CN111792928A - Preparation method of 3D printing ceramic and product thereof - Google Patents
Preparation method of 3D printing ceramic and product thereof Download PDFInfo
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- CN111792928A CN111792928A CN202010517694.1A CN202010517694A CN111792928A CN 111792928 A CN111792928 A CN 111792928A CN 202010517694 A CN202010517694 A CN 202010517694A CN 111792928 A CN111792928 A CN 111792928A
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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
- B33Y10/00—Processes of additive manufacturing
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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
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- 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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- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention discloses a preparation method of 3D printing ceramic and a product thereof. The invention discloses a preparation method of 3D printing ceramic, which comprises the following steps: s1: adding ceramic powder into a mixed solution of a binder and an organic solvent, and uniformly stirring to obtain slurry; s2: extruding and molding the slurry by adopting microflow extrusion molding equipment to obtain a ceramic blank, immediately immersing the printed ceramic blank into an inorganic solution for rapid molding, wherein the organic solvent and the inorganic solution are mutually soluble; s3: taking out and drying the ceramic blank after the ceramic blank is cured and hardened; s4: removing the binder; s5: and (4) calcining at high temperature to obtain the ceramic. The ceramic slurry provided by the invention has good fluidity and stability, has proper solid content, has excellent shape retention capacity, and is porous and not easy to crack; the porosity is regulated and controlled by the proportion of the organic solvent and the ceramic powder, a hierarchical pore structure is realized, and ceramic parts with complex geometric shapes can be prepared.
Description
Technical Field
The invention relates to the technical field of ceramic 3D printing, in particular to a preparation method of 3D printing ceramic and a product thereof.
Background
As a traditional inorganic non-metallic material, the ceramic has excellent properties of high strength, corrosion resistance, wear resistance, high temperature resistance and the like, and is widely concerned and applied in various industries such as biological medicine, electronics, aerospace and the like.
Additive Manufacturing (AM), commonly known as 3D printing, is a new and advanced material forming technology which is popular at present, and numerous domestic and foreign research institutions and enterprises participate in research, development and innovation of the technology. The ceramic 3D printing technology is used as a combination of the ceramic material and the 3D printing technology, so that the ceramic product with a complex shape can be manufactured, and the ceramic product has the advantages of high forming speed, low cost, high forming precision and the like. In view of the current situation of ceramic 3D printing, the development of the current ceramic 3D printing technology is not mature enough, and many problems to be solved, such as how to prepare ceramic slurry with good viscosity, low fluidity and uniform mixing, exist. In the sintering process, the blank is easy to generate the defects of cracks, deformation, different shrinkage rates in all directions and the like, and the sintering difficulty is increased.
Disclosure of Invention
The invention aims to provide a preparation method of a 3D printing ceramic and a product thereof, aiming at the defects in the prior art.
The invention discloses a preparation method of 3D printing ceramic, which comprises the following steps:
s1: adding ceramic powder into a mixed solution of a binder and an organic solvent, and uniformly stirring to obtain slurry;
s2: extruding and molding the slurry by adopting microflow extrusion molding equipment to obtain a ceramic blank, immediately immersing the printed ceramic blank into an inorganic solution for rapid molding, wherein the organic solvent and the inorganic solution are mutually soluble;
s3: taking out and drying the ceramic blank after the ceramic blank is cured and hardened;
s4: preserving the heat of the dried ceramic blank at 500-600 ℃ for 3h to remove the binder;
s5: and (4) calcining the ceramic body obtained in the step S4 at a high temperature to obtain the ceramic product.
Further, in the step S5, the calcination temperature is 1100-1500 ℃, the temperature rise rate is 5-20 ℃/min, and the time is 2.5-6 h.
Further, the mass ratio of the binder to the organic solvent to the ceramic powder is 2.8-4.2: 1: 1.
Further, the binder comprises polyether sulfone and/or polyvinyl alcohol.
Further, the organic solvent comprises one or more of N-methyl-2-pyrrolidone, dimethylformamide or dimethyl sulfoxide.
Further, the inorganic solution includes deionized water or distilled water.
Further, the ceramic powder includes ZrO2、Al2O3、TiO2And SiC.
Further, the particle size of the ceramic powder is in the nanometer or submicron level.
Further, the drying temperature in the step S3 is 75-85 ℃, and the drying time is 12-14 h.
A ceramic prepared by the method.
The ceramic slurry provided by the invention has good fluidity and stability, has proper solid content, has excellent shape retention capacity, and is porous and not easy to crack; the method has the advantages of one-step molding, controllable shape, simple process, low cost and high molding precision, the porosity is regulated and controlled by the proportion of the organic solvent and the ceramic powder, the hierarchical pore structure is realized, the higher the mass ratio of the organic solvent to the ceramic powder is, the higher the porosity is, the hierarchical pore structure is realized, the organic solvent and the inorganic solution in the ceramic blank are mutually dissolved and separated, and meanwhile, the polymer binder in the ceramic blank forms macromolecular gel, so that the rapid curing molding of the ceramic blank is realized, the calcining condition is controlled, the ceramic strength value is increased, the porosity of the prepared ceramic is more than 10 percent, the strength is more than 1500MPa, and the ceramic part with complex geometric shape can be prepared.
Drawings
Fig. 1 is a flow chart of a 3D printing ceramic preparation method of the present invention.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
Example 1
As shown in figure 1, 3.34g of polyethersulfone was slowly added into 10.02g of N-methyl-2-pyrrolidone solvent, and stirred at a constant temperature of 70 ℃ for 1.5h under 800r/min in a magnetic stirrer until the polyethersulfone was uniformly dissolved in the solvent to obtain premix 1. Then 10.00g of ceramic powder is added into the premixed liquid 1 to obtain a premixed liquid 2, and a magnetic stirrer is used for stirring for 12 hours at the constant temperature of 800r/min and the temperature of 65 ℃ to obtain uniform ceramic slurry. And then, extruding and molding by adopting a microflow extrusion molding device, printing a ceramic blank 1, immediately and slowly immersing the printed ceramic blank 1 into deionized water, standing for 12 hours until the exchange of the organic solvent and water is finished, and curing and hardening the blank to obtain a ceramic blank 2. All ceramic bodies 2 were then dried at 75 ℃ for 12 h. And (3) preserving the heat of the dried ceramic body 2 at 600 ℃ for 3h to remove the polyether sulfone binder, then calcining at 1200 ℃ for 5h at the heating rate of 10 ℃/min to obtain the ceramic product with the porosity of 13.2% and the strength of 1648 Mpa.
Example 2
Slowly adding 3.33g of polyethylene glycol into 10.10g of N-methyl-2-pyrrolidone solvent, and stirring and processing for 1.5h at the constant temperature of 70 ℃ under the condition of 800r/min by a magnetic stirrer until the polyether sulfone is uniformly dissolved in the solvent to obtain a premixed solution 1. Then 10.00g of ceramic powder is added into the premixed liquid 1 to obtain a premixed liquid 2, and a magnetic stirrer is used for stirring for 12 hours at the constant temperature of 800r/min and the temperature of 65 ℃ to obtain uniform ceramic slurry. And then, extruding and molding by adopting a microflow extrusion molding device, printing a ceramic blank 1, immediately and slowly immersing the printed ceramic blank 1 into deionized water, standing for 12 hours until the exchange of the organic solvent and water is finished, and curing and hardening the blank to obtain a ceramic blank 2. All ceramic bodies 2 were then dried at 75 ℃ for 12 h. And (3) preserving the heat of the dried ceramic body 2 at 550 ℃ for 3h to remove the binder polyethylene glycol, calcining at 1250 ℃ for 3h at a heating rate of 10 ℃/min to obtain the ceramic product with the porosity of 12.5% and the strength of 1705 Mpa.
Example 3
4.10g of polyethersulfone is slowly added into 12.30g of dimethylformamide solvent, and stirred for 1.5h at the constant temperature of 70 ℃ under the condition of 800r/min by a magnetic stirrer until the polyethersulfone is uniformly dissolved in the solvent to obtain a premixed solution 1. Then, 12.00g of ceramic powder is added into the premixed liquid 1 to obtain a premixed liquid 2, and a magnetic stirrer is used for stirring for 12 hours at the constant temperature of 800r/min and the temperature of 65 ℃ to obtain uniform ceramic slurry. And then extruding and forming by adopting a microflow extrusion forming device, printing the ceramic blank 1, immediately and slowly immersing the printed ceramic blank 1 into deionized water, standing for 12h until the exchange of the organic solvent and water is finished, and curing and hardening the blank to obtain the ceramic blank 2. All ceramic bodies 2 were then dried at 75 ℃ for 12 h. And (3) preserving the heat of the dried ceramic body 2 at 550 ℃ for 3h to remove the polyether sulfone binder, calcining at 1300 ℃ for 3h at the high temperature with the heating rate of 12 ℃/min to obtain the ceramic product with the porosity of 11.3% and the strength of 1850 MPa.
Example 4
Slowly adding 5.05g of polyethersulfone into 15.15g of dimethylformamide solvent, and stirring and processing for 1.5h at the constant temperature of 70 ℃ under the condition of 800r/min by using a magnetic stirrer until the polyethersulfone is uniformly dissolved in the solvent to obtain a premixed solution 1. Then 15.05g of ceramic powder is added into the premixed liquid 1 to obtain a premixed liquid 2, and a magnetic stirrer is used for stirring for 12 hours at the constant temperature of 800r/min and the temperature of 65 ℃ to obtain uniform ceramic slurry. And then, extruding and molding by adopting a microflow extrusion molding device, printing a ceramic blank 1, immediately and slowly immersing the printed ceramic blank 1 into deionized water, standing for 12 hours until the exchange of the organic solvent and water is finished, and curing and hardening the blank to obtain a ceramic blank 2. All ceramic bodies 2 were then dried at 75 ℃ for 12 h. And (3) preserving the heat of the dried ceramic blank 2 at 600 ℃ for 3h to remove the polyether sulfone binder, calcining at 1150 ℃ for 6h at the high temperature of 5 ℃/min to obtain the ceramic product with the porosity of 15.2% and the strength of 1580 Mpa.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. A preparation method of 3D printing ceramic is characterized by comprising the following steps: the method comprises the following steps:
s1: adding ceramic powder into a mixed solution of a binder and an organic solvent, and uniformly stirring to obtain slurry;
s2: extruding and molding the slurry by adopting microflow extrusion molding equipment to obtain a ceramic blank, immediately immersing the printed ceramic blank into an inorganic solution for rapid molding, wherein the organic solvent and the inorganic solution are mutually soluble;
s3: taking out and drying the ceramic blank after the ceramic blank is cured and hardened;
s4: preserving the heat of the dried ceramic blank at 500-600 ℃ for 3h to remove the binder;
s5: and (4) calcining the ceramic body obtained in the step S4 at a high temperature to obtain the ceramic product.
2. The method for preparing 3D printed ceramics according to claim 1, wherein: in the step S5, the calcination temperature is 1100-1500 ℃, the temperature rise rate is 5-20 ℃/min, and the time is 2.5-6 h.
3. A method of preparing a 3D printed ceramic as claimed in claim 1 or 2, wherein: the mass ratio of the binder to the organic solvent to the ceramic powder is 2.8-4.2: 1: 1.
4. A method of preparing a 3D printed ceramic as claimed in claim 1 or 2, wherein: the binder comprises polyether sulfone and/or polyvinyl alcohol.
5. The method for preparing 3D printing ceramic according to claim 4, wherein the method comprises the following steps: the organic solvent comprises one or more of N-methyl-2-pyrrolidone, dimethylformamide and dimethyl sulfoxide.
6. The method for preparing 3D printing ceramic according to claim 5, wherein the method comprises the following steps: the inorganic solution includes deionized or distilled water.
7. The method for preparing 3D printing ceramic according to claim 4, wherein the method comprises the following steps: the ceramic powder comprises ZrO2、Al2O3、TiO2And SiC.
8. The method for preparing 3D printed ceramics according to claim 7, wherein: the particle size of the ceramic powder is in the nanometer or submicron level.
9. The method for preparing 3D printed ceramics according to claim 1, wherein: in the step S3, the drying temperature is 75-85 ℃, and the drying time is 12-14 h.
10. A ceramic prepared by a method of preparing a 3D printed ceramic as claimed in any one of claims 1 to 9.
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Cited By (2)
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CN113275590A (en) * | 2021-04-27 | 2021-08-20 | 江苏大学 | Method for preparing component with through cavity by direct-writing printing and pressure sintering |
CN113372114A (en) * | 2021-07-16 | 2021-09-10 | 合肥工业大学 | Preparation method of zirconia ceramic material extrusion type 3D printing material |
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2020
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WO2009027525A2 (en) * | 2007-08-29 | 2009-03-05 | Vito Nv | Method for producing a three-dimensional macroporous filament construct based on phase inversion and construct thereby obtained |
CN106588000A (en) * | 2016-11-24 | 2017-04-26 | 上海交通大学 | Manufacturing process of helical wire type ceramic spring |
CN110142957A (en) * | 2019-06-03 | 2019-08-20 | 北京化工大学 | A kind of polymer 3D printing forming method based on solid separation separating technology |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113275590A (en) * | 2021-04-27 | 2021-08-20 | 江苏大学 | Method for preparing component with through cavity by direct-writing printing and pressure sintering |
CN113372114A (en) * | 2021-07-16 | 2021-09-10 | 合肥工业大学 | Preparation method of zirconia ceramic material extrusion type 3D printing material |
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