CN112341165A - A preparation method of high solid content and low viscosity Al2O3 ceramic slurry for UV light curing 3D printing - Google Patents
A preparation method of high solid content and low viscosity Al2O3 ceramic slurry for UV light curing 3D printing Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 67
- 239000002002 slurry Substances 0.000 title claims abstract description 63
- 238000010146 3D printing Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000007787 solid Substances 0.000 title claims abstract description 18
- 238000003848 UV Light-Curing Methods 0.000 title claims description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title description 25
- 229910052593 corundum Inorganic materials 0.000 title description 18
- 229910001845 yogo sapphire Inorganic materials 0.000 title description 18
- 238000000016 photochemical curing Methods 0.000 claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 28
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000000178 monomer Substances 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000011268 mixed slurry Substances 0.000 claims abstract description 6
- 238000007873 sieving Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- PSGCQDPCAWOCSH-UHFFFAOYSA-N (4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl) prop-2-enoate Chemical compound C1CC2(C)C(OC(=O)C=C)CC1C2(C)C PSGCQDPCAWOCSH-UHFFFAOYSA-N 0.000 claims description 7
- OCIFJWVZZUDMRL-UHFFFAOYSA-N 6-hydroxyhexyl prop-2-enoate Chemical compound OCCCCCCOC(=O)C=C OCIFJWVZZUDMRL-UHFFFAOYSA-N 0.000 claims description 7
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 7
- 125000001931 aliphatic group Chemical group 0.000 claims description 6
- 229910052594 sapphire Inorganic materials 0.000 claims description 5
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims 1
- 238000003801 milling Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 14
- 238000000034 method Methods 0.000 description 13
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 5
- 238000007639 printing Methods 0.000 description 5
- 238000001723 curing Methods 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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Abstract
The invention relates to the technical field of ceramic slurry, and particularly relates to high-solid-content low-viscosity Al for UV (ultraviolet) photocuring 3D printing2O3The preparation method of the ceramic slurry comprises the following steps: 1) alpha-Al is added2O3Drying the powder, grinding, crushing and sieving; 2) preparing UV light-cured monomers and oligomers into UV light-cured premixed liquid according to a proportion, and uniformly stirring; 3) adding a certain amount of dispersant into the UV photocuring premixed liquid, uniformly mixing, and adding the alpha-Al obtained in the step 1)2O3Mixing the powder, adding a certain amount of photoinitiator, and mixing to obtain mixed slurry; 4) mixing the mixed slurry obtained in the step 3) in a reactorBall milling for a certain time at a constant rotating speed; 5) removing bubbles: and removing bubbles from the mixture slurry after ball milling. UV photocuring Al prepared by the invention2O3The ceramic slurry has high solid content, low viscosity and excellent stability.
Description
Technical Field
The invention relates to the technical field of ceramic slurry, in particular to a high-solid-content UV (ultraviolet) photocuring 3D printing inkContaining low-viscosity Al2O3A preparation method of ceramic slurry.
Background
The ceramic photocuring 3D printing technology is a new ceramic molding processing technology, and the principle is that UV photocuring ceramic slurry is selectively cured by utilizing ultraviolet light, the ceramic slurry is polymerized into a single-layer solid, then the next layer of curing is continuously carried out by moving a printing platform, the steps are circulated in such a way to obtain a final solid body, and the ceramic device can be obtained by carrying out glue discharge and sintering treatment on the body. According to the type of Light source and the printing process, the ceramic photocuring 3D printing technology can be divided into a stereo photocuring molding technology (SLA) and a Digital Light Processing technology (DLP), wherein the SLA photocuring technology is a technology that uses a laser as a Light source and prints in a dot-to-line, line-to-surface, and surface-to-body manner, and the DLP photocuring 3D printing technology is a technology that uses a Digital Light Processing projector as a Light source and prints in a layer-to-body manner. The ceramic photocuring 3D printing technology has obvious advantages in preparing various ceramic devices with high precision and complex shapes, does not need to use a mold, and has the characteristics of high efficiency and low cost. Ceramics prepared by applying the photocuring 3D printing technology at present comprise aluminum oxide, silicon oxide, zirconium oxide, silicon nitride, silicon carbide, hydroxyapatite and the like. The key of the ceramic UV photocuring 3D printing technology lies in the preparation of ceramic slurry with high solid content, low viscosity, high stability and excellent self-leveling property, and the ceramic slurry has significant influence on the continuity and integrity of the printing process and the performance of a final ceramic device.
The alumina ceramic is one of ceramic materials with the widest application range, has excellent physical and chemical properties, and is a research hotspot for preparing the ceramic by applying a UV (ultraviolet) photocuring 3D printing technology. Currently, UV-light-cured Al is prepared2O3The volume fraction of the ceramic slurry is concentrated at 30-50 vol%, the solid content is improved, and the corresponding viscosity is also increased rapidly, so that the slurry recoating in the photocuring 3D printing process is not facilitated.
As the text of the Chinese invention patent 'A photocuring 3D printing alumina ceramic slurry and preparation' (201910550744.3), n-octanol and polyethylene are selectedGlycol, oleic acid, etc. as dispersant, which produces UV-light-cured Al2O3The mass fraction of the ceramic slurry is 66.6 wt%, and the volume fraction is lower than 40 vol%. The invention of Chinese patent of invention, a rapid degreasing sintering method of photocuring formed ceramic body (201910605007.9), uses phosphate as dispersant to prepare UV photocuring Al2O3The volume fraction of the ceramic slurry was 40 vol%. The literature "The effect of The surfactants on The formulation of UV-curable SLA aluminum dispersion" (Central. Int.43(2017)4761-2O3The maximum solid content of the ceramic slurry is 40 vol% and 30s-1The corresponding viscosity was 2.12 pas. The document "A study on the biomedical and mechanical properties of photo-curable ceramic/polymer compositions with differential silane coupling agents for SLA 3D printing technology" (nanomaterials 8(2) (2018)1-12) reports UV-light-cured Al prepared by silane coupling agents2O3Ceramic slurry with maximum solid content of 27 vol% for 30s-1The corresponding viscosity was 2 pas. The volume fraction of the alumina slurry prepared by the method is below 40 vol%, and the viscosity is above 2 pas.
Disclosure of Invention
The invention aims to provide a preparation method of high-solid-content low-viscosity Al2O3 ceramic slurry for UV photocuring 3D printing, and the prepared UV photocuring Al2O3Compared with the traditional method, the ceramic slurry has the advantages of high solid content, low viscosity, excellent stability and obvious self-leveling behavior.
The scheme adopted by the invention for realizing one of the purposes is as follows: high-solid-content low-viscosity Al for UV photocuring 3D printing2O3The preparation method of the ceramic slurry comprises the following steps:
1) alpha-Al is added2O3Drying the powder, grinding, crushing and sieving;
2) preparing UV light-cured monomers and oligomers into UV light-cured premixed liquid according to a proportion, and uniformly stirring;
3) adding a certain amount of dispersant into the UV light curing premix liquid to mixAfter uniform mixing, adding the alpha-Al obtained in the step 1)2O3Mixing the powder, adding a certain amount of photoinitiator, and mixing to obtain mixed slurry;
4) ball-milling the mixed slurry obtained in the step 3) for a certain time at a certain rotating speed;
5) removing bubbles: removing bubbles from the ball-milled mixture slurry to obtain the high-solid-content low-viscosity Al for the UV photocuring 3D printing2O3Ceramic slurry.
Preferably, in the step 2): the UV light curing monomer is a mixture of 1,6 hexanediol acrylate, isobornyl acrylate and trimethylolpropane triacrylate, the oligomer is aliphatic urethane acrylate, and the mass ratio of the UV light curing monomer to the oligomer is 8: 2-7: 3.
Preferably, the volume ratio of the 1,6 hexanediol acrylate, the isobornyl acrylate and the trimethylolpropane triacrylate is 5: 2: 3.
Preferably, in the step 3), the dispersant is any one of BYK110, BYK111, BYK163, BYK180, TEGO630 and TEGO700, and the addition amount of the dispersant is alpha-Al2O32 to 4 weight percent of the powder.
Preferably, in the step 3), 50-55 vol% of alpha-Al in the ball milling tank is added in batches2O3And (3) powder.
Preferably, in the step 3), the photoinitiator is TPO or 819, and the addition amount of the photoinitiator is 1-3 wt% of the UV light curing monomer.
Preferably, in the step 4), ball milling is carried out for 12-24 hours at the rotating speed of 300-400 rpm.
Preferably, the V photocuring 3D printing high-solid-content low-viscosity Al obtained in the step 5)2O3The solid content of the ceramic slurry is more than 55 vol% and 30s-1The viscosity at shear rate is 1.042 pas or less.
The invention has the following advantages and beneficial effects:
UV photocuring Al prepared by the invention2O3The ceramic slurry has high solid content, low viscosity and excellent stability. At the same time, the user can select the desired position,the degree of a slurry network structure is reduced through uniform dispersion, the solid content is improved, and meanwhile, the viscosity is kept low, so that the performance of the slurry is closer to that of liquid, the slurry can be automatically leveled on a printing platform, the self-leveling behavior of the slurry prepared by the method is obviously improved compared with that of the slurry prepared by the traditional method, and the completeness and the continuity of the printing process are improved.
UV photocuring Al prepared by the invention2O3The solid content of the ceramic slurry is high and reaches 55 vol% for 30s-1The viscosity at the shear rate is only 1.042 pas, the stability is excellent, no obvious sedimentation exists within 10 days of standing, the self-leveling behavior is obvious, and the technical requirements of the alumina ceramic slurry for UV photocuring 3D printing and the preparation of high-precision ceramic products can be met.
Drawings
FIG. 1 is a graph of viscosity versus solids content for ceramic slurries prepared in example 1 of the present invention;
FIG. 2 is a settling curve for ceramic slurries prepared in example 1 of the present invention;
FIG. 3 is a flow flat image of a ceramic slurry prepared according to example 1 of the present invention.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
Example 1:
1)Al2O3pretreatment of ceramic powder: alpha-Al is added2O3Drying the powder at 200 ℃ for 12h to remove residual moisture in the powder, and drying the alpha-Al2O3Grinding and crushing the powder and sieving the powder by a 80-mesh sieve;
2) preparing a UV light curing premix liquid: preparing UV light-cured monomers (the UV light-cured monomers are a mixture of 1,6 hexanediol acrylate, isobornyl acrylate and trimethylolpropane triacrylate according to the volume ratio of 5: 2: 3) and oligomer aliphatic urethane acrylate according to the mass ratio of 8:2 into UV light-cured premixed liquid, and uniformly mixing the UV light-cured premixed liquid through magnetic stirring;
3) disposition of Al2O3Ceramic slurry: adding the UV light-cured premixed solution into a ballAdding 2 wt% of BYK111 dispersant into a grinding tank, fully stirring, and then adding 55 vol% of alpha-Al in batches2O3Powder is mixed evenly, and finally 2 wt% of photoinitiator TPO is added and mixed evenly;
4) ball milling: curing the above UV light to obtain Al2O3Ball-milling the ceramic slurry for 12 hours at the rotating speed of 400 rpm;
5) removing bubbles: ball-milled Al2O3The ceramic slurry is put into a vacuum defoaming machine for 2 hours to remove bubbles generated in the ball milling process.
Through testing, the UV light-cured Al prepared by the invention2O3The ceramic slurry has high solid content, up to 55 vol% (see figure I), 30s-1The viscosity at the shear rate is only 1.042Pa s (shown in figure 1), the stability is excellent, no obvious sedimentation is generated after standing for 10 days (shown in figure 2), the self-leveling behavior is obvious (shown in figure 3), and the technical requirements of UV photocuring alumina ceramic slurry for 3D printing and preparation of high-precision ceramic products can be met.
Example 2:
1)Al2O3pretreatment of ceramic powder: alpha-Al is added2O3Drying the powder at 200 ℃ for 12h to remove residual moisture in the powder, and drying the alpha-Al2O3Grinding and crushing the powder and sieving the powder by a 80-mesh sieve;
2) preparing a UV light curing premix liquid: preparing a UV light curing monomer (the UV light curing monomer is a mixture of 1,6 hexanediol acrylate, isobornyl acrylate and trimethylolpropane triacrylate according to the volume ratio of 5: 2: 3) and oligomer aliphatic urethane acrylate according to the mass ratio of 7:3 into UV light curing premix liquid, and uniformly mixing the UV light curing premix liquid through magnetic stirring;
3) disposition of Al2O3Ceramic slurry: adding the UV light-cured premixed liquid into a ball milling tank, adding 4 wt% of BYK163 dispersing agent, fully stirring, and then adding 50 vol% of alpha-Al in batches2O3Powder is mixed evenly, and finally 1 wt% of photoinitiator 819 is added and mixed evenly;
4) ball milling: curing the above UV light to obtain Al2O3Ball-milling the ceramic slurry for 24 hours at the rotating speed of 300rpm；
5) Removing bubbles: ball-milled Al2O3The ceramic slurry was placed in a vacuum defoaming machine for 3 hours to remove bubbles generated during the ball milling process.
Through testing, the UV light-cured Al prepared by the invention2O3The ceramic slurry has high solid content, up to 55 vol% (see figure I), 30s-1The viscosity at the shear rate is only 1.122 pas, the stability is excellent, no obvious settlement occurs within 10 days of standing, the self-leveling behavior is obvious, the self-spreading angle is 61.2 degrees, and the technical requirements of the alumina ceramic slurry for UV photocuring 3D printing and the preparation of high-precision ceramic products can be met.
Example 3:
1)Al2O3pretreatment of ceramic powder: alpha-Al is added2O3Drying the powder at 200 ℃ for 12h to remove residual moisture in the powder, and drying the alpha-Al2O3Grinding and crushing the powder and sieving the powder by a 80-mesh sieve;
2) preparing a UV light curing premix liquid: preparing a UV light curing monomer (the UV light curing monomer is a mixture of 1,6 hexanediol acrylate, isobornyl acrylate and trimethylolpropane triacrylate according to the volume ratio of 5: 2: 3) and oligomer aliphatic urethane acrylate according to the mass ratio of 7.5:2.5 into UV light curing premix, and uniformly mixing the UV light curing premix and the oligomer aliphatic urethane acrylate through magnetic stirring;
3) disposition of Al2O3Ceramic slurry: adding the UV photocuring premixed solution into a ball milling tank, adding 3 wt% of BYK110 dispersant, fully stirring, and then adding 55 vol% of alpha-Al in batches2O3Powder is mixed evenly, and finally 3 wt% of photoinitiator TPO is added and mixed evenly;
4) ball milling: curing the above UV light to obtain Al2O3Ball-milling the ceramic slurry for 16 hours at the rotating speed of 350 rpm;
5) removing bubbles: ball-milled Al2O3The ceramic slurry is put into a vacuum defoaming machine for 2 hours to remove bubbles generated in the ball milling process.
Through testing, the UV light-cured Al prepared by the invention2O3The ceramic slurry has high solid content up to 55 vol%(see FIG. 1), 30s-1The viscosity at the shear rate is only 1.212 pas, the stability is excellent, no obvious settlement is generated after standing for 10 days, the self-leveling behavior is obvious, the self-spreading angle is 60.7 degrees, and the technical requirements of the alumina ceramic slurry for UV photocuring 3D printing and the preparation of high-precision ceramic products can be met.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (8)
1. High-solid-content low-viscosity Al for UV photocuring 3D printing2O3The preparation method of the ceramic slurry is characterized by comprising the following steps:
1) alpha-Al is added2O3Drying the powder, grinding, crushing and sieving;
2) preparing UV light-cured monomers and oligomers into UV light-cured premixed liquid according to a proportion, and uniformly stirring;
3) adding a certain amount of dispersant into the UV photocuring premixed liquid, uniformly mixing, and adding the alpha-Al obtained in the step 1)2O3Mixing the powder, adding a certain amount of photoinitiator, and mixing to obtain mixed slurry;
4) ball-milling the mixed slurry obtained in the step 3) for a certain time at a certain rotating speed;
5) removing bubbles: removing bubbles from the ball-milled mixture slurry to obtain the high-solid-content low-viscosity Al for the UV photocuring 3D printing2O3Ceramic slurry.
2. High-solid-content low-viscosity Al for UV photocuring 3D printing according to claim 12O3The preparation method of the ceramic slurry is characterized by comprising the following steps: in the step 2): the UV light curing monomer is a mixture of 1,6 hexanediol acrylate, isobornyl acrylate and trimethylolpropane triacrylate, and the oligomer is aliphatic urethane acrylateAnd the mass ratio of the UV light curing monomer to the oligomer is 8: 2-7: 3.
3. High-solid-content low-viscosity Al for UV photocuring 3D printing according to claim 22O3The preparation method of the ceramic slurry is characterized by comprising the following steps: the volume ratio of the 1,6 hexanediol acrylate, the isobornyl acrylate and the trimethylolpropane triacrylate is 5: 2: 3.
4. High-solid-content low-viscosity Al for UV photocuring 3D printing according to claim 12O3The preparation method of the ceramic slurry is characterized by comprising the following steps: in the step 3), the dispersant is any one of BYK110, BYK111, BYK163, BYK180, TEGO630 and TEGO700, and the addition amount of the dispersant is alpha-Al2O32 to 4 weight percent of the powder.
5. High-solid-content low-viscosity Al for UV photocuring 3D printing according to claim 12O3The preparation method of the ceramic slurry is characterized by comprising the following steps: in the step 3), 50-55 vol% of alpha-Al in the ball-milling tank is added in batches2O3And (3) powder.
6. High-solid-content low-viscosity Al for UV photocuring 3D printing according to claim 12O3The preparation method of the ceramic slurry is characterized by comprising the following steps: in the step 3), the photoinitiator is TPO or 819, and the addition amount of the photoinitiator is 1-3 wt% of the UV light curing monomer.
7. High-solid-content low-viscosity Al for UV photocuring 3D printing according to claim 12O3The preparation method of the ceramic slurry is characterized by comprising the following steps: in the step 4), ball milling is carried out for 12-24 hours at the rotating speed of 300-400 rpm.
8. High-solid-content low-viscosity Al for UV photocuring 3D printing according to claim 12O3The preparation method of the ceramic slurry is characterized by comprising the following steps: said step 5) The obtained high-solid-content low-viscosity Al for V photocuring 3D printing2O3The solid content of the ceramic slurry is more than 55 vol% and 30s-1The viscosity at shear rate is 1.042 pas or less.
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