CN114933486B - Method for preparing porous ceramic block body based on water-based slurry through 3D printing - Google Patents
Method for preparing porous ceramic block body based on water-based slurry through 3D printing Download PDFInfo
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Abstract
The invention relates to the technical field of porous ceramic material preparation, in particular to a method for preparing a porous ceramic block by 3D printing based on water-based slurry. The ingredients comprise: 25-55 parts of graded alumina powder, 0-55 parts of starch, 15-25 parts of binder, 1-2 parts of photoinitiator, 1-4 parts of dispersing agent and 20-35 parts of solvent; the mixing mode is as follows: ball-milling and mixing graded alumina powder, starch, a binder, a photoinitiator, a dispersing agent and a solvent to obtain photosensitive slurry; curing and forming the obtained photosensitive slurry by adopting a 3D ceramic printer to obtain a ceramic green body; and (3) placing the ceramic green body in a tubular furnace for degreasing and sintering to finally obtain the porous alumina ceramic.
Description
Technical Field
The invention relates to a method for preparing a porous ceramic block by 3D printing based on water-based slurry, belonging to the technical field of porous ceramic material preparation.
Background
Porous ceramic materials are widely used in the fields of automobile industry, catalyst loading, gas/liquid filters, etc. because of their low density, low specific heat, high specific surface area, high permeability, high strength and hardness, strong dimensional stability, high wear resistance and corrosion resistance, excellent chemical stability, etc. As a porous ceramic material with low cost, easy availability and good performance, the effective preparation method of the porous alumina is being widely researched. The traditional method for preparing the porous alumina mainly adopts die casting molding and slurry casting molding, and the prepared porous alumina ceramic material has simple morphology and structure and is difficult to meet the demands of production and life.
3D printing techniques are often used for the formation of complex samples due to their unique additive manufacturing processes. The design idea can be automatically, quickly, accurately and directly converted into the physical model through 3D printing, the 3D printing is not limited by the types of the dies, the shape and the size of a required sample can be changed at will, and the development cost of the product is greatly reduced. Direct-writing 3D printing has been widely studied in the aspect of porous ceramic molding, namely, an inkjet method in the conventional printing technology is adopted, a spray head selectively sprays a binder to a position designed in advance under the condition of not directly contacting with the surface of powder, and then printing is carried out layer by layer, so that the molding of a complex shape and the design of a three-dimensional pore structure are realized. However, direct-write 3D printing has disadvantages of slow printing speed, low precision, long adhesive curing time, and the like. Therefore, a molding mode with high molding speed, high precision and complex morphology structure is sought, and the important research is still needed at present.
Disclosure of Invention
Aiming at the problems that the current mature 3D ceramic printing technology is high in density and difficult to prepare porous materials such as heat insulation and sound insulation, the invention provides a method for preparing a porous ceramic block by 3D printing based on water-based slurry, and the alumina ceramic obtained by the method forms a macroporous structure with high porosity, controllability and uniform pore size distribution, is free from warping and low in shrinkage rate during sintering, is beneficial to maintaining the size and shape of the materials, and accurately controls the complex molding of the porous ceramic materials.
The technical scheme of the invention is as follows: a method for preparing a porous ceramic block based on 3D printing of water-based slurry,
1) The ingredients comprise: 25-55 parts of graded alumina powder, 0-55 parts of starch, 15-25 parts of binder, 1-2 parts of photoinitiator, 1-4 parts of dispersing agent and 20-35 parts of solvent;
2) The mixing mode is as follows: ball-milling and mixing graded alumina powder, starch, a binder, a photoinitiator, a dispersing agent and a solvent to obtain photosensitive slurry;
3) Curing and forming the photosensitive slurry obtained in the step 2) by adopting a 3D ceramic printer to obtain a ceramic green body;
4) And (3) placing the ceramic green body in a tubular furnace for degreasing and sintering to finally obtain the porous alumina ceramic.
Preferably, in the method for preparing the porous ceramic block based on the 3D printing of the water-based slurry, in the step 1), the binder is PEG400DA, the dispersant is glycerol, and the solvent is water; the photoinitiator was 2-hydroxy-2-methyl-1-phenyl-1-propanone.
Preferably, in the above method for preparing a porous ceramic block based on 3D printing of water-based slurry, in step 1), the size grading of the graded alumina powder is specifically: 200-400 parts of 0.2 mu m alumina, 600-800 parts of 1-3 mu m alumina.
Preferably, in the above method for preparing porous ceramic blocks based on 3D printing of water-based slurry, in step 2), the rotation speed of ball milling and mixing is 150-200 rpm, and the ball milling time is 2-4 hours.
Preferably, in the above method for preparing a porous ceramic block based on 3D printing of water-based slurry, in step 4), the degreasing process is heated to 200-650 ℃ at a heating rate of 0.5-2 ℃/min, and the holding time is 1-3 hours.
Preferably, in the above method for preparing a porous ceramic block based on 3D printing of water-based slurry, in step 4), the sintering process is heated to 650-1300 ℃ at a heating rate of 3-5 ℃/min for 2-6 hours.
The beneficial effects of the invention are as follows:
the photosensitive slurry contains the modified alumina powder with reasonable grading so as to form a uniform and controllable pore structure, so that the proper viscosity and photosensitive property of the photosensitive slurry are ensured, the shrinkage rate of a blank body is small in the sintering process, the blank body is not easy to warp and deform, the size and shape of the material are kept, and the complex forming of the porous ceramic material is accurately controlled. And simultaneously, the invention selects the starch as a pore-forming agent, and the starch is removed in the sintering degreasing process, so that a microstructure with uniform pore size distribution, high porosity and adjustability is formed. Compared with other pore formers, the adoption of the starch as the pore former has three advantages, namely, compared with other organic polymers, the chemical purity of the starch is relatively high, generally only C, H, O (a small amount of trace elements) elements are contained, and residual byproducts are not generated after sintering; secondly, the grain sizes of different types of starch are different, and the size and shape of the hole can be controlled by selecting different types of starch. Thirdly, the color of the starch is lighter, the influence on the light transmittance of the photosensitive paste is small, and the photo-curing molding is easy. Compared with the traditional die casting molding and direct writing type 3D printing molding, the method can prepare the porous alumina ceramic material with complex shape, and the photo-curing molding has the advantages of high molding efficiency, high molding resolution, high molding speed, high resolution and the like.
The porosity of the porous alumina ceramic material prepared by the method can be adjusted by the sintering temperature and the starch adding amount, the porosity of the porous ceramic material prepared by the existing precision forming technology is more than 45-60%, and the porosity of the sample prepared by the method can be adjusted between 45-80%. The porous alumina prepared by the invention has the advantages of high strength and hardness, strong dimensional stability, high wear resistance, corrosion resistance, high temperature resistance, oxidation resistance, small thermal expansion coefficient and the like, and has wide development prospect in the fields of automobile industry, catalyst loading, gas/liquid filters and the like, porous sound absorption materials, phase change packaging materials and the like.
Meanwhile, the photosensitive paste disclosed by the invention mainly comprises the following raw materials: starch, alumina powder, PEG400DA and water, low cost, simple mixing formula, easy industrial production, long quality guarantee period of the photosensitive slurry obtained by mixing, and rapid prototyping by photo-curing, and can be used for preparing porous alumina ceramic materials with complex shapes on a large scale.
Drawings
Fig. 1 shows an optical photograph of a ceramic green body prepared by 3D printing and a ceramic block after sintering treatment.
Fig. 2 shows graphs of bulk density and open porosity of the alumina prepared in examples 1, 2, 3 of the present invention.
Fig. 3 shows graphs of bulk density and open porosity of the aluminas prepared in examples 2, 4, 5, 6, 7 of the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings and the following embodiments, it being understood that the drawings and the following embodiments are only for the purpose of illustrating the invention, not for limiting the same.
Example 1
A method for preparing a porous ceramic block based on 3D printing of water-based slurry, which comprises the following steps:
(a) A preparation method of photosensitive slurry comprises the following components in parts by weight: 55 parts of graded alumina powder (wherein 0.2 μm alumina 300 parts, 1-3 μm alumina 700 parts), 18 parts of PEG400DA,2 parts of glycerol as a dispersant, 1 part of photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, 24 parts of water;
(b) Ball milling and mixing the raw materials in the step (a), wherein the conditions are as follows: the rotation speed is 150 rpm, the ball milling time is 4 hours, and the photosensitive slurry which is evenly mixed and has moderate viscosity is obtained;
(c) Curing and forming the slurry in the step (b) by adopting a 3D ceramic printer to prepare a ceramic green body with a complex shape;
the parameters of the printer in step (c) are set as follows: the layer thickness is 40 mu m, the release speed is 1.2mm/s, the curing time of the first layer and the curing time are 40000ms and 8000ms respectively, the curing light intensity is 60%, and the scraper speed is 10mm/s.
(d) And (3) placing the ceramic green body in a tubular furnace for degreasing and sintering to finally obtain the porous alumina ceramic.
The degreasing conditions in the step (d) are as follows: the temperature rise rate of 2 ℃/min is raised to 650 ℃, and the heat preservation time is 1 hour.
The sintering conditions in step (d) are: the temperature rise rate of 5 ℃/min is raised to 1300 ℃, and the heat preservation time is 2 hours.
Example 2
A method for preparing a porous ceramic block based on 3D printing of water-based slurry, which comprises the following steps:
(a) A preparation method of photosensitive slurry comprises the following components in parts by weight: 36.6 parts of graded alumina powder (wherein 0.2 μm alumina 300 parts, 1-3 μm alumina 700 parts), 18 parts of PEG400DA,2 parts of glycerol as dispersant, 1 part of photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, 24 parts of water, 18.3 parts of starch;
(b) Ball milling and mixing the raw materials in the step (a), wherein the conditions are as follows: the rotation speed is 150 rpm, the ball milling time is 4 hours, and the photosensitive slurry which is evenly mixed and has moderate viscosity is obtained;
(c) Curing and forming the slurry in the step (b) by adopting a 3D ceramic printer to prepare a ceramic green body with a complex shape;
the parameters of the printer in step (c) are set as follows: the layer thickness is 40 mu m, the release speed is 1.2mm/s, the curing time of the first layer and the curing time are 40000ms and 8000ms respectively, the curing light intensity is 60%, and the scraper speed is 10mm/s.
(d) And (3) placing the ceramic green body in a tubular furnace for degreasing and sintering to finally obtain the porous alumina ceramic.
The degreasing conditions in the step (d) are as follows: the temperature rise rate of 2 ℃/min is raised to 650 ℃, and the heat preservation time is 1 hour.
The sintering conditions in step (d) are: the temperature rise rate of 5 ℃/min is raised to 1300 ℃, and the heat preservation time is 2 hours.
Example 3
A method for preparing a porous ceramic block based on 3D printing of water-based slurry, which comprises the following steps:
(a) A preparation method of photosensitive slurry comprises the following components in parts by weight: 27.5 parts of graded alumina powder (wherein 0.2 μm alumina 300 parts, 1-3 μm alumina 700 parts, 18 parts PEG400DA,2 parts glycerol as dispersant, 1 part photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, 24 parts water, 27.5 parts starch;
(b) Ball milling and mixing the raw materials in the step (a), wherein the conditions are as follows: the rotation speed is 150 rpm, the ball milling time is 4 hours, and the photosensitive slurry which is evenly mixed and has moderate viscosity is obtained;
(c) Curing and forming the slurry in the step (b) by adopting a 3D ceramic printer to prepare a ceramic green body with a complex shape;
the parameters of the printer in step (c) are set as follows: the layer thickness is 40 mu m, the release speed is 1.2mm/s, the curing time of the first layer and the curing time are 40000ms and 8000ms respectively, the curing light intensity is 60%, and the scraper speed is 10mm/s.
(d) And (3) placing the ceramic green body in a tubular furnace for degreasing and sintering to finally obtain the porous alumina ceramic.
The degreasing conditions in the step (d) are as follows: the temperature rise rate of 2 ℃/min is raised to 650 ℃, and the heat preservation time is 1 hour.
The sintering conditions in step (d) are: the temperature rise rate of 5 ℃/min is raised to 1300 ℃, and the heat preservation time is 2 hours.
Example 4
A method for preparing a porous ceramic block based on 3D printing of water-based slurry, which comprises the following steps:
(a) A preparation method of photosensitive slurry comprises the following components in parts by weight: 36.6 parts of a graded alumina powder (wherein 0.2 μm alumina 300 parts, 1-3 μm alumina 700 parts), 18 parts of PEG400DA,2 parts of glycerol as dispersant, 1 part of photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, 24 parts of water, 18.3 parts of starch.
(b) Ball milling and mixing the raw materials in the step (a), wherein the conditions are as follows: the rotation speed is 150 rpm, the ball milling time is 4 hours, and the photosensitive slurry which is evenly mixed and has moderate viscosity is obtained;
(c) Curing and forming the slurry in the step (b) by adopting a 3D ceramic printer to prepare a ceramic green body with a complex shape;
the parameters of the printer in step (c) are set as follows: the layer thickness is 40 mu m, the release speed is 1.2mm/s, the curing time of the first layer and the curing time are 40000ms and 8000ms respectively, the curing light intensity is 60%, and the scraper speed is 10mm/s.
(d) And (3) placing the ceramic green body in a tubular furnace for degreasing and sintering to finally obtain the porous alumina ceramic.
The degreasing conditions in the step (d) are as follows: the temperature rise rate of 2 ℃/min is raised to 650 ℃, and the heat preservation time is 1 hour.
The sintering conditions in step (d) are: the temperature rise rate of 5 ℃/min is raised to 1200 ℃, and the heat preservation time is 2 hours.
Example 5
A method for preparing a porous ceramic block based on 3D printing of water-based slurry, which comprises the following steps:
(a) A preparation method of photosensitive slurry comprises the following components in parts by weight: 36.6 parts of graded alumina powder (wherein 0.2 μm alumina 300 parts, 1-3 μm alumina 700 parts), 18 parts of PEG400DA,2 parts of glycerol as dispersant, 1 part of photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, 24 parts of water, 18.3 parts of starch;
(b) Ball milling and mixing the raw materials in the step (a), wherein the conditions are as follows: the rotation speed is 150 rpm, the ball milling time is 4 hours, and the photosensitive slurry which is evenly mixed and has moderate viscosity is obtained;
(c) Curing and forming the slurry in the step (b) by adopting a 3D ceramic printer to prepare a ceramic green body with a complex shape;
the parameters of the printer in step (c) are set as follows: the layer thickness is 40 mu m, the release speed is 1.2mm/s, the curing time of the first layer and the curing time are 40000ms and 8000ms respectively, the curing light intensity is 60%, and the scraper speed is 10mm/s.
(d) And (3) placing the ceramic green body in a tubular furnace for degreasing and sintering to finally obtain the porous alumina ceramic.
The degreasing conditions in the step (d) are as follows: the temperature rise rate of 2 ℃/min is raised to 650 ℃, and the heat preservation time is 1 hour.
The sintering conditions in step (d) are: the temperature rise rate of 5 ℃/min is raised to 1400 ℃, and the heat preservation time is 2 hours.
Example 6
A method for preparing a porous ceramic block based on 3D printing of water-based slurry, which comprises the following steps:
(a) A preparation method of photosensitive slurry comprises the following components in parts by weight: 36.6 parts of graded alumina powder (wherein 0.2 μm alumina 300 parts, 1-3 μm alumina 700 parts), 18 parts of PEG400DA,2 parts of glycerol as dispersant, 1 part of photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, 24 parts of water, 18.3 parts of starch;
(b) Ball milling and mixing the raw materials in the step (a), wherein the conditions are as follows: the rotation speed is 150 rpm, the ball milling time is 4 hours, and the photosensitive slurry which is evenly mixed and has moderate viscosity is obtained;
(c) Curing and forming the slurry in the step (b) by adopting a 3D ceramic printer to prepare a ceramic green body with a complex shape;
the parameters of the printer in step (c) are set as follows: the layer thickness is 40 mu m, the release speed is 1.2mm/s, the curing time of the first layer and the curing time are 40000ms and 8000ms respectively, the curing light intensity is 60%, and the scraper speed is 10mm/s.
(d) And (3) placing the ceramic green body in a tubular furnace for degreasing and sintering to finally obtain the porous alumina ceramic.
The degreasing conditions in the step (d) are as follows: the temperature rise rate of 2 ℃/min is raised to 650 ℃, and the heat preservation time is 1 hour.
The sintering conditions in step (d) are: the temperature rise rate of 5 ℃/min is raised to 1500 ℃, and the heat preservation time is 2 hours.
Example 7
A method for preparing a porous ceramic block based on 3D printing of water-based slurry, which comprises the following steps:
(a) A preparation method of photosensitive slurry comprises the following components in parts by weight: 36.6 parts of a graded alumina powder (wherein 0.2 μm alumina 300 parts, 1-3 μm alumina 700 parts), 18 parts of PEG400DA,2 parts of glycerol as dispersant, 1 part of photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, 24 parts of water, 18.3 parts of starch.
(b) Ball milling and mixing the raw materials in the step (a), wherein the conditions are as follows: the rotation speed is 150 rpm, the ball milling time is 4 hours, and the photosensitive slurry which is evenly mixed and has moderate viscosity is obtained;
(c) Curing and forming the slurry in the step (b) by adopting a 3D ceramic printer to prepare a ceramic green body with a complex shape;
the parameters of the printer in step (c) are set as follows: the layer thickness is 40 mu m, the release speed is 1.2mm/s, the curing time of the first layer and the curing time are 40000ms and 8000ms respectively, the curing light intensity is 60%, and the scraper speed is 10mm/s.
(d) And (3) placing the ceramic green body in a tubular furnace for degreasing and sintering to finally obtain the porous alumina ceramic.
The degreasing conditions in the step (d) are as follows: the temperature rise rate of 2 ℃/min is raised to 650 ℃, and the heat preservation time is 1 hour.
The sintering conditions in step (d) are: the temperature rise rate of 5 ℃/min is raised to 1600 ℃, and the heat preservation time is 2 hours.
Claims (3)
1. A method for preparing a porous ceramic block based on 3D printing of water-based slurry is characterized in that,
1) The ingredients comprise: 25-55 parts of graded alumina powder, 0-55 parts of starch, 15-25 parts of binder, 1-2 parts of photoinitiator, 1-4 parts of dispersing agent and 20-35 parts of solvent;
2) The mixing mode is as follows: ball-milling and mixing graded alumina powder, starch, a binder, a photoinitiator, a dispersing agent and a solvent to obtain photosensitive slurry;
3) Curing and forming the photosensitive slurry obtained in the step 2) by adopting a 3D ceramic printer to obtain a ceramic green body;
4) Placing the ceramic green body in a tubular furnace for degreasing and sintering to finally obtain porous alumina ceramic;
in the step 1), the binder is PEG400DA, the dispersing agent is glycerol, and the solvent is water; the photoinitiator is 2-hydroxy-2-methyl-1-phenyl-1-acetone;
in the step 1), the size grading of the graded alumina powder is specifically as follows: 200-400 parts of 0.2 mu m alumina, 600-800 parts of 1-3 mu m alumina;
in the step 4), the degreasing process is heated to 200-650 ℃ at a heating rate of 0.5-2 ℃/min, and the temperature is kept for 1-3 hours.
2. The method for preparing a porous ceramic block based on 3D printing of water-based slurry according to claim 1, wherein in step 2), the rotational speed of the ball mill mixing is 150-200 rpm, and the ball milling time is 2-4 hours.
3. The method for preparing a porous ceramic block based on 3D printing of water-based slurry according to claim 1, wherein in step 4), the sintering process is heated to 650-1300 ℃ at a heating rate of 3-5 ℃/min for 2-6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210459889.4A CN114933486B (en) | 2022-04-28 | 2022-04-28 | Method for preparing porous ceramic block body based on water-based slurry through 3D printing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202210459889.4A CN114933486B (en) | 2022-04-28 | 2022-04-28 | Method for preparing porous ceramic block body based on water-based slurry through 3D printing |
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| CN103342544A (en) * | 2013-07-03 | 2013-10-09 | 镇江市江南矿山机电设备有限公司 | Method for preparing porous alumina ceramic |
| CN106747360A (en) * | 2017-01-18 | 2017-05-31 | 武汉纺织大学 | A kind of preparation method of 3D printing photocuring ceramic size |
| CN109485395A (en) * | 2018-01-15 | 2019-03-19 | 杭州创屹机电科技有限公司 | A kind of method of 3D printing high-strength ceramic mold |
| CN108178659B (en) * | 2018-02-05 | 2021-01-15 | 郑州大学 | Molding material for 3D printing |
| CN112390626A (en) * | 2019-08-16 | 2021-02-23 | 上海魅湃实业有限公司 | Preparation of ceramic slurry for 3D printing and 3D printing photocuring forming method thereof |
| CN110950651A (en) * | 2019-11-26 | 2020-04-03 | 兰州大学 | Method for preparing multi-stage porous ceramic based on ink direct writing 3D printing technology |
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