CN117362016A - Silicon oxide ceramic core and preparation method thereof - Google Patents
Silicon oxide ceramic core and preparation method thereof Download PDFInfo
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- CN117362016A CN117362016A CN202311074281.0A CN202311074281A CN117362016A CN 117362016 A CN117362016 A CN 117362016A CN 202311074281 A CN202311074281 A CN 202311074281A CN 117362016 A CN117362016 A CN 117362016A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910052814 silicon oxide Inorganic materials 0.000 title claims abstract description 57
- 239000011224 oxide ceramic Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000919 ceramic Substances 0.000 claims abstract description 191
- 238000010438 heat treatment Methods 0.000 claims abstract description 65
- 239000011159 matrix material Substances 0.000 claims abstract description 54
- 239000002245 particle Substances 0.000 claims abstract description 51
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 44
- 239000002002 slurry Substances 0.000 claims abstract description 44
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 38
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000000016 photochemical curing Methods 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 238000010146 3D printing Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000007598 dipping method Methods 0.000 claims abstract description 6
- 239000000178 monomer Substances 0.000 claims description 34
- 239000000377 silicon dioxide Substances 0.000 claims description 27
- 238000006116 polymerization reaction Methods 0.000 claims description 25
- 239000011347 resin Substances 0.000 claims description 21
- 229920005989 resin Polymers 0.000 claims description 21
- 239000002270 dispersing agent Substances 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 19
- 229920000642 polymer Polymers 0.000 claims description 13
- 239000003085 diluting agent Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 9
- INQDDHNZXOAFFD-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOC(=O)C=C INQDDHNZXOAFFD-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 5
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 5
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 4
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 4
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 4
- 229920000053 polysorbate 80 Polymers 0.000 claims description 4
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims description 4
- 229910001950 potassium oxide Inorganic materials 0.000 claims description 4
- 238000001694 spray drying Methods 0.000 claims description 4
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 3
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 3
- LWZFANDGMFTDAV-BURFUSLBSA-N [(2r)-2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O LWZFANDGMFTDAV-BURFUSLBSA-N 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 235000011067 sorbitan monolaureate Nutrition 0.000 claims description 3
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims 3
- 230000000996 additive effect Effects 0.000 claims 3
- 238000005266 casting Methods 0.000 abstract description 13
- 239000011148 porous material Substances 0.000 abstract description 10
- 239000000243 solution Substances 0.000 description 21
- 230000009286 beneficial effect Effects 0.000 description 12
- 238000000465 moulding Methods 0.000 description 9
- 238000005058 metal casting Methods 0.000 description 8
- 238000001723 curing Methods 0.000 description 7
- 238000005452 bending Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229920001451 polypropylene glycol Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 229940113115 polyethylene glycol 200 Drugs 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical group [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- 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
- C04B35/14—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 silica
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/3873—Silicon nitrides, e.g. silicon carbonitride, silicon oxynitride
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6026—Computer aided shaping, e.g. rapid prototyping
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The invention discloses a silicon oxide ceramic core and a preparation method thereof, wherein the preparation method of the silicon oxide ceramic core comprises the following steps: preparing ceramic slurry, wherein the ceramic slurry comprises ceramic particles, and the ceramic particles comprise silicon oxide and silicon nitride; preparing a ceramic matrix blank by photocuring 3D printing based on the ceramic slurry; pre-sintering the ceramic matrix blank to obtain a ceramic matrix; preparing an auxiliary agent solution, dipping the auxiliary agent solution into a ceramic matrix, and then carrying out heating reaction; then sintering to obtain a silicon oxide ceramic core; the problem that scattering phenomenon is easy to occur due to low relative refractive index of ceramic slurry in the process of preparing the silicon oxide ceramic core by the photo-curing 3D printing mode is solved, and accordingly the reduction of forming precision is avoided; and the ceramic core is easy to demould, and meanwhile, the problem that the surface of a casting piece is not smooth due to high pores when the ceramic core is cast is avoided.
Description
Technical Field
The invention relates to the technical field of ceramic cores, in particular to a silicon oxide ceramic core and a preparation method thereof.
Background
Along with the development of aerospace technology, the shape of a ceramic core for casting nickel-based superalloy is more and more complex, the traditional hot-press injection molding cannot meet the requirement of rapid manufacturing of novel hollow blades, rapid manufacturing of a silicon oxide core can be realized through a photocuring 3D printing mode, but due to the fact that the relative refractive index of silicon oxide ceramic and photocuring resin is low, scattering phenomena are prone to occurring in the photocuring process, forming precision is reduced, and the requirement of high precision of core casting cannot be met.
Therefore, improving the molding accuracy in the process of preparing the silicon oxide ceramic core by the 3D printing mode becomes a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to provide a preparation method of a silicon oxide ceramic core, which solves the problems that the relative refractive index of ceramic slurry is low and scattering phenomenon is easy to occur in the process of preparing the silicon oxide ceramic core by a 3D printing mode, thereby avoiding the reduction of molding precision; the critical exposure energy of the silicon oxide ceramic slurry is more than or equal to 173.14mj/cm 2 The critical curing thickness is less than or equal to 356.38 mu m, so that the molding precision is high, the high precision requirement of ceramic core casting is met, the silicon oxide content in the prepared ceramic core is more than or equal to 99.5%, the porosity is high, the demolding is easy, and the problem that the surface of a casting piece is not smooth due to the high porosity when the ceramic core is cast is avoided.
According to one aspect of the present invention, there is provided a method for preparing a silica ceramic core, comprising the steps of:
preparing ceramic slurry, wherein the ceramic slurry comprises ceramic particles, and the ceramic particles comprise silicon oxide and silicon nitride; preparing a ceramic matrix blank by photocuring 3D printing based on the ceramic slurry;
pre-sintering the ceramic matrix blank to obtain a ceramic matrix;
preparing an auxiliary agent solution, dipping the auxiliary agent solution into a ceramic matrix, and then carrying out heating reaction;
then sintering to obtain a silicon oxide ceramic core; preferably, the critical exposure energy of the ceramic slurry is more than or equal to 178 units mj/cm 2 The critical curing thickness is more than or equal to 320 mu m, and the silicon oxide content in the prepared ceramic core is more than or equal to 99.5%.
Compared with the prior art, the invention has the beneficial effects that the ceramic particles comprise silicon oxide and silicon nitride, namely, the relative refractive index of the ceramic slurry is high when the ceramic slurry is used for preparing a ceramic matrix blank body through 3D printing by introducing the silicon nitride, and the scattering phenomenon is obviously reduced in the photo-curing process, so that the critical exposure energy of the ceramic slurry is larger than or equal to 178mj/cm 2 The critical curing thickness is less than or equal to 320 mu m, so that the ceramic matrix blank has high molding precision;
the auxiliary agent solution is prepared, the auxiliary agent solution is immersed into the ceramic matrix, and then the heating reaction is carried out, so that the auxiliary agent is introduced into the ceramic matrix, the auxiliary agent is beneficial to reacting with silicon nitride in the ceramic matrix, the silicon nitride is changed into silicon oxide, and the content of silicon oxide in a finished silicon oxide ceramic core is improved; meanwhile, the surface compactness of the silicon oxide ceramic core is improved through the auxiliary agent, and the smoothness of the surface of a casting piece obtained during the casting of the silicon oxide ceramic core is facilitated.
Further, the ceramic slurry also comprises light-cured resin and a dispersing agent, and is formed by mixing raw materials comprising the ceramic particles, the light-cured resin and the dispersing agent;
the mass ratio of the ceramic particles to the photo-curing resin to the dispersing agent is (40-55): (30-40): (2-5);
the dispersing agent comprises one or more of span 20, tween 80, pick 103 and triton 114;
the light-cured resin comprises a first polymerization monomer, a second polymerization monomer, a diluent and a photoinitiator;
the mass ratio of the first polymerization monomer to the second polymerization monomer to the diluent to the photoinitiator is (60-70): (10-30): (5-15): (0.1-5).
The technical proposal of the last step has the advantages that the ceramic matrix blank body is prepared by 3D printing and has grid-shaped pores; the second silicon nitride ceramic matrix slurry does not comprise a pore-forming agent, so that the problem of carbon residue after volatilization of the pore-forming agent in the ceramic matrix is avoided, disordered volatilization of volatile matters in the sintering process of the ceramic matrix is avoided, uneven pores on the surface of a ceramic core are avoided, and finally the problem of unsmooth surface of a metal piece prepared by casting with the ceramic core is avoided;
the ceramic particles, the photo-curing resin and the dispersing agent are mixed according to the mass proportion, so that the photo-curing resin content is low, and the problem of high porosity of the surface of the ceramic core after sintering is avoided;
the ratio of the first polymerized monomer to the second polymerized monomer is (60-70): (10-30) realizing good fluidity of the ceramic slurry, wherein the green body strength of the silicon nitride ceramic matrix is enough, and the fluidity and dispersibility of the second silicon nitride ceramic matrix slurry are not obviously reduced when the content of the photo-curing resin of the ceramic matrix slurry is low; simultaneously, the pore diameter is uniform when the first polymerization monomer and the second polymerization monomer volatilize in the sintering process, and the problems of difficult volatilization, cracking or damage of the ceramic core and the like are avoided.
Further, the mass ratio of the silicon nitride to the silicon oxide is (1-30): (70-99).
The technical scheme of the above step has the beneficial effects that the mass ratio of the added silicon nitride to the silicon oxide is (1-30): (70-99), namely, the problems of low relative refractive index and easy occurrence of scattering phenomenon in 3D printing are solved, and the silicon oxide content in the finished ceramic core is up to more than 99.5 percent.
Further, the first polymeric monomer comprises one or more of hydroxyethyl acrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate;
the second polymer monomer comprises one or more of pentaerythritol triacrylate, triethylene glycol diacrylate and 1, 6-hexanediol diacrylate;
the diluent comprises n-butanol or isopropanol.
The technical proposal of the above step has the beneficial effects that the chemical formulas of the first polymerization monomer and the second polymerization monomer contain the alcoholic hydroxyl groups, so that the dispersion effect of silicon nitride and silicon oxide in ceramic slurry is obviously improved; the first polymerization monomer has small molecular weight, high curing speed in photoinitiated polymerization, and low molecular weight after polymerization reaction, thereby being beneficial to volatilization in the subsequent sintering process;
the second polymer monomer comprises a plurality of double bond groups, so that the strength of the silicon nitride ceramic matrix blank body is improved, and the forming precision of the ceramic matrix is further improved.
Further, the auxiliary agent solution comprises an auxiliary agent and a solvent; the auxiliary agent comprises one or more of silica sol, zirconium silicate, zirconium oxide, potassium oxide and magnesium oxide; the mass fraction of the auxiliary agent in the auxiliary agent solution is 30-70%.
The technical scheme of the last step has the advantages that after the auxiliary agent solution is immersed in the ceramic matrix, silica sol, zirconium silicate, zirconium oxide, potassium oxide and magnesium oxide in the ceramic auxiliary agent solution react with silicon nitride in the ceramic matrix to change the silicon nitride into silicon oxide, and meanwhile, the surface density of the ceramic core is improved, and the mass fraction of the auxiliary agent solution is 30-70%, so that the impregnation is facilitated, and meanwhile, the surface density of the ceramic core is also facilitated to be high.
Further, the specific process of pre-sintering the ceramic matrix blank is as follows: heating from normal temperature to 400-450 ℃ at a heating rate of 10-14.5 ℃/min, and then heating from 400-450 ℃ to 500-650 ℃ at a heating rate of 5-7 ℃/min; preferably, the temperature is 50-60 ℃ in the process of controlling the ceramic slurry.
The upper technical scheme has the beneficial effects that the temperature is controlled to be 50-60 ℃ by the photo-curing resin, so that the reaction rate during photo-curing is improved;
the temperature is raised to 400-450 ℃ from normal temperature, the heating rate is 10-14.5 ℃/min, the dispersing agent with small molecular weight is favorable for realizing high volatilization speed, pores are slightly larger and are through holes when volatilized although the molecular weight is small, the subsequent polymer with large molecular weight is favorable for volatilizing under the pore diameter generated by the polymer, partial macromolecular polymer is decomposed under the temperature, the rapid heating is favorable for realizing the decomposition of the macromolecular polymer but not volatilized, and the macromolecular polymer is prevented from volatilizing on the basis of the pores generated by volatilization of the original small molecular substance, so that the problems of closed pore generation or nonuniform pore distribution or crack or damage are avoided; the temperature is raised from 400-450 ℃ to 500-650 ℃ at a temperature rise rate of 5-7 ℃/min, so that the volatilization of the macromolecular polymer on the basis of pores caused by volatilization of the original micromolecular substances after the macromolecular polymer is decomposed is facilitated.
Further, the specific process of dipping the auxiliary agent solution into the silicon nitride ceramic matrix and then carrying out the heating reaction is as follows:
heating the silicon nitride ceramic matrix impregnated with the auxiliary agent solution step by step in an air atmosphere; heating from normal temperature to 400-450 ℃ at a heating rate of 10-14.5 ℃/min, heating from 400-450 ℃ to 780-820 ℃ at a heating rate of 5-7 ℃/min, and preserving heat for 2-4 hours at 780-820 ℃.
The technical proposal of the upper part has the advantages that the temperature is increased from normal temperature to 400-450 ℃ through the heating rate of 10-14.5 ℃/min, which is beneficial to the rapid volatilization of the water immersed on the surface and inside of the ceramic matrix and the rapid and uniform adhesion of the auxiliary agent inside the ceramic matrix; the silicon oxide is obtained by the reaction of the auxiliary agent and the silicon nitride in the ceramic matrix through heating from 400-450 ℃ to 780-820 ℃ at the heating rate of 5-7 ℃/min and preserving heat for 2-4 hours, and simultaneously the nitrogen-containing volatile generated by the reaction volatilizes slowly, so that the problem of uneven gaps on the surface of the ceramic matrix caused by the volatilization of the nitrogen-containing volatile is avoided.
Further, the ceramic particles are prepared by granulating silicon nitride and silicon oxide powder, and the specific ceramic particle preparation process comprises the following steps:
preparing ceramic particle slurry, wherein the mass ratio of silicon nitride powder to silicon oxide powder to solvent to carbon powder to binder is (1-30): (70-99): (100-120): (30-35): (10-15) mixing;
then spray drying to obtain a ceramic particle blank; preferably, the binder comprises one or two of polyethylene glycol 200, polyethylene glycol 400, polypropylene glycol 200, polypropylene glycol 400; the solvent is water.
And heating the ceramic particle blank to obtain ceramic particles, wherein the heating treatment process of the ceramic particle blank is that the heat treatment temperature is 300-500 ℃.
The upper technical scheme has the beneficial effects that the silicon nitride and the silicon oxide powder in the ceramic particles are uniformly mixed through granulation, the high internal porosity of the ceramic particles is mainly realized, the low porosity among the ceramic particles is high, and the density is high, so that the ceramic core is easy to break and separate from the metal casting when the ceramic core is separated from the metal casting after casting metal liquid, the metal casting is not damaged, and the surface of the ceramic core is compact, so that the surface of the metal casting is smooth.
Further, the sintering temperature of the ceramic matrix is 1050-1150 ℃.
The upper technical scheme has the beneficial effects that the ceramic core meets the strength and is beneficial to separating the core from the metal casting after casting through the sintering temperature of 1050-1150 ℃.
Another aspect of the present invention provides a silica ceramic core prepared according to the preparation method of the silica ceramic core; preferably, the bending strength of the silicon oxide ceramic mold core is more than or equal to 35MPa, and the molding precision of the silicon oxide ceramic mold is 0.05-0.2mm.
Compared with the prior art, the invention has the beneficial effects that the ceramic particles comprise silicon oxide and silicon nitride, namely, the relative refractive index of the ceramic slurry is high when the ceramic slurry is used for preparing a ceramic matrix blank body through 3D printing by introducing the silicon nitride, and the scattering phenomenon is obviously reduced in the photo-curing process, so that the critical exposure energy of the ceramic slurry is more than or equal to 178mj/cm 2 The critical curing thickness is less than or equal to 320 mu m, so that the ceramic matrix blank has high molding precision; the silicon oxide content in the silicon oxide ceramic core is more than or equal to 99.5 percent;
the surface compactness of the silica ceramic core is beneficial to realizing smooth surface of a casting piece obtained during casting of the silica ceramic core, and the silica ceramic core is easy to separate from a metal casting after casting, so that the problem of metal casting damage caused by separating the silica ceramic core from the metal casting is avoided.
Detailed Description
In order to better understand the technical scheme of the invention, the invention is further described below with reference to specific embodiments and specifications.
Example 1:
in one aspect of this embodiment, a method for preparing a silica ceramic mandrel is provided, including the steps of:
preparing ceramic slurry, wherein the ceramic slurry comprises ceramic particles, photo-curing resin and a dispersing agent; the ceramic particles comprise silicon oxide powder and silicon nitride powder;
mixing the silicon oxide powder, the silicon nitride powder, the photo-curing resin and the dispersing agent in grinding equipment, and dispersing uniformly to obtain the ceramic slurry; the critical exposure energy of the ceramic slurry is 178mj/cm 2 The critical curing thickness is 320 μm.
The mass ratio of the ceramic particles, the photo-curing resin and the dispersing agent is 48:35:3.5; the dispersing agent comprises span 20 and tween 80; the mass ratio of the silicon nitride powder to the silicon oxide powder is 10:90.
the light-cured resin comprises a first polymerization monomer, a second polymerization monomer, a diluent and a photoinitiator; the mass ratio of the first polymerization monomer to the second polymerization monomer to the diluent to the photoinitiator is 65:20:10:2.6;
the first polymerization monomer comprises hydroxyethyl acrylate and hydroxyethyl methacrylate;
the second polymer monomer comprises pentaerythritol triacrylate and triethylene glycol diacrylate; the diluent comprises n-butanol.
Preparing a ceramic matrix blank from the ceramic slurry by photocuring 3D printing based on the ceramic slurry; pre-sintering the ceramic matrix blank to obtain a ceramic matrix;
the specific process of pre-sintering the ceramic matrix blank body is as follows: heating from normal temperature to 425 ℃ at a heating rate of 12 ℃/min, and then heating from 425 ℃ to 575 ℃ at a heating rate of 6 ℃/min; preferably, the temperature is 55 ℃ during the control of the ceramic slurry.
Preparing an auxiliary agent solution, dipping the auxiliary agent solution into a ceramic matrix, and then carrying out heating reaction;
the auxiliary agent solution comprises an auxiliary agent and a solvent; the auxiliary agent comprises silica sol, zirconium silicate and magnesium oxide; the mass fraction of the auxiliary agent in the auxiliary agent solution is 50%;
the specific process of dipping the auxiliary agent solution into the silicon nitride ceramic matrix and then carrying out heating reaction is as follows: heating the silicon nitride ceramic matrix impregnated with the auxiliary agent solution step by step in an air atmosphere; heating from normal temperature to 425 ℃ at a heating rate of 12 ℃/min; heating from 425 ℃ to 800 ℃ at a heating rate of 6 ℃/min, and preserving heat for 3 hours;
then sintering to obtain a silicon oxide ceramic core; the sintering temperature of the ceramic matrix was 1100 ℃.
In another aspect of this embodiment, a silica ceramic mandrel is provided, which is made according to the method of making the silica ceramic mandrel.
The silicon oxide content in the prepared ceramic core is 99.9%, the bending strength of the silicon oxide ceramic core is 35MPa, and the molding accuracy of the silicon oxide ceramic core is 0.12mm.
Example 2:
the same contents of this embodiment as those of embodiment 1 will not be described again; the embodiment differs from embodiment 1 in the following manner:
in one aspect of the embodiment, a preparation method of a silicon oxide ceramic core is provided, wherein the ceramic particles are prepared by granulating silicon nitride and silicon oxide powder, and the preparation process of the specific ceramic particles is as follows:
preparing ceramic particle slurry, namely mixing silicon nitride powder, silicon oxide powder, a solvent, carbon powder and polypropylene glycol 200 according to the mass ratio of 20:80:110:32:12, mixing; then spray drying to obtain a ceramic particle blank; the solvent is water;
heating the ceramic particle blank to obtain ceramic particles, wherein the heating process of the ceramic particle blank is that the heat treatment temperature is 400 ℃;
and mixing the ceramic particles, the photo-curing resin and the dispersing agent in grinding equipment, and uniformly dispersing to obtain the ceramic slurry.
Critical exposure energy of ceramic slurry 180mj/cm 2 Critical cure thickness 315 μm.
The mass ratio of the ceramic particles, the photo-curing resin and the dispersing agent is 53:32:4, a step of; the dispersing agent comprises Pick 103 and triton 114.
The mass ratio of the first polymerization monomer to the second polymerization monomer to the diluent to the photoinitiator is 62:25:13:4, a step of;
the first polymeric monomer comprises hydroxypropyl methacrylate; the second polymer monomer comprises triethylene glycol diacrylate and 1, 6-hexanediol diacrylate; the diluent comprises isopropanol.
The specific process of pre-sintering the ceramic matrix blank body is as follows: heating from normal temperature to 430 ℃ at a heating rate of 13 ℃/min, and then heating from 430 ℃ to 640 ℃ at a heating rate of 6.5 ℃/min; the temperature was 58 ℃ during the control of the ceramic slurry.
The auxiliary agent comprises silica sol, zirconia and potassium oxide; the mass fraction of the auxiliary agent in the auxiliary agent solution is 60%;
carrying out distributed heating on the silicon nitride ceramic matrix impregnated with the auxiliary agent solution in an air atmosphere; heating from normal temperature to 440 ℃ at a heating rate of 13.5 ℃/min; heating from 440 ℃ to 810 ℃ at a heating rate of 6.5 ℃/min, and preserving heat for 2.5 hours; the ceramic substrate was sintered at 1130 ℃.
In another aspect of the embodiment, a silica ceramic core is provided, wherein the silica content in the prepared ceramic core is 99.8%, the bending strength of the silica ceramic core is 36MPa, and the molding accuracy of the silica ceramic mold is 0.06mm.
Example 3:
the content of this embodiment, which is the same as that of embodiment 2, will not be described again; the embodiment differs from embodiment 2 in the following manner:
in one aspect of the embodiment, a preparation method of a silicon oxide ceramic core is provided, wherein the ceramic particles are prepared by granulating silicon nitride and silicon oxide powder, and the preparation process of the specific ceramic particles is as follows:
preparing ceramic particle slurry, namely mixing silicon nitride powder, silicon oxide powder, a solvent, carbon powder and polyethylene glycol 200 according to the mass ratio of 28:72:115:31:11, mixing; then spray drying to obtain a ceramic particle blank;
heating the ceramic particle blank to obtain ceramic particles, wherein the heating process of the ceramic particle blank is that the heat treatment temperature is 450 ℃;
and mixing the ceramic particles, the photo-curing resin and the dispersing agent in grinding equipment, and uniformly dispersing to obtain the ceramic slurry.
Critical exposure energy 181mj/cm of ceramic slurry 2 The critical curing thickness is 312 μm.
The mass ratio of the ceramic particles, the photo-curing resin and the dispersing agent is 43:38:3, a step of; the dispersing agent comprises tween 80 and Pick 103.
The mass ratio of the first polymerization monomer to the second polymerization monomer to the diluent to the photoinitiator is 78:15:8:1, a step of;
the first polymerization monomer comprises hydroxyethyl acrylate and hydroxypropyl methacrylate;
the second polymer monomer comprises pentaerythritol triacrylate and 1, 6-hexanediol diacrylate;
the specific process of pre-sintering the ceramic matrix blank body is as follows: after the temperature was raised from normal temperature to 410℃at a temperature-raising rate of 11/min, the temperature was raised from 410℃to 580℃at a temperature-raising rate of 5.5℃per minute.
The auxiliary agent comprises zirconium silicate and magnesium oxide; the mass fraction of the auxiliary agent in the auxiliary agent solution is 40%;
carrying out distributed heating on the silicon nitride ceramic matrix impregnated with the auxiliary agent solution in an air atmosphere; heating from normal temperature to 410 ℃ at a heating rate of 11 ℃/min; the temperature was raised from 410℃to 785℃at a heating rate of 5.5℃per minute, and the temperature was kept for 3.5 hours. The sintering temperature of the ceramic matrix is 1080 ℃.
In another aspect of the embodiment, a silica ceramic core is provided, the silica content in the prepared ceramic core is greater than 99.6%, the flexural strength of the silica ceramic core is 37MPa, and the molding accuracy of the silica ceramic core is 0.1mm.
The foregoing description is only of the preferred embodiments of the present application and is presented as a description of the principles of the technology being utilized. It will be appreciated by persons skilled in the art that the scope of the invention referred to in this application is not limited to the specific combinations of features described above, but it is intended to cover other embodiments in which any combination of features described above or equivalents thereof is possible without departing from the spirit of the invention. Such as the features described above, have similar functionality as disclosed (but not limited to) in this application.
Claims (10)
1. The preparation method of the silicon oxide ceramic core is characterized by comprising the following steps:
preparing ceramic slurry, wherein the ceramic slurry comprises ceramic particles, and the ceramic particles comprise silicon oxide and silicon nitride;
preparing a ceramic matrix blank by photocuring 3D printing based on the ceramic slurry;
pre-sintering the ceramic matrix blank to obtain a ceramic matrix;
preparing an auxiliary agent solution, dipping the auxiliary agent solution into a ceramic matrix, and then carrying out heating reaction;
and then sintering to obtain the silicon oxide ceramic core.
2. The method for producing a silica ceramic core according to claim 1, wherein the ceramic slurry further comprises a photocurable resin and a dispersant, and the ceramic slurry is formed by mixing raw materials comprising the ceramic particles, the photocurable resin and the dispersant;
the mass ratio of the ceramic particles to the photo-curing resin to the dispersing agent is (40-55): (30-40): (2-5);
the dispersing agent comprises one or more of span 20, tween 80, pick 103 and triton 114;
the light-cured resin comprises a first polymerization monomer, a second polymerization monomer, a diluent and a photoinitiator;
the mass ratio of the first polymerization monomer to the second polymerization monomer to the diluent to the photoinitiator is (60-70): (10-30): (5-15): (0.1-5).
3. The method of producing a silica ceramic mandrel according to claim 1, wherein the mass ratio of silicon nitride to silicon oxide is (1-30): (70-99).
4. The method of preparing a silica ceramic mandrel according to claim 2, wherein the first polymeric monomer comprises one or more of hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate;
the second polymer monomer comprises one or more of pentaerythritol triacrylate, triethylene glycol diacrylate and 1, 6-hexanediol diacrylate;
the diluent comprises n-butanol or isopropanol.
5. The method for preparing a silica ceramic core according to claim 1, wherein the additive solution comprises an additive and a solvent; the auxiliary agent comprises one or more of silica sol, zirconium silicate, zirconium oxide, potassium oxide and magnesium oxide; the mass fraction of the auxiliary agent in the auxiliary agent solution is 30-70%.
6. The method for preparing a silica ceramic core according to claim 1, wherein the ceramic base body is pre-sintered by the following steps:
heating from normal temperature to 400-450 ℃ at a heating rate of 10-14.5 ℃/min, and then heating from 400-450 ℃ to 500-650 ℃ at a heating rate of 5-7 ℃/min.
7. The method for preparing a silica ceramic core according to claim 1, wherein the specific process of immersing the additive solution in the ceramic matrix and then performing the heating reaction is as follows:
heating the ceramic matrix impregnated with the auxiliary agent solution step by step in an air atmosphere; heating from normal temperature to 400-450 ℃ at a heating rate of 10-14.5 ℃/min, and then heating from 400-450 ℃ to 780-820 ℃ at a heating rate of 5-7 ℃/min; and preserving the temperature for 2 to 4 hours at 780 to 820 ℃.
8. The preparation method of the silicon oxide ceramic core according to claim 1, wherein the ceramic particles are prepared by granulating silicon nitride and silicon oxide powder, and the specific ceramic particle preparation process is as follows:
preparing ceramic particle slurry, wherein the mass ratio of silicon nitride powder to silicon oxide powder to solvent to carbon powder to binder is (1-30): (70-99): (100-120): (30-35): (10-15) mixing;
then spray drying to obtain a ceramic particle blank;
and heating the ceramic particle blank to obtain ceramic particles, wherein the heating treatment process of the ceramic particle blank is that the heat treatment temperature is 300-500 ℃.
9. The method of producing a silica ceramic core according to claim 1, wherein the sintering temperature of the ceramic matrix is 1050-1150 ℃.
10. A silica ceramic core, characterized in that it is produced according to the method for producing a silica ceramic core according to any one of claims 1 to 9.
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