CN113880559A - Preparation method of hard-to-cure ceramic based on photocuring forming and product - Google Patents
Preparation method of hard-to-cure ceramic based on photocuring forming and product Download PDFInfo
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- CN113880559A CN113880559A CN202111271406.XA CN202111271406A CN113880559A CN 113880559 A CN113880559 A CN 113880559A CN 202111271406 A CN202111271406 A CN 202111271406A CN 113880559 A CN113880559 A CN 113880559A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 120
- 238000000016 photochemical curing Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 42
- 239000002002 slurry Substances 0.000 claims abstract description 38
- 239000004005 microsphere Substances 0.000 claims abstract description 29
- 229920000642 polymer Polymers 0.000 claims abstract description 22
- 239000002131 composite material Substances 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 17
- 238000002835 absorbance Methods 0.000 claims abstract description 16
- 239000011347 resin Substances 0.000 claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- 235000015895 biscuits Nutrition 0.000 claims abstract description 14
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 13
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052451 lead zirconate titanate Inorganic materials 0.000 claims abstract description 12
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 9
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000011230 binding agent Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 32
- 238000001816 cooling Methods 0.000 claims description 16
- 239000003999 initiator Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical group CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 claims description 9
- GTELLNMUWNJXMQ-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical class OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCC(CO)(CO)CO GTELLNMUWNJXMQ-UHFFFAOYSA-N 0.000 claims description 8
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 7
- ZDQNWDNMNKSMHI-UHFFFAOYSA-N 1-[2-(2-prop-2-enoyloxypropoxy)propoxy]propan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COCC(C)OC(=O)C=C ZDQNWDNMNKSMHI-UHFFFAOYSA-N 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 6
- 239000004793 Polystyrene Substances 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- -1 polyethylene Polymers 0.000 claims description 6
- VAZQKPWSBFZARZ-UHFFFAOYSA-N 2-(2-phenylphenoxy)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC1=CC=CC=C1C1=CC=CC=C1 VAZQKPWSBFZARZ-UHFFFAOYSA-N 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920002223 polystyrene Polymers 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 4
- 238000005303 weighing Methods 0.000 description 8
- 238000001723 curing Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003462 bioceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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Abstract
The invention belongs to the related technical field of photocuring forming, and discloses a preparation method of a photocuring forming-based hard-to-cure ceramic and a product. The method comprises the following steps: s1, selecting photosensitive resin, polyethylene glycol, a dispersing agent and a photoinitiator, mixing to form a uniformly mixed solution, adding ceramic powder into the mixed solution, and stirring to obtain ceramic slurry; s2, adding polymer microspheres with low absorbance and refractive index into the ceramic slurry, and carrying out vacuum stirring and defoaming treatment to obtain composite ceramic slurry with uniform components; s3, presetting technological parameters of photocuring forming, using the composite ceramic slurry to awaken photocuring forming to obtain a ceramic biscuit, and carrying out binder removal and reactive sintering treatment on the ceramic biscuit so as to obtain the required high-performance ceramic part. The invention solves the difficult problems of photocuring manufacturing of ceramic powder such as silicon carbide, silicon nitride, barium titanate, lead zirconate titanate and the like with high refractive index and high absorbance, and greatly expands the photocuring forming material system.
Description
Technical Field
The invention belongs to the related technical field of photocuring forming, and particularly relates to a preparation method of a hard-to-cure ceramic based on photocuring forming and a product.
Background
The high-performance ceramic has the characteristics of high strength, high hardness, high temperature resistance, corrosion resistance, good thermal, optical, electrical and the like, and is widely applied to the fields of aerospace, biomedical, electronics, machinery, energy and the like. At present, the traditional ceramic forming method depends on a mould too much, so that the defects of long development period, high cost and the like exist, the high-performance ceramic part with a complex structure is difficult to prepare, and the application and development of the high-performance ceramic part are severely limited.
The ceramic photocuring forming technology has high forming precision and surface quality, can form a specific complex structure, and opens up a new path for preparing high-performance ceramic. However, this technique is greatly limited by the printing material system, and mainly focuses on the preparation of bioceramics and structural ceramics, and for ceramic powders such as silicon carbide, silicon nitride, barium titanate, lead zirconate titanate, etc., the single-layer curing thickness of the ceramic slurry is very low due to the high ultraviolet light absorption rate, strong scattering effect, large difference in refractive index with photosensitive resin, etc., and thus it is difficult to form the ceramic powder by the photo-curing forming technique.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides a preparation method and a product of photocuring forming-based hard-to-cure ceramic, which solve the photocuring manufacturing problems of high refractive index and high absorbance of ceramic powder such as silicon carbide, silicon nitride, barium titanate, lead zirconate titanate and the like, and greatly expand a photocuring forming material system.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for preparing a hard-to-cure ceramic based on photocuring forming, the method comprising the steps of:
s1, selecting photosensitive resin, polyethylene glycol, a dispersing agent and a photoinitiator, mixing to form a uniformly mixed solution, adding ceramic powder into the mixed solution, and stirring to obtain ceramic slurry;
s2, adding polymer microspheres with low absorbance and refractive index into the ceramic slurry, and carrying out vacuum stirring and defoaming treatment to obtain composite ceramic slurry with uniform components;
s3, presetting technological parameters of photocuring forming, using the composite ceramic slurry to awaken photocuring forming to obtain a ceramic biscuit, and carrying out binder removal and reactive sintering treatment on the ceramic biscuit so as to obtain the required high-performance ceramic part.
Further preferably, in step S1, the ceramic powder is one or more of silicon carbide, silicon nitride, barium titanate, lead zirconate titanate, alumina, zirconia, silica, and the like, and has a particle size of submicron or micron.
Further preferably, in step S2, the polymer microspheres are one or more of polymethyl methacrylate, polyethylene, polystyrene and polypropylene.
Further preferably, the volume ratio of the polymer microspheres to the ceramic powder is 1: 4-7: 3.
Further preferably, in step S1, the photosensitive resin is one or more of o-phenylphenoxyethyl acrylate, 1, 6-hexanediol diacrylate, tripropylene glycol diacrylate, and ethoxylated trimethylolpropane triacrylate.
Further preferably, in step S1, the mass ratio of the photosensitive resin to the polyethylene glycol is 9:1 to 4: 1.
Further preferably, in step S1, the photoinitiator is 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, and the mass of the initiator is 1% to 7% of the sum of the mass of the photosensitive resin and the mass of the polyethylene glycol.
Further preferably, in step S1, the mass of the dispersant is 1% to 6% of the total mass of the ceramic powder and the polymer microspheres.
Further preferably, in step S3, the glue discharging process is performed according to the following steps: heating the mixture from room temperature to 500-700 ℃ at a heating rate of 0.1-2 ℃/min, keeping the temperature for 1-3 h, and then cooling the mixture to room temperature along with the furnace; the sintering is carried out according to the following steps: heating from room temperature to 1100-2100 ℃ at 2-6 ℃/min, keeping the temperature for 2-4 h, and cooling to room temperature along with the furnace.
According to another aspect of the present invention, there is provided a ceramic part obtained by the above-mentioned production method.
Generally, compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1. one or more of oligomeric methyl methacrylate, polyethylene, polystyrene and polypropylene with the absorbance and the refractive index are selected, and the addition of the polymer microspheres reduces the absorption of ultraviolet light by the powder and the refractive index difference between the powder and photosensitive resin, so that the curing performance of the ceramic slurry can be improved; the functional ceramic with high impurity requirement is not influenced, and can be completely removed in the later glue discharging and sintering processes;
2. the volume ratio of the polymer microspheres to the ceramic powder is 1: 4-7: 3, because if the content of the polymer microspheres is too low, the effect of improving the curing performance of the ceramic slurry cannot be achieved, and photocuring forming cannot be achieved; if the content is too high, the viscosity of the ceramic slurry is sharply increased, and the probability of generating defects is increased;
3. the binder removal temperature is increased from room temperature to 500-700 ℃ at a heating rate of 0.1-2 ℃/min, because the heating rate can prevent deformation and cracking of a blank body, the temperature interval can also ensure complete discharge of organic matters, the sintering temperature is increased from room temperature to 1100-2100 ℃ at a heating rate of 2-6 ℃/min, because the heating rate can obtain ceramic parts with complete and flawless surfaces, and the temperature interval covers the sintering temperature range of each ceramic;
4. the amount of the photosensitive resin, the polyethylene glycol and the dispersant in the present invention is determined according to the properties of the ceramic powder and the total amount of the ceramic powder and the polymeric microspheres added, and is selected because it can ensure the fluidity of the ceramic slurry required for photocuring.
Drawings
FIG. 1 is a flow chart of a method for making a hard-to-cure ceramic based on photocuring profiling constructed in accordance with a preferred embodiment of the present invention;
FIG. 2 is a diagram of a lead zirconate titanate green body constructed in accordance with preferred embodiment 1 of the present invention;
FIG. 3 is a diagram of a barium titanate biscuit constructed in accordance with a preferred embodiment 2 of the present invention;
fig. 4 is a barium titanate ceramic part constructed in accordance with a preferred embodiment 6 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The preparation method of the hard-to-cure ceramic based on photocuring forming has strong universality, simple flow and short preparation period, can effectively solve the photocuring manufacturing problems of high refractive index and high absorbance of ceramic powder such as silicon carbide, silicon nitride, barium titanate, lead zirconate titanate and the like, and greatly expands a photocuring forming material system.
Specifically, as shown in fig. 1, the preparation method mainly comprises the following steps:
(1) uniformly mixing photosensitive resin, polyethylene glycol, a dispersant and a photoinitiator to prepare a mixed solution;
the photosensitive resin is one or more of o-phenylphenoxyethyl acrylate, 1, 6-hexanediol diacrylate, tripropylene glycol diacrylate and ethoxylated trimethylolpropane triacrylate. The mass ratio of the photosensitive resin to the polyethylene glycol is preferably 9: 1-4: 1, the photoinitiator is 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, the mass of the initiator is preferably 1-7% of the mass sum of the photosensitive resin and the polyethylene glycol, and the mass of the dispersant is preferably 1-6% of the mass of the composite ceramic powder.
(2) Adding the initial ceramic powder into the mixed solution, and performing vacuum stirring and defoaming treatment to obtain ceramic slurry with uniform components;
wherein, the initial ceramic powder is one or more of silicon carbide, silicon nitride, barium titanate, lead zirconate titanate, alumina, zirconia, silicon oxide and the like, and the particle size is preferably submicron or micron.
(3) Adding polymer microspheres with low absorbance and low refractive index into the ceramic slurry, and carrying out vacuum stirring and defoaming treatment to obtain composite ceramic slurry with uniform components;
the polymer microspheres with low absorbance and low refractive index are one or more of PMMA, PE, PS and PP, and the volume ratio of the polymer microspheres with low absorbance and low refractive index to the ceramic powder is 1: 4-7: 3; the content, the grain diameter and the shape of the polymer microspheres can be controlled by adjusting the parameters, so that the performance of the ceramic part can be regulated.
(4) Presetting technological parameters of photocuring forming, and forming a ceramic biscuit by combining data information obtained by slicing; then carrying out binder removal and reaction sintering treatment to obtain the required high-performance ceramic part;
the binder removal temperature is preferably 500-700 ℃, the binder removal time is preferably 1-3 h, the sintering temperature is preferably 1100-2100 ℃, and the sintering time is preferably 2-4 h.
The present invention is further described in detail below with reference to several specific examples.
Example 1
(1) Weighing 5.4081g, 2.7040g and 0.9013g of 1, 6-hexanediol diacrylate, tripropylene glycol diacrylate and ethoxylated trimethylolpropane triacrylate, respectively, weighing 1.5906g of polyethylene glycol, 0.5302g of initiator 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide and 0.9g of dispersant which is 3 percent of the composite powder;
(2) 26.627g of lead zirconate titanate ceramic powder is added into the ceramic powder and is uniformly mixed by a vacuum stirring and defoaming machine to obtain ceramic slurry;
(3) 3.373g of polymer microsphere PE microspheres with low absorbance and low refractive index are added into the ceramic slurry obtained in the step (2), and are uniformly mixed by a vacuum stirring defoaming machine to obtain composite ceramic slurry;
(4) establishing a CAD model with an extremely-small curved surface structure, introducing data information into Digital Light Processing (DLP) forming equipment after processing by slicing software, obtaining a ceramic biscuit after photocuring, as shown in figure 2, heating from room temperature to 600 ℃ at a heating rate of 0.5 ℃/min, preserving heat for 2h, cooling to room temperature along with a furnace, heating from room temperature to 1200 ℃ at 5 ℃/min, preserving heat for 2h, and cooling to room temperature along with the furnace to obtain the lead zirconate titanate piezoelectric ceramic.
Example 2
(1) Weighing 6.7055g and 4.4703g of 1, 6-hexanediol diacrylate and tripropylene glycol diacrylate, 1.9722g of polyethylene glycol, 0.3944g of initiator 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 0.45g of dispersant which are 1.5 percent of the composite powder;
(2) 25.911g of barium titanate ceramic powder is added into the ceramic powder, and the mixture is uniformly mixed by a vacuum stirring and defoaming machine to obtain ceramic slurry;
(3) 4.089g of low-absorbance and low-refractive-index polymer microsphere PP microspheres are added into the ceramic slurry obtained in the step (2), and the mixture is uniformly mixed by a vacuum stirring defoaming machine to obtain composite ceramic slurry;
(4) establishing a CAD model of a tiny curved surface structure, introducing data information into Stereolithography (SL) forming equipment after processing by slicing software, obtaining a ceramic biscuit after photocuring, as shown in figure 3, then heating from room temperature to 500 ℃ at a heating rate of 0.2 ℃/min, preserving heat for 3h, then cooling to room temperature along with a furnace, heating from room temperature to 1320 ℃ at 3 ℃/min, preserving heat for 2h, and cooling to room temperature along with the furnace to obtain the barium titanate piezoelectric ceramic.
Example 3
(1) Weighing 11.6556g and 7.7704g of 1, 6-hexanediol diacrylate and ethoxylated trimethylolpropane triacrylate, 3.4281g of polyethylene glycol, 0.9142g of initiator 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 0.6g of dispersant, wherein the mass of the dispersant is 2 percent of the composite powder;
(2) 22.998g of silicon nitride ceramic powder is added into the ceramic powder, and the ceramic powder is uniformly mixed by a vacuum stirring and defoaming machine to obtain ceramic slurry;
(3) 7.002g of low-absorbance and low-refractive-index polymer microsphere PS microspheres are added into the ceramic slurry obtained in the step (2), and are uniformly mixed by a vacuum stirring defoaming machine to obtain composite ceramic slurry;
(4) establishing a CAD model of a tiny curved surface structure, introducing data information into Digital Light Processing (DLP) forming equipment after processing by slicing software, obtaining a ceramic biscuit after photocuring, then heating from room temperature to 650 ℃ at a heating rate of 0.6 ℃/min, preserving heat for 2h, then cooling to room temperature along with a furnace, heating from room temperature to 1800 ℃ at a heating rate of 2 ℃/min, preserving heat for 2h, and cooling to room temperature along with the furnace to obtain the silicon nitride ceramic.
Example 4
(1) Weighing 10.601g and 7.0673g of tripropylene glycol diacrylate and ethoxylated trimethylolpropane triacrylate, 3.1179g of polyethylene glycol, 0.6236g of initiator 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 1.2g of dispersant which is 4 percent of the composite powder;
(2) 23.133g of silicon carbide ceramic powder is added into the ceramic powder, and the mixture is uniformly mixed by a vacuum stirring and defoaming machine to obtain ceramic slurry;
(3) adding 6.867g of low-absorbance and low-refractive-index polymer microsphere PP microspheres into the ceramic slurry obtained in the step (2), and uniformly mixing the mixture by using a vacuum stirring defoaming machine to obtain composite ceramic slurry;
(4) establishing a CAD model of a tiny curved surface structure, introducing data information into Stereolithography (SL) forming equipment after processing by slicing software, obtaining a ceramic biscuit after photocuring, then heating up to 600 ℃ from room temperature at a heating rate of 1 ℃/min, preserving heat for 2h, then cooling to room temperature along with a furnace, heating up to 2100 ℃ from room temperature at a heating rate of 4 ℃/min, preserving heat for 2h, and cooling to room temperature along with the furnace to obtain the silicon carbide ceramic.
Example 5
(1) Weighing 1.3507g, 4.7273g and 1.7668g of o-phenylphenoxyethyl acrylate, 1, 6-hexanediol diacrylate and ethoxylated trimethylolpropane triacrylate, respectively, weighing 1.1918g of polyethylene glycol, 0.3973g of initiator 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 0.3g of dispersant which is 1 percent of the composite powder;
(2) 28.455g of lead zirconate titanate ceramic powder is added into the ceramic powder and is uniformly mixed by a vacuum stirring and defoaming machine to obtain ceramic slurry;
(3) adding 1.545g of low-absorbance and low-refractive-index polymer microsphere PE microspheres into the ceramic slurry obtained in the step (2), and uniformly mixing the mixture by using a vacuum stirring defoaming machine to obtain composite ceramic slurry;
(4) establishing a CAD model of an extremely-small curved surface structure, introducing data information into Stereolithography (SL) forming equipment after processing by slicing software, obtaining a ceramic biscuit after photocuring, then heating up to 600 ℃ from room temperature at a heating rate of 1.5 ℃/min, preserving heat for 3h, then cooling to room temperature along with a furnace, heating up to 1250 ℃ from room temperature at a heating rate of 2 ℃/min, preserving heat for 3h, and cooling to room temperature along with the furnace to obtain the lead zirconate titanate ceramic.
Example 6
(1) Weighing 4.617g and 10.7740g of o-phenylphenoxyethyl acrylate and ethoxylated trimethylolpropane triacrylate, 1.7101g of polyethylene glycol, 0.5130g of initiator 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 1.5g of dispersant which is 5 percent of the composite powder;
(2) 21.322g of barium titanate ceramic powder is added into the ceramic powder, and the mixture is uniformly mixed by a vacuum stirring and defoaming machine to obtain ceramic slurry;
(3) 8.678g of low-absorbance and low-refractive-index polymer microsphere PS microspheres are added into the ceramic slurry obtained in the step (2), and are uniformly mixed by a vacuum stirring defoaming machine to obtain composite ceramic slurry;
(4) establishing a CAD model of a tiny curved surface structure, introducing data information into Digital Light Processing (DLP) forming equipment after processing by slicing software, obtaining a ceramic biscuit after photocuring, then heating from room temperature to 600 ℃ at a heating rate of 0.1 ℃/min, preserving heat for 2h, then cooling to room temperature along with a furnace, heating from room temperature to 1320 ℃ at a heating rate of 6 ℃/min, preserving heat for 2h, and cooling to room temperature along with the furnace to obtain barium titanate ceramic, as shown in figure 4.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of hard-to-cure ceramics based on photocuring forming is characterized by comprising the following steps:
s1, selecting photosensitive resin, polyethylene glycol, a dispersing agent and a photoinitiator, mixing to form a uniformly mixed solution, adding ceramic powder into the mixed solution, and stirring to obtain ceramic slurry;
s2, adding polymer microspheres with low absorbance and refractive index into the ceramic slurry, and carrying out vacuum stirring and defoaming treatment to obtain composite ceramic slurry with uniform components;
s3, presetting technological parameters of photocuring forming, using the composite ceramic slurry to awaken photocuring forming to obtain a ceramic biscuit, and carrying out binder removal and reactive sintering treatment on the ceramic biscuit so as to obtain the required high-performance ceramic part.
2. The method of claim 1, wherein in step S1, the ceramic powder is one or more of silicon carbide, silicon nitride, barium titanate, lead zirconate titanate, alumina, zirconia, and silica, and the particle size is submicron or micron.
3. The method of claim 2, wherein in step S2, the polymer microspheres are one or more selected from the group consisting of polymethyl methacrylate, polyethylene, polystyrene and polypropylene.
4. The preparation method of the photocuring-forming-based hard-to-cure ceramic, according to claim 3, wherein the volume ratio of the polymer microspheres to the ceramic powder is 1: 4-7: 3.
5. The method of claim 2, wherein in step S1, the photosensitive resin is one or more selected from the group consisting of o-phenylphenoxyethyl acrylate, 1, 6-hexanediol diacrylate, tripropylene glycol diacrylate, and ethoxylated trimethylolpropane triacrylate.
6. The method of claim 5, wherein in step S1, the ratio of the photosensitive resin to the polyethylene glycol is 9: 1-4: 1.
7. The method of claim 1, wherein in step S1, the photo-initiator is 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, and the mass of the photo-initiator is 1-7% of the sum of the mass of the photosensitive resin and the mass of the polyethylene glycol.
8. The method of claim 1, wherein in step S1, the dispersant accounts for 1-6% of the total mass of the ceramic powder and the polymer microspheres.
9. The method for preparing a hard-to-cure ceramic based on photocuring forming of claim 1, wherein in step S3, the glue removing process is performed according to the following steps: heating the mixture from room temperature to 500-700 ℃ at a heating rate of 0.1-2 ℃/min, keeping the temperature for 1-3 h, and then cooling the mixture to room temperature along with the furnace; the sintering is carried out according to the following steps: heating from room temperature to 1100-2100 ℃ at 2-6 ℃/min, keeping the temperature for 2-4 h, and cooling to room temperature along with the furnace.
10. A ceramic part produced by the production method as set forth in any one of claims 1 to 9.
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