CN114907133B - Silicon-based ceramic core material, preparation method and silicon-based ceramic core - Google Patents
Silicon-based ceramic core material, preparation method and silicon-based ceramic core Download PDFInfo
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- 239000011162 core material Substances 0.000 title claims abstract description 229
- 239000000919 ceramic Substances 0.000 title claims abstract description 218
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 145
- 239000010703 silicon Substances 0.000 title claims abstract description 145
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 182
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 42
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000011819 refractory material Substances 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 65
- 239000004014 plasticizer Substances 0.000 claims description 51
- 238000005728 strengthening Methods 0.000 claims description 36
- 238000005245 sintering Methods 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 21
- 239000002002 slurry Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 239000000377 silicon dioxide Substances 0.000 claims description 17
- -1 borides Chemical class 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 235000015895 biscuits Nutrition 0.000 claims description 14
- 239000004698 Polyethylene Substances 0.000 claims description 12
- 239000012188 paraffin wax Substances 0.000 claims description 12
- 229920000573 polyethylene Polymers 0.000 claims description 12
- 235000013871 bee wax Nutrition 0.000 claims description 11
- 239000012166 beeswax Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 239000012744 reinforcing agent Substances 0.000 claims description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 238000001746 injection moulding Methods 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- 150000001247 metal acetylides Chemical class 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
- 239000004482 other powder Substances 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 238000005056 compaction Methods 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- 239000000306 component Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 8
- 238000000227 grinding Methods 0.000 description 7
- 238000003837 high-temperature calcination Methods 0.000 description 7
- 238000000465 moulding Methods 0.000 description 7
- 238000005266 casting Methods 0.000 description 6
- 238000005495 investment casting Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 230000001089 mineralizing effect Effects 0.000 description 4
- 239000008358 core component Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 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
- 239000002356 single layer Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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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
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/10—Cores; Manufacture or installation of cores
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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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- 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
- 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
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63408—Polyalkenes
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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
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63496—Bituminous materials, e.g. tar, pitch
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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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
- C04B2235/3248—Zirconates or hafnates, e.g. zircon
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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
- C04B2235/65—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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- C04B2235/656—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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The invention provides a silicon-based ceramic core material, which comprises silicon-based ceramic core powder, wherein the silicon-based ceramic core powder comprises refractory material powder and mineralizer, and is characterized in that the refractory material powder accounts for 65-85% of the silicon-based ceramic core powder in percentage by mass, the mineralizer comprises zirconium silicate powder and silicon nitride powder, the zirconium silicate powder accounts for 5-15% of the silicon-based ceramic core powder in percentage by mass, and the silicon nitride powder accounts for 5-30% of the silicon-based ceramic core powder in percentage by mass. The invention also provides a corresponding preparation method of the silicon-based ceramic core and the silicon-based ceramic core. By applying the technical scheme of the invention, the problems of large size shrinkage, inconsistent thickness shrinkage, low high-temperature strength, large high-temperature deflection and the like of the silicon-based ceramic core are solved.
Description
Technical Field
The invention relates to a preparation method of a silicon-based ceramic core and the silicon-based ceramic core, in particular to a preparation method of a silicon-based ceramic core for near-zero shrinkage investment casting and the silicon-based ceramic core.
Background
The gas turbine has the advantages of compact structure, high power density, flexible start and stop, cleanness, high efficiency, wide application range of fuel and the like, is core equipment in the fields of aviation, ships and energy, has extremely high military value and economic value, is known as a 'bright bead on crown' in equipment manufacturing industry, and is a 'national heavy device' related to national security and national economic development. Turbine blades are the core components of high performance gas turbines, and as the performance requirements for gas turbines are increasing, higher requirements are also being placed on the heat resistance of the turbine blades.
Blade cooling technology is one of the most effective approaches to improving turbine blade heat resistance. With the development of blade cooling technology, the blade cooling mode has been developed from the initial modes of convection cooling, impact cooling, film cooling and the like to the current more advanced blade cooling modes of divergent cooling, laminate cooling and the like. The hollow blade has finer and more complicated cavity shape design, and a single-layer wall structure, a double-layer wall structure and even a multi-layer wall structure are sequentially arranged. How to manufacture the blade with the complex inner cavity structure is a challenge, conventional processing modes such as forging and pressing, electrochemical processing and the like cannot meet the manufacturing requirements of the blade, and precision investment manufacturing becomes a key means for solving the manufacturing of the hollow blade, so that the method has wide application at present. The ceramic core is a core component in the precision investment manufacturing process, plays a decisive role in the quality of castings, and the manufacturing level of the ceramic core has important significance on the quality, manufacturing cost, product qualification rate and the like of hollow blades.
Silica-based ceramic cores are one of the most widely used ceramic cores at present. The firing temperature of the silicon-based ceramic core is 1150-1250 ℃, the use temperature is 1520-1560 ℃, and the finished product rate is higher under the casting condition of 1500-1550 ℃, and the core is easy to be corroded and removed by alkali liquor. However, because the inner cavity structure of the part is more refined, the difference of the sizes of the thick wall and the thin wall is large, the produced ceramic core is inconsistent in shrinkage, so that the problems of core fracture, low high-temperature strength, large high-temperature deflection and the like can be caused, and the core deviation, core exposure and core breakage in the investment casting process can be caused. In particular to a ceramic core with double-layer walls, multi-layer walls and large-size structures, the thick and thin connecting parts of the ceramic core still have larger deformation and cracks in the sintering process, and the production efficiency is reduced.
The prior art CN104384452A discloses a preparation process of a thin-wall silicon-based ceramic core, wherein the ceramic core material consists of 70% -85% of quartz glass powder and 15% -30% of M75 type mullite powder, and the plasticizer consists of 97% of white paraffin and 3% of polyethylene; the core pressing process parameters are as follows: the preheating temperature of the die is 30-45 ℃, the slurry temperature is 95-110 ℃, the injection pressure is 2.0-3.0 MPa, and the pressure maintaining time is 15-20 s; the core sintering process parameters are as follows: heat preservation at 200 ℃ for 4h,400 ℃ for 4h,600 ℃ for 1h,900 ℃ for 1h, and final firing temperature 1150-1160 ℃ for 4h; after sintering, adopting an ethyl silicate reinforcing agent to carry out high-temperature reinforcement, and adopting a low-temperature reinforcing agent prepared from epoxy resin, polyamide resin and acetone according to a certain proportion to carry out low-temperature reinforcement; and finally baking. The thin-wall silicon-based ceramic core prepared by the process has the advantages that the yield can reach more than 85%, the core interruption rate in the casting process is lower than 8%, the shrinkage rate is small, the room-temperature and high-temperature strength is good, the dimensional accuracy is high, the thin-wall silicon-based ceramic core is not deformed in the casting process, the core is easy to take off, and the casting requirement of a thin-wall casting with a complex cavity can be met.
However, the preparation method of the silicon-based ceramic core in the prior art still has the problems of inconsistent core shrinkage, low high-temperature strength, large high-temperature deflection and the like, and then the problems of core deformation, cracking and even fracture are caused.
Disclosure of Invention
The invention mainly aims to provide a silicon-based ceramic core powder, a preparation method of a silicon-based ceramic core and the silicon-based ceramic core, so as to solve the problems in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a silica-based ceramic core material comprising a silica-based ceramic core powder comprising a refractory powder and a mineralizer, wherein the refractory powder comprises 65 to 85% by mass of the silica-based ceramic core powder, the mineralizer comprises a zirconium silicate powder and a silicon nitride powder, the zirconium silicate powder comprises 5 to 15% by mass of the silica-based ceramic core powder, and the silicon nitride powder comprises 5 to 30% by mass of the silica-based ceramic core powder.
Further, the refractory material powder is quartz glass powder, and the particle size is 100-300 meshes.
Further, the silicon nitride powder is irregularly-shaped beta-Si 3 N 4 The powder has a particle size of 200-400 mesh.
Further, the grain size of the zirconium silicate powder is 300-350 meshes, and the zirconium silicate powder accounts for 10% of the mass of the silicon-based ceramic core powder.
Further, the silicon-based ceramic core powder comprises the following components in percentage by weight:
80% of quartz glass powder, 10% of zirconium silicate powder and 10% of silicon nitride powder; or alternatively
75% of quartz glass powder, 10% of zirconium silicate powder and 15% of silicon nitride powder; or alternatively
70% of quartz glass powder, 10% of zirconium silicate powder and 20% of silicon nitride powder; or alternatively
65% of quartz glass powder, 10% of zirconium silicate powder and 25% of silicon nitride powder.
Further, the silicon-based ceramic core powder also includes other powder components including one or more of other oxides, carbides, borides, and nitrides.
Further, the refractory material powder, the zirconium silicate powder and the silicon nitride powder are mixed by a three-dimensional mixer to form the silicon-based ceramic core powder.
Further, the ceramic core material also comprises a plasticizer, wherein the mass of the plasticizer is 12-20% of that of the silicon-based ceramic core material.
Further, the mass of the plasticizer is 16% of the mass of the silicon-based ceramic core material.
Further, the plasticizer is a mixture of paraffin wax, beeswax and polyethylene.
According to another aspect of the present invention, there is provided a method for producing a silica-based ceramic core, comprising a powder mixing step, a slurry preparation step, a green compact pressing step and a sintering step, which are sequentially performed, wherein the above-mentioned silica-based ceramic core powder is used in the powder mixing step.
Further, in the slurry preparation step, a plasticizer is mixed with the silicon-based ceramic core powder, the mass of the plasticizer being 12-20% of the mass of the silicon-based ceramic core material.
Further, the mass of the plasticizer is 16% of the mass of the silicon-based ceramic core material.
Further, the plasticizer is a mixture of paraffin wax, beeswax and polyethylene.
Further, a strengthening step is further included, which is performed after the sintering step, in which the strength of the silicon-based ceramic core is improved using a strengthening agent.
Further, in the powder mixing step, the silicon-based ceramic core powder is filled into a ball milling tank for mixing, the mass ratio of the silicon-based ceramic core powder to zirconia balls is 1:2, the rotating speed of the ball milling machine is 200r/min, the ball milling time is 12h, and the uniformly mixed silicon-based ceramic core powder is subjected to drying treatment for 10h.
Further, in the step of preparing the slurry, the plasticizer is placed into a mixing barrel at 90 ℃, after the plasticizer is completely melted, the dried silicon-based ceramic core powder is added into the mixing barrel in batches, stirring is carried out under high vacuum, 0.1% of oleic acid is added in the process, and after all the silicon-based ceramic core powder is added, stirring is continued to be carried out under vacuum for 4 hours uniformly, so that the slurry is obtained.
Further, in the biscuit pressing step, a biscuit is pressed by adopting a hot-pressing injection molding method, the slurry is placed into a ceramic core pressing injection machine, the slurry temperature is set to 90 ℃, the injection pressure is set to 4MPa, the dwell time is set to 25S, and the slurry is pressed into a die to prepare the biscuit.
Further, in the sintering step, the corrected biscuit is buried in a sagger of alpha-Al 2O3 powder, the thickness of filler at the top of the biscuit is not less than 25mm, after the biscuit is completely filled in the sagger, the filler is compacted by a rubber hammer, and then the biscuit is placed in a box-type resistance furnace for sintering, wherein the sintering system is as follows: heating to 250 ℃ at a heating rate of 0.1-3 ℃/min, preserving heat for 200-300 min, heating to 600 ℃ at a heating rate of 0.1-3 ℃/min, preserving heat for 100-200 min, heating to 1200 ℃ at a heating rate of 0.1-5 ℃/min, preserving heat for 100-200 min, and cooling to room temperature along with a furnace to obtain the silicon-based ceramic core.
Further, the strengthening step includes at least one of a high temperature strengthening step and a room temperature strengthening step.
Further, in the high-temperature strengthening step, the sintered silicon-based ceramic core is immersed in a high-temperature strengthening agent under vacuum for 6 hours, the silicon-based ceramic core is taken out after bubbles completely disappear, residual liquid on the surface of the silicon-based ceramic core is wiped off, and the silicon-based ceramic core after high-temperature strengthening is obtained after the silicon-based ceramic core is self-dried for more than 24 hours, wherein the high-temperature strengthening agent is liquid silica sol.
Further, in the room temperature strengthening step, the ceramic core is completely soaked in a room temperature strengthening agent, the ceramic core is placed in a vacuum drying oven, vacuumizing is carried out for 3-5 min at room temperature for 10min, excessive liquid on the surface is wiped off until the surface is smooth and clean, the ceramic core is placed in the vacuum drying oven at 55 ℃ for heat preservation for 1h for drying treatment, and the ceramic core is taken out after cooling, so that the silicon-based ceramic core after the room temperature strengthening is obtained, wherein the room temperature strengthening agent is epoxy resin: polyamide: acetone: methanol=3.4: 2:3.8:0.8 of a reinforcing agent.
According to another aspect of the present invention, there is provided a silicon-based ceramic core, characterized in that the silicon-based ceramic core is prepared using the preparation method of the silicon-based ceramic core.
By applying the technical scheme of the invention, at least the following beneficial effects are realized:
1. the invention starts from the excellent performance of the silicon-based ceramic core, improves the types of mineralizing agents, and combines zirconium silicate and silicon nitride as the mineralizing agents, thereby establishing the ceramic core of a complex ternary system and solving the problems of large size shrinkage, inconsistent thickness wall shrinkage, low high-temperature strength, large high-temperature deflection and the like of the silicon-based ceramic core.
2. The invention also optimizes and adjusts the mineralizer content, especially the content of silicon nitride, of the added core, so that the shrinkage rate of the ceramic core after sintering is close to zero, and the comprehensive performance of the ceramic core is further improved, and the prepared silicon-based ceramic core can be applied to preparing single crystal blades with more complex cavities.
3. The invention also provides a solution for the corresponding ceramic core preparation process, so that the performance of the ceramic core can be further improved by utilizing a proper process on the basis of selecting reasonable material proportion, and the yield and the product precision of investment casting are improved.
4. According to the invention, a certain amount of plasticizer is used in the preparation of the ceramic core, and the components and the dosage of the plasticizer are specially adjusted and optimized, so that the improvement of the preparation effect of the ceramic core is facilitated.
5. The invention sets the strengthening step in the preparation process of the ceramic core, and further improves the performances such as strength and the like of the ceramic core by utilizing the strengthening step.
Detailed Description
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other. The present invention will be described in detail with reference to examples.
The invention is described in further detail below in connection with specific examples which are not to be construed as limiting the scope of the invention as claimed.
Example 1
The preparation of the near-zero shrinkage silicon-based ceramic core material and the silicon-based ceramic mold comprises silicon-based ceramic core powder and plasticizer, wherein the silicon-based ceramic core powder comprises the following components in percentage by mass: 80% of quartz glass powder, 10% of zirconium silicate powder and 10% of silicon nitride powder, wherein the plasticizer accounts for 16% of the total mass of the ceramic core material. Preferably, the plasticizer is a mixture of paraffin wax, beeswax, polyethylene.
Preferably, the particle size of the quartz glass powder is 200 meshes, and the silicon nitride powder is irregularly shaped beta-Si 3 N 4 The powder has a particle size of 300 meshes, the zirconium silicate has a particle size of 325 meshes, and the powder is prepared by high-temperature calcination, grinding and self-making.
Preferably, the quartz glass powder, zirconium silicate and silicon nitride are mixed by a three-dimensional mixer.
The embodiment also provides a preparation method of the near-zero shrinkage ceramic core, which comprises the following steps:
mixing powder: the mixed silicon-based ceramic core powder required by the experiment is prepared according to a certain proportion, the prepared powder is filled into a ball milling tank for mixing, the mass ratio of the mixed powder to zirconia balls is 1:2, the rotating speed of the ball milling machine is 200r/min, and the ball milling time is 12h. And drying the uniformly mixed powder for 10 hours.
And (3) preparing slurry: weighing a certain amount of plasticizer, putting into a mixing barrel at 90 ℃, after the plasticizer is completely melted, adding the dried powder into the mixing barrel in batches according to a certain amount, and stirring under high vacuum. 0.1% oleic acid is added in the mixing process. After the powder is completely added, continuously stirring for 4 hours under vacuum uniformly, and obtaining the slurry with the powder uniformly dispersed in the plasticizer.
And (3) biscuit pressing: the biscuit is pressed by adopting a hot-pressing injection molding method. And (3) placing the ceramic core slurry into a ceramic core pressing and injecting machine, and pressing the ceramic core slurry into a die to prepare a ceramic core biscuit when parameters of the pressing and injecting machine are consistent with set values (the slurry temperature is 90 ℃, the injection pressure is 4Mpa and the pressure maintaining time is 25S).
Sintering: the corrected biscuit is filled in a sagger filled with alpha-Al 2O3 powder with the grain diameter of about 100 meshes. And the thickness of the filler at the top of the core biscuit is not less than 25mm, and after the core biscuit is completely filled into the sagger, the filler is subjected to compaction by a rubber hammer and then is placed into a box-type resistance furnace for sintering. Sintering system: heating to 250 ℃ at a heating rate of 0.1-3 ℃/min, preserving heat for 200-300 min, heating to 600 ℃ at a heating rate of 0.1-3 ℃/min, preserving heat for 100-200 min, heating to 1200 ℃ at a heating rate of 0.1-5 ℃/min, preserving heat for 100-200 min, and cooling to room temperature along with a furnace to obtain the silicon-based ceramic core.
Strengthening: and (3) selecting liquid silica sol for high-temperature strengthening, immersing the sintered core in a high-temperature strengthening agent under vacuum for 6 hours, taking out after bubbles completely disappear, wiping off residual liquid on the surface of the core, and self-drying for more than 24 hours to obtain the ceramic core after high-temperature strengthening. Room temperature reinforcing selected epoxy resin: polyamide: acetone: methanol=3.4: 2:3.8: 0.8. The ceramic core is completely soaked in the core strengthening liquid, placed in a vacuum drying oven, vacuumized for 3-5 min at room temperature and soaked for 10min. And taking out and wiping off superfluous protective liquid on the surface until the surface is smooth and clean. And (5) placing the ceramic core in a vacuum drying box at 55 ℃ for heat preservation for 1h for drying treatment, cooling and taking out the ceramic core to obtain the ceramic core reinforced at room temperature.
The silicon-based ceramic core prepared by the embodiment has the molding rate of more than 95%, the sintering shrinkage rate of 0.52%, the room temperature strength of 24.2MPa, the high temperature strength of 22.8MPa and the high temperature deflection of 0.71mm.
Example 2
The preparation of the near-zero shrinkage silicon-based ceramic core material and the silicon-based ceramic mold comprises silicon-based ceramic core powder and plasticizer, wherein the silicon-based ceramic core powder comprises the following components in percentage by mass: 75% of quartz glass powder, 10% of zirconium silicate powder and 15% of silicon nitride powder, wherein the plasticizer accounts for 16% of the total mass of the ceramic core material.
Preferably, the plasticizer is a mixture of paraffin wax, beeswax, polyethylene.
Preferably, the particle size of the quartz glass powder is 200 meshes, and the silicon nitride powder is irregularly shaped beta-Si 3 N 4 The powder has a particle size of 300 meshes, the zirconium silicate has a particle size of 325 meshes, and the powder is prepared by high-temperature calcination, grinding and self-making.
Preferably, the quartz glass powder, zirconium silicate and silicon nitride are mixed by a three-dimensional mixer.
The preparation process of the silicon-based ceramic core of this example is the same as that of example 1 and the process parameters are finely adjusted according to the difference of materials.
The silicon-based ceramic core prepared by the embodiment has the molding rate of more than 95%, the sintering shrinkage rate of 0.31%, the room temperature strength of 22.8MPa, the high temperature strength of 21.3MPa and the high temperature deflection of 0.82mm.
Example 3
The preparation of the near-zero shrinkage silicon-based ceramic core material and the silicon-based ceramic mold comprises silicon-based ceramic core powder and plasticizer, wherein the silicon-based ceramic core powder comprises the following components in percentage by mass: 70% of quartz glass powder, 10% of zirconium silicate powder and 20% of silicon nitride powder, wherein the plasticizer accounts for 16% of the total mass of the ceramic core material.
Preferably, the plasticizer is a mixture of paraffin wax, beeswax, polyethylene.
Preferably, the particle size of the quartz glass powder is 200 meshes, and the silicon nitride powder is irregularly shaped beta-Si 3 N 4 The powder has a particle size of 300 meshes, the zirconium silicate has a particle size of 325 meshes, and the powder is prepared by high-temperature calcination, grinding and self-making.
Preferably, the quartz glass powder, zirconium silicate and silicon nitride are mixed by a three-dimensional mixer.
The preparation process of the silicon-based ceramic core of this example is the same as that of example 1 and the process parameters are finely adjusted according to the difference of materials.
The silicon-based ceramic core prepared by the embodiment has the molding rate of more than 96%, the sintering shrinkage rate of 0.09%, the room temperature strength of 20.1MPa, the high temperature strength of 20.8MPa and the high temperature deflection of 0.85mm, and is suitable for manufacturing single crystal blades with higher inner cavity size precision.
Example 4
The preparation of the near-zero shrinkage silicon-based ceramic core material and the silicon-based ceramic mold comprises silicon-based ceramic core powder and plasticizer, wherein the silicon-based ceramic core powder comprises the following components in percentage by mass: 65% of quartz glass powder, 10% of zirconium silicate powder and 25% of silicon nitride powder, wherein the plasticizer accounts for 16% of the total mass of the ceramic core material.
Preferably, the plasticizer is a mixture of paraffin wax, beeswax, polyethylene.
Preferably, the particle size of the quartz glass powder is 200 meshes, and the silicon nitride powder is irregularly shaped beta-Si 3 N 4 The powder has a particle size of 300 meshes, the zirconium silicate has a particle size of 325 meshes, and the powder is prepared by high-temperature calcination, grinding and self-making.
Preferably, the quartz glass powder, zirconium silicate and silicon nitride are mixed by a three-dimensional mixer.
The preparation process of the silicon-based ceramic core of this example is the same as that of example 1 and the process parameters are finely adjusted according to the difference of materials.
The silicon-based ceramic core prepared by the embodiment has the molding rate of more than 95%, the sintering shrinkage rate of-0.04%, the room temperature strength of 18.4MPa, the high temperature strength of 15.6MPa and the high temperature deflection of 0.97mm.
Example 5
The preparation of the near-zero shrinkage silicon-based ceramic core material and the silicon-based ceramic mold comprises silicon-based ceramic core powder and plasticizer, wherein the silicon-based ceramic core powder comprises the following components in percentage by mass: 75% of quartz glass powder, 5% of zirconium silicate powder and 20% of silicon nitride powder, wherein the plasticizer accounts for 12% of the total mass of the ceramic core material.
Preferably, the plasticizer is a mixture of paraffin wax, beeswax, polyethylene.
Preferably, the particle size of the quartz glass powder is 100 meshes, and the silicon nitride powder is irregularly shaped beta-Si 3 N 4 The powder has a grain size of 200 meshes, the zirconium silicate has a grain size of 300 meshes, and the powder is prepared by high-temperature calcination, grinding and self-making。
Preferably, the quartz glass powder, zirconium silicate and silicon nitride are mixed by a three-dimensional mixer.
The preparation process of the silicon-based ceramic core of this example is the same as that of example 1 and the process parameters are finely adjusted according to the difference of materials.
The silicon-based ceramic core prepared by the embodiment has the molding rate of more than 95 percent, the sintering shrinkage rate of 0.12 percent, the room temperature strength of 21.1MPa, the high temperature strength of 21.0MPa and the high temperature deflection of 0.83mm.
Example 6
The preparation of the near-zero shrinkage silicon-based ceramic core material and the silicon-based ceramic mold comprises silicon-based ceramic core powder and plasticizer, wherein the silicon-based ceramic core powder comprises the following components in percentage by mass: 75% of quartz glass powder, 15% of zirconium silicate powder and 10% of silicon nitride powder, wherein the plasticizer accounts for 20% of the total mass of the ceramic core material.
Preferably, the plasticizer is a mixture of paraffin wax, beeswax, polyethylene.
Preferably, the particle size of the quartz glass powder is 300 meshes, and the silicon nitride powder is irregularly shaped beta-Si 3 N 4 The powder has the particle size of 400 meshes, the particle size of zirconium silicate is 350 meshes, and the zirconium silicate is prepared by high-temperature calcination, grinding and self-making.
Preferably, the quartz glass powder, zirconium silicate and silicon nitride are mixed by a three-dimensional mixer.
The preparation process of the silicon-based ceramic core of this example is the same as that of example 1 and the process parameters are finely adjusted according to the difference of materials.
The silicon-based ceramic core prepared by the embodiment has the molding rate of more than 95%, the sintering shrinkage rate of 0.49%, the room temperature strength of 23.9MPa, the high temperature strength of 21.9MPa and the high temperature deflection of 0.75mm.
Example 7
The preparation of the near-zero shrinkage silicon-based ceramic core material and the silicon-based ceramic mold comprises silicon-based ceramic core powder and plasticizer, wherein the silicon-based ceramic core powder comprises the following components in percentage by mass: 65% of quartz glass powder, 5% of zirconium silicate powder and 30% of silicon nitride powder, wherein the plasticizer accounts for 16% of the total mass of the ceramic core material.
Preferably, the plasticizer is a mixture of paraffin wax, beeswax, polyethylene.
Preferably, the particle size of the quartz glass powder is 300 meshes, and the silicon nitride powder is irregularly shaped beta-Si 3 N 4 The powder has the particle size of 400 meshes, the particle size of zirconium silicate is 350 meshes, and the zirconium silicate is prepared by high-temperature calcination, grinding and self-making.
Preferably, the quartz glass powder, zirconium silicate and silicon nitride are mixed by a three-dimensional mixer.
The preparation process of the silicon-based ceramic core of this example is the same as that of example 1 and the process parameters are finely adjusted according to the difference of materials.
The silicon-based ceramic core prepared by the embodiment has the molding rate of more than 95%, the sintering shrinkage rate of-0.05%, the room temperature strength of 18.1MPa, the high temperature strength of 15.2MPa and the high temperature deflection of 0.99mm.
Example 8
The preparation of the near-zero shrinkage silicon-based ceramic core material and the silicon-based ceramic mold comprises silicon-based ceramic core powder and plasticizer, wherein the silicon-based ceramic core powder comprises the following components in percentage by mass: 80% of quartz glass powder, 10% of zirconium silicate powder and 10% of silicon nitride powder, wherein the plasticizer accounts for 16% of the total mass of the ceramic core material.
The preparation process of the silicon-based ceramic core in this embodiment differs from that in embodiment 1 in that no strengthening step is provided after the sintering step, and after the sintering step, the properties of the ceramic core are still in the ideal range, and the requirements of the complex single crystal blade on the sintering shrinkage rate, the room temperature strength, the high temperature strength and the high temperature deflection of the ceramic core can still be satisfied.
It should be added that, in order to regulate the performance of the silicon-based ceramic core, the silicon-based ceramic core powder may further include an appropriate amount of other powder components including one or more of other oxides, carbides, borides and nitrides, such as alumina, silicon carbide, etc.
The technical scheme of the invention can be used for manufacturing turbine blades of gas turbines, and can be applied to manufacturing turbine blades, superalloy blades and other investment casting in other fields to obtain ideal effects.
From the above description, it can be seen that the above embodiments of the present invention achieve the following technical effects:
1. the invention starts from the excellent performance of the silicon-based ceramic core, improves the types of mineralizing agents, and combines zirconium silicate and silicon nitride as the mineralizing agents, thereby establishing the ceramic core of a complex ternary system and solving the problems of large size shrinkage, inconsistent thickness wall shrinkage, low high-temperature strength, large high-temperature deflection and the like of the silicon-based ceramic core.
2. The invention also optimizes and adjusts the mineralizer content, especially the content of silicon nitride, of the added core, so that the shrinkage rate of the ceramic core after sintering is close to zero, and the comprehensive performance of the ceramic core is further improved, and the prepared silicon-based ceramic core can be applied to preparing single crystal blades with more complex cavities.
3. The invention also provides a solution for the corresponding ceramic core preparation process, so that the performance of the ceramic core can be further improved by utilizing a proper process on the basis of selecting reasonable material proportion, and the yield and the product precision of investment casting are improved.
4. According to the invention, a certain amount of plasticizer is used in the preparation process of the ceramic core, and the components and the dosage of the plasticizer are specially adjusted and optimized, so that the preparation effect of the ceramic core is improved.
5. According to the invention, the strengthening step can be arranged in the preparation process of the ceramic core, and the strength and other performances of the ceramic core are further improved by utilizing the strengthening step.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (21)
1. The silicon-based ceramic core material comprises silicon-based ceramic core powder, wherein the silicon-based ceramic core powder comprises refractory material powder and mineralizer, and is characterized in that the refractory material powder accounts for 65-85% of the silicon-based ceramic core powder in percentage by mass, the mineralizer comprises zirconium silicate powder and silicon nitride powder, the zirconium silicate powder accounts for 5-10% of the silicon-based ceramic core powder in percentage by mass, the silicon nitride powder accounts for 20-30% of the silicon-based ceramic core powder in percentage by mass, and the silicon nitride powder is irregularly-shaped beta-Si 3 N 4 The refractory material powder is quartz glass powder with the particle size of 200-400 meshes and further comprises a plasticizer, wherein the mass of the plasticizer is 12-20% of the mass of the silicon-based ceramic core material.
2. The silicon-based ceramic core material according to claim 1, wherein the refractory powder has a particle size of 100-300 mesh.
3. The silicon-based ceramic core material according to claim 1, wherein the particle size of the zirconium silicate powder is 300-350 meshes, and the zirconium silicate powder accounts for 10% of the mass of the silicon-based ceramic core powder.
4. The silicon-based ceramic core material according to claim 1, wherein the silicon-based ceramic core powder comprises the following components in percentage by weight:
70% of quartz glass powder, 10% of zirconium silicate powder and 20% of silicon nitride powder; or alternatively
65% of quartz glass powder, 10% of zirconium silicate powder and 25% of silicon nitride powder.
5. The silicon-based ceramic core material of any one of claims 1-4, wherein the silicon-based ceramic core powder further comprises other powder components including one or more of other oxides, carbides, borides, and nitrides.
6. The silica-based ceramic core material according to any one of claims 1 to 4, wherein the refractory powder, zirconium silicate powder and silicon nitride powder are mixed by a three-dimensional mixer to form the silica-based ceramic core powder.
7. The silicon-based ceramic core material according to claim 1, wherein the mass of the plasticizer is 16% of the mass of the silicon-based ceramic core material.
8. The silicon-based ceramic core material of claim 7, wherein the plasticizer is a mixture of paraffin wax, beeswax and polyethylene.
9. A method for producing a silicon-based ceramic core comprising a powder mixing step, a slurry preparation step, a green compact pressing step and a sintering step which are sequentially carried out, characterized in that the silicon-based ceramic core powder as defined in any one of claims 1 to 6 is used in the powder mixing step.
10. The method of producing a silica-based ceramic core according to claim 9, wherein in the slurry producing step, a plasticizer is mixed with the silica-based ceramic core powder, the mass of the plasticizer being 12 to 20% of the mass of the silica-based ceramic core material.
11. The method of manufacturing a silicon-based ceramic core according to claim 10, wherein the mass of the plasticizer is 16% of the mass of the silicon-based ceramic core material.
12. The method of claim 11, wherein the plasticizer is a mixture of paraffin wax, beeswax and polyethylene.
13. The method of manufacturing a silicon-based ceramic core according to claim 9, further comprising a strengthening step performed after the sintering step, wherein a strengthening agent is used to increase the strength of the silicon-based ceramic core.
14. The method for producing a silica-based ceramic core according to any one of claims 9 to 13, wherein in the powder mixing step, the silica-based ceramic core powder is charged into a ball mill tank for mixing, the mass ratio of the silica-based ceramic core powder to zirconia balls is 1:2, the rotation speed of the ball mill is 200r/min, the ball milling time is 12 hours, and the uniformly mixed silica-based ceramic core powder is subjected to drying treatment for 10 hours.
15. The method for preparing a silicon-based ceramic core according to claim 14, wherein in the step of preparing slurry, the plasticizer is placed into a mixing barrel at 90 ℃, after the plasticizer is melted completely, the dried silicon-based ceramic core powder is added into the mixing barrel in batches, stirring is performed under high vacuum, 0.1% of oleic acid is added in the process, and after the silicon-based ceramic core powder is completely added, stirring is continued to be performed under vacuum for 4 hours uniformly, so as to obtain the slurry.
16. The method of manufacturing a silicon-based ceramic core according to claim 15, wherein in the green body pressing step, a green body is pressed by a hot-press injection molding method, the slurry is put into a ceramic core press, the slurry temperature is set to 90 ℃, the injection pressure is set to 4MPa, the dwell time is set to 25S, and the slurry is pressed into a mold to manufacture the green body.
17. The method of producing a silicon-based ceramic core according to claim 16, wherein in the sintering step, the green compact is filled with α -Al 2 O 3 The powder sagger is filled with the top filler with the thickness not less than 25mm, and after the biscuit is fully filled into the sagger, the filler is filled by a rubber hammerAnd (3) vibrating compaction, and then sintering in a box-type resistance furnace, wherein the sintering system is as follows: heating to 250 ℃ at a heating rate of 0.1-3 ℃/min, preserving heat for 200-300 min, heating to 600 ℃ at a heating rate of 0.1-3 ℃/min, preserving heat for 100-200 min, heating to 1200 ℃ at a heating rate of 0.1-5 ℃/min, preserving heat for 100-200 min, and cooling to room temperature along with a furnace to obtain the silicon-based ceramic core.
18. The method of manufacturing a silicon-based ceramic core according to claim 13, wherein the strengthening step includes at least one of a high temperature strengthening step and a room temperature strengthening step.
19. The method according to claim 18, wherein in the high temperature strengthening step, the sintered silicon-based ceramic core is immersed in a high temperature strengthening agent under vacuum for 6 hours, the sintered silicon-based ceramic core is taken out after bubbles completely disappear, residual liquid on the surface of the silicon-based ceramic core is wiped off, and the silicon-based ceramic core after high temperature strengthening is obtained after the sintered silicon-based ceramic core is air-dried for more than 24 hours, wherein the high temperature strengthening agent is liquid silica sol.
20. The method for manufacturing a silicon-based ceramic core according to claim 18, wherein in the room temperature strengthening step, the ceramic core is completely soaked in a room temperature strengthening agent, the ceramic core is placed in a vacuum drying oven, the vacuum drying oven is vacuumized at room temperature for 3-5 min, the soaking time is 10min, the surface excess liquid is removed to be smooth and clean, the ceramic core is placed in the vacuum drying oven at 55 ℃ for heat preservation for 1h for drying treatment, and the ceramic core is taken out after cooling, so that the silicon-based ceramic core after room temperature strengthening is obtained, wherein the room temperature strengthening agent is epoxy resin: polyamide: acetone: methanol=3.4: 2:3.8:0.8 of a reinforcing agent.
21. A silicon-based ceramic core, characterized in that the silicon-based ceramic core is prepared using the preparation method according to any one of claims 9 to 20.
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