CN114907133A - 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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- CN114907133A CN114907133A CN202210489553.2A CN202210489553A CN114907133A CN 114907133 A CN114907133 A CN 114907133A CN 202210489553 A CN202210489553 A CN 202210489553A CN 114907133 A CN114907133 A CN 114907133A
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- 239000011162 core material Substances 0.000 title claims abstract description 224
- 239000000919 ceramic Substances 0.000 title claims abstract description 200
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 239000010703 silicon Substances 0.000 title claims abstract description 146
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 146
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 174
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 43
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 43
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000011819 refractory material Substances 0.000 claims abstract description 8
- 239000004014 plasticizer Substances 0.000 claims description 52
- 238000000034 method Methods 0.000 claims description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 35
- 238000005728 strengthening Methods 0.000 claims description 33
- 238000005245 sintering Methods 0.000 claims description 29
- 239000002002 slurry Substances 0.000 claims description 20
- 235000015895 biscuits Nutrition 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 14
- -1 polyethylene Polymers 0.000 claims description 13
- 239000004698 Polyethylene Substances 0.000 claims description 12
- 239000000203 mixture 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
- 239000003795 chemical substances by application Substances 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
- 238000003825 pressing Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 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
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000001746 injection moulding Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 238000002791 soaking Methods 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
- 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
- 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
- 239000000463 material Substances 0.000 abstract description 15
- 239000000306 component Substances 0.000 description 15
- 238000000227 grinding Methods 0.000 description 7
- 238000000465 moulding Methods 0.000 description 7
- 238000003837 high-temperature calcination Methods 0.000 description 6
- 238000005266 casting Methods 0.000 description 5
- 238000005495 investment casting Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000002787 reinforcement Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 3
- 239000008358 core component Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process 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
- 239000004482 other powder Substances 0.000 description 2
- 238000004321 preservation Methods 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
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 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
- 239000003623 enhancer Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011226 reinforced ceramic Substances 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
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910001845 yogo sapphire 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
- C04B35/66—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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- 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
- C04B35/01—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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- 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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- C04B2235/02—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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- C04B2235/656—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
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- Inorganic Chemistry (AREA)
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- Molds, Cores, And Manufacturing Methods Thereof (AREA)
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Abstract
The invention provides a silicon-based ceramic core material which comprises a silicon-based ceramic core powder material, wherein the silicon-based ceramic core powder material comprises a refractory material powder and a mineralizer, and is characterized in that the refractory material powder accounts for 65-85% of the mass of the silicon-based ceramic core powder material, the mineralizer comprises a zirconium silicate powder and a silicon nitride powder, the zirconium silicate powder accounts for 5-15% of the mass of the silicon-based ceramic core powder material, and the silicon nitride powder accounts for 5-30% of the mass of the silicon-based ceramic core powder material. The invention also provides a preparation method of the corresponding 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 shrinkage of thick and thin walls, 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 investment casting with near zero shrinkage 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 fuel application range 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 'imperial pearl' in equipment manufacturing industry, and is 'national heavy equipment' which is concerned with national safety and national economic development. The turbine blade is a core component of a high-performance gas turbine, and as the performance of the gas turbine is more and more required, the heat resistance of the turbine blade is also more and more required.
Blade cooling technology is one of the most effective ways to improve the thermal resistance of turbine blades. With the development of blade cooling technology, blade cooling methods have been developed from initial convection cooling, impingement cooling, film cooling, etc. to more advanced blade cooling methods such as divergent cooling, laminate cooling, etc. at present. The shape design of the inner cavity of the hollow blade is more elaborate and complicated, and a single-wall structure, a double-wall structure or even a multi-wall structure appears in succession. How to manufacture the blade with the complex inner cavity structure also becomes a challenge, the conventional processing modes such as forging and stamping, electrochemical machining and the like cannot meet the manufacturing requirements of the blade, investment precision manufacturing becomes a key means for solving the problem of manufacturing the hollow blade, and the investment precision manufacturing is widely applied at present. The ceramic core is a core component in the precise manufacturing process of the investment mold, plays a decisive role in the quality of a casting, and has important significance in the manufacturing level of the ceramic core on the quality, the manufacturing cost, the product percent of pass and the like of the hollow blade.
Silica-based ceramic cores are one of the most used ceramic cores today. The firing temperature of the silicon-based ceramic core is 1150-1250 ℃, the use temperature is 1520-1560 ℃, the yield is higher under the casting condition of 1500-1550 ℃, and the core is easy to corrode and strip by alkali liquor. However, the inner cavity structure of the part is more refined, the size difference of the thick wall and the thin wall is large, and 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 further the core deviation, core exposure and core fracture in the investment casting process can be caused. Particularly for ceramic cores with double-layer walls, multi-layer walls and large-size structures, the thick and thin connecting parts of the ceramic cores 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 core material of the ceramic core consists of 70-85% of quartz glass powder and 15-30% of M75 type mullite powder, and a plasticizer consists of 97% of white paraffin and 3% of polyethylene; the parameters of the core pressing process are as follows: preheating the mould at 30-45 deg.c, material slurry at 95-110 deg.c, pressure injection pressure of 2.0-3.0 MPa and pressure maintaining time of 15-20 s; the parameters of the core sintering process are as follows: keeping the temperature at 200 ℃ for 4h, keeping the temperature at 400 ℃ for 4h, keeping the temperature at 600 ℃ for 1h, keeping the temperature at 900 ℃ for 1h, and keeping the final sintering temperature at 1150-1160 ℃ for 4 h; after sintering, adopting ethyl silicate reinforcer to carry out high-temperature reinforcement, and using low-temperature reinforcer prepared by 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 breaking rate in the pouring process is lower than 8%, the shrinkage rate is small, the room-temperature and high-temperature strength is good, the size precision is high, the core is not deformed in the casting process and is easy to fall off, and the casting requirement of a thin-wall casting with a complex cavity channel can be met.
However, the preparation method of the silicon-based ceramic core in the prior art still has the problems of inconsistent shrinkage of the core, low high-temperature strength, large high-temperature deflection and the like, and then causes the problems of deformation, cracks, even fracture and the like of the core.
Disclosure of Invention
The invention mainly aims to provide 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 silicon-based ceramic core material, comprising a silicon-based ceramic core powder, wherein the silicon-based ceramic core powder comprises a refractory material powder and a mineralizer, and is characterized in that the refractory material powder accounts for 65-85% by mass of the silicon-based ceramic core powder, the mineralizer comprises zirconium silicate powder and silicon nitride powder, the zirconium silicate powder accounts for 5-15% by mass of the silicon-based ceramic core powder, and the silicon nitride powder accounts for 5-30% by mass of the silicon-based ceramic core powder.
Furthermore, the refractory material powder is quartz glass powder with the particle size of 100-300 meshes.
Further, the silicon nitride powder is irregular-shaped beta-Si 3 N 4 Powder with the particle size of 200-400 meshes.
Further, 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.
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
75% of quartz glass powder, 10% of zirconium silicate powder and 15% of silicon nitride powder; or
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 frit may further comprise other frit components, and the other frit components may comprise 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 through a three-dimensional mixer to form the silicon-based ceramic core powder.
Further, the silicon-based ceramic core material further comprises a plasticizer, and the mass of the plasticizer is 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, beeswax and polyethylene.
According to another aspect of the invention, a method for preparing a silicon-based ceramic core is provided, which comprises a powder mixing step, a slurry preparation step, a biscuit pressing step and a sintering step which are sequentially carried out, and is characterized in that the silicon-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, wherein the mass of the plasticizer is 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, beeswax and polyethylene.
Further, a strengthening step is included, wherein the strengthening step is performed after the sintering step, and a strengthening agent is used for improving the strength of the silicon-based ceramic core.
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 mill is 200r/min, the ball milling time is 12 hours, the uniformly mixed silicon-based ceramic core powder is dried, and the drying time is 10 hours.
Further, in the slurry preparation step, the plasticizer is placed into a mixing barrel at the temperature of 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 the silicon-based ceramic core powder is completely added, the uniform stirring is carried out for 4 hours under vacuum continuously, so that the slurry is obtained.
Further, in the biscuit pressing step, a biscuit is pressed by a hot pressing injection molding method, the slurry is put into a ceramic core injection press, the slurry temperature is set to 90 ℃, the injection pressure is set to 4MPa, and the pressure holding time is set to 25S, and the slurry is pressed into a mold to prepare the biscuit.
Further, in the sintering step, the corrected biscuit is filled in a sagger of alpha-Al 2O3 powder, the thickness of the filler on 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 is placed in a box-type resistance furnace for sintering, and 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 the 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, taken out after bubbles completely disappear, wiped off residual liquid on the surface of the silicon-based ceramic core, and dried by air for more than 24 hours to obtain the silicon-based ceramic core after high-temperature strengthening, wherein the high-temperature strengthening agent is liquid silica sol.
Further, in the room temperature strengthening step, completely soaking the ceramic core in a room temperature strengthening agent, placing the ceramic core in a vacuum drying oven, vacuumizing for 3-5 min at room temperature, soaking for 10min, taking out, wiping off redundant liquid on the surface until the surface is smooth and clean, placing the ceramic core in a vacuum drying oven at 55 ℃ for heat preservation for 1h for drying treatment, cooling and taking out to obtain the silicon-based ceramic core strengthened at room temperature, wherein the room temperature strengthening agent is epoxy resin: polyamide: acetone: methanol 3.4: 2: 3.8: 0.8 of a fortifier.
According to another aspect of the invention, a silicon-based ceramic core is provided, wherein the silicon-based ceramic core is prepared by 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 improves the type of mineralizer from the excellent performance of the silicon-based ceramic core, and compositely adds zirconium silicate and silicon nitride as the mineralizer, thereby establishing the ceramic core of a complex ternary system and solving the problems of large size shrinkage, inconsistent thickness and thin 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 content of the mineralizer added into the core, particularly the content of silicon nitride, 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, so that the prepared silicon-based ceramic core can be applied to the preparation of 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 using a proper process on the basis of selecting a 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 amount of the plasticizer are specially adjusted and optimized, so that the preparation effect of the ceramic core is improved.
5. The invention sets a strengthening step in the preparation process of the ceramic core, and the strengthening step is utilized to further improve the properties of the ceramic core, such as strength and the like.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
The present invention is described in further detail below with reference to specific examples, which are not to be construed as limiting the scope of the invention as claimed.
Example 1
The silicon-based ceramic core material comprises silicon-based ceramic core powder and a 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, 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 with the grain diameter of 300 meshes and the grain diameter of 325 meshes is prepared by high-temperature calcining and grinding.
Preferably, the quartz glass powder, the zirconium silicate and the silicon nitride are mixed by a three-dimensional mixer.
The embodiment also provides a preparation method of the ceramic core with near-zero shrinkage, which comprises the following steps:
mixing powder: the method comprises the steps of preparing mixed silicon-based ceramic core powder required by an experiment according to a certain proportion, and filling the prepared powder into a ball milling tank for mixing, wherein the mass ratio of the mixed powder to zirconia balls is 1:2, the rotating speed of a ball mill is 200r/min, and the ball milling time is 12 hours. And drying the uniformly mixed powder for 10 hours.
Preparing slurry: weighing a certain amount of plasticizer, putting the plasticizer into a mixing barrel at the temperature of 90 ℃, adding the dried powder into the mixing barrel in batches according to a certain amount after the plasticizer is completely melted, and stirring under high vacuum. 0.1 percent of oleic acid is added in the process of mixing materials. After the powder is completely added, the mixture is continuously and uniformly stirred for 4 hours under vacuum, and the slurry with the powder uniformly dispersed in the plasticizer can be obtained.
Biscuit pressing: and pressing the biscuit by adopting a hot-pressing injection molding method. And (3) putting the ceramic core slurry into a ceramic core injection molding machine, and pressing the ceramic core slurry into a mold when the parameters of the injection molding machine are consistent with the set values (the slurry temperature is 90 ℃, the injection pressure is 4Mpa, and the pressure maintaining time is 25S), so as to prepare the ceramic core biscuit.
And (3) sintering: the corrected biscuit was filled in a sagger containing α -Al2O3 powder having a particle size of about 100 mesh. The thickness of the filler on the top of the core biscuit is not less than 25mm, after the core biscuit is completely loaded into a sagger, a rubber hammer is used for compacting the filler, and then the core biscuit is placed into a box-type resistance furnace for sintering. 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 the furnace to obtain the silicon-based ceramic core.
Strengthening: and (3) selecting liquid silica sol for high-temperature reinforcement, immersing the sintered core into a high-temperature reinforcement agent under vacuum for 6 hours, taking out the core after bubbles disappear completely, wiping off residual liquid on the surface of the core, and drying the core for more than 24 hours by air to obtain the high-temperature reinforced ceramic core. And (3) room-temperature reinforced selection of epoxy resin: polyamide: acetone: methanol 3.4: 2: 3.8: 0.8 of the proportion to prepare the enhancer. And completely soaking the ceramic core in the core strengthening liquid, putting the core strengthening liquid in a vacuum drying oven, and vacuumizing for 3-5 min at room temperature for 10 min. Taking out and wiping off the redundant protective solution on the surface until the surface is smooth and clean. And (3) placing the ceramic core in a vacuum drying box at the temperature of 55 ℃ for heat preservation for 1h for drying treatment, and taking out the ceramic core after cooling to obtain the room-temperature-strengthened ceramic core.
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 0.71 mm.
Example 2
The silicon-based ceramic core material comprises silicon-based ceramic core powder and a 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, beeswax and 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 with the grain diameter of 300 meshes and the grain diameter of 325 meshes is prepared by high-temperature calcination and grinding.
Preferably, the quartz glass powder, the zirconium silicate and the silicon nitride are mixed by a three-dimensional mixer.
The silicon-based ceramic core of this example was prepared in the same process as in example 1 and the process parameters were fine-tuned according to the material differences.
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 0.82 mm.
Example 3
The silicon-based ceramic core material comprises silicon-based ceramic core powder and a 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, beeswax and 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 with the grain diameter of 300 meshes and the grain diameter of 325 meshes is prepared by high-temperature calcination and grinding.
Preferably, the quartz glass powder, the zirconium silicate and the silicon nitride are mixed by a three-dimensional mixer.
The silicon-based ceramic core of this example was prepared in the same process as in example 1 and the process parameters were fine-tuned according to the material differences.
The silicon-based ceramic core prepared by the embodiment has the molding rate of more than 96 percent, the sintering shrinkage rate of 0.09 percent, 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 and using single crystal blades with higher inner cavity dimensional precision.
Example 4
The silicon-based ceramic core material comprises silicon-based ceramic core powder and a 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, 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 with the grain diameter of 300 meshes and the grain diameter of 325 meshes is prepared by high-temperature calcination and grinding.
Preferably, the quartz glass powder, the zirconium silicate and the silicon nitride are mixed by a three-dimensional mixer.
The silicon-based ceramic core of this example was prepared in the same process as in example 1 and the process parameters were fine-tuned according to the material differences.
The silicon-based ceramic core prepared by the embodiment has the molding rate of more than 95 percent, the sintering shrinkage rate of-0.04 percent, the room temperature strength of 18.4MPa, the high temperature strength of 15.6MPa and the high temperature deflection of 0.97 mm.
Example 5
A silicon-based ceramic core material with near zero shrinkage and preparation of a silicon-based ceramic mold are disclosed, wherein the silicon-based ceramic core material comprises silicon-based ceramic core powder and a plasticizer, and 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, beeswax and 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 with the grain diameter of 200 meshes and the grain diameter of 300 meshes is prepared by high-temperature calcination and grinding.
Preferably, the quartz glass powder, the zirconium silicate and the silicon nitride are mixed by a three-dimensional mixer.
The silicon-based ceramic core of this example was prepared in the same process as in example 1 and the process parameters were fine-tuned according to the material differences.
The silicon-based ceramic core prepared by the embodiment has the molding rate of more than 95%, the sintering shrinkage rate of 0.12%, the room temperature strength of 21.1MPa, the high temperature strength of 21.0MPa and the high temperature deflection of 0.83 mm.
Example 6
The silicon-based ceramic core material comprises silicon-based ceramic core powder and a 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, beeswax and 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 with the grain diameter of 400 meshes and the grain diameter of 350 meshes is prepared by high-temperature calcination and grinding.
Preferably, the quartz glass powder, the zirconium silicate and the silicon nitride are mixed by a three-dimensional mixer.
The silicon-based ceramic core of this example was prepared in the same process as in example 1 and the process parameters were fine-tuned according to the material differences.
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 0.75 mm.
Example 7
The silicon-based ceramic core material comprises silicon-based ceramic core powder and a 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, beeswax and 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 with the grain diameter of 400 meshes and the grain diameter of 350 meshes is prepared by high-temperature calcination and grinding.
Preferably, the quartz glass powder, the zirconium silicate and the silicon nitride are mixed by a three-dimensional mixer.
The silicon-based ceramic core of this example was prepared in the same process as in example 1 and the process parameters were fine-tuned according to the material differences.
The silicon-based ceramic core prepared by the embodiment has the molding rate of over 95 percent, the sintering shrinkage rate of-0.05 percent, the room temperature strength of 18.1MPa, the high temperature strength of 15.2MPa and the high temperature deflection of 0.99 mm.
Example 8
The silicon-based ceramic core material comprises silicon-based ceramic core powder and a 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 of the embodiment is different from that of the embodiment 1 in that a strengthening step is not arranged after the sintering step, and after the sintering step, various properties of the ceramic core are still within an 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 be still met.
It is added that, in order to regulate and control the performance of the silicon-based ceramic core, the silicon-based ceramic core powder can also comprise other powder components in proper amount, and the other powder components comprise one or more of other oxides, carbides, borides and nitrides, such as aluminum oxide, silicon carbide and the like.
The technical scheme of the invention can be applied to the manufacturing of turbine blades of gas turbines, the manufacturing of turbine blades and high-temperature alloy blades in other fields and other investment casting to obtain ideal effects.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
1. the invention improves the type of mineralizer from the excellent performance of the silicon-based ceramic core, and compositely adds zirconium silicate and silicon nitride as the mineralizer, thereby establishing the ceramic core of a complex ternary system and solving the problems of large size shrinkage, inconsistent thickness and thin 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 content of the mineralizer added into the core, particularly the content of silicon nitride, 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, so that the prepared silicon-based ceramic core can be applied to the preparation of 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 using a proper process on the basis of selecting a 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 amount of the plasticizer are specially adjusted and optimized, so that the preparation effect of the ceramic core is improved.
5. The ceramic core preparation process can be provided with a strengthening step, and the strengthening step is utilized to further improve the properties of the ceramic core such as strength and the like.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (23)
1. The silicon-based ceramic core material comprises 65-85% of refractory material powder by mass, and 5-15% of mineralizer powder by mass, and 5-30% of silicon nitride powder by mass.
2. The silicon-based ceramic core material as recited in claim 1, wherein the refractory material powder is silica glass powder with a particle size of 100-300 mesh.
3. The silicon-based ceramic core material of claim 1, wherein the silicon nitride powder is irregularly shaped β -Si 3 N 4 Powder with the particle size of 200-400 meshes.
4. The silicon-based ceramic core material as recited in claim 1, wherein the zirconium silicate powder has a particle size of 300-350 mesh, and the zirconium silicate powder accounts for 10% by mass of the silicon-based ceramic core powder.
5. 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:
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
70% of quartz glass powder, 10% of zirconium silicate powder and 20% of silicon nitride powder; or
65% of quartz glass powder, 10% of zirconium silicate powder and 25% of silicon nitride powder.
6. The silicon-based ceramic core material according to any of claims 1-5, wherein the silicon-based ceramic core frit further comprises other frit components, the other frit components comprising one or more of other oxides, carbides, borides and nitrides.
7. The silicon-based ceramic core material according to any one of claims 1 to 5, wherein the refractory 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.
8. The silicon-based ceramic core material according to any of claims 1-5, further comprising a plasticizer, the mass of the plasticizer being 12-20% of the mass of the silicon-based ceramic core material.
9. The silicon-based ceramic core material according to claim 8, wherein the mass of the plasticizer is 16% of the mass of the silicon-based ceramic core material.
10. The silicon-based ceramic core material according to claim 8, wherein the plasticizer is a mixture of paraffin wax, beeswax and polyethylene.
11. A method for the preparation of a silicon-based ceramic core comprising a powder mixing step, a slurry preparation step, a biscuit pressing step and a sintering step carried out in sequence, characterized in that a powder for a silicon-based ceramic core according to any one of claims 1 to 10 is used in the powder mixing step.
12. The method of claim 11, wherein a plasticizer is mixed with the silicon-based ceramic core powder in the slurry preparation step, wherein the mass of the plasticizer is 12-20% of the mass of the silicon-based ceramic core material.
13. The method of claim 12, wherein the plasticizer comprises 16% by mass of the silicon-based ceramic core material.
14. The method of making a silicon-based ceramic core as recited in claim 13 wherein the plasticizer is a mixture of paraffin wax, beeswax and polyethylene.
15. The method of claim 11, 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.
16. The method for preparing the silicon-based ceramic core according to any one of claims 11 to 15, wherein 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 rotation speed of the ball mill is 200r/min, the ball milling time is 12 hours, and the silicon-based ceramic core powder after uniform mixing is dried for 10 hours.
17. The method for preparing the silicon-based ceramic core according to claim 16, wherein in the slurry preparation step, the plasticizer is put into a mixing barrel with the temperature of 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 the silicon-based ceramic core powder is completely added, uniform stirring is carried out for 4 hours under vacuum continuously to obtain the slurry.
18. The method of claim 17, wherein in the green body pressing step, the green body is pressed by a hot press injection molding method, the slurry is put into a ceramic core injection press, the slurry temperature is set to 90 ℃, the injection pressure is set to 4MPa, and the dwell time is set to 25S, and the green body is manufactured by pressing the slurry into a mold.
19. The method of claim 18, wherein the corrected biscuit is embedded in α -Al during the sintering step 2 O 3 In a powder sagger, the thickness of the filler at the top of the biscuit is not less than 25mm, after the biscuit is completely loaded into the sagger, the filler is compacted by a rubber hammer and then is put into a box-type resistance furnace for sintering, and 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 the furnace to obtain the silicon-based ceramic core.
20. The method of preparing a silicon-based ceramic core of claim 15, wherein the strengthening step comprises at least one of a high temperature strengthening step and a room temperature strengthening step.
21. The method for preparing the silicon-based ceramic core according to claim 20, 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, taken out after bubbles completely disappear, wiped off residual liquid on the surface of the silicon-based ceramic core, and dried for more than 24 hours by self-drying to obtain the silicon-based ceramic core after high temperature strengthening, wherein the high temperature strengthening agent is liquid silica sol.
22. The method for preparing the silicon-based ceramic core according to claim 20, 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 ceramic core is taken out to wipe off redundant liquid on the surface until the surface is smooth and clean, the ceramic core is placed in a vacuum drying oven at 55 ℃ and is kept for 1h for drying treatment, and the silicon-based ceramic core is taken out after cooling to obtain the room temperature strengthened silicon-based ceramic core, wherein the room temperature strengthening agent is epoxy resin: polyamide: acetone: methanol 3.4: 2: 3.8: 0.8 of a fortifier.
23. A silicon-based ceramic core, characterized in that it is produced using the production method according to one of claims 11 to 22.
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