CN116102364B - Anti-cracking inert ceramic core and preparation method thereof - Google Patents
Anti-cracking inert ceramic core and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 87
- 238000005336 cracking Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 62
- 239000011248 coating agent Substances 0.000 claims abstract description 61
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000006255 coating slurry Substances 0.000 claims abstract description 27
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- 230000007704 transition Effects 0.000 claims abstract description 9
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 239000010410 layer Substances 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 7
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 7
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 7
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000005642 Oleic acid Substances 0.000 claims description 7
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 7
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 7
- 239000012188 paraffin wax Substances 0.000 claims description 7
- 229910052727 yttrium Inorganic materials 0.000 claims description 7
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 5
- 239000002344 surface layer Substances 0.000 claims description 5
- 230000001680 brushing effect Effects 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 22
- 229910001069 Ti alloy Inorganic materials 0.000 abstract description 19
- 238000005266 casting Methods 0.000 abstract description 12
- 239000011224 oxide ceramic Substances 0.000 abstract description 7
- 238000005495 investment casting Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000010304 firing Methods 0.000 abstract description 2
- 230000000704 physical effect Effects 0.000 abstract description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000012797 qualification Methods 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000004512 die casting Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical group [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910001928 zirconium oxide 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
-
- 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
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Mold Materials And Core Materials (AREA)
- Molds, Cores, And Manufacturing Methods Thereof (AREA)
Abstract
The invention belongs to the technical field of titanium alloy precision casting, and particularly relates to an anti-cracking inert ceramic core and a preparation method thereof. Step one: forming a silica-based ceramic preform; step two: the alumina coating slurry and the yttria coating slurry are attached to the surface of the silica-based ceramic preform; step three: and sintering the silica-based ceramic preform and the surface composite coating integrally. The anti-cracking inert ceramic core takes silicon oxide ceramic as a matrix, a yttrium oxide coating as a surface inert layer and an alumina transition layer is arranged between the matrix and the coating, and is obtained by integral sintering, so that the problem of unmatched physical properties of yttrium oxide and silicon oxide at high temperature is solved, the cracking of the coating is obviously reduced, the adhesiveness is improved, and the anti-cracking inert ceramic core can be used for near-net forming of a titanium alloy complex structure with high quality, easy core removal and low cost. The anti-cracking inert ceramic core is obtained by integral firing, so that the manufacturing process is simplified, the energy consumption is reduced, the core cost is reduced, and the production requirement of a large number of titanium alloy casting products is met.
Description
Technical Field
The invention belongs to the technical field of titanium alloy precision casting, and particularly relates to an anti-cracking inert ceramic core and a preparation method thereof, in particular to an inert ceramic core which can be used for manufacturing a titanium alloy casting with a complex inner cavity.
Background
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or suggestion that this information is already known in the art to those of ordinary skill in the art.
The titanium alloy has excellent comprehensive performance, low density, high specific strength, good corrosion resistance and wide temperature application range, becomes an indispensable advanced structural material in the modern industry, has wide application in the fields of aerospace, military equipment, petrochemical industry, medical appliances and the like, and is praised as future metal. However, its relatively high chemical activity, low thermal conductivity and low plasticity also makes it relatively difficult to shape in conventional processing. The investment precision casting method for producing the titanium alloy casting has the following advantages: high utilization rate of raw materials, accurate size, capability of casting various castings with complex structures and lower production cost. With the rapid increase of the demands of national defense military products and high-end civil products on titanium alloy near-net-shape parts, the shape and inner cavity structure of titanium alloy castings are more and more complex, and the demands on high-quality cores for titanium alloy near-net-shape are also aggravated.
Silica-based cores and alumina-based cores are commonly used because of their excellent economy. However, the titanium alloy has great activity at high temperature, and reacts with the two ceramics, and a large number of air holes are formed in the casting, so that the two ceramics cannot be directly applied to the titanium alloy investment casting process.
The zirconium oxide and the yttrium oxide have high chemical inertness and can be used as ceramic cores or shells to prepare titanium alloy castings. However, the ceramic core is produced by adopting zirconia and yttria, so that the cost is high, the core is difficult to remove due to high strength, and the ceramic core is not suitable for being used as a titanium alloy ceramic core.
The silica-based ceramic core has great potential by combining the production cost and the core-removing difficulty factors. In order to solve the problem of the reaction of the silicon oxide ceramic with the titanium liquid at high temperature, scientific researchers developed a process technique of coating the outer layer of the core with an inert coating. The prior investment casting scale production of titanium alloy is zirconia and yttria, zirconia is mainly used for producing civil products and yttria is used for producing aviation components. Wherein, yttrium oxide hardly reacts with titanium liquid at high temperature, so that the defect of air holes caused by the reaction of titanium liquid and silicon oxide ceramic can be avoided. However, as the thermal expansion of the yttrium oxide and the silicon oxide is not cooperated, the yttrium oxide coating on the surface is easy to crack due to temperature change, and especially in a complex temperature environment with high and low temperature change, the cracking rate of the yttrium oxide coating is obviously improved, and once the coating cracks, titanium liquid directly reacts with silicon oxide ceramic, so that an effective protection effect is difficult to play. In practice, therefore, the inhibition of cracking of yttria coatings, particularly in the case of large changes in ambient temperature in the production site, is one of the key and difficult points to limit the improvement of the porosity defects of titanium alloy castings.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides an anti-cracking inert ceramic core and a preparation method thereof. The invention firstly aims to provide an inert ceramic core which is easy to remove and does not react with titanium liquid, and secondly aims to inhibit the surface cracking of the ceramic core as much as possible and improve the adaptability of the ceramic core to the environmental temperature as much as possible on the basis of the aim, thereby improving the quality of titanium alloy castings.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the anti-cracking inert ceramic core is prepared by the following preparation method:
step one: pressing and forming a silica-based ceramic preform;
step two: the surface of the silica-based ceramic preform is adhered with Al 2 O 3 Coating slurry, drying and then adhering Y 2 O 3 Coating slurry, waiting for drying;
step three: and dewaxing and sintering the silica-based ceramic preform and the surface composite coating integrally.
Preferably, in the first step, the ceramic die-casting slurry is prepared by mixing, by mass, 70% -90% of silicon oxide powder, 8.5% -22.0% of paraffin and 1.5% -8.0% of oleic acid at 60-100 ℃.
Preferably, in the first step, the ceramic slurry is injected into a metal mold through compressed air, and after the sample is solidified, the sample is dried for 24-48 hours at the drying temperature of 24-50 ℃.
Preferably, in the second step, al 2 O 3 Or Y 2 O 3 The coating slurry is formed by mixing oxide powder with 80-325 meshes with silica sol or yttrium sol, wherein the mass ratio of powder to liquid is 2.5:1-4:1, and the stirring time is more than 8 hours.
Preferably, in the second step, al 2 O 3 Coating paste and Y 2 O 3 The coating sizing agent adopts spraying,The ceramic core is adhered by soaking or brushing.
Preferably, in the second step, al 2 O 3 Drying the coating for 12-48 h, and then carrying out Y 2 O 3 The coating is coated and dried for 12 hours at normal temperature.
Preferably, in the second step, al 2 O 3 Coating and Y 2 O 3 The thickness of the coating is 0.5-180 μm respectively.
Preferably, in the third step, the ceramic preform and the composite coating are dewaxed and sintered integrally, the dewaxing temperature is 135-200 ℃, and the heat preservation time is 1-2 h; sintering temperature is
The temperature is 1350-1500 ℃ and the heat preservation time is 2-6 h.
Advantageous effects
The anti-cracking inert ceramic core provided by the invention is prepared by taking silicon oxide ceramic as a matrix, yttrium oxide coating as a surface inert layer and an alumina transition layer between the silicon oxide ceramic and the yttrium oxide coating, and integrally sintering the matrix and the coating. The integrated firing technology is realized, the manufacturing process is simplified, the energy consumption is reduced, the core cost is reduced, and the production requirement of mass titanium alloy casting products is met. The silicon oxide ceramic has lower matrix cost and is easy to be core-removed. The composite coating with yttrium oxide as the surface layer effectively blocks the reaction of titanium liquid and a silicon oxide core in investment casting, and reduces the generation of casting defects. The alumina has stable structure, and respectively reacts with the silicon oxide and the yttrium oxide in the heating process, so that the bonding strength of the coating is improved, and meanwhile, the transitional expansion coefficient difference is also realized so as to inhibit the cracking of the coating, so that the stability and the reliability of the inert coating are greatly improved, and the adaptability of the coating in a low-temperature environment is improved. Further experimental study also proves that the anti-cracking inert ceramic core provided by the invention overcomes the problem of unmatched physical properties of yttrium oxide and silicon oxide at high temperature, obviously reduces cracking of the coating and improves adhesion. In summary, the anti-cracking inert ceramic core provided by the invention can be used for near net forming of a titanium alloy complex structure with high quality, easy core removal and low cost.
Drawings
FIG. 1 is a microstructure of a composite coating on a silica ceramic mandrel (scale 200 μm).
FIG. 2 is a pictorial view of a sample of a failed ceramic core.
Fig. 3 is an enlarged view of a portion of the crack portion of fig. 2.
Fig. 4 is a pictorial view of a sample of acceptable ceramic cores.
Detailed Description
The invention is further illustrated by the following specific examples, which are intended to illustrate the problem and to explain the invention, without limiting it.
Example 1
Injecting ceramic slurry (formed by mixing 70% silicon oxide powder, 22.0% paraffin and 8.0% oleic acid) into a metal mold through compressed air, curing, drying at room temperature for 12h, and then continuously drying in a drying oven for 36h at 35 ℃; using 80 mesh Al 2 O 3 Mixing powder and silica sol, wherein the mass ratio of the powder to the solution is 2.5:1, and stirring for 12 hours to prepare alumina coating slurry; will be 100 mesh Y 2 O 3 Mixing the powder with yttrium sol, wherein the mass ratio of the powder to the liquid is 2.5:1, and stirring for 12 hours to obtain yttrium oxide coating slurry; coating the alumina coating slurry on the surface of the preform in a soaking mode, drying for 12 hours at normal temperature, immersing the preform in the yttria coating slurry, and drying for 12 hours at normal temperature; ceramic preform and coating integral dewaxing and sintering adopt a step heating mode: dewaxing temperature is 135 ℃, heat preservation is carried out for 2 hours, sintering temperature is 1350 ℃, and heat preservation time is 6 hours.
And cooling the ceramic furnace to be fired to below 300 ℃, discharging the ceramic furnace at the room temperature of 23-30 ℃ and the low temperature of-2-8 ℃ respectively, observing cracks on the surface of the coating and cracking conditions of the coating, and counting the qualification rate of the coating.
Example 2
Injecting ceramic slurry (formed by mixing 80.0% silicon oxide powder, 14.0% paraffin and 6.0% oleic acid) into a metal mold through compressed air, curing, drying at room temperature for 24 hours, and then continuously drying in a drying oven for 24 hours at 45 ℃; 100 mesh Al is adopted 2 O 3 Mixing powder and silica sol, wherein the mass ratio of powder to liquid is 3:1, stirring for 10 hours, and preparing oxygenAluminum coating sizing agent; y of 200 meshes 2 O 3 Mixing the powder with yttrium sol, wherein the mass ratio of the powder to the liquid is 3:1, and stirring for 10 hours to obtain yttrium oxide coating slurry; coating the alumina coating slurry on the surface of the preform in a soaking mode, drying for 24 hours at normal temperature, soaking the preform in the yttria coating slurry, and drying for 12 hours at normal temperature; ceramic preform and coating integral dewaxing and sintering adopt a step heating mode: dewaxing temperature is 160 ℃, heat preservation is carried out for 1.5h, sintering temperature is 1450 ℃, and heat preservation time is 4h.
And cooling the ceramic furnace to be fired to below 300 ℃, discharging the ceramic furnace at the room temperature of 23-30 ℃ and the low temperature of-2-8 ℃ respectively, observing cracks on the surface of the coating and cracking conditions of the coating, and counting the qualification rate of the coating.
Example 3
Injecting ceramic slurry (formed by mixing 90.0% silicon oxide powder, 12.0% paraffin and 8.0% oleic acid) into a metal mold through compressed air, drying at room temperature for 36h after solidification, and continuing to dry in a drying oven for 12h at 50 ℃; 200 mesh Al is adopted 2 O 3 Mixing powder and silica sol, wherein the mass ratio of the powder to the solution is 3.5:1, and stirring for 8 hours to prepare alumina coating slurry; will Y of 325 mesh 2 O 3 Mixing the powder with yttrium sol, wherein the mass ratio of the powder to the liquid is 3.5:1, and stirring for 8 hours to obtain yttrium oxide coating slurry; the alumina coating slurry is coated on the surface of the preform in a soaking mode, and is dried for 48 hours at normal temperature, and then the preform is soaked in the yttria coating slurry and is dried for 12 hours at normal temperature; ceramic preform and coating integral dewaxing and sintering adopt a step heating mode: dewaxing temperature is 200 ℃, heat preservation is carried out for 1h, sintering temperature is 1500 ℃, and heat preservation time is 2h.
And cooling the ceramic furnace to be fired to below 300 ℃, discharging the ceramic furnace at the room temperature of 23-30 ℃ and the low temperature of-2-8 ℃ respectively, observing cracks on the surface of the coating and cracking conditions of the coating, and counting the qualification rate of the coating.
Comparative example 1
Injecting ceramic slurry (formed by mixing 90.0% silicon oxide powder, 12.0% paraffin and 8.0% oleic acid) into a metal mold through compressed air, curing, drying at room temperature for 24 hours, and then continuously drying in a drying oven for 24 hours at 50 ℃; collectingWith 200 mesh Y 2 O 3 Mixing powder and yttrium sol, wherein the mass ratio of the powder to the solution is 3:1, and stirring for 10 hours to prepare coating slurry; y is Y 2 O 3 Coating the coating slurry on the surface of the preform by adopting a soaking mode, and drying for 12 hours at normal temperature; ceramic preform and coating integral dewaxing and sintering adopt a step heating mode: dewaxing temperature is 160 ℃, heat preservation is carried out for 1.5h, sintering temperature is 1450 ℃, and heat preservation time is 4h.
And cooling the ceramic furnace to be fired to below 300 ℃, discharging the ceramic furnace at the room temperature of 23-30 ℃ and the low temperature of-2-8 ℃ respectively, observing cracks on the surface of the coating and cracking conditions of the coating, and counting the qualification rate of the coating.
Comparative example 2
Injecting ceramic slurry (formed by mixing 90.0% silicon oxide powder, 12.0% paraffin and 8.0% oleic acid) into a metal mold through compressed air, curing, drying at room temperature for 24 hours, and then continuously drying in a drying oven for 24 hours at 50 ℃; 100 mesh Al is adopted 2 O 3 Powder and 200 mesh Y 2 O 3 Mixing powder and yttrium sol, wherein the mass ratio of the powder to the solution is 3:1, and stirring for 10 hours to prepare coating slurry; al (Al) 2 O 3 And Y 2 O 3 The mixed coating slurry is coated on the surface of the preform in a soaking mode, and is dried for 24 hours at normal temperature; ceramic preform and coating integral dewaxing and sintering adopt a step heating mode: dewaxing temperature is 160 ℃, heat preservation is carried out for 1.5h, sintering temperature is 1450 ℃, and heat preservation time is 4h.
And cooling the ceramic furnace to be fired to below 300 ℃, discharging at the room temperature of 23-30 ℃ and the low temperature of-2-8 ℃ respectively, observing cracks on the surface of the coating and cracking conditions of the coating, if cracking or peeling phenomena (shown in fig. 2 and 3) occur, judging the ceramic furnace to be unqualified, and if no cracking or peeling phenomena (shown in fig. 4) occur, judging the ceramic furnace to be qualified, and counting the qualification rate of the coating.
Silica-based ceramic cores were prepared according to the above examples, and the coating pass rate was calculated as shown in table 1.
TABLE 1
As can be seen from the test results in Table 1, the present invention sequentially coats Al on a silicon oxide substrate 2 O 3 Transition layer and Y 2 O 3 The ceramic core prepared by the integrated sintering of the surface layer has higher qualification rate in normal temperature and low temperature environments. Further examination of the microstructure revealed that the surface was Y 2 O 3 Between the layer and the silicon oxide matrix through Al 2 O 3 Forming a transitional fusion integrated combination state (shown in figure 1), realizing that the surface of the ceramic core is inert Y 2 O 3 Layer, again realize Y 2 O 3 A strong bond between the layer and the silicon oxide substrate; in addition, due to the presence of Al 2 O 3 When the ambient temperature changes, al 2 O 3 The layer can be opposite to Y 2 O 3 The expansion and contraction difference between the layer and the silicon oxide matrix forms transition and buffering, so that the ceramic core has better cracking resistance and reliability under a complex temperature environment. Y in comparative example 1 2 O 3 The coating is directly combined with the silicon oxide substrate, the shrinkage conditions of the core substrate and the coating are greatly different, and the cracking resistance at normal temperature is good, but the cracking at low temperature is obviously increased. In comparative example 2, Y 2 O 3 And Al 2 O 3 The combination condition of the mixed coating and the matrix is slightly improved, but the embodiment has a certain gap and the surface of the core has a certain Al 2 O 3 Exposing. In conclusion, al is adopted 2 O 3 The composite coating as the transition layer is more beneficial to the working condition of complicated temperature change in production.
The above embodiments are illustrative for the purpose of illustrating the technical concept and features of the present invention so that those skilled in the art can understand the content of the present invention and implement it accordingly, and thus do not limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (9)
1. A preparation method of an anti-cracking inert ceramic core is characterized by comprising the following steps: the anti-cracking inert ceramic core comprises a ceramic matrix, a transition layer and an inert surface layer; the ceramic matrix is a silica-based ceramic matrix, the transition layer is an alumina transition layer, and the inert surface layer is an yttrium oxide layer;
the preparation method of the anti-cracking inert ceramic core comprises the following steps:
step one: manufacturing a silica-based ceramic preform;
step two: attaching alumina coating slurry on the surface of the silica-based ceramic preform, drying, and then attaching yttrium oxide coating slurry, and curing and forming the alumina coating slurry;
step three: the silica-based ceramic preform and the composite coating on the surface are integrally sintered and molded to obtain the anti-cracking inert ceramic core;
in the second step, the alumina coating slurry is formed by stirring and mixing 80-325 mesh alumina powder and silica sol, wherein the mass ratio of the powder to the liquid is 2.5:1-4:1; the yttrium oxide coating slurry is formed by stirring and mixing yttrium oxide powder with the particle size of 80-325 meshes and yttrium sol, wherein the mass ratio of the powder to the liquid is 2.5:1-4:1;
the thickness of the transition layer is in the range of 0.5-180 mu m, and the thickness of the inert surface layer is in the range of 0.5-180 mu m.
2. The method for preparing the anti-cracking inert ceramic core according to claim 1, wherein the method comprises the following steps: in the first step, the silica-based ceramic preform is obtained by curing and forming ceramic slurry, wherein the ceramic slurry is prepared by mixing 70% -90% by mass of silica powder, 8.5% -22.0% by mass of paraffin and 1.5% -8.0% by mass of oleic acid at 60-100 ℃.
3. The method for preparing the anti-cracking inert ceramic core according to claim 2, wherein: injecting the ceramic slurry into a metal mold through compressed air, and continuously drying for 24-48 hours after curing to obtain the silica-based ceramic preform; the drying temperature is 24-50 ℃.
4. The method for preparing the anti-cracking inert ceramic core according to claim 1, wherein the method comprises the following steps: in the second step, the stirring time is more than 8h.
5. The method for preparing the anti-cracking inert ceramic core according to claim 4, wherein the method comprises the following steps: in the second step, the alumina coating slurry and the yttria coating slurry are attached to the ceramic core in a spraying, soaking or brushing mode.
6. The method for preparing the anti-cracking inert ceramic core according to claim 4, wherein the method comprises the following steps: and step two, drying the alumina coating for 12-48 hours, then coating the yttrium oxide coating, and drying at normal temperature for 12 hours.
7. The method for preparing the anti-cracking inert ceramic core according to claim 4, wherein the method comprises the following steps: in the third step, the ceramic preform and the composite coating are dewaxed and sintered integrally.
8. The method for preparing the anti-cracking inert ceramic core according to claim 7, wherein: in the third step, dewaxing and sintering are continuously carried out through temperature programming; dewaxing temperature is 100-200 ℃, and heat preservation time is 1-2 hours; the sintering temperature is 950-1450 ℃, and the heat preservation time is 2-6 hours.
9. An anti-crack inert ceramic core, characterized in that: the method for preparing the anti-cracking inert ceramic core according to claim 1.
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