CN116410013A - Silicon carbide ceramic and preparation method thereof - Google Patents
Silicon carbide ceramic and preparation method thereof Download PDFInfo
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- CN116410013A CN116410013A CN202310433850.XA CN202310433850A CN116410013A CN 116410013 A CN116410013 A CN 116410013A CN 202310433850 A CN202310433850 A CN 202310433850A CN 116410013 A CN116410013 A CN 116410013A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 91
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title description 5
- 239000000843 powder Substances 0.000 claims abstract description 74
- 235000015895 biscuits Nutrition 0.000 claims abstract description 48
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 26
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 238000000110 selective laser sintering Methods 0.000 claims abstract description 13
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- 239000000654 additive Substances 0.000 claims abstract description 8
- 230000000996 additive effect Effects 0.000 claims abstract description 8
- 239000011230 binding agent Substances 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims description 29
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 26
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- 239000000243 solution Substances 0.000 claims description 26
- 229910052710 silicon Inorganic materials 0.000 claims description 25
- 239000010703 silicon Substances 0.000 claims description 25
- 238000001723 curing Methods 0.000 claims description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000007787 solid Substances 0.000 claims description 21
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- 238000000227 grinding Methods 0.000 claims description 18
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 18
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 14
- 239000004215 Carbon black (E152) Substances 0.000 claims description 12
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 12
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- NLSFWPFWEPGCJJ-UHFFFAOYSA-N 2-methylprop-2-enoyloxysilicon Chemical compound CC(=C)C(=O)O[Si] NLSFWPFWEPGCJJ-UHFFFAOYSA-N 0.000 claims description 3
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- HGPXWXLYXNVULB-UHFFFAOYSA-M lithium stearate Chemical compound [Li+].CCCCCCCCCCCCCCCCCC([O-])=O HGPXWXLYXNVULB-UHFFFAOYSA-M 0.000 claims description 3
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
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- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 3
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 3
- 239000005052 trichlorosilane Substances 0.000 claims description 3
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims description 3
- 229910003465 moissanite Inorganic materials 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 10
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a method for manufacturing silicon carbide ceramics, which comprises the following steps: s1: mixing carbon powder, binder, curing agent, lubricant and additive according to a certain proportion and sequence to form composite powder; s2: performing selective laser sintering 3D printing on the composite powder to obtain a ceramic biscuit; s3: degreasing the ceramic biscuit at high temperature to obtain a degreased ceramic biscuit; s4: and (3) densifying the degreased ceramic biscuit to obtain the silicon carbide ceramic. The method for preparing the silicon carbide composite ceramic by selective laser sintering SLS-3D printing provided by the invention has the advantages of high powder bulk density, high biscuit strength and high sintering strength, can solve the problem that a precise silicon carbide structural member with a rice-grade large-size complex special-shaped hollow structure is difficult to prepare, and can also improve the production efficiency of the precise silicon carbide structural member so as to be suitable for industrial mass production.
Description
Technical Field
The invention relates to the technical field of advanced manufacturing and additive manufacturing, in particular to the intelligent manufacturing field of selective laser sintering SiC ceramics and composite materials thereof.
Background
Silicon carbide (SiC) ceramics have higher heat conductivity coefficient, low thermal expansion coefficient, high thermal stability and good corrosion resistance, are excellent structural materials, and have been widely applied to the fields of aviation, aerospace, petrochemical industry, mechanical manufacturing, nuclear industry, microelectronics and the like. At present, the requirements for a high-end precision SiC structural member matched with a diffusion furnace for production in the photovoltaic industry and a precision high-purity SiC structural member for production process of an electronic semiconductor high-end chip are gradually increased for a nuclear reactor core SiC material in the field of large-size complex-shape nuclear industry, a SiC workpiece table for a photoetching machine for manufacturing an integrated circuit, a guide rail, a reflecting mirror, a ceramic sucker, an arm and the like for producing a new energy lithium battery. However, siC is a covalent bond compound having a strong si—c bond, and has a hardness inferior to that of diamond, extremely high hardness, remarkable brittleness, and great difficulty in precision processing. Therefore, the preparation difficulty of the precise SiC structural member with a large-size and complex special-shaped hollow structure is high, the wide application of SiC ceramic in the manufacturing field of high-end equipment such as integrated circuits is limited, the difficulty can be effectively solved by the 3D printing technology, and the preparation technology of the 3D printing SiC ceramic has become one of the main development directions of the research and the application of the SiC ceramic at present. In the future, the 3D printing technology can be widely applied to intelligent workshops, intelligent factories and intelligent supply chains in various fields of manufacturing industry, and effectively promotes the cultivation of modern manufacturing industry and the transformation and upgrading of traditional manufacturing industry.
The selective laser sintering technology (Selective Laser Sintering) SLS is one of 3D printing methods, mainly adopts an infrared laser as energy, and uses a molding material which is mostly a powder material. During processing, firstly preheating the powder to a temperature slightly lower than the melting point of the powder, and then paving the powder under the action of a shaving roller; the laser beam is selectively sintered under the control of a computer according to the layering section information, the next layer of sintering is carried out after one layer of sintering is completed, and redundant powder is removed after all sintering is completed, so that a sintered part can be obtained. The forming method has the advantages of simple manufacturing process, high flexibility, wide material selection range, low material price, low cost, high material utilization rate, no need of building support in the printing process and high forming speed, and is one of the preferred methods for manufacturing the precise SiC ceramic structural member with large-size and complex special-shaped hollow structure. However, the existing SLS-3D technology has low powder bulk density, weak biscuit strength and small strength after sintering in the printing process, and cannot realize efficient preparation of precise silicon carbide structural members with large-size complex special-shaped hollow structures.
Disclosure of Invention
Aiming at the problem that the traditional method is difficult to prepare the SiC ceramic with the large-size complex hollow structure and the composite material structural member thereof, the invention aims to provide the method for preparing the silicon carbide composite ceramic by selective laser sintering SLS-3D printing, which can solve the problem that the precise silicon carbide structural member with the large-size complex special-shaped hollow structure is difficult to prepare, and can also improve the production efficiency of the precise silicon carbide structural member so as to adapt to industrial mass production.
The invention provides a method for manufacturing silicon carbide ceramics, which comprises the following steps: s1: mixing carbon powder, binder, curing agent, lubricant and additive according to a certain proportion and sequence to form composite powder; s2: performing selective laser sintering 3D printing on the composite powder to obtain a ceramic biscuit; s3: degreasing the ceramic biscuit at high temperature to obtain a degreased ceramic biscuit; s4: and (3) densifying the degreased ceramic biscuit to obtain the silicon carbide ceramic.
According to an embodiment of the present invention, the carbon-containing powder is one or more of carbon powder, chopped carbon fiber powder, and silicon carbide powder; the content of the carbon powder or the chopped carbon fiber powder is 0-100wt% and the content of the silicon carbide powder is 100-0wt% based on 100% of the total mass of the carbon-containing powder; the particle size of the carbon-containing powder is 10-600 μm, preferably 10-300 μm, more preferably 100-150 μm; the angular coefficient of the powder is less than or equal to 1.63; the binder is thermoplastic solid phenolic resin; the curing agent is white or colorless crystalline powder urotropine; the lubricant is one or more of white powdery calcium stearate, sodium stearate, lithium stearate, stearic acid and stearic acid amide, preferably calcium stearate; the additive is a silane colorless transparent liquid coupling agent: one or more of vinyl silane, amino silane and methacryloxy silane, preferably 3-aminopropyl triethoxy silane.
According to another embodiment of the invention, the thermoplastic solid phenolic resin is 1-3wt% of the carbon powder-containing body, the urotropin is 15-30wt% of the thermoplastic solid phenolic resin content, the lubricant is 2.5-6wt% of the thermoplastic solid phenolic resin content, and the coupling agent is 1-2wt% of the thermoplastic solid phenolic resin; wherein, the urotropine adopts 40wt% urotropine aqueous solution, and the coupling agent adopts 30wt% coupling agent aqueous solution.
According to another embodiment of the present invention, the step S1 includes: s11: heating the carbon-containing powder to 220-230 ℃, and mixing and grinding for 60-120s to obtain first raw powder; s12: adding the thermoplastic solid phenolic resin after the temperature of the first raw powder is reduced, and mixing and grinding for 60-90s; preferably, the thermoplastic solid phenolic resin is added when the temperature of the first raw powder is reduced to 120+/-5 ℃; s13: adding the coupling agent, and mixing and grinding for 30-60s; s14: adding 50% of the calcium stearate powder, and mixing and grinding for 40-100s to obtain second raw powder; s15: adding urotropine as the curing agent after the temperature of the second raw powder is reduced, and mixing and grinding for 60-120s; preferably, when the temperature of the second raw powder is reduced to 95+/-5 ℃, adding the curing agent urotropine; s16: adding the rest 50% of the calcium stearate powder, and mixing and grinding for 50-100s to form the composite powder.
According to another embodiment of the present invention, in the step S2, the selective laser sintering 3D printing parameters include: the laser power is 12-45W, the scanning speed is 1500-3000mm/s, the scanning interval is 0.05-0.2mm, and the single-layer thickness is 0.1-0.4mm.
According to another embodiment of the present invention, in the step S3, the degreasing temperature is not higher than 1200 ℃, preferably 900 to 1100 ℃; degreasing time is 12-48 h.
According to another embodiment of the present invention, in the step S4, the densification process includes: a precursor polymer solution impregnation treatment and/or a precursor polymer chemical vapor infiltration treatment.
According to another embodiment of the present invention, the precursor polymer solution impregnation treatment process is as follows: putting the degreased ceramic biscuit into a precursor polymer solution for dipping, crosslinking and curing; then, the precursor polymer is converted into cracked carbon or SiC ceramic through high-temperature cracking; the precursor polymer solution is a high-carbon-residue carbon precursor solution or a high-residue Si-based ceramic precursor solution, and the high-carbon-residue carbon precursor is one or more of phenolic resin, pitch resin, sucrose and furan resin; the precursor of the Gao Can Si-based ceramic is one or more of polycarbosilane, polysiloxane and polysilazane; wherein, when the high carbon residue carbon precursor solution is adopted for impregnation treatment, the time for impregnation and crosslinking curing is 4-12h, preferably 10h; degreasing and siliconizing are further carried out after the impregnation, the cross-linking and the solidification, and finally the SiC ceramic is obtained through the high-temperature cracking.
According to another embodiment of the invention, the precursor polymer chemical vapor infiltration treatment process is: at least one or more hydrocarbon or silicon-based gases are adopted as carburizing or silicon-based ceramic media, and after pyrolysis and polycondensation, the hydrocarbon or silicon-based gases are converted into carbon or silicon-based ceramic and deposited in the degreased ceramic biscuit to obtain SiC ceramic; wherein the precursor polymer vapor permeation treatment is performed in a chemical vapor deposition apparatus; controlling the flow rate of the hydrocarbon or silicon-based gas to be 200-300mL/min; the pressure is controlled at 100-300 torr, the temperature of high-temperature decomposition polycondensation is 1000-1300 ℃, the time is 1-10 days, the hydrocarbon is one or more of methane, ethylene and propylene, and the silicon-based gas is one or more of silicon halide (SiX) and trichlorosilane (MTS); when the chemical vapor infiltration treatment of the precursor polymer is carried out by adopting at least one or more hydrocarbons as carburization, siliconizing is also carried out.
The invention also provides silicon carbide ceramic manufactured by the manufacturing method. The silicon carbide ceramic of the invention has the relative density of 90-99%, the silicon content of 0-48 vol% and the density of 2.80-3.15 g/cm 3 Three-point bending strength of 200-500 MPa, elastic modulus of 100-460 GPa and fracture toughness of 2.0-4.5 MPam 1/2 Thermal conductivity is 80-200W/mK, thermal expansion coefficient (RT-400) is 2.0-4.0X10 -6 。
The method for preparing the silicon carbide composite ceramic by selective laser sintering SLS-3D printing provided by the invention has the advantages of high powder bulk density, high biscuit strength and high sintering strength, can solve the problem that a precise silicon carbide structural member with a rice-grade large-size complex special-shaped hollow structure is difficult to prepare, and can also improve the production efficiency of the precise silicon carbide structural member so as to be suitable for industrial mass production.
Drawings
FIG. 1 is a flow chart of a method for producing a silicon carbide ceramic according to the present invention.
FIG. 2 is a flow chart showing the step S1 of the method for producing a silicon carbide ceramic according to the present invention.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
As shown in fig. 1, the method for producing a silicon carbide ceramic according to the present invention comprises: s1: mixing carbon powder, binder, curing agent, lubricant and additive according to a certain proportion and sequence to form composite powder;
s2: carrying out selective laser sintering 3D printing on the composite powder to obtain a ceramic biscuit; s3: degreasing the ceramic biscuit at high temperature to obtain a degreased ceramic biscuit; s4: and (3) densifying the degreased ceramic biscuit to obtain the silicon carbide ceramic. According to the manufacturing method, the powder with high bulk density is obtained by selecting proper powder; by selecting a proper curing agent and a corresponding treatment process, the high-strength biscuit is obtained, the strength of the sintered product is high, the difficult problem that the precise silicon carbide structural member with the large-size complex special-shaped hollow structure in the rice grade is difficult to prepare can be solved, and the production efficiency can be improved so as to be suitable for industrial mass production.
In the step S1, the carbon-containing powder is one or more of carbon powder, chopped carbon fiber powder and silicon carbide powder. The total mass of the carbon powder is 100%, the content of the carbon powder or chopped carbon fiber powder is 0-100% by weight, and the content of the silicon carbide powder is 100-0% by weight. The particle size of the carbon-containing powder is 10 to 600. Mu.m, preferably 10 to 300. Mu.m, more preferably 100to 150. Mu.m. The angular coefficient of the powder is less than or equal to 1.63. The binder is thermoplastic solid phenolic resin. The curing agent is white or colorless crystalline powder urotropine. The lubricant is one or more of white powdery calcium stearate, sodium stearate, lithium stearate, stearic acid and stearic acid amide, preferably calcium stearate. The additive is silane colorless transparent liquid coupling agent: one or more of vinyl silane, amino silane and methacryloxy silane, preferably 3-aminopropyl triethoxy silane.
The thermoplastic solid phenolic resin accounts for 1-3wt% of the carbon-containing powder, the urotropine accounts for 15-30wt% of the thermoplastic solid phenolic resin, the lubricant accounts for 2.5-6wt% of the thermoplastic solid phenolic resin, and the coupling agent accounts for 1-2wt% of the thermoplastic solid phenolic resin; wherein, the urotropine adopts a urotropine aqueous solution with 40 weight percent, and the coupling agent adopts a coupling agent aqueous solution with 30 weight percent.
As shown in fig. 2, the above materials may be mixed to obtain a composite powder by: s11: heating the carbon-containing powder to 220-230 ℃, and mixing and grinding for 60-120s to obtain first raw powder; s12: adding thermoplastic solid phenolic resin after the temperature of the first raw powder is reduced, and mixing and grinding for 60-90s; s13: adding a coupling agent, and mixing and grinding for 30-60s; s14: adding 50% calcium stearate powder, and mixing and grinding for 40-100s to obtain second raw powder; s15: adding urotropine as curing agent after the temperature of the second raw powder is reduced, and mixing and grinding for 60-120s; s16: adding the rest 50% of calcium stearate powder, and mixing and grinding for 50-100s to form composite powder. Preferably, in step S12, the thermoplastic solid phenolic resin is added when the temperature of the primary raw powder is reduced to 120 ℃ ± 5 ℃. Preferably, in the step S15, when the temperature of the second raw powder is reduced to 95+/-5 ℃, the curing agent urotropine is added.
In step S2, the selective laser sintering 3D printing parameters include: the laser power is 12-45W, the scanning speed is 1500-3000mm/s, the scanning interval is 0.05-0.2mm, and the single-layer thickness is 0.1-0.4mm.
In the step S3, the degreasing temperature is not higher than 1200 ℃, and is preferably 900-1100 ℃; degreasing time is 12-48 h.
In step S4, the densification process includes: a precursor polymer solution impregnation treatment and/or a precursor polymer chemical vapor infiltration treatment.
The process of the dipping treatment of the precursor polymer solution comprises the following steps: putting the degreased ceramic biscuit into a precursor polymer solution for dipping, crosslinking and curing; the precursor polymer is then converted to a cracked carbon or SiC ceramic by pyrolysis. The precursor polymer solution may be a high carbon residue carbon precursor solution or a high residue Si based ceramic precursor solution. The carbon precursor with high carbon residue is one or more of phenolic resin, pitch resin, sucrose and furan resin. The precursor of the high-residue Si-based ceramic is one or more of polycarbosilane, polysiloxane and polysilazane. When the impregnation treatment is performed with a carbon precursor solution of high carbon residue, the time for impregnation and crosslinking curing is 4 to 12 hours, preferably 10 hours. Degreasing and siliconizing are also carried out after impregnation and cross-linking solidification, and finally SiC ceramic is obtained through high-temperature pyrolysis. The impregnation-curing-pyrolysis process may be sufficiently performed, and the number of repetitions may be 1 to 3.
The chemical vapor infiltration treatment process of the precursor polymer comprises the following steps: at least one or more hydrocarbon or silicon-based gases are adopted as carburizing or silicon-based ceramic media, and after high-temperature decomposition and polycondensation, the hydrocarbon or silicon-based gases are converted into carbon or silicon-based ceramic and deposited in the degreasing ceramic biscuit to obtain SiC ceramic. The precursor polymer vapor permeation treatment is performed in a chemical vapor deposition apparatus. Controlling the flow rate of hydrocarbon or silicon-based gas to be 200-300mL/min; the pressure is controlled between 100torr and 300torr, the temperature of high temperature decomposition polycondensation is 1000 ℃ to 1300 ℃, and the time is 1 day to 10 days. The hydrocarbon is one or more of methane, ethylene and propylene. The silicon-based gas is one or more of silicon halide (SiX) and trichlorosilane (MTS).
The invention also provides silicon carbide ceramic manufactured by the manufacturing method. The silicon carbide ceramic of the invention has the relative density of 90-99%, the silicon content of 0-48 vol% and the density of 2.80-3.15 g/cm 3 Three-point bending strength of 200-500 MPa, elastic modulus of 100-460 GPa and fracture toughness of 2.0-4.5 MPam 1/2 Thermal conductivity is 80-200W/mK, thermal expansion coefficient (RT-400) is 2.0-4.0X10 -6 。
The present invention will be further illustrated by the following examples. It should also be understood that the following examples are given by way of illustration only and are not to be construed as limiting the scope of the invention, since various insubstantial modifications and adaptations of the invention to those skilled in the art based on the foregoing disclosure are intended to be within the scope of the invention and the specific process parameters and the like set forth below are merely one example of a suitable range within which one skilled in the art would choose from the description herein without being limited to the specific values set forth below.
In the following examples and comparative examples, reagents, materials and instruments used, unless otherwise specified, were commercially available.
Example 1
Taking carbon powder with the particle size d50=150 mu m as 100kg of carbon-containing powder, wherein the angular coefficient of the powder is=1.63, and the raw materials are mixed and prepared according to the following process:
according to the design model, the powder is placed into selective laser SLS printing equipment for 3D printing, the laser power is 40W, the scanning speed is 2000mm/s, the scanning interval is 0.1mm, and the single-layer thickness is 0.3mm, so that the ceramic biscuit is obtained. And (3) degreasing the ceramic material biscuit at a high temperature of 900 ℃/12h to obtain a degreased biscuit sample. Will take offAnd immersing the post-fat biscuit sample in furan resin solution for densification treatment, wherein the crosslinking curing time is 12h. And degreasing the densified ceramic biscuit at 1000 ℃/24h, and then further carrying out siliconizing reaction sintering at 1600 ℃ for 120 minutes to obtain the silicon carbide ceramic. Its density is 2.80g/cm 3 Three-point bending strength 200MPa, elastic modulus 230GPa and fracture toughness 2.2MPam 1/2 Thermal conductivity 180W/mK, thermal expansion coefficient (RT-400) 4.0X10 -6 。
Example 2
Taking silicon carbide powder with the particle size d50=50 μm and carbon powder with the particle size d50=10 μm as 100kg raw materials, wherein the mass ratio is 3:2, the angular coefficient of the powder is=1.20, and the raw materials are mixed and prepared according to the following process:
according to the design model, the powder is placed into selective laser SLS printing equipment for 3D printing, the laser power is 35W, the scanning speed is 1500mm/s, the scanning interval is 0.1mm, and the single-layer thickness is 0.2mm, so that the ceramic biscuit is obtained. And (3) degreasing the ceramic material biscuit at a high temperature of 1000 ℃/24h to obtain a degreased biscuit sample. And (3) immersing the degreased biscuit sample in a polycarbosilane resin solution for densification treatment, wherein the cross-linking curing time is 10 hours, and sintering the densified ceramic biscuit at a high temperature of 1600 ℃/1 hour to obtain the silicon carbide ceramic. Its density is 2.95g/cm 3 Three-point bending strength 300MPa, elastic modulus 300GPa and fracture toughness 2.5MPam 1/2 Thermal conductivity 120W/mK, thermal expansion coefficient (RT-400) 3.7X10 -6 。
Example 3
Taking silicon carbide powder with the particle size D50=50 mu m and carbon fiber with the particle size D50=60 mu m as 100kg of raw materials, wherein the mass ratio is 4:1, the angular coefficient of the powder is=1.6, and the raw materials are mixed and prepared according to the following process:
according to the design model, the powder is placed into selective laser SLS printing equipment for 3D printing, the laser power is 35W, the scanning speed is 2000mm/s, the scanning interval is 0.1mm, and the single-layer thickness is 0.2mm, so that the ceramic biscuit is obtained. And (3) degreasing the ceramic material biscuit at a high temperature of 1000 ℃/24h to obtain a degreased biscuit sample. And (3) immersing the defatted biscuit sample in a polycarbosilane resin solution for densification treatment, wherein the crosslinking curing time is 10h. And sintering the densified ceramic biscuit at a high temperature of 1600 ℃/1h to obtain the carbon fiber reinforced silicon carbide ceramic composite material. Its density is 2.90g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Three-point bending strength 310MPa, elastic modulus 150GPa and fracture toughness 4.5MPam 1/2 Thermal conductivity 106W/mK, thermal expansion coefficient (RT-400) 3.7X10 -6 。
Example 4
100kg of silicon carbide powder with the particle size d50=110 mu m is taken as a raw material, the angular coefficient of the powder is=1.20, and the raw materials are mixed and prepared according to the following process:
according to the design model, the powder is placed into selective laser SLS printing equipment for 3D printing, the laser power is 20W, the scanning speed is 3000mm/s, the scanning interval is 0.1mm, and the single-layer thickness is 0.2mm, so that the ceramic biscuit is obtained. And (3) degreasing the ceramic material biscuit at a high temperature of 900 ℃/12h to obtain a degreased biscuit sample. And (3) carrying out phenolic resin solution impregnation densification treatment on the defatted biscuit sample, wherein the crosslinking curing time is 10h, and carrying out phenolic resin solution impregnation densification treatment on the ceramic biscuit subjected to the first densification treatment after the ceramic biscuit is degreased at 1200 ℃/48h, wherein the crosslinking curing time is 10h. And degreasing the densified ceramic biscuit at 1200 ℃/48h, and then further carrying out siliconizing reaction sintering at 1800 ℃ for 120 minutes to obtain the high-density silicon carbide ceramic. Its density is 3.15g/cm 3 Three-point bending strength 500MPa, elastic modulus 450GPa and fracture toughness 4.0MPam 1/2 Thermal conductivity 190W/mK, thermal expansion coefficient (RT-400) 4.0X10 -6 。
The present embodiment is merely illustrative of the present application, and the present application is not limited thereto, and a worker can make various changes and modifications without departing from the scope of the technical idea of the present application. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of claims.
Claims (10)
1. A method for producing a silicon carbide ceramic, comprising:
s1: mixing carbon powder, binder, curing agent, lubricant and additive according to a certain proportion and sequence to form composite powder;
s2: performing selective laser sintering 3D printing on the composite powder to obtain a ceramic biscuit;
s3: degreasing the ceramic biscuit at high temperature to obtain a degreased ceramic biscuit; and
s4: and (3) densifying the degreased ceramic biscuit to obtain the silicon carbide ceramic.
2. The method for producing a silicon carbide ceramic according to claim 1, wherein,
the carbon-containing powder is one or more of carbon powder, chopped carbon fiber powder and silicon carbide powder; the content of the carbon powder or the chopped carbon fiber powder is 0-100wt% and the content of the silicon carbide powder is 100-0wt% based on 100% of the total mass of the carbon-containing powder; the particle size of the carbon-containing powder is 10-600 μm, preferably 10-300 μm, more preferably 100-150 μm; the angular coefficient of the powder is less than or equal to 1.63;
the binder is thermoplastic solid phenolic resin;
the curing agent is white or colorless crystalline powder urotropine;
the lubricant is one or more of white powdery calcium stearate, sodium stearate, lithium stearate, stearic acid and stearic acid amide, preferably calcium stearate;
the additive is a silane colorless transparent liquid coupling agent: one or more of vinyl silane, amino silane and methacryloxy silane, preferably 3-aminopropyl triethoxy silane.
3. The method for producing a silicon carbide ceramic according to claim 2, wherein,
the thermoplastic solid phenolic resin is 1-3wt% of the carbon-containing powder, the urotropine is 15-30wt% of the thermoplastic solid phenolic resin, the lubricant is 2.5-6wt% of the thermoplastic solid phenolic resin, and the coupling agent is 1-2wt% of the thermoplastic solid phenolic resin;
wherein, the urotropine adopts 40wt% urotropine aqueous solution, and the coupling agent adopts 30wt% coupling agent aqueous solution.
4. The method for producing silicon carbide ceramic according to claim 2, wherein the step S1 comprises:
s11: heating the carbon-containing powder to 220-230 ℃, and mixing and grinding for 60-120s to obtain first raw powder;
s12: adding the thermoplastic solid phenolic resin after the temperature of the first raw powder is reduced, and mixing and grinding for 60-90s; preferably, the thermoplastic solid phenolic resin is added when the temperature of the first raw powder is reduced to 120+/-5 ℃;
s13: adding the coupling agent, and mixing and grinding for 30-60s;
s14: adding 50% of the calcium stearate powder, and mixing and grinding for 40-100s to obtain second raw powder;
s15: adding urotropine as the curing agent after the temperature of the second raw powder is reduced, and mixing and grinding for 60-120s; preferably, when the temperature of the second raw powder is reduced to 95+/-5 ℃, adding the curing agent urotropine; and
s16: adding the rest 50% of the calcium stearate powder, and mixing and grinding for 50-100s to form the composite powder.
5. The method of manufacturing silicon ceramic according to claim 1, wherein in the S2 step, the selective laser sintering 3D printing parameters include: the laser power is 12-45W, the scanning speed is 1500-3000mm/s, the scanning interval is 0.05-0.2mm, and the single-layer thickness is 0.1-0.4mm.
6. The method for producing a silicon carbide ceramic according to claim 1, wherein in the step S3, the degreasing temperature is not higher than 1200 ℃, preferably 900 to 1100 ℃; degreasing time is 12-48 h.
7. The method for producing a silicon carbide ceramic according to claim 1, wherein in the step S4, the densification process comprises: a precursor polymer solution impregnation treatment and/or a precursor polymer chemical vapor infiltration treatment.
8. The method for producing silicon carbide ceramic according to claim 7, wherein the precursor polymer solution impregnation treatment is performed by: putting the degreased ceramic biscuit into a precursor polymer solution for dipping, crosslinking and curing; then, the precursor polymer is converted into cracked carbon or SiC ceramic through high-temperature cracking;
the precursor polymer solution is a high-carbon-residue carbon precursor solution or a high-residue Si-based ceramic precursor solution, and the high-carbon-residue carbon precursor is one or more of phenolic resin, pitch resin, sucrose and furan resin; the precursor of the Gao Can Si-based ceramic is one or more of polycarbosilane, polysiloxane and polysilazane;
wherein, when the high carbon residue carbon precursor solution is adopted for impregnation treatment, the time for impregnation and crosslinking curing is 4-12h, preferably 10h; degreasing and siliconizing are further carried out after the impregnation, the cross-linking and the solidification, and finally the SiC ceramic is obtained through the high-temperature cracking.
9. The method for producing silicon carbide ceramic according to claim 7, wherein the chemical vapor infiltration treatment of the precursor polymer is performed by: at least one or more hydrocarbon or silicon-based gases are adopted as carburizing or silicon-based ceramic media, and after pyrolysis and polycondensation, the hydrocarbon or silicon-based gases are converted into carbon or silicon-based ceramic and deposited in the degreased ceramic biscuit to obtain SiC ceramic;
wherein the precursor polymer vapor permeation treatment is performed in a chemical vapor deposition apparatus; controlling the flow rate of the hydrocarbon or silicon-based gas to be 200-300mL/min; the pressure is controlled at 100-300 torr, the temperature of high-temperature decomposition polycondensation is 1000-1300 ℃, the time is 1-10 days, the hydrocarbon is one or more of methane, ethylene and propylene, and the silicon-based gas is one or more of silicon halide and trichlorosilane;
when the chemical vapor infiltration treatment of the precursor polymer is carried out by adopting at least one or more hydrocarbons as carburization, siliconizing is also carried out.
10. A silicon carbide ceramic manufactured by the manufacturing method according to any one of claims 1 to 9; preferably, the silicon carbide ceramic has a relative density of 90-99%, a silicon content of 0-48 vol% and a density of 2.80-3.15 g/cm 3 Three-point bending strength of 200-500 MPa, elastic modulus of 100-460 GPa and fracture toughness of 2.0-4.5 MPam 1/2 Thermal conductivity is 80-200W/mK, thermal expansion coefficient (RT-400) is 2.0-4.0X10 -6 。
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