CN116283254A - High-temperature-resistant silicon-based ceramic core and preparation method and application thereof - Google Patents
High-temperature-resistant silicon-based ceramic core and preparation method and application thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 148
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 49
- 239000010703 silicon Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 120
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000005245 sintering Methods 0.000 claims abstract description 34
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000004014 plasticizer Substances 0.000 claims abstract description 26
- 239000002002 slurry Substances 0.000 claims abstract description 25
- 239000010431 corundum Substances 0.000 claims abstract description 24
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims description 39
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 28
- 239000003822 epoxy resin Substances 0.000 claims description 27
- 229920000647 polyepoxide Polymers 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 239000000413 hydrolysate Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000005728 strengthening Methods 0.000 claims description 14
- 238000001746 injection moulding Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000004952 Polyamide Substances 0.000 claims description 9
- 229920002647 polyamide Polymers 0.000 claims description 9
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000011226 reinforced ceramic Substances 0.000 claims description 7
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- 238000000748 compression moulding Methods 0.000 claims description 5
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- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000002347 injection Methods 0.000 abstract description 7
- 239000007924 injection Substances 0.000 abstract description 7
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- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 239000011162 core material Substances 0.000 description 100
- 238000012360 testing method Methods 0.000 description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 11
- 238000001514 detection method Methods 0.000 description 7
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- 238000005516 engineering process Methods 0.000 description 4
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Abstract
The invention provides a high-temperature-resistant silicon-based ceramic core and a preparation method and application thereof, and belongs to the technical field of ceramic materials. The invention adopts grain diameter of 75 mu m, 45 mu m and 25 mu m as grading, the grain size is controlled below 100 mu m, and the sintering shrinkage rate of the ceramic core can be reduced and the high-temperature strength can be improved by adopting larger grain diameter proportion; according to the invention, the high-temperature strength is improved by adding the zirconium silicate powder and the corundum powder, and then the high-temperature strength can be further improved by utilizing the grain size grading of the quartz glass powder; the invention utilizes the quartz glass powder grading and the plasticizer of the ceramic slurry to control the fluidity of the ceramic slurry, and simultaneously the quartz powder grading can control the shrinkage rate and improve the sintering success rate of the ceramic core pressed injection green body. The high-temperature-resistant silicon-based ceramic core prepared by the method has the advantages of low sintering shrinkage rate, high-temperature strength and good corrosion resistance, and is suitable for more ceramic core inner cavity structures.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a high-temperature-resistant silicon-based ceramic core, and a preparation method and application thereof.
Background
In order to improve the thrust-weight ratio of a modern aeroengine, firstly, the temperature of turbine fuel gas is improved, and because of the limitation of the melting point of metal materials, the engine blade adopts an air-cooled hollow blade technology, thereby improving the cooling efficiency of the blade, and further improving the service life and the safety of the blade. However, the shape of the inner cavity of the efficient air-cooled blade is tortuous and complicated, the complicated inner cavity cannot be machined, and the precise size of the inner cavity of the blade can be controlled by adopting an investment precision casting technology, wherein a ceramic core is one of key technologies of the investment precision casting technology. The ceramic core requires moderate high temperature strength, and also has excellent heat stability, good removability and the like.
The existing ceramic core material is a mixed material of quartz glass powder and zirconium silicate, and because the existing ceramic core prepared from the quartz powder and the zirconium silicate material has low strength, the problems of core leakage, core deviation, core breakage and the like easily occur in the casting process, the success rate of casting the blade is reduced, and the cost is increased. The XD-1 developed by Beijing aviation material institute is represented by the XD-1, has excellent solubility and lower expansion coefficient, is suitable for part of directional and single crystal casting, but has the strength of about 8MPa at 1500 ℃, has lower strength and is not suitable for a more complex ceramic core structure.
Disclosure of Invention
In view of the above, the invention aims to provide a high-temperature resistant silicon-based ceramic core, and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a high-temperature-resistant silicon-based ceramic core, which comprises the following steps:
mixing quartz glass powder with different grades with zirconium silicate powder and corundum powder to obtain mixed ceramic powder; the quartz glass powder with different gradations comprises the following components in percentage by mass:
0-50% of 75 mu m quartz glass powder;
20-70% of 45 mu m quartz glass powder;
20-50% of 25 mu m quartz glass powder;
heating, mixing and cooling the mixed ceramic powder and the plasticizer to obtain a ceramic slurry condensate;
performing compression molding and sintering on the ceramic slurry condensate to obtain a sintered ceramic core;
placing the sintered ceramic core in ethyl silicate hydrolysate for first strengthening to obtain a pre-strengthened ceramic core;
and placing the pre-reinforced ceramic core in epoxy resin liquid for second reinforcement to obtain the high-temperature-resistant silicon-based ceramic core.
Preferably, the grain size of the zirconium silicate powder and the corundum powder is independently 10-20 mu m;
the mass of the zirconium silicate powder is 10-20% of the total mass of the mixed ceramic powder;
the mass of the corundum powder is 2-5% of the total mass of the mixed ceramic powder.
Preferably, the plasticizer comprises, in mass percent:
70-80% of paraffin;
15-25% of beeswax;
polyethylene 1-3%;
2-5% of stearic acid.
Preferably, the mass of the plasticizer is 16-20% of the mass of the mixed ceramic powder;
the temperature of the heating and mixing is 110-120 ℃.
Preferably, the pressure of the injection molding is 2-5 MPa, the time for injecting the slurry is 10-20 s, and the pressure maintaining time is 20-30 s; the temperature of the die is 30-40 ℃ during the injection molding.
Preferably, the sintering process includes:
heating to 200 ℃, and preserving heat for 3-5 h;
heating from 200 ℃ to 450 ℃, and preserving heat for 1-2 h;
heating from 450 ℃ to 600 ℃ and preserving heat for 1-2 h;
heating from 600 ℃ to 900 ℃, and preserving heat for 1-2 h;
heating from 900 ℃ to 1170-1230 ℃ and preserving heat for 6-10 h.
Preferably, the components of the ethyl silicate hydrolysate comprise ethyl silicate, hydrochloric acid, ethanol and water;
the time of the first reinforcement is 10-40 min.
Preferably, the components of the epoxy resin liquid comprise epoxy resin, polyamide and acetone;
the second strengthening time is 10-40 min.
The invention provides the high-temperature-resistant silicon-based ceramic core prepared by the preparation method.
The invention provides application of the high-temperature-resistant silicon-based ceramic core in preparing engine blades.
The invention provides a preparation method of a high-temperature-resistant silicon-based ceramic core, which comprises the following steps: mixing quartz glass powder with different grades with zirconium silicate powder and corundum powder to obtain mixed ceramic powder; the quartz glass powder with different gradations comprises the following components in percentage by mass: heating, mixing and cooling the mixed ceramic powder and the plasticizer to obtain a ceramic slurry condensate; performing compression molding and sintering on the ceramic slurry condensate to obtain a sintered ceramic core; placing the sintered ceramic core in ethyl silicate hydrolysate for first strengthening to obtain a pre-strengthened ceramic core; and placing the pre-reinforced ceramic core in epoxy resin liquid for second reinforcement to obtain the high-temperature-resistant silicon-based ceramic core. The invention adopts grain diameter of 75 mu m, 45 mu m and 25 mu m as grading, the grain size is controlled below 100 mu m, and the sintering shrinkage rate of the ceramic core can be reduced and the high-temperature strength can be improved by adopting larger grain diameter proportion; according to the invention, the high-temperature strength is improved by adding the zirconium silicate powder and the corundum powder, and then the high-temperature strength can be further improved by utilizing the grain size grading of the quartz glass powder; the invention utilizes the quartz glass powder grading and the plasticizer of the ceramic slurry to control the fluidity of the ceramic slurry, and simultaneously the quartz powder grading can control the shrinkage rate and improve the sintering success rate of the ceramic core pressed injection green body. The high-temperature-resistant silicon-based ceramic core prepared by the method has the advantages of low sintering shrinkage rate, high-temperature strength and good corrosion resistance, and is suitable for more ceramic core inner cavity structures. The example results show that the high temperature strength of the high temperature resistant silicon-based ceramic core provided by the invention at 1540 ℃ is 15-30 MPa, and the sintering shrinkage rate is 0.67-0.85%.
Furthermore, the invention can control the size range of the high-temperature strength by adjusting the gradation proportion of the quartz glass powder of 75 mu m, 45 mu m and 25 mu m, and more kinds of inner cavities of the ceramic core are applied.
Drawings
FIG. 1 is a flow chart of the preparation of a refractory silicon-based ceramic core of example 1;
FIG. 2 is a 100-fold enlarged microstructure of the sintered ceramic core obtained after sintering in example 4;
FIG. 3 is a 200-fold enlarged microstructure of the sintered ceramic core obtained after sintering in example 4.
Detailed Description
The invention provides a preparation method of a high-temperature-resistant silicon-based ceramic core, which comprises the following steps:
mixing quartz glass powder with different grades with zirconium silicate powder and corundum powder to obtain mixed ceramic powder;
heating, mixing and cooling the mixed ceramic powder and the plasticizer to obtain a ceramic slurry condensate;
performing compression molding and sintering on the ceramic slurry condensate to obtain a sintered ceramic core;
placing the sintered ceramic core in ethyl silicate hydrolysate for first strengthening to obtain a pre-strengthened ceramic core;
and placing the pre-reinforced ceramic core in epoxy resin liquid for second reinforcement to obtain the high-temperature-resistant silicon-based ceramic core.
The sources of the raw materials used in the present invention are all commercially available unless otherwise specified.
The invention mixes quartz glass powder with different grades with zirconium silicate powder and corundum powder to obtain mixed ceramic powder. In the invention, the quartz glass powder with different gradations comprises the following components in percentage by mass:
0 to 50%, preferably 10 to 40%, more preferably 20 to 30% of 75 μm quartz glass powder;
20 to 70%, preferably 30 to 60%, more preferably 40 to 50% of 45 μm quartz glass powder;
the silica glass powder of 25 μm is 20 to 50%, preferably 25 to 45%, and more preferably 30 to 40%.
In the present invention, the particle diameter of the zirconium silicate powder is preferably 10 to 20. Mu.m, more preferably 15. Mu.m; the mass of the zirconium silicate powder is preferably 10 to 20%, more preferably 12 to 18%, and even more preferably 15% of the total mass of the mixed ceramic powder. In the present invention, the zirconium silicate powder functions as a mineralizer. In the invention, the zirconium silicate has small thermal expansion coefficient and strong high temperature resistance, does not generate crystal form transformation, reduces the negative influence of precipitation of cristobalite from quartz glass powder, and improves the strength and the thermal stability of the ceramic core.
In the present invention, the corundum powder preferably has a particle diameter of 10 to 20. Mu.m, more preferably 15. Mu.m; the mass of the corundum powder is preferably 2 to 5% of the total mass of the mixed ceramic powder, more preferably 3 to 4%. In the invention, the corundum powder has the function of improving the high-temperature strength and the normal-temperature strength of the ceramic core.
In the present invention, the mixing means is preferably ball milling mixing. In the present invention, the ball milling is preferably dry ball milling, and the ball milling rate is preferably 150 to 300r/min, more preferably 200 to 250r/min; the time of the ball milling is preferably 2 hours.
After the mixed ceramic powder is obtained, the mixed ceramic powder and the plasticizer are heated, mixed and cooled to obtain the ceramic slurry condensate. In the present invention, the plasticizer preferably includes, in mass percent:
70-80% paraffin wax, preferably 72-78%, more preferably 75%;
15-25% of beeswax, preferably 18-22%, more preferably 20%;
polyethylene 1-3%, preferably 2%;
stearic acid 2-5%, preferably 3%.
In the invention, the melting point of the paraffin is preferably 60 ℃, and the melting point of the beeswax is preferably 62-67 ℃; the number average molecular weight of the polyethylene is preferably 40000 to 300000, more preferably 100000 ～ 200000.
In the present invention, the mass of the plasticizer is preferably 16 to 20% of the mass of the mixed ceramic powder, more preferably 17 to 18%.
In the invention, the feeding mode of the ceramic powder and the plasticizer is preferably as follows: firstly, heating and melting raw materials of the plasticizer, and then adding mixed ceramic powder in batches.
In the present invention, the plasticizer is preferably melted by heating at a temperature of 110 to 120 ℃, more preferably 115 ℃. In the present invention, the mixed ceramic powder is preferably added in 3 to 5 times.
The temperature of the heated mixture is preferably 110 to 120 ℃, more preferably 115 ℃. In the invention, the heating and mixing mode is preferably stirring and mixing firstly and then vacuum mixing; in the present invention, the stirring and mixing time is preferably 3 to 5 hours, more preferably 4 hours; the time for the vacuum mixing is preferably 1 to 2 hours, more preferably 1.5 hours.
In the present invention, the cooling means is preferably: and pouring the ceramic powder and the plasticizer which are heated and mixed into a block shape and naturally cooling.
After the ceramic slurry condensate is obtained, the ceramic slurry condensate is subjected to compression molding and sintering to obtain the sintered ceramic core. In the present invention, the injection molding is preferably performed in an injection molding machine. In the present invention, the temperature of the injection molding machine at the time of injection is preferably 110 to 120 ℃, more preferably 115 ℃. The invention carries out pressure injection at the temperature, the ceramic slurry condensate is converted into ceramic slurry, the filling capacity is better, the plasticizer in the ceramic slurry is not easy to volatilize, and the stability of the slurry is easy to control.
In the present invention, the pressure of the injection molding is preferably 2 to 5MPa, more preferably 3 to 4MPa; the time for injecting the slurry is preferably 10 to 20 seconds, more preferably 15 seconds; the dwell time is preferably 20 to 30s, more preferably 25s. In the present invention, the dwell time is the time between the injection of the slurry and the lifting of the upper die of the injection molding machine.
In the present invention, the temperature of the mold at the time of the injection molding is preferably 30 to 40 ℃, more preferably 35 ℃. And after the press-injection molding, obtaining a ceramic core press-injection green body.
After the injection molding, the method is used for preferably checking whether the ceramic core injection molding green body has defects or not, trimming and deburring, and cleaning residues on the surface.
The invention preferably sinters a ceramic core green compact in an alumina filler. In the present invention, the alumina is preferably calcined alumina, and the temperature of the calcination is preferably 1400 to 1600 ℃, more preferably 1500 ℃. The particle size of the alumina filler is preferably 150 to 320 mesh. In the present invention, the calcined alumina serves to stabilize the alumina crystal form to alpha-alumina.
The calcination is preferably carried out in a sagger; according to the invention, alumina filler is preferably placed at the position of 1/3 of the height of the sagger, then ceramic core pressed green bodies are inserted, the spacing between the ceramic core pressed green bodies is preferably 3-5 cm, and finally alumina filler is added to embed the ceramic core pressed green bodies.
In the present invention, the sintering process preferably includes:
(1) heating to 200 ℃, and preserving heat for 3-5 hours, wherein the heating rate is preferably 3-5 ℃/min;
(2) heating from 200 ℃ to 450 ℃, and preserving heat for 1-2 h, wherein the heating rate is preferably 1-2 ℃/min;
(3) heating from 450 ℃ to 600 ℃, and preserving heat for 1-2 h, wherein the heating rate is preferably 2-4 ℃/min;
(4) heating from 600 ℃ to 900 ℃, and preserving heat for 1-2 h, wherein the heating rate is preferably 5 ℃/min;
(5) heating from 900 ℃ to 1170-1230 ℃, preferably 1200 ℃, and preserving heat for 6-10 h, wherein the heating rate is preferably 5 ℃/min.
In the sintering process, the ceramic core press-injection green body is easy to dewax in a low-temperature dewaxing stage at the temperature of between room temperature and 600 ℃ and is not easy to bulge, crack and deform; in the sintering stage of the core at 600-1200 ℃, the temperature equalizing area of the sagger can be well controlled, and enough cristobalite is separated out.
After the sintered ceramic core is obtained, the sintered ceramic core is placed in ethyl silicate hydrolysate for first strengthening, so that the pre-strengthened ceramic core is obtained. In the invention, the components of the ethyl silicate hydrolysate comprise ethyl silicate, hydrochloric acid, ethanol and water; the volume ratio of the ethyl silicate to the hydrochloric acid to the ethanol to the water is preferably 85-90:1-2:3-4:4-10, and more preferably 86-88:1-2:3-4:5-8. The ethyl silicate hydrolysate can promote the hydrolysis of ethyl silicate fast and raise the high temperature strength of ceramic core by about one time.
In the present invention, the preparation method of the ethyl silicate hydrolysate preferably comprises the following steps:
mixing ethyl silicate, hydrochloric acid, ethanol and water to obtain ethyl silicate hydrolysate.
In the present invention, the temperature of the mixing is preferably 30 to 35℃and the time is preferably 30 to 40 minutes. In the present invention, the mixing is preferably performed under stirring.
In the present invention, the time of the first strengthening is preferably 10 to 40min, preferably 30min, and the temperature is preferably 30 ℃. In the invention, after the first strengthening, the pre-strengthened ceramic core is taken out and naturally dried for more than 24 hours.
After the pre-reinforced ceramic core is obtained, the pre-reinforced ceramic core is placed in epoxy resin liquid for second reinforcement, and the high-temperature-resistant silicon-based ceramic core is obtained. In the invention, the components of the epoxy resin liquid comprise epoxy resin, polyamide and acetone; the mass ratio of the epoxy resin to the polyamide to the acetone is preferably 1-2:1:4-6, and more preferably 1:1:4. In the invention, the epoxy resin liquid of the component can uniformly disperse the epoxy resin, improve the strength of the reinforced ceramic core by 2-3 times, ensure that the reinforcing agent is moderately adhered to the ceramic core and has no influence on the size of the core.
In the present invention, the preparation method of the epoxy resin liquid preferably includes the steps of:
mixing epoxy resin, acetone and polyamide to obtain epoxy resin liquid.
In the present invention, the temperature of the mixing is preferably 30 to 40 ℃, more preferably 35 ℃; the mixing means is preferably stirring mixing.
In the present invention, the time of the second strengthening is preferably 10 to 40min, preferably 30min, and the temperature is preferably 30 ℃. In the invention, after the second strengthening, the high-temperature-resistant silicon-based ceramic core is taken out, naturally dried for 24 hours and dried. In the present invention, the temperature of the drying is preferably 150℃and the time is preferably 30 minutes.
As a specific embodiment of the invention, a preparation flow chart of the high-temperature-resistant silicon-based ceramic core is shown in FIG. 1.
The invention provides the high-temperature-resistant silicon-based ceramic core prepared by the preparation method. The high-temperature-resistant silicon-based ceramic core prepared by the method has the advantages of low sintering shrinkage rate, high-temperature strength and good corrosion resistance, and is suitable for more ceramic core inner cavity structures. The example results show that the high temperature strength of the high temperature resistant silicon-based ceramic core provided by the invention at 1540 ℃ is 15-30 MPa, and the sintering shrinkage rate is 0.67-0.85%.
The invention provides application of the high-temperature-resistant silicon-based ceramic core in preparing engine blades.
The high temperature resistant silicon-based ceramic cores, the preparation method and application thereof provided by the invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the invention.
Example 1
The quartz glass powder adopts the composition of average grain diameter of 75 μm, 45 μm and 25 μm with the mass ratio of 5:3:2. The stone powder glass powder accounts for 82% of the total powder weight, the mineralizer zirconium silicate accounts for 15%, the additive corundum powder accounts for 3%, the zirconium silicate granularity adopts 320 meshes, the corundum granularity adopts 800 meshes, wherein the addition amount of the plasticizer is 20% of the total powder weight, and the stone powder glass powder consists of paraffin wax, polyethylene and stearic acid in a mass ratio of 70:25:2:3.
The ethyl silicate hydrolysate consists of ethyl silicate, hydrochloric acid, alcohol and distilled water, and the mass ratio is 85:1:4:10.
The epoxy resin liquid consists of epoxy resin, polyamide and acetone in the mass ratio of 1:1:4.
The preparation method of the high-temperature-resistant silicon-based ceramic core comprises the following steps:
mixing quartz glass powder with zirconium silicate powder and corundum powder through ball milling to obtain mixed ceramic powder, and drying;
after the plasticizer is melted at 117 ℃, adding ceramic powder in 5 batches, stirring for 5 hours, vacuumizing for 2 hours, cooling and shaping to obtain ceramic slurry condensate;
and (3) placing the ceramic slurry condensate into a pressing and injecting machine for pressing and injecting, wherein the temperature is controlled at 120 ℃, the pressing and injecting pressure is controlled at 3MPa, the pressing and injecting time is 15s, the pressure maintaining time is 20s, and the temperature of a die is 30 ℃ to obtain the ceramic core pressing and injecting green compact.
Placing the ceramic core pressed green compact into alumina filler for sintering, wherein the sintering procedure is as follows: (1) heating to 200 ℃, and preserving heat for 4 hours, wherein the heating rate is 5 ℃/min; (2) heating from 200 ℃ to 450 ℃, and preserving heat for 2 hours, wherein the heating rate is 2 ℃/min; (3) heating from 450 ℃ to 600 ℃, and preserving heat for 2 hours, wherein the heating rate is 3 ℃/min; (4) heating from 600 ℃ to 900 ℃, and preserving heat for 2 hours, wherein the heating rate is 5 ℃/min; (5) heating from 900 ℃ to 1200 ℃, and preserving heat for 6 hours, wherein the heating rate is 5 ℃/min.
After sintering, cleaning the residual filler on the surface of the sintered ceramic core, placing the sintered ceramic core in ethyl silicate hydrolysate for strengthening for 30min, and placing the sintered ceramic core in epoxy resin liquid for strengthening for 30min to obtain the high-temperature-resistant silicon-based ceramic core.
The shrinkage of the high-temperature-resistant silicon-based ceramic core obtained by testing the normal-temperature bending strength and the high Wen Wanshe strength (1540 ℃ for 30 min) of the high-temperature-resistant silicon-based ceramic core obtained by testing the part 3 of the performance test method of HB5353.3-2004 investment casting ceramic core is tested by testing the part 2 of the performance test method of HB5353.2-2004 investment casting ceramic core. Through testing, the high-temperature resistant silicon-based ceramic core has the flexural strength of 24.02MPa at normal temperature, the flexural strength at high temperature of 16.89MPa and the sintering shrinkage rate of 0.67 percent.
Example 2
The quartz glass powder is graded by adopting an average particle size of 75 mu m, 45 mu m and 25 mu m, the mass ratio is 3:5:2, the stone powder glass powder accounts for 82% of the total powder mass, the mineralizer zirconium silicate accounts for 15% of the total powder mass, the additive corundum powder accounts for 3% of the total powder mass, the zirconium silicate granularity adopts 320 meshes, the corundum granularity adopts 800 meshes, wherein the addition amount of the plasticizer is 20% of the total powder mass, and the quartz glass powder consists of paraffin wax, polyethylene and stearic acid with the mass ratio of 70:25:2:3.
The ethyl silicate hydrolysate consists of ethyl silicate, hydrochloric acid, alcohol and distilled water, and the mass ratio is 90:1.5:3.5:5; the epoxy resin liquid consists of epoxy resin, polyamide and acetone in the mass ratio of 1:1:4.
The preparation method and the performance detection method of the high-temperature-resistant silicon-based ceramic core are the same as in example 1.
Through testing, the high-temperature resistant silicon-based ceramic core has the flexural strength of 26.75MPa at normal temperature, the flexural strength at high temperature of 20.79MPa and the sintering shrinkage rate of 0.72 percent.
Example 3
The quartz glass powder is graded by adopting an average grain diameter of 75 mu m, 45 mu m and 25 mu m, the mass ratio is 3:2:5, the stone powder glass powder accounts for 82% of the total powder mass, the mineralizer zirconium silicate accounts for 15%, the additive corundum powder is 3%, the zirconium silicate granularity adopts 320 meshes, the corundum granularity adopts 800 meshes, wherein the addition amount of the plasticizer is 20% of the total powder, and the additive is composed of paraffin: beeswax: polyethylene: stearic acid mass ratio is 70:25:2:3.
The ethyl silicate hydrolysate consists of ethyl silicate, hydrochloric acid, alcohol and distilled water, and the mass ratio is 90:1.5:3.5:5; the epoxy resin liquid consists of epoxy resin, polyamide and acetone in the mass ratio of 1:1:4.
The preparation method and the performance detection method of the high-temperature-resistant silicon-based ceramic core are the same as in example 1.
Through testing, the high-temperature resistant silicon-based ceramic core has the flexural strength of 29.75MPa at normal temperature, the flexural strength at high temperature of 26.39MPa and the sintering shrinkage rate of 0.82 percent.
Example 4
The quartz glass powder is graded by adopting average grain diameter 45 mu m and 25 mu m, the mass ratio is 6:4, the stone powder glass powder accounts for 82% of the total powder mass, the mineralizer zirconium silicate accounts for 15%, the additive corundum powder accounts for 3%, the zirconium silicate granularity adopts 320 meshes, the corundum granularity adopts 800 meshes, wherein the addition amount of the plasticizer is 18% of the total powder mass, and the quartz glass powder consists of paraffin wax, polyethylene and stearic acid with the mass ratio of 70:25:2:3.
The ethyl silicate hydrolysate consists of ethyl silicate, hydrochloric acid, alcohol and distilled water, wherein the mass ratio of the ethyl silicate hydrolysate to the distilled water is 90:1.5:3.5:5; the epoxy resin liquid consists of epoxy resin, polyamide and acetone in the mass ratio of 1:1:4.
The preparation method and the performance detection method of the high-temperature-resistant silicon-based ceramic core are the same as in example 1.
Through testing, the high-temperature resistant silicon-based ceramic core has the flexural strength of 35.99MPa at normal temperature, the flexural strength at high temperature of 30.12MPa and the sintering shrinkage rate of 0.85 percent.
The 100-fold enlarged microstructure of the sintered ceramic core obtained after sintering is shown in fig. 2, and the 200-fold enlarged microstructure is shown in fig. 3. As can be seen from fig. 2 and 3, the sintered ceramic core takes large-particle quartz as a framework, small-particle quartz fills gaps, zirconium silicate and corundum are distributed among quartz powder aggregates, and a porous ceramic core with uniform pore distribution is formed.
Comparative example 1
The preparation method of the silica glass powder was the same as in example 1 except that the silica glass powder was added to a gradation of 54%,10 μm was 26%, zirconium silicate was added to 15%, alumina was 5%, and plasticizer was added to 20% of the total powder mass.
Through testing, the high-temperature resistant silicon-based ceramic core has the flexural strength of 36.17MPa at normal temperature, the flexural strength at high temperature of 18.16MPa and the sintering shrinkage rate of 1.02 percent.
Comparative example 2
The quartz glass powder is graded by adopting the composition of average grain diameter of 75 mu m, 45 mu m and 25 mu m, the mass ratio is 7:2:1, and the rest is the same as the embodiment 1.
The preparation method and the performance detection method of the high-temperature-resistant silicon-based ceramic core are the same as in example 1.
Through testing, the high-temperature resistant silicon-based ceramic core has the flexural strength of 21.5MPa at normal temperature, the flexural strength at high temperature of 12.32MPa and the sintering shrinkage rate of 0.39 percent.
Comparative example 3
In comparison with example 4, only the plasticizer content was changed, the plasticizer content was 22%, and otherwise the same was found.
The preparation method and the performance detection method of the high-temperature-resistant silicon-based ceramic core are the same as in example 1.
Through testing, the high-temperature resistant silicon-based ceramic core has the flexural strength of 42.7MPa at normal temperature, the flexural strength at high temperature of 23.54MPa and the sintering shrinkage rate of 1.38%.
Comparative example 4
In comparison with example 4, no strengthening of the ethyl silicate hydrolysate was performed, and the same was true.
The preparation method and the performance detection method of the high-temperature-resistant silicon-based ceramic core are the same as in example 1.
Through testing, the high-temperature resistant silicon-based ceramic core has the flexural strength of 37.82MPa at normal temperature, the flexural strength at high temperature of 15.70MPa and the sintering shrinkage rate of 0.85%.
Comparative example 5
The same as in example 4 was not performed with the epoxy resin liquid reinforcement, and the other was performed in the same manner.
The preparation method and the performance detection method of the high-temperature-resistant silicon-based ceramic core are the same as in example 1.
Through testing, the high-temperature resistant silicon-based ceramic core has the flexural strength of 13.88MPa at normal temperature, the flexural strength at high temperature of 30.12MPa and the sintering shrinkage rate of 0.85 percent.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A preparation method of a high-temperature-resistant silicon-based ceramic core comprises the following steps:
mixing quartz glass powder with different grades with zirconium silicate powder and corundum powder to obtain mixed ceramic powder; the quartz glass powder with different gradations comprises the following components in percentage by mass:
0-50% of 75 mu m quartz glass powder;
20-70% of 45 mu m quartz glass powder;
20-50% of 25 mu m quartz glass powder;
heating, mixing and cooling the mixed ceramic powder and the plasticizer to obtain a ceramic slurry condensate;
performing compression molding and sintering on the ceramic slurry condensate to obtain a sintered ceramic core;
placing the sintered ceramic core in ethyl silicate hydrolysate for first strengthening to obtain a pre-strengthened ceramic core;
and placing the pre-reinforced ceramic core in epoxy resin liquid for second reinforcement to obtain the high-temperature-resistant silicon-based ceramic core.
2. The preparation method according to claim 1, wherein the particle sizes of the zirconium silicate powder and the corundum powder are independently 10-20 μm;
the mass of the zirconium silicate powder is 10-20% of the total mass of the mixed ceramic powder;
the mass of the corundum powder is 2-5% of the total mass of the mixed ceramic powder.
3. The preparation method according to claim 1, wherein the plasticizer comprises, in mass percent:
70-80% of paraffin;
15-25% of beeswax;
polyethylene 1-3%;
2-5% of stearic acid.
4. A method of producing according to claim 1 or 3, wherein the mass of the plasticizer is 16 to 20% of the mass of the mixed ceramic powder;
the temperature of the heating and mixing is 110-120 ℃.
5. The preparation method according to claim 1, wherein the pressure of the injection molding is 2 to 5MPa, the time for injecting the slurry is 10 to 20s, and the dwell time is 20 to 30s; the temperature of the die is 30-40 ℃ during the injection molding.
6. The method of claim 1, wherein the sintering process comprises:
heating to 200 ℃, and preserving heat for 3-5 h;
heating from 200 ℃ to 450 ℃, and preserving heat for 1-2 h;
heating from 450 ℃ to 600 ℃ and preserving heat for 1-2 h;
heating from 600 ℃ to 900 ℃, and preserving heat for 1-2 h;
heating from 900 ℃ to 1170-1230 ℃ and preserving heat for 6-10 h.
7. The method according to claim 1, wherein the components of the ethyl silicate hydrolysate include ethyl silicate, hydrochloric acid, ethanol and water;
the time of the first reinforcement is 10-40 min.
8. The method of claim 1, wherein the components of the epoxy resin liquid include epoxy resin, polyamide and acetone;
the second strengthening time is 10-40 min.
9. The high temperature resistant silicon-based ceramic core prepared by the preparation method of any one of claims 1 to 8.
10. Use of the refractory silicon-based ceramic core of claim 9 in the manufacture of an engine blade.
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