
Example 2
Weighing 90 parts of distilled water, slowly adding 15 parts of water-based styrene-acrylic acid copolymer resin, and stirring until the mixture is fully dissolved. And finally, adding 0.3 part of surfactant (dodecyl ammonium bromide), uniformly stirring and fully dissolving, wherein the viscosity of the binder is 8.1mPa.s, the surface tension is 40.3mN/m, the contact angle of the binder and the silicon nitride ceramic powder is 33.58 degrees, and the use temperature is 27 ℃.
Adopting 3DP method three-dimensional printing technology, the binder dosage is 18 percent, and the strength of the formed blank body is obtained5.2MPa, sintering density of 92 percent and dielectric loss of silicon nitride ceramic of 1.9 multiplied by 10-3。
Example 3
100 parts of distilled water is weighed, 20 parts of water-based styrene-acrylic acid copolymer resin is slowly added, and the mixture is stirred until the mixture is fully dissolved. And finally, adding 1 part of surfactant (absolute ethyl alcohol), uniformly stirring and fully dissolving, wherein the viscosity of the binder is 9.2mPa.s, the surface tension is 32.39mN/m, the contact angle of the binder and the silicon nitride ceramic powder is 34.18 degrees, and the use temperature is 25 ℃.
Adopting 3DP method three-dimensional printing technology, 15% binder consumption, obtaining the formed blank with strength of 5.6MPa, sintering density of 97%, and silicon nitride ceramic dielectric loss of 1.2X 10-3。
Example 4
Weighing 90 parts of distilled water, slowly adding 15 parts of water-based styrene-acrylic acid copolymer resin, and stirring until the mixture is fully dissolved. And finally, adding 1 part of surfactant (dodecyl ammonium bromide), uniformly stirring and fully dissolving, wherein the viscosity of the binder is 8.7mPa.s, the surface tension is 35.62mN/m, the contact angle of the binder and the alumina ceramic powder is 27.56 degrees, and the use temperature is 23 ℃.
Adopting 3DP method three-dimensional printing technology, 16% of binder consumption, obtaining the formed blank with the strength of 5.5MPa, the sintering density of 95%, and the dielectric loss of alumina ceramic of 1.7 multiplied by 10-3。
Example 5
100 parts of distilled water is weighed, 1 part of water-based styrene-acrylic acid copolymer resin is slowly added, and the mixture is stirred until the mixture is fully dissolved. And finally, adding 1 part of surfactant (absolute ethyl alcohol), uniformly stirring and fully dissolving, wherein the viscosity of the binder is 9.6mPa.s, the surface tension is 38.75mN/m, the contact angle of the binder and the alumina ceramic powder is 23.18 degrees, and the use temperature is 22 ℃.
Adopting 3DP method three-dimensional printing technology, the binder dosage is 18%, the strength of the obtained formed blank is 5.3MPa, the sintering density is 92%, and the dielectric loss of the alumina ceramic is 1.5 multiplied by 10-3。
Comparative example 1
100 parts of distilled water is weighed, 15 parts of polyvinylpyrrolidone is slowly added, and the mixture is stirred until the polyvinylpyrrolidone is fully dissolved. And finally, adding 0.5 part of surfactant (absolute ethyl alcohol), uniformly stirring and fully dissolving, wherein the viscosity of the binder is 1.33mPa.s, the surface tension is 37.16mN/m, the contact angle of the binder and the silicon nitride ceramic powder is 34.57 degrees, and the use temperature is 21 ℃.
Adopting 3DP method three-dimensional printing technology, the binder dosage is 13%, the strength of the obtained formed blank is 1.0MPa, the sintering density is 54%, and the dielectric loss of the silicon nitride ceramic is 36 multiplied by 10-3。
Comparative example 2
100 parts of distilled water is weighed, 18 parts of polyvinylpyrrolidone is slowly added, and the mixture is stirred until the mixture is fully dissolved. And finally, adding 0.5 part of surfactant (absolute ethyl alcohol), uniformly stirring and fully dissolving, wherein the viscosity of the binder is 1.87mPa.s, the surface tension is 38.03mN/m, the contact angle of the binder and the alumina ceramic powder is 21.36 degrees, and the use temperature is 27 ℃.
Adopting 3DP method three-dimensional printing technology, with 24% binder consumption, to obtain a molded blank with strength of 1.8MPa, sintering density of 65%, and dielectric loss of alumina ceramic of 14 × 10-3。
Comparative example 3
100 parts of distilled water was weighed, and 15 parts of phosphate was slowly added to dissolve sufficiently. And finally, adding 0.5 part of surfactant (absolute ethyl alcohol), uniformly stirring and fully dissolving, wherein the viscosity of the binder is 433.23mPa.s, the surface tension is 58.45mN/m, the contact angle of the binder and the silicon nitride ceramic powder is 122.15 ℃, and the use temperature is 22 ℃. And 3DP method three-dimensional printing technology is adopted, so that the 3DP blank cannot be bonded and molded.
Comparative example 4
90 parts of distilled water was weighed, and 17 parts of glutaraldehyde was slowly added to dissolve it sufficiently. Finally, 0.5 part of surfactant (dodecyl ammonium bromide) is added, the mixture is uniformly stirred and fully dissolved, the viscosity of the adhesive is 87.11Pa.s, the surface tension is 48.32mN/m, and the contact angle between the adhesive and the chitosan-coated silicon nitride ceramic powder is 42 degrees, and the use temperature is 27 ℃.
Adopting 3DP method three-dimensional printing technology, 33% of binder consumption, obtaining the formed blank with the strength of 5.6MPa, the sintering compactness of 40% and the dielectric loss of 25 multiplied by 10 of silicon nitride ceramic-3。
As can be seen from the SEM photograph of the silicon nitride ceramic obtained in example 1 of fig. 1 and comparative examples 1 to 4, the density of the article obtained by using the styrene-acrylic acid copolymer resin aqueous solution is much greater than that of the article obtained in the comparative example, and the density of the article obtained in example 3 is the highest in the example, 43% higher than that of the article obtained in comparative example 1, 32% higher than that of the article obtained in comparative example 2, and 57% higher than that of comparative example 4; in addition, the strength of the 3DP blank and the dielectric loss are far better than those of the comparative example. In conclusion, the powder and binder formula and the process method of the invention are beneficial to improving the compactness of the finished piece, thereby being beneficial to obtaining the high-strength finished piece, reducing the dielectric loss of the ceramic and greatly reducing the process production cost.
The above examples are intended only to illustrate the technical solution of the invention, and not to limit it; although the invention of the present application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (8)
1. The adhesive is characterized by comprising the following components in parts by mass: 90-100 parts of base material, 15-20 parts of water-soluble styrene-acrylic acid copolymer resin and 0.1-1 part of surfactant.
2. Adhesive according to claim 1, characterized in that it has a viscosity of 2-12mpa.s and a surface tension of 30-38 mN/m.
3. The binder of claim 1 wherein the binder is distilled water.
4. The binder of claim 1 wherein the surfactant is one of dodecylammonium bromide and absolute ethanol.
5. The adhesive of claim 1, wherein the adhesive is used at a temperature of 21-27 ℃.
6. A method for preparing the adhesive according to claims 1 to 5, comprising the steps of:
s01, weighing the raw materials according to the mass parts of the claim 1;
s02, slowly adding the cross-linked polymer weighed in the S01 weight part into the weighed distilled water, and stirring until the cross-linked polymer is fully dissolved;
and S03, finally adding the surfactant weighed in the S01 in parts by weight, uniformly stirring and fully dissolving.
7. The method for producing the adhesive according to claim 6, wherein the viscosity of the adhesive is controlled to 2 to 12mPa.s and the surface tension is controlled to 30 to 38 mN/m.
8. The use of the binder of claims 1-5, wherein the binder is used for bonding ceramic powder in a 3DP forming process, wherein the ceramic powder is one of silicon nitride ceramic powder or aluminum oxide ceramic powder; the contact angle between the binder and the ceramic powder is 20-35 degrees, and the dielectric loss of the sintered ceramic is 1.2 multiplied by 10-3-1.9×10-3。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115572071A (en) * | 2022-10-14 | 2023-01-06 | 山东工业陶瓷研究设计院有限公司 | False tooth preparation method |
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| WO1995030503A1 (en) * | 1994-05-06 | 1995-11-16 | Dtm Corporation | Binder compositions for selective laser sintering processes |
| CN1508209A (en) * | 2002-11-08 | 2004-06-30 | 株式会社村田制作所 | Water-soluble propenoic-acids adhesive and its preparation method, ceramic slurry composition and preparation method thereof |
| CN1733652A (en) * | 2005-06-30 | 2006-02-15 | 北京科技大学 | Preparation method of ceramic powder material applying in precinct laser sintering for quick formation |
| WO2019131710A1 (en) * | 2017-12-26 | 2019-07-04 | 昭和電工株式会社 | Binder for nonaqueous battery electrodes, slurry for nonaqueous battery electrodes, nonaqueous battery electrode, and nonaqueous battery |
| CN110177638A (en) * | 2017-02-24 | 2019-08-27 | 惠普发展公司，有限责任合伙企业 | 3 D-printing |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995030503A1 (en) * | 1994-05-06 | 1995-11-16 | Dtm Corporation | Binder compositions for selective laser sintering processes |
| CN1508209A (en) * | 2002-11-08 | 2004-06-30 | 株式会社村田制作所 | Water-soluble propenoic-acids adhesive and its preparation method, ceramic slurry composition and preparation method thereof |
| CN1733652A (en) * | 2005-06-30 | 2006-02-15 | 北京科技大学 | Preparation method of ceramic powder material applying in precinct laser sintering for quick formation |
| CN110177638A (en) * | 2017-02-24 | 2019-08-27 | 惠普发展公司，有限责任合伙企业 | 3 D-printing |
| WO2019131710A1 (en) * | 2017-12-26 | 2019-07-04 | 昭和電工株式会社 | Binder for nonaqueous battery electrodes, slurry for nonaqueous battery electrodes, nonaqueous battery electrode, and nonaqueous battery |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115572071A (en) * | 2022-10-14 | 2023-01-06 | 山东工业陶瓷研究设计院有限公司 | False tooth preparation method |
| CN115572071B (en) * | 2022-10-14 | 2024-05-24 | 山东工业陶瓷研究设计院有限公司 | Denture preparation method |
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Application publication date: 20201103 |