CN108503365B - Silicon carbide ceramic based on photocuring technology and preparation method thereof - Google Patents
Silicon carbide ceramic based on photocuring technology and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of 3D printing, discloses a silicon carbide ceramic based on a photocuring technology and a preparation method thereof, and solves the problem that a silicon carbide part with a complex shape cannot be prepared by the conventional process at present. The method comprises the following steps: mixing and stirring the premixed liquid, the photoinitiator, the dispersant, the sintering aid and the silicon carbide powder uniformly, and performing ball milling to obtain silicon carbide slurry; taking out the ball-milled slurry, placing the ball-milled slurry on a tray of a 3D printer, obtaining required sample parameters through digital modeling, and then carrying out photocuring treatment on the ceramic slurry by using ultraviolet light; degreasing and sintering the cured ceramic-based blank to obtain the silicon carbide ceramic. The invention has the advantages of simple preparation process, controllable process, convenient adjustment of material system, direct manufacture of ceramics by photocuring and suitability for batch production; the method is suitable for preparing the carbide ceramic parts and the carbide ceramic matrix composite materials with complex shapes.
Description
Technical Field
The invention belongs to the technical field of 3D printing, and particularly relates to a silicon carbide ceramic based on a photocuring technology and a preparation method thereof.
Background
Silicon carbide has the characteristics of stable chemical property, high thermal conductivity, small thermal expansion coefficient, small density, good wear resistance, high hardness, high mechanical strength, chemical corrosion resistance and the like, and is rapidly developed in the field of materials. The silicon carbide ceramic has the characteristics of low density, small thermal expansion coefficient, high hardness, high temperature resistance, large elastic modulus, corrosion resistance and the like, and is widely applied to the fields of ceramic ball bearings, valves, semiconductor materials, gyroscopes, measuring instruments, aerospace and the like. The silicon carbide parts manufactured by the traditional process are difficult in post-processing process, have high dependence on a die, are difficult to demould, are easy to crack and deform, cause material waste and have low utilization rate. The silicon carbide parts with complex shapes are manufactured by utilizing one of the 3D printing technologies, the material waste can be avoided by the additive manufacturing, and the utilization rate of the silicon carbide parts is improved.
Disclosure of Invention
In order to overcome the defects that the forming method of the silicon carbide ceramic in the prior art has large dependence on a mould and cannot prepare a complex precise structure, the invention mainly aims to provide the silicon carbide ceramic based on the photocuring technology.
The invention also aims to provide a preparation method of the silicon carbide ceramic based on the photocuring technology.
The purpose of the invention is realized by the following technical scheme:
a preparation method of silicon carbide ceramic based on photocuring technology comprises the following steps:
(1) preparing slurry: mixing the premix liquid, the photoinitiator, the dispersant and amorphous silicon dioxide as a sintering aid to obtain a premix, mixing 30-50% of the premix with 50-70% of silicon carbide powder by mass, uniformly stirring, ultrasonically dispersing for 5-10 minutes, and ball milling to obtain silicon carbide slurry;
(2) molding: curing and molding the slurry obtained in the step (1) on a 3D printer platform to obtain a blank body;
(3) and (3) post-treatment: and (3) sequentially curing, drying, degreasing and sintering the blank obtained in the step (2) to obtain the silicon carbide ceramic.
The components of the premix liquid in the step (1) comprise 25-35% of acrylate, 30-40% of n-octanol and 35-45% of polyethylene glycol by mass; the using amount of the photoinitiator is 3% of the mass of the acrylate; the using amount of the dispersing agent is 3% of the mass of the silicon carbide powder; the amorphous silicon dioxide is used in an amount of 2% by mass of the silicon carbide powder.
Preferably, the components of the premix liquid comprise 30 mass percent of acrylate, 35 mass percent of n-octanol and 35 mass percent of polyethylene glycol.
The photoinitiator in the step (1) is more than one of 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxycyclohexyl phenyl ketone and phenyl bis (2,4, 6-trimethyl benzoyl) phosphine oxide; the dispersing agent is more than one of BYK-9076, BYK-163, BYK-9076 and BYK-9077.
When the silicon carbide powder in the step (1) is silicon carbide powder with the particle size of less than or equal to 1 mu m, the silicon carbide powder is directly used for preparing silicon carbide slurry, and the solid phase content of ceramic particles in the prepared silicon carbide slurry reaches 45 percent by mass percent;
when the silicon carbide powder in the step (1) is silicon carbide powder with the particle size larger than 1 mu m, ball milling is firstly adopted to break up the agglomeration to obtain oxidized silicon carbide powder, and the oxidized silicon carbide powder is then used for preparing silicon carbide slurry, wherein the solid phase content of ceramic particles in the prepared silicon carbide slurry reaches 70 percent by mass.
The ball milling in the step (1) is carried out at the rotating speed of 250-.
In the curing and forming process in the step (2), the exposure time of the base layer is 30-60 s, the number of layers of the base layer is 8-10, the single-layer printing time is 15-30 s, the single-layer thickness is 20-50 mu m, and the exposure is 220-768J/cm2The wavelength is 287-405 nm.
Curing and drying the blank body treated by ultraviolet light for 10-24 hours, and performing vacuum degreasing and air degreasing on the dried blank body; and the sintering method comprises the steps of heating the degreased blank, preserving heat, and cooling after heat preservation to obtain the silicon carbide ceramic.
The vacuum degreasing method comprises the following steps: heating to 400-750 ℃ at the speed of 1-5 ℃/min, preserving heat for 3-5 h, preserving heat for 30-60 min every 100 ℃ in the heating process, and cooling to room temperature;
the air degreasing method comprises the following steps: heating to 600-900 ℃ at the speed of 1-5 ℃/min, preserving heat for 3-5 h, and cooling to room temperature;
the sintering method comprises the steps of heating the degreased blank to 1950 ℃ at the speed of 5-10 ℃/min, preserving heat for 1-2 hours, and cooling after heat preservation to obtain silicon carbide ceramic; the sintering mode is hot-pressing sintering or atmosphere sintering.
The silicon carbide ceramic prepared by the preparation method is based on the photocuring technology.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention solves the problem that the traditional technology can not prepare hard and brittle ceramic parts with complex shapes and difficult processing in one step.
(2) The invention has the advantages of simple preparation process, controllable process, convenient adjustment of material system, capability of manufacturing layered ceramics and gradient ceramics, suitability for batch production and suitability for preparing the existing carbide ceramics.
Detailed Description
The present invention is further illustrated by the following specific examples in combination, but should not be construed as limiting the scope of the invention, and it is within the scope of the invention that one skilled in the art may make insubstantial changes and modifications from the above disclosure.
Example 1
(1) Preparing slurry: mixing the premixed liquid, the photoinitiator (2-hydroxy-2-methyl-1-phenyl-1-acetone), the dispersant BYK-9076 and the amorphous silicon dioxide as the sintering aid to obtain a premix, mixing the premix with the mass fraction of 50% with silicon carbide powder (the silicon carbide powder with the particle size of less than or equal to 1 mu m) with the mass fraction of 50%, and uniformly stirring; the components of the premix liquid comprise 30 mass percent of acrylic ester, 35 mass percent of n-octanol and 35 mass percent of polyethylene glycol; the using amount of the photoinitiator is 3% of the mass of the acrylate; the using amount of the dispersing agent is 3% of the mass of the silicon carbide powder; the amount of the amorphous silicon dioxide is 2% of the mass of the silicon carbide powder;
(2) putting the uniformly stirred ceramic slurry into an ultrasonic dispersion machine for ultrasonic dispersion for 5 minutes, then putting the ceramic slurry subjected to ultrasonic dispersion into a plastic tank, and carrying out ball milling (the ball milling medium is tungsten carbide or zirconium oxide) at the rotating speed of 400r/min for 1.5 hours to obtain slurry;
(3) molding: curing and molding the slurry obtained in the step (2) on a 3D printer platform to obtain a blank body; in the curing and forming process, the exposure time of the base layer is 30s, the number of the base layer is 8, the single-layer printing time is 15s, the single-layer thickness is 20 mu m, and the exposure amount is 220J/cm2The wavelength is 405 nm;
(4) and (3) post-treatment: curing and drying the blank obtained in the step (3) for 18h by ultraviolet light treatment; and (3) carrying out vacuum degreasing on the dried blank: heating to 400 ℃ at the speed of 1-5 ℃/min, preserving heat for 5h, preserving heat for 30min every 100 ℃ in the heating process, and cooling to room temperature; and then carrying out air degreasing: heating to 600 ℃ at the speed of 1-5 ℃/min, preserving the heat for 5 hours, and cooling to room temperature; and heating the degreased blank to 1950 ℃ at the speed of 5-10 ℃/min, preserving the temperature for 2 hours, and cooling after the heat preservation is finished to obtain the silicon carbide ceramic.
Example 2
The difference between the embodiment and the embodiment 1 is that the components of the premix liquid in the step (1) comprise 25 mass percent of acrylate, 30 mass percent of n-octanol and 45 mass percent of polyethylene glycol; other steps and parameters are the same as in the example.
Example 3
The difference between the embodiment and the embodiment 1 is that the components of the premix in the step (1) comprise 35% by mass of acrylic ester, 30% by mass of n-octanol and 35% by mass of polyethylene glycol; other steps and parameters are the same as in the example.
Example 4
The difference between the present embodiment and embodiment 1 is that the ultrasonic dispersion time in step (2) is 10 minutes; the rotation speed of the ball milling is 350r/min, and the ball milling time is 2 h; other steps and parameters are the same as in the example.
Example 5
The difference between the present example and example 1 is that the time for ultrasonic dispersion in step (2) is 8 minutes; the rotation speed of the ball milling is 380r/min, and the ball milling time is 1.8 h; other steps and parameters are the same as in the example.
Example 6
The difference between the embodiment and the embodiment 1 is that the exposure time of the base layer in the step (3) is 30-60 s, the number of the base layer is 8-10, the single-layer printing time is 15-30 s, the single-layer thickness is 20-50 μm, and the exposure amount is 220-768J/cm2The wavelength is 287-405 nm; other steps and parameters are the same as in the example.
Example 7
This example is different from example 1 in that the base layer exposure time in the step (3) is 60s, the number of the basic layers is 10, the single-layer printing time is 30s, the single-layer thickness is 50 mu m, and the exposure is 768J/cm2The wavelength is 287 nm; other steps and parameters are the same as in the example.
Example 8
This example is different from example 1 in that the exposure time of the foundation layer in the step (3) was 50 seconds, the number of layers of the foundation layer was 9, the printing time of the single layer was 25 seconds, the thickness of the single layer was 30 μm, and the exposure amount was 550J/cm2The wavelength is 300 nm; other steps and parameters are the same as in the example.
Example 9
The difference between the embodiment and the embodiment 1 is that the green body in the step (4) is cured and dried by ultraviolet light treatment for 10 hours; other steps and parameters are the same as in the example.
Example 10
The difference between the embodiment and the embodiment 1 is that the green body in the step (4) is cured and dried by ultraviolet light treatment for 24 hours; other steps and parameters are the same as in the example.
Example 11
The difference between the embodiment and the embodiment 1 is that in the step (4), the temperature is raised to 750 ℃ at a rate of 1-5 ℃/min and is kept for 3 hours, and the temperature is kept for 60 minutes every 100 ℃ in the temperature raising process; other steps and parameters are the same as in the example.
Example 12
The difference between the embodiment and the embodiment 1 is that in the step (4), the vacuum degreasing is performed by heating to 500 ℃ at a rate of 1-5 ℃/min and keeping the temperature for 4 hours, and the temperature is kept for 50 minutes every 100 ℃ in the heating process; other steps and parameters are the same as in the example.
Example 13
The difference between the embodiment and the embodiment 1 is that the air degreasing in the step (4) is carried out by heating to 900 ℃ at the speed of 1-5 ℃/min and keeping the temperature for 3 h; other steps and parameters are the same as in the example.
Example 14
The difference between the embodiment and the embodiment 1 is that the air degreasing in the step (4) is carried out by heating to 800 ℃ at the speed of 1-5 ℃/min and keeping the temperature for 4 h; other steps and parameters are the same as in the example.
Example 15
The difference between the embodiment and the embodiment 1 is that in the step (4), the degreased blank is heated to 1950 ℃ at the speed of 5-10 ℃/min and is kept warm for 1 h; other steps and parameters are the same as in the example.
Example 16
The difference between the embodiment and embodiment 1 is that the particle size of the silicon carbide powder in step (1) is larger than 1 μm, the silicon carbide powder is ball-milled to break up agglomerates before use, oxidized silicon carbide powder is obtained, and then the silicon carbide powder is mixed with other raw materials, and the use amount of each raw material is adjusted, so that the solid phase content of ceramic particles in the silicon carbide slurry reaches 70% by mass percent; other steps and parameters are the same as in the example.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A preparation method of silicon carbide ceramic based on photocuring technology is characterized by comprising the following steps:
(1) preparing slurry: mixing the premix liquid, the photoinitiator, the dispersant and amorphous silicon dioxide as a sintering aid to obtain a premix, mixing 30-50% of the premix with 50-70% of silicon carbide powder by mass, uniformly stirring, ultrasonically dispersing for 5-10 minutes, and ball milling to obtain silicon carbide slurry; the components of the premix liquid comprise 25 to 35 mass percent of acrylate, 30 to 40 mass percent of n-octanol and 35 to 45 mass percent of polyethylene glycol;
when the silicon carbide powder in the step (1) is silicon carbide powder with the particle size of less than or equal to 1 mu m, the silicon carbide powder is directly used for preparing silicon carbide slurry, and the solid phase content of ceramic particles in the prepared silicon carbide slurry reaches 45 percent by mass percent;
when the silicon carbide powder in the step (1) is silicon carbide powder with the particle size larger than 1 mu m, ball milling is firstly adopted to break up the agglomeration to obtain oxidized silicon carbide powder, and the oxidized silicon carbide powder is then used for preparing silicon carbide slurry, wherein the solid phase content of ceramic particles in the prepared silicon carbide slurry reaches 70 percent by mass;
(2) molding: curing and molding the slurry obtained in the step (1) on a 3D printer platform to obtain a blank body;
(3) and (3) post-treatment: curing and drying the blank obtained in the step (2) by ultraviolet light treatment for 10-24 h, and performing vacuum degreasing and air degreasing on the dried blank; sintering the degreased blank to obtain silicon carbide ceramic; the sintering mode is hot-pressing sintering or atmosphere sintering.
2. The method of claim 1, wherein: the using amount of the photoinitiator in the step (1) is 3% of the mass of the acrylate; the using amount of the dispersing agent is 3% of the mass of the silicon carbide powder; the amorphous silicon dioxide is used in an amount of 2% by mass of the silicon carbide powder.
3. The method of claim 1, wherein: the components of the premix liquid comprise 30 mass percent of acrylic ester, 35 mass percent of n-octanol and 35 mass percent of polyethylene glycol.
4. The method of claim 1, wherein: the photoinitiator in the step (1) is more than one of 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxycyclohexyl phenyl ketone and phenyl bis (2,4, 6-trimethyl benzoyl) phosphine oxide; the dispersing agent is more than one of BYK-9076, BYK-163 and BYK-9077.
5. The method of claim 1, wherein: the ball milling in the step (1) is carried out at the rotating speed of 250-.
6. According to claim 1The preparation method is characterized by comprising the following steps: in the curing and forming process in the step (2), the exposure time of the base layer is 30-60 s, the number of layers of the base layer is 8-10, the single-layer printing time is 15-30 s, the single-layer thickness is 20-50 mu m, and the exposure is 220-768J/cm2The wavelength is 287-405 nm.
7. The method of claim 1, wherein: and (3) heating the degreased blank, preserving heat, and cooling to obtain the silicon carbide ceramic.
8. The production method according to claim 1 or 7, characterized in that: the vacuum degreasing method comprises the following steps: heating to 400-750 ℃ at the speed of 1-5 ℃/min, preserving heat for 3-5 h, preserving heat for 30-60 min every 100 ℃ in the heating process, and cooling to room temperature;
the air degreasing method comprises the following steps: heating to 600-900 ℃ at the speed of 1-5 ℃/min, preserving heat for 3-5 h, and cooling to room temperature;
the sintering method comprises the steps of heating the degreased blank to 1950 ℃ at the speed of 5-10 ℃/min, preserving heat for 1-2 hours, and cooling after heat preservation to obtain the silicon carbide ceramic.
9. A silicon carbide ceramic based on photocuring technology, which is produced by the production method according to any one of claims 1 to 8.
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| CN110395986A (en) * | 2019-08-05 | 2019-11-01 | 上海应用技术大学 | A kind of method of long wavelength laser printed material |
| CN112171848A (en) * | 2020-09-29 | 2021-01-05 | 江西金石三维智能制造科技有限公司 | Photocuring silicon carbide ceramic slurry and preparation method and application thereof |
| CN115215661B (en) * | 2021-04-15 | 2023-06-20 | 南京航空航天大学 | Photo-curing 3D printing silicon carbide ceramic component and near-net forming 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 |
| CN115180955A (en) * | 2021-10-19 | 2022-10-14 | 中国科学院沈阳自动化研究所 | Silicon carbide ceramic slurry, preparation method thereof and pyrolysis process of photocuring formed body |
| CN115010498A (en) * | 2022-06-15 | 2022-09-06 | 西安铂力特增材技术股份有限公司 | Forming method of SiC complex component |
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