CN118026692A - Preparation method and application of silicon carbide ceramic slurry for photo-curing 3D printing - Google Patents
Preparation method and application of silicon carbide ceramic slurry for photo-curing 3D printing Download PDFInfo
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- CN118026692A CN118026692A CN202410436760.0A CN202410436760A CN118026692A CN 118026692 A CN118026692 A CN 118026692A CN 202410436760 A CN202410436760 A CN 202410436760A CN 118026692 A CN118026692 A CN 118026692A
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- silicon carbide
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 170
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 135
- 239000000919 ceramic Substances 0.000 title claims abstract description 109
- 238000010146 3D printing Methods 0.000 title claims abstract description 106
- 239000002002 slurry Substances 0.000 title claims abstract description 98
- 238000000016 photochemical curing Methods 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 238000001723 curing Methods 0.000 claims abstract description 55
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 239000003085 diluting agent Substances 0.000 claims abstract description 15
- 239000000178 monomer Substances 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 239000012686 silicon precursor Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 229920001296 polysiloxane Polymers 0.000 claims description 29
- -1 polysiloxane Polymers 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 25
- 239000002243 precursor Substances 0.000 claims description 15
- 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 11
- 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 10
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical compound 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 10
- XQTJQXCPQYOAIJ-UHFFFAOYSA-N 4-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OC(CC)CCCOC(=O)C=C XQTJQXCPQYOAIJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000013007 heat curing Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- MPIAGWXWVAHQBB-UHFFFAOYSA-N [3-prop-2-enoyloxy-2-[[3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propoxy]methyl]-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C MPIAGWXWVAHQBB-UHFFFAOYSA-N 0.000 claims description 3
- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 claims description 3
- 229920003257 polycarbosilane Polymers 0.000 claims description 3
- 229920001709 polysilazane Polymers 0.000 claims description 3
- 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 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 2
- ZCZFEIZSYJAXKS-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] prop-2-enoate Chemical compound OCC(CO)(CO)COC(=O)C=C ZCZFEIZSYJAXKS-UHFFFAOYSA-N 0.000 claims description 2
- FXIVKZGDYRLHKF-UHFFFAOYSA-N C(C)OP(OC(C1=C(C=C(C=C1C)C)C)=O)(=O)C1=CC=CC=C1 Chemical compound C(C)OP(OC(C1=C(C=C(C=C1C)C)C)=O)(=O)C1=CC=CC=C1 FXIVKZGDYRLHKF-UHFFFAOYSA-N 0.000 claims 1
- 238000007639 printing Methods 0.000 abstract description 27
- 239000007787 solid Substances 0.000 abstract description 21
- 230000001678 irradiating effect Effects 0.000 description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000004005 microsphere Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- YMCOIFVFCYKISC-UHFFFAOYSA-N ethoxy-[2-(2,4,6-trimethylbenzoyl)phenyl]phosphinic acid Chemical compound CCOP(O)(=O)c1ccccc1C(=O)c1c(C)cc(C)cc1C YMCOIFVFCYKISC-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 238000007613 slurry method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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Abstract
The invention belongs to the technical field of 3D printing ceramics, and particularly relates to a preparation method and application of silicon carbide ceramic slurry for photo-curing 3D printing. The preparation method comprises the following steps: (1) Uniformly dispersing silicon carbide into an organic silicon precursor, and curing to obtain silicon carbide powder coated by the organic silicon precursor; (2) And mixing and stirring the reactive diluent monomer, the photoinitiator and the dispersing agent, then adding the silicon carbide powder coated by the organic silicon precursor, and continuously stirring to obtain the silicon carbide ceramic slurry for photocuring 3D printing. The preparation method has the advantages of simple process and low cost, and the prepared silicon carbide ceramic slurry has the advantages of good curing depth, high solid content and excellent printing forming performance, thereby laying a foundation for the subsequent preparation of high-precision and high-performance silicon carbide ceramics.
Description
Technical Field
The invention belongs to the technical field of 3D printing ceramics, and particularly relates to a preparation method and application of silicon carbide ceramic slurry for photo-curing 3D printing.
Background
With the rapid development of modern technology, the requirements on the material performance are increasingly improved, and in particular, in the high-end fields of aerospace, chemical industry, machinery, integrated circuits and the like, stringent standards are provided for corrosion resistance, high-temperature stability, mechanical properties and the like of the material. Silicon carbide ceramics are widely used in these fields as a structural ceramic material with excellent properties due to good corrosion resistance, high-temperature stability and excellent mechanical properties.
Conventional methods of silicon carbide ceramic formation such as dry press forming, cold isostatic pressing, slip casting, cast forming, injection molding, etc., while capable of producing silicon carbide ceramics of a certain quality and density, exhibit significant limitations in the manufacture of ceramic articles of high precision, high complexity construction. In addition, these conventional processes are time consuming and costly, limiting the large-scale production and use of silicon carbide ceramic materials.
In recent years, the 3D printing technology provides a new idea for preparing ceramic materials by virtue of the unique design flexibility and the high material utilization rate. The photocuring 3D printing technology has great potential in the field of ceramic material manufacturing due to the characteristics of high precision, high speed and high complexity. However, photo-curing 3D printed dark ceramic materials, particularly silicon carbide ceramics, still face a number of challenges. Due to the mismatch of refractive indexes of the ceramic powder and the photo-curing resin, and the scattering and reflection of light in the silicon carbide slurry, the curing depth is limited and the solid content is low, thereby affecting the quality and performance of the final product. Therefore, developing a method capable of effectively solving the problems of poor curing depth and low solid content of silicon carbide ceramic slurry and improving the precision and quality of photo-curing 3D printing silicon carbide ceramic is an urgent need in the current field.
Chinese patent CN114436658a discloses a photo-curing silicon carbide ceramic slurry, and preparation method and application thereof, the preparation method comprises: (1) Modifying the silicon carbide powder to obtain modified silicon carbide powder coated with silicon dioxide on the surface; (2) And mixing the modified silicon carbide powder, the photosensitive resin and the dispersing agent, and performing ball milling treatment to obtain the photo-curing silicon carbide ceramic slurry. The prepared photo-curing silicon carbide ceramic slurry has good fluidity and strong curing capability, realizes 3D printing of a silicon carbide ceramic green body with high solid content, and provides guarantee for mechanical properties of the silicon carbide ceramic green body after degreasing and sintering. However, the silicon carbide powder is oxidized and treated at different temperatures, the period is long, the cost is high, and although the solid content in the slurry is improved to a certain extent, the method still has a great room for improvement.
Chinese patent CN117069498a discloses a silicon carbide ceramic slurry for 3D printing, a preparation method, application and silicon carbide ceramic, wherein the silicon carbide ceramic slurry for 3D printing is prepared from the following raw materials in parts by weight: 55-70 parts of silicon carbide powder, 22-42 parts of photosensitive resin, 2-3 parts of dispersing agent and 1-5 parts of initiator; the silicon carbide slurry has smaller scattering in the printing process of the additive manufacturing digital light processing photocuring 3D printer, the size precision of the printed sample is better, and a more complex structure can be printed. However, the silicon carbide slurry with different solid contents is prepared by the grain composition of the powder, the effect of the gray powder of the silicon carbide on light cannot be changed, and the solid content in the silicon carbide slurry cannot be well broken through.
Chinese patent CN116283299a discloses a method for manufacturing ceramic microsphere reinforced precursor ceramic by additive, firstly, balling the organosilicon precursor emulsion, then placing in a tube furnace, protecting with nitrogen or argon atmosphere, and pyrolyzing to obtain ceramic microsphere; secondly, mixing ceramic microspheres, an organosilicon precursor, a reactive diluent and a photoinitiator to obtain uniformly dispersed slurry; and printing a ceramic blank body with a complex shape by using additive manufacturing equipment, and post-treating to obtain the silicon-based composite ceramic. However, the organosilicon precursor (containing photo-curing groups and having high synthesis cost) is converted into amorphous silicon-based ceramics after heat treatment, and the sample prepared by the method has large shrinkage and high porosity and can only be used for preparing some small-size silicon-based ceramics. Therefore, to achieve the preparation of silicon carbide ceramics of large size, wall thickness, and high purity and complex structure, it is necessary to prepare a slurry with high solid content.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of silicon carbide ceramic slurry for photo-curing 3D printing, which has the advantages of simple process and low cost, and the prepared silicon carbide ceramic slurry has the advantages of good curing depth, high solid content and excellent printing forming property, thereby laying a foundation for the subsequent preparation of high-precision and high-performance silicon carbide ceramics;
another object of the present invention is to provide an application of the silicon carbide ceramic slurry for photo-curing 3D printing.
The technical scheme adopted by the invention is as follows:
The preparation method of the silicon carbide ceramic slurry for photo-curing 3D printing comprises the following steps:
(1) Uniformly dispersing silicon carbide into an organic silicon precursor, and placing the organic silicon precursor into a blast drying oven for curing at the curing temperature of 50-100 ℃ to obtain silicon carbide powder coated by the organic silicon precursor after curing, wherein the mass ratio of the silicon carbide to the organic silicon precursor is (2-5);
(2) Adding an active diluent monomer, a photoinitiator and a dispersing agent into a magnetic stirrer, mixing and stirring at a mixing and stirring speed of 400-500 r/min for 2-4 hours, then adding silicon carbide powder coated by an organosilicon precursor, continuously stirring for 2-4 hours, and uniformly stirring for 1-10 minutes to obtain the silicon carbide ceramic slurry for photocuring 3D printing; the addition amount of the photoinitiator is 2.9-5.1 wt% of the total amount of the reactive diluent monomer and the photoinitiator, the addition amount of the reactive diluent monomer is 20-32 wt% of the total amount of the reactive diluent monomer and the silicon carbide powder coated by the organosilicon precursor, and the addition amount of the dispersing agent is 2.7-7.1 wt% of the total amount of the silicon carbide powder coated by the organosilicon precursor and the dispersing agent.
The particle size of the silicon carbide is 6-9 mu m.
And 2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, ultraviolet light with the wavelength of 405nm is used for irradiating for 5-20 s, and the curing depth is tested.
The organosilicon precursor is one of polycarbosilane, polysilazane, polyborosilazane or polysiloxane.
The reactive diluent monomer is more than one of 1, 6-hexanediol diacrylate, 1, 4-hexanediol diacrylate, tripropylene glycol diacrylate, hydroxyethyl acrylate, trimethylolpropane triacrylate, dipentaerythritol hexaacrylate or pentaerythritol acrylate.
The photoinitiator is one of 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide, 2,4, 6-trimethylbenzoyl phenyl phosphonic acid ethyl ester, phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide or 2-phenylbenzyl-2-dimethyl amine-1- (4-morpholinophenyl) butanone.
The dispersing agent is one of BYK410, KOS110 or KOS 2000.
The silicon carbide ceramic slurry for photocuring 3D printing is applied, and the silicon carbide blank is prepared from the silicon carbide ceramic slurry for photocuring 3D printing, which is prepared by the preparation method of the silicon carbide ceramic slurry for photocuring 3D printing.
The application of the silicon carbide ceramic slurry for photo-curing 3D printing is used for preparing silicon carbide blanks.
The preparation method of the silicon carbide blank comprises the following steps:
(1) Adding the silicon carbide ceramic slurry for photocuring 3D printing into 3D printing equipment to print into a blank;
(2) Placing the blank in a vacuum curing box for secondary curing, wherein the secondary curing is heat curing, the curing temperature is 90-100 ℃, and the curing time is 20-40 min;
(3) And placing the blank after secondary solidification in a tube furnace, introducing nitrogen, heating from room temperature to 200-300 ℃ at a heating rate of 1-3 ℃/min, preserving heat for 1-2 h, continuously heating to 400-600 ℃ at a heating rate of 1-3 ℃/min, preserving heat for 2-4 h, heating to 800-1000 ℃ at a heating rate of 2-4 ℃/min, preserving heat for 1-2 h, and cooling to room temperature to obtain the silicon carbide blank.
Compared with the prior art, the invention has the following beneficial effects:
Compared with the traditional silicon carbide powder or slurry with the same solid content prepared by adopting an oxidation treatment silicon carbide powder or particle grading method, the preparation method of the silicon carbide ceramic slurry for photocuring 3D printing has the advantages that the curing efficiency of the slurry is improved, and the precision and stability of a printing finished product are ensured; in addition, the preparation method of the silicon carbide ceramic slurry for photo-curing 3D printing can further increase the solid content in the slurry, the prepared silicon carbide slurry with high solid content can better maintain the shape and the dimensional stability in the printing process, the deformation and the cracking phenomenon in the printing process are effectively reduced, and the preparation method of the silicon carbide ceramic slurry with high precision and high performance further has huge application potential in the aspect of subsequent preparation of silicon carbide ceramics.
Drawings
FIG. 1 is a scanning electron microscope image of silicon carbide according to example 1;
fig. 2 is a scanning electron microscope image of a silicone precursor-coated silicon carbide powder described in example 1.
Detailed Description
The invention is further illustrated below with reference to examples, which are not intended to limit the practice of the invention.
The raw materials used in examples and comparative examples are conventional commercial raw materials unless otherwise specified, and the process methods used in examples and comparative examples are conventional in the art unless otherwise specified.
Example 1
The preparation method of the silicon carbide ceramic slurry for photo-curing 3D printing comprises the following steps:
(1) Uniformly dispersing silicon carbide into polysiloxane, and placing the polysiloxane into a blast drying oven for curing at the curing temperature of 50 ℃ to obtain polysiloxane-coated silicon carbide powder, wherein the mass ratio of the silicon carbide to the polysiloxane is 1:2;
(2) Adding 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide and KOS110 into a magnetic stirrer, mixing and stirring at the speed of 400r/min for 2h, adding polysiloxane-coated silicon carbide powder, continuously stirring for 2h, and uniformly stirring for 5min to obtain silicon carbide ceramic slurry for photocuring 3D printing, wherein the viscosity is 279.5 mPa.s; wherein the amounts of 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, KOS110 and polysiloxane-coated silicon carbide powder were 3g, 0.18g, 0.67g, 12.75g, respectively, with a solids content of 68wt.%. The method for calculating the solid content comprises the following steps: the total amount of reactive diluent monomer was m 1, the amount of polysiloxane coated silicon carbide powder was m 2, the solid content (wt.%) =m 2/(m1+m2) ×100.
The grain diameter of the silicon carbide is 7.5+/-1.5 mu m.
2G of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is 163 mu m.
The preparation method of the silicon carbide blank comprises the following steps:
(1) Adding the silicon carbide ceramic slurry for photocuring 3D printing into 3D printing equipment to print into a blank;
(2) Placing the blank in a vacuum curing box for secondary curing, wherein the secondary curing is heat curing, the curing temperature is 100 ℃, and the curing time is 20min;
(3) And (3) placing the blank after secondary solidification in a tube furnace, introducing nitrogen, heating from room temperature to 300 ℃ at a heating rate of 1 ℃/min, preserving heat for 1h, continuously heating to 400 ℃ at a heating rate of 1 ℃/min, preserving heat for 2h, heating to 1000 ℃ at a heating rate of 2 ℃/min, preserving heat for 1h, and cooling to room temperature to obtain the silicon carbide blank. The surface of the prepared silicon carbide blank body is smooth and flat, and no cracking exists.
The scanning electron microscope test is carried out on the silicon carbide and the silicon carbide powder coated by the polysiloxane respectively, the test results are shown in figures 1-2, and as can be seen from figures 1-2, the surface of the silicon carbide powder coated by the polysiloxane obtained after the polysiloxane treatment is smooth, no small particles on the surface of the silicon carbide before the treatment exist, and the effect of the polysiloxane on the silicon carbide powder is demonstrated.
Example 2
The difference from example 1 is that:
The dispersing agent is KOS2000;
The viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 122.9 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is 165 mu m.
Example 3
The difference from example 1 is that:
the dispersing agent is BYK410;
the viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 479.5 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is measured to be 164 mu m.
Example 4
The difference from example 2 is that:
The amounts of 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, KOS2000 and polysiloxane coated silicon carbide powder were 3g, 0.18g, 0.39g, 12.75g, respectively, with a solids content of 68wt.%.
The viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 153.6 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is 163 mu m.
Example 5
The difference from example 2 is that:
The amounts of 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, KOS2000 and polysiloxane coated silicon carbide powder were 3g, 0.18g, 0.96g, 12.75g, respectively, with a solids content of 68wt.%.
The viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 189.5 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is measured to be 164 mu m.
Example 6
The difference from example 2 is that:
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 5s, so that the curing depth is measured to be 95 mu m.
Example 7
The difference from example 2 is that:
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 15s, so that the curing depth is measured to be 201 mu m.
Example 8
The difference from example 2 is that:
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 20s, so that the curing depth is measured to be 234 mu m.
Example 9
The difference from example 2 is that:
In the step (1) of the preparation method of the silicon carbide ceramic slurry for photo-curing 3D printing, the mass ratio of silicon carbide to polysiloxane is 1:3;
the viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 125.6 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is measured to be 172 mu m.
Example 10
The difference from example 2 is that:
In the step (1) of the preparation method of the silicon carbide ceramic slurry for photo-curing 3D printing, the mass ratio of silicon carbide to polysiloxane is 1:5;
the viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 123.8 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is measured to be 174 mu m.
Example 11
The difference from example 2 is that:
The amounts of 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, KOS2000 and polysiloxane coated silicon carbide powder were 3g, 0.18g, 0.67g, 15.43g, respectively, with a solids content of 72wt.%.
The viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 597.4 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is measured to be 134 mu m.
Example 12
The difference from example 2 is that:
the amounts of 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, KOS2000 and polysiloxane coated silicon carbide powder were 3g, 0.18g, 0.67g, 19g, respectively, with a solids content of 76wt.%.
The viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 1373.1 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is measured to be 96 mu m.
Example 13
The difference from example 2 is that:
The amounts of 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, KOS2000 and polysiloxane coated silicon carbide powder were 3g, 0.18g, 0.67g, 24g, respectively, with a solids content of 80wt.%.
The viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 2646.2 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is measured to be 64 mu m.
Example 14
The difference from example 2 is that:
the amounts of 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, KOS2000 and polysiloxane coated silicon carbide powder were 3g, 0.32g, 0.67g, 12.75g, respectively, with a solids content of 68wt.%.
The viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 123.1 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is measured to be 156 mu m.
Example 15
The difference from example 2 is that:
the organosilicon precursor is polycarbosilane;
the reactive diluent monomer is a mixture of 1, 4-hexanediol diacrylate and trimethylolpropane triacrylate with equal mass;
the photoinitiator is phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide;
The viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 123.5 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is measured to be 164 mu m.
Example 16
The difference from example 2 is that:
the organic silicon precursor is polysilazane;
the reactive diluent monomer is a mixture of 1, 4-hexanediol diacrylate and dipentaerythritol hexaacrylate with equal mass;
The photoinitiator is 2-phenylbenzyl-2-dimethylamine-1- (4-morpholinophenyl) butanone;
The viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 176.4 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is 169 mu m.
Example 17
The difference from example 2 is that:
In the preparation method of the silicon carbide ceramic slurry for photo-curing 3D printing, in the step (1), the curing temperature is 100 ℃; in the step (2), the mixing and stirring rotating speed is 500r/min, and the stirring time is 4h; and adding the silicon carbide powder coated by the organosilicon precursor, and continuing stirring for 4 hours.
The viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 122.4 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is 162 mu m.
The preparation method of the silicon carbide blank comprises the following steps:
(1) Adding the silicon carbide ceramic slurry for photocuring 3D printing into 3D printing equipment to print into a blank;
(2) Performing secondary curing on the blank, wherein the secondary curing is performed to heat curing, the curing temperature is 90 ℃, and the curing time is 40min;
(3) And (3) placing the blank after the secondary solidification in a tube furnace, heating from room temperature to 300 ℃ at a heating rate of 3 ℃/min, preserving heat for 2 hours, continuously heating to 600 ℃ at a heating rate of 3 ℃/min, preserving heat for 4 hours, heating to 800 ℃ at a heating rate of 4 ℃/min, preserving heat for 2 hours, and cooling to room temperature to obtain the silicon carbide blank. The surface of the prepared silicon carbide blank body is smooth and flat, and no cracking exists.
Comparative example 1
The difference from example 2 is that:
in the step (1) of the preparation method of the silicon carbide ceramic slurry for photo-curing 3D printing, the mass ratio of silicon carbide to polysiloxane is 1:1;
the viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 123.7 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is measured to be 106 mu m. The mass ratio of silicon carbide to polysiloxane in the formula has little influence on the viscosity of the ceramic slurry, but the silicon carbide powder is influenced to refract ultraviolet light due to the low thickness of the silicon carbide powder coated by the polysiloxane, so that the curing depth of the ceramic slurry is reduced.
Comparative example 2
The difference from example 2 is that:
In the step (1) of the preparation method of the silicon carbide ceramic slurry for photo-curing 3D printing, the mass ratio of silicon carbide to polysiloxane is 1:10;
The viscosity of the prepared silicon carbide ceramic slurry for photocuring 3D printing is 178.9 mPa.s;
2g of the prepared silicon carbide ceramic slurry for photo-curing 3D printing is placed on a printing platform of 3D printing equipment, and ultraviolet light with the wavelength of 405nm is used for irradiating for 10s, so that the curing depth is 168 mu m. When the polysiloxane content is too large, the coated silicon carbide is caused to contain a large amount of cured polysiloxane powder, resulting in an increase in the viscosity of the slurry. In addition, after the thickness of the polysiloxane coated with silicon carbide reaches a certain value, the curing depth of the slurry is not influenced.
Claims (10)
1. The preparation method of the silicon carbide ceramic slurry for photo-curing 3D printing is characterized by comprising the following steps of:
(1) Uniformly dispersing silicon carbide into an organic silicon precursor, and curing to obtain silicon carbide powder coated by the organic silicon precursor, wherein the mass ratio of the silicon carbide to the organic silicon precursor is 1 (2-5);
(2) Mixing and stirring a reactive diluent monomer, a photoinitiator and a dispersing agent, then adding silicon carbide powder coated by an organosilicon precursor, and continuously stirring to obtain silicon carbide ceramic slurry for photocuring 3D printing; the addition amount of the photoinitiator is 2.9-5.1 wt% of the total amount of the reactive diluent monomer and the photoinitiator, the addition amount of the reactive diluent monomer is 20-32 wt% of the total amount of the reactive diluent monomer and the silicon carbide powder coated by the organosilicon precursor, and the addition amount of the dispersing agent is 2.7-7.1 wt% of the total amount of the silicon carbide powder coated by the organosilicon precursor and the dispersing agent.
2. The method for preparing the silicon carbide ceramic slurry for photo-curing 3D printing according to claim 1, wherein the particle size of the silicon carbide is 6-9 μm.
3. The method for preparing a silicon carbide ceramic slurry for photo-curing 3D printing according to claim 1, wherein the organosilicon precursor is one of polycarbosilane, polysilazane, polyborosilazane or polysiloxane.
4. The method for preparing the silicon carbide ceramic slurry for photocuring 3D printing according to claim 1, wherein the reactive diluent monomer is one or more of 1, 6-hexanediol diacrylate, 1, 4-hexanediol diacrylate, tripropylene glycol diacrylate, hydroxyethyl acrylate, trimethylolpropane triacrylate, dipentaerythritol hexaacrylate or pentaerythritol acrylate.
5. The method for preparing a silicon carbide ceramic slurry for photo-curing 3D printing according to claim 1, wherein the photoinitiator is one of 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide, ethyl 2,4, 6-trimethylbenzoyl phenylphosphonate, phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide or 2-phenylbenzyl-2-dimethylamine-1- (4-morpholinophenyl) butanone.
6. The method for preparing the silicon carbide ceramic slurry for photo-curing 3D printing according to claim 1, wherein the dispersing agent is one of BYK410, KOS110 and KOS 2000.
7. The method for preparing the silicon carbide ceramic slurry for photo-curing 3D printing according to claim 1, wherein in the step (1), the curing temperature is 50-100 ℃; in the step (2), the mixing and stirring rotation speed is 400-500 r/min, and the stirring time is 2-4 h; and adding the silicon carbide powder coated by the organic silicon precursor, and continuing stirring for 2-4 hours.
8. The application of the silicon carbide ceramic slurry for photocuring 3D printing is characterized in that the silicon carbide ceramic slurry for photocuring 3D printing prepared by the preparation method of the silicon carbide ceramic slurry for photocuring 3D printing is adopted to prepare a silicon carbide blank body.
9. The use of a silicon carbide ceramic slurry for photo-cured 3D printing according to claim 8, wherein the method for preparing the silicon carbide blank comprises the steps of:
(1) Adding the silicon carbide ceramic slurry for photocuring 3D printing into 3D printing equipment to print into a blank;
(2) Performing secondary curing on the blank;
(3) And (3) placing the blank after secondary solidification in a tube furnace, heating from room temperature to 200-300 ℃ at a heating rate of 1-3 ℃/min, preserving heat for 1-2h, continuously heating to 400-600 ℃ at a heating rate of 1-3 ℃/min, preserving heat for 2-4 h, heating to 800-1000 ℃ at a heating rate of 2-4 ℃/min, preserving heat for 1-2h, and cooling to room temperature to obtain the silicon carbide blank.
10. The application of the silicon carbide ceramic slurry for photo-curing 3D printing according to claim 9, wherein in the step (2), the secondary curing is heat curing, the curing temperature is 90-100 ℃, and the curing time is 20-40 min.
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