CN115504782A - High-solid-content and low-viscosity zirconia ceramic slurry for photocuring 3D printing - Google Patents
High-solid-content and low-viscosity zirconia ceramic slurry for photocuring 3D printing Download PDFInfo
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- CN115504782A CN115504782A CN202211340876.1A CN202211340876A CN115504782A CN 115504782 A CN115504782 A CN 115504782A CN 202211340876 A CN202211340876 A CN 202211340876A CN 115504782 A CN115504782 A CN 115504782A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/486—Fine ceramics
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- 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
- C04B35/62605—Treating the starting powders individually or as mixtures
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- 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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- 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
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- 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
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63488—Polyethers, e.g. alkylphenol polyglycolether, polyethylene glycol [PEG], polyethylene oxide [PEO]
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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Abstract
The invention discloses a high-solid-content and low-viscosity zirconia slurry for photocuring 3D printing and a preparation method thereof, wherein the high-solid-content and low-viscosity zirconia slurry for photocuring 3D printing comprises the following components in percentage by mass: nano zirconia powder (3 mol yttria-stabilized zirconia): 60% -85%; light-curing resin: 10% -40%; dispersing agent: 1% -15%; plasticizer: 1% -10%; auxiliary agent: 0.5-10%, high solid content and low viscosityZrO 2 The ceramic slurry has the characteristics of simple operation, good stability, high forming precision of a printed piece, low shrinkage rate of a sample piece and the like. The method is suitable for zirconia ceramic parts with high precision and complex structures.
Description
Technical Field
The invention relates to the technical field of additive manufacturing, in particular to zirconia ceramic slurry with high solid content and low viscosity for photocuring 3D printing.
Background art:
ZrO 2 the ceramic is widely applied to the fields of chemical industry, machinery, electronics, aerospace, biomedicine and the like due to excellent physical properties of mechanical strength, high temperature resistance, chemical stability, acoustoelectric magneto-thermal property and the like; most of the traditional manufacturing methods need to manufacture a mold in advance, so that the whole production period is longer, and ceramic parts with highly complex structures, particularly hollow and porous ceramic parts cannot be formed; 3D printing can flexibly manufacture a highly complex structure which cannot be realized by the traditional method, and the efficiency is improved; the ceramic photocuring 3D printing forming process based on the photopolymerization principle has the characteristics of high forming precision, good surface quality of a sample piece and the like, so that the ceramic photocuring 3D printing forming process has a wide application prospect; zrO of high solid content and low viscosity 2 The ceramic slurry can reduce the shrinkage rate of the ceramic piece after printing, reduce defects and improve the printing efficiency; thus, high-solid, low-viscosity ZrO was investigated 2 The ceramic slurry and the preparation process are very critical.
Disclosure of Invention
The invention aims to provide zirconia ceramic slurry with high solid content and low viscosity for photocuring 3D printing, wherein the zirconia slurry with high solid content can make the whole system of the slurry more stable and prevent the slurry from settling; the low viscosity can improve the printability of the paste.
The invention adopts the following technical scheme to achieve the aim:
the high-solid-content and low-viscosity zirconia slurry for photocuring 3D printing is characterized by comprising the following components in parts by weight: the zirconia slurry comprises the following components in percentage by mass: nano zirconium powder: 60% -85%; photosensitive resin: 10% -40%; dispersing agent: 1% -15%; plasticizer: 1% -10%; the nano zirconia powder is zirconia nano powder with 3mol yttria stabilization, and the grain size distribution is 100-200nm.
The photosensitive resin is prepared by blending an auxiliary agent and a light-cured resin, wherein the ratio of the auxiliary agent to the light-cured resin is 0.5-10%: 90 to 99.5 percent; the light-cured resin is butyl acrylate.
The dispersant is any one of sodium hexametaphosphate and citric acid.
The plasticizer is one or a mixture of polyethylene glycol-400, polyethylene glycol-600 and polyethylene glycol-800;
the auxiliary agent for adjusting the viscosity of the slurry is ethanol or methyl phthalate.
The invention provides a high-solid-content and low-viscosity zirconia slurry for photocuring 3D printing, which adopts the technical scheme and has the following beneficial effects:
1. the photocuring 3D printing zirconia ceramic slurry prepared by the technical scheme is simple in method, easy to operate and easy to industrialize; the zirconia particles prepared by the spray granulation method are spherical and have good fluidity and uniform particle size distribution, and the particle size distribution is between 100 and 200nm, thereby being beneficial to improving the solid content of zirconia in the slurry, reducing the viscosity of the slurry and improving the fluidity of the slurry. Solves the problems of large shrinkage, cracks and the like of printed materials after heat treatment due to low solid content of the sizing agent.
2. In the technical scheme, sodium hexametaphosphate or citric acid belongs to an ionic dispersing agent, so that the surfaces of zirconia particles have charges, and the charges of the same kind are mutually exclusive, the agglomeration phenomenon of zirconia in a resin solution is effectively solved, the stability of the slurry is improved, and the stable zirconia ceramic slurry is obtained.
3. The plasticizer in the technical scheme effectively solves the problem of forming of low-viscosity slurry printing, improves printing efficiency and printing precision, and is suitable for the technical field with high requirement precision and complex shape.
4. The auxiliary agent and the auxiliary dispersing agent in the technical scheme enable the nano zirconia particles to be better and more dispersed in the slurry, and further ensure the excellent dispersibility and stability of the zirconia slurry.
5. The sample formed in the technical scheme has good mechanical property, good wear resistance and high toughness, thereby having wide application prospect.
Detailed Description
The present invention will be described in detail with reference to specific examples:
example 1
(1) Taking ethanol as an auxiliary agent, and ultrasonically dispersing 1% ethanol and 99% photosensitive resin for 10min to obtain modified photosensitive resin;
(2) Adding 65% of nano zirconia powder into 33% of modified photosensitive resin to obtain slurry 1;
(3) Taking citric acid as a dispersing agent, adding 1% of the dispersing agent into the slurry 1, stirring for 10min by a homogenizer, and uniformly mixing to obtain a slurry 2;
(4) And (3) uniformly stirring 99% of the slurry 2 and 1% of polyethylene glycol-800 to obtain the zirconia slurry for 3D printing.
Example 2
(1) Adding ethanol as an auxiliary agent and 3% ethanol into 97% photosensitive resin, and performing ultrasonic dispersion for 10min to obtain photosensitive resin 1;
(2) Taking 70% of nano zirconia powder, and adding the nano zirconia powder into 23% of photosensitive resin 1 to obtain slurry 3;
(3) Taking sodium hexametaphosphate as a dispersing agent, adding 5% of the dispersing agent into 95% of the slurry 3, stirring for 10min by a homogenizer, and uniformly mixing to obtain a slurry 4;
(4) And mixing 98% of the slurry 4 with 2% of polyethylene glycol-600, and uniformly stirring to obtain the zirconia slurry for 3D printing.
Example 3
(1) Adding 5% of methyl phthalate into 95% of photosensitive resin by taking methyl phthalate as an auxiliary agent, and performing ultrasonic dispersion for 15min to obtain photosensitive resin 2;
(2) Adding 78% of nano zirconia powder into 17% of photosensitive resin 2 to obtain slurry 5;
(3) Taking a sodium hexametaphosphate solution as a dispersing agent, adding 4.5% of the dispersing agent into the slurry 5, stirring for 15min by a homogenizer, and uniformly mixing to obtain a slurry 6;
(4) And mixing 99.5% of the slurry 6 with 0.5% of polyethylene glycol-400, and uniformly stirring to obtain the zirconia slurry for 3D printing.
Example 4
(1) Adding 4% of methyl phthalate serving as an auxiliary agent into 96% of photosensitive resin, and performing ultrasonic dispersion for 15min to obtain photosensitive resin 3;
(2) Adding 82% of nano zirconia powder into 13% of photosensitive resin 3 to obtain slurry 7;
(3) Taking a citric acid solution as a dispersing agent, adding 4% of the dispersing agent into 96% of the slurry 7, stirring for 20min by a homogenizer, and uniformly mixing to obtain a slurry 8;
(4) And adding 1% of polyethylene glycol-400 into the 99% of slurry 8, and uniformly stirring to obtain the zirconia slurry for 3D printing.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive efforts, which shall be considered within the scope of the present invention.
Claims (5)
1. The high-solid-content and low-viscosity zirconia slurry for photocuring 3D printing is characterized in that: the zirconia slurry comprises the following components in percentage by mass: nano zirconium powder: 60% -85%; photosensitive resin: 10% -40%; dispersing agent: 1% -15%; plasticizer: 1% -10%; the nano zirconia powder is zirconia nano powder stabilized by 3mol of yttria, and the grain size distribution is 100-200nm.
2. The high-solid content, low-viscosity zirconia slurry for photocuring 3D printing of claim 1, wherein: the photosensitive resin is prepared by blending an auxiliary agent and a light-cured resin, wherein the ratio of the auxiliary agent to the light-cured resin is 0.5-10%: 90% -99.5%; the light-cured resin is butyl acrylate.
3. The high-solids, low-viscosity zirconia slurry for photocurable 3D printing according to claim 1, wherein: the dispersant is any one of sodium hexametaphosphate and citric acid.
4. The high-solids, low-viscosity zirconia slurry for photocurable 3D printing according to claim 1, wherein: the plasticizer is one or a mixture of polyethylene glycol-400, polyethylene glycol-600 and polyethylene glycol-800.
5. The high-solids, low-viscosity zirconia slurry for photocurable 3D printing according to claim 1, wherein: the auxiliary agent for adjusting the viscosity of the slurry is ethanol or methyl phthalate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211340876.1A CN115504782A (en) | 2022-10-30 | 2022-10-30 | High-solid-content and low-viscosity zirconia ceramic slurry for photocuring 3D printing |
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| CN202211340876.1A CN115504782A (en) | 2022-10-30 | 2022-10-30 | High-solid-content and low-viscosity zirconia ceramic slurry for photocuring 3D printing |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116655374A (en) * | 2023-06-28 | 2023-08-29 | 深圳新致美精密齿研有限公司 | High solid-phase zirconia ceramic slurry and preparation method and application thereof |
| CN120157473A (en) * | 2025-05-19 | 2025-06-17 | 浙江摩克激光智能装备有限公司 | A low-shrinkage 3D printed zirconia ceramic and its preparation process |
Citations (4)
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|---|---|---|---|---|
| CN109437893A (en) * | 2019-01-09 | 2019-03-08 | 北京理工大学 | A kind of high solids content/low viscosity photocuring zirconia ceramics slurry and preparation method thereof |
| CN113336542A (en) * | 2021-05-15 | 2021-09-03 | 江苏京科智镕新材料科技有限公司 | High-transmittance zirconia ceramic formula, paste preparation method and dental crown preparation method |
| US20210292243A1 (en) * | 2018-08-31 | 2021-09-23 | 3M Innovative Properties Company | Additive manufacturing method for making non-oxide ceramic articles, and aerogels, xerogels, and porous ceramic articles |
| CN114921115A (en) * | 2022-03-25 | 2022-08-19 | 深圳职业技术学院 | Yttrium-stabilized zirconia ceramic slurry and preparation method and application thereof |
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2022
- 2022-10-30 CN CN202211340876.1A patent/CN115504782A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210292243A1 (en) * | 2018-08-31 | 2021-09-23 | 3M Innovative Properties Company | Additive manufacturing method for making non-oxide ceramic articles, and aerogels, xerogels, and porous ceramic articles |
| CN109437893A (en) * | 2019-01-09 | 2019-03-08 | 北京理工大学 | A kind of high solids content/low viscosity photocuring zirconia ceramics slurry and preparation method thereof |
| CN113336542A (en) * | 2021-05-15 | 2021-09-03 | 江苏京科智镕新材料科技有限公司 | High-transmittance zirconia ceramic formula, paste preparation method and dental crown preparation method |
| CN114921115A (en) * | 2022-03-25 | 2022-08-19 | 深圳职业技术学院 | Yttrium-stabilized zirconia ceramic slurry and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116655374A (en) * | 2023-06-28 | 2023-08-29 | 深圳新致美精密齿研有限公司 | High solid-phase zirconia ceramic slurry and preparation method and application thereof |
| CN120157473A (en) * | 2025-05-19 | 2025-06-17 | 浙江摩克激光智能装备有限公司 | A low-shrinkage 3D printed zirconia ceramic and its preparation process |
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Inventor after: Wang Jia Inventor after: Sun Xiaofei Inventor after: Chen Yafang Inventor after: Qing Ge Inventor after: Meng Ye Inventor before: Wang Jia Inventor before: Sun Xiaofei Inventor before: Chen Yafang Inventor before: Qing Ge Inventor before: Meng Ye |
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Application publication date: 20221223 |