CN116409997A - Silicon carbide composite ceramic and preparation method thereof - Google Patents
Silicon carbide composite ceramic and preparation method thereof Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 66
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000919 ceramic Substances 0.000 title claims description 49
- 238000000034 method Methods 0.000 claims abstract description 54
- 235000015895 biscuits Nutrition 0.000 claims abstract description 52
- 239000000843 powder Substances 0.000 claims abstract description 37
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 238000010146 3D printing Methods 0.000 claims abstract description 19
- 238000000280 densification Methods 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 10
- 238000005086 pumping Methods 0.000 claims abstract description 5
- 238000001723 curing Methods 0.000 claims description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 20
- 229910052710 silicon Inorganic materials 0.000 claims description 20
- 239000010703 silicon Substances 0.000 claims description 20
- 239000011230 binding agent Substances 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 claims description 17
- 238000007639 printing Methods 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 15
- 229920000642 polymer Polymers 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- 238000005238 degreasing Methods 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 238000005470 impregnation Methods 0.000 claims description 8
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 7
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims description 7
- 238000004132 cross linking Methods 0.000 claims description 7
- 239000007849 furan resin Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 229920001568 phenolic resin Polymers 0.000 claims description 7
- 239000005011 phenolic resin Substances 0.000 claims description 7
- 239000004215 Carbon black (E152) Substances 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 229930195733 hydrocarbon Natural products 0.000 claims description 6
- 150000002430 hydrocarbons Chemical class 0.000 claims description 6
- 230000008595 infiltration Effects 0.000 claims description 6
- 238000001764 infiltration Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005336 cracking Methods 0.000 claims description 5
- 238000013001 point bending Methods 0.000 claims description 5
- 238000005475 siliconizing Methods 0.000 claims description 5
- WHOZNOZYMBRCBL-OUKQBFOZSA-N (2E)-2-Tetradecenal Chemical compound CCCCCCCCCCC\C=C\C=O WHOZNOZYMBRCBL-OUKQBFOZSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 229940092714 benzenesulfonic acid Drugs 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
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- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 4
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- 229920005989 resin Polymers 0.000 claims description 4
- 238000013461 design Methods 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 229920003257 polycarbosilane Polymers 0.000 claims description 3
- 238000006068 polycondensation reaction Methods 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 238000005255 carburizing Methods 0.000 claims description 2
- 239000012700 ceramic precursor Substances 0.000 claims description 2
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- 239000003822 epoxy resin Substances 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- 229910003465 moissanite Inorganic materials 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 229920001709 polysilazane Polymers 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 238000000605 extraction Methods 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 238000005406 washing Methods 0.000 description 6
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- 230000008021 deposition Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 241000252254 Catostomidae Species 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000000110 selective laser sintering Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007652 sheet-forming process Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
- C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
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Abstract
The invention discloses a silicon carbide composite ceramic material and a preparation method thereof, wherein silicon carbide powder with specific parameters (particle size, angular coefficient and bulk density) is taken as a raw material, and the operation of pumping air and vibrating at low frequency is combined with layering powder in the 3D printing process, so that a high-density silicon carbide ceramic material biscuit is realized, and the density of the prepared silicon carbide ceramic material biscuit can reach 1.90g/cm 3 . The silicon carbide composite ceramic material with the same biscuit density is prepared, the subsequent densification times are reduced, the process is simplified, and the energy is saved.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a silicon carbide composite ceramic material and a preparation method thereof.
Background
The silicon carbide ceramic has high elastic modulus and specific stiffness, is not easy to deform, has higher heat conductivity coefficient, low thermal expansion coefficient, high thermal stability and good corrosion resistance, so that the silicon carbide ceramic is an excellent structural material and has been widely applied to the fields of aviation, aerospace, petrochemical industry, mechanical manufacturing, nuclear industry, microelectronics industry and the like. The silicon carbide ceramic material can be particularly applied to nuclear reactor core materials in the field of nuclear industry, silicon carbide workpiece tables, guide rails, reflectors, ceramic suckers, arms and the like for manufacturing key equipment photoetching machines of integrated circuits, and high-end precise SiC structural members matched with the production of new energy lithium batteries and high-end precise SiC structural members matched with diffusion furnaces for the production of photovoltaic industry and precise high-purity SiC structural members for the production process of electronic semiconductor high-end chips.
However, since silicon carbide is a covalent bond compound having a strong Si-C bond, the hardness is inferior to that of diamond, and it has extremely high hardness and remarkable brittleness, and difficulty in precision processing. Therefore, the difficulty of manufacturing precise silicon carbide structural members with large-size and complex special-shaped hollow structures is high, and the wide application of silicon carbide ceramics in the field of manufacturing high-end equipment such as integrated circuits is limited.
The 3D printing technique is an additive manufacturing technique that is distinct from traditional material processing methods. The 3D printing technology is based on three-dimensional digital model design, and the three-dimensional entity is manufactured by carrying out layered processing, stacking and bonding on materials such as ceramic powder, resin, metal powder and the like through a software layered discrete and numerical control forming system and finally carrying out superposition forming. Compared with the traditional manufacturing method, the 3D printing technology saves raw materials, is easy to quickly manufacture materials with complex structures, shortens the research and development period, and is more suitable for the production of personalized products. The method is suitable for preparing the precise silicon carbide structural member with the complicated special-shaped hollow structure.
The SiC ceramic 3D printing forming method mainly comprises laser selective sintering (selective laser sintering, SLS) and three-dimensional jet printing (thread-dimensional printing or binder casting, 3DP or BJ); slurry/paste forming processes include photo curing (SL) and ink direct write forming (direct ink writing, DIW); particle/wire forming processes generally refer to fused deposition forming (fused deposition modeling, FDM); the sheet forming process is generally referred to as sheet laminate forming (laminated object manufacturing, LOM). Although all 3D printing methods have advantages, the problem of low production efficiency of these direct 3D printing forming methods is not suitable for industrial mass production.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a method for preparing silicon carbide composite ceramic by combining 3D printing with precursor dipping and cracking and chemical vapor infiltration, which can solve the problem that a precise silicon carbide structural member with a complicated special-shaped hollow structure is difficult to prepare and can improve the production efficiency so as to be suitable for industrial mass production.
In order to overcome the problems in the prior art, the invention provides a preparation method of silicon carbide composite ceramic, which is characterized by comprising the following steps:
s1, taking silicon carbide powder as a raw material, pickling the silicon carbide powder, and then cleaning the silicon carbide powder to be neutral by using clear water to obtain a silicon carbide powder raw material;
s2, uniformly mixing the silicon carbide powder raw material obtained in the step S1 with a curing agent to obtain a silicon carbide-curing agent mixture;
and S3, performing 3D printing on the silicon carbide-curing agent mixture obtained in the step S2 to obtain a silicon carbide ceramic material biscuit.
According to an embodiment of the invention, in step S1, the silicon carbide powder has a particle size of 1 to 600um, preferably 10 to 300um, more preferably 100to 150um;
the invention is beneficial to improving the density of the obtained silicon carbide ceramic material biscuit by controlling the grain size of the raw material powder within the range of 1-600 um.
In the invention, the purpose of acidizing the silicon carbide powder is to remove impurities in the raw material powder and improve the strength of the printing biscuit
According to one embodiment of the invention, the angular coefficient of the silicon carbide powder is less than or equal to 1.63;
in the invention, the angular coefficient of the silicon carbide powder is controlled to be less than or equal to 1.63, so that the density of the obtained silicon carbide ceramic material biscuit is improved.
According to one embodiment of the invention, the bulk density of the silicon carbide powder is 1.20-2.00 g.cm -3 ；
The bulk density of the raw material powder is controlled to be 1.20-2.00 g.cm -3 In the range, the density of the obtained silicon carbide ceramic material biscuit is improved. If the bulk density of the raw material powder is too small, the ceramic prepared by post-sintering has low density or the number of densification is too large. According to one embodiment of the invention, the standard of the clean water to be washed to be neutral is that the pH value is 6-8, and the acid consumption value of the powder is less than or equal to 5.0.
According to an embodiment of the present invention, in step S2, the content of the curing agent is 30 to 70wt% of the binder content; controlling the acidity of the curing agent to be 18-28; the curing agent is as follows: one or more of dilute sulfuric acid, hydrochloric acid, phosphoric acid, boric acid, oxalic acid, maleic anhydride, citric acid, malic acid, benzenesulfonic acid or phenolsulfonic acid, preferably benzenesulfonic acid or phenolsulfonic acid, more preferably p-toluenesulfonic acid; the mixing time is 30-120 s.
According to a specific embodiment of the invention, in step S3, the specific operation steps are selecting a proper binder, setting printing parameters, performing 3D printing according to a CAD design, simultaneously pumping air from the layed powder during printing, and vibrating at low frequency to obtain a biscuit of silicon carbide ceramic material;
according to the invention, the density of the obtained silicon carbide ceramic material biscuit can be improved by simultaneously carrying out air extraction on the layering powder in the 3D printing process and carrying out low-frequency vibration operation.
According to one embodiment of the invention, the binder comprises one or more of phenolic resin, furan resin, polyvinyl alcohol (PVA), polyvinyl butyral (PVB), polymethyl methacrylate (PMMA), or epoxy resin.
According to a specific embodiment of the present invention, the specific operation steps of the 3D printing are: the printing parameters include: the spraying amount of the binder is 0.8-2.0% of the mass of the silicon carbide powder, the printing temperature is controlled at 15-25 ℃, the humidity is controlled at 50-70%, the spraying scanning speed is 0.4-1 m/s, and the scanning interval is 0.1-0.5 mm; the thickness of the printed layer is controlled to be 0.15-0.6 mm.
According to one embodiment of the invention, the vacuum degree of the air suction operation is controlled to be lower than 1000Pa, and the powder is vibrated at a low frequency, wherein the vibration frequency is 15-50 Hz, preferably 30Hz.
The density of the obtained silicon carbide ceramic material biscuit can be improved by simultaneously carrying out air extraction operation on the layering powder in the 3D printing process and low-frequency vibration operation.
According to one embodiment of the present invention, the above preparation method further comprises the steps of:
s4, degreasing the silicon carbide ceramic material biscuit obtained in the step S3 at a high temperature to obtain a degreased silicon carbide ceramic biscuit;
s5, densifying the degreased silicon carbide ceramic biscuit obtained in the step S4 to obtain a densified silicon carbide composite ceramic biscuit;
and S6, performing high-temperature sintering or siliconizing sintering on the silicon carbide composite ceramic biscuit obtained in the step S5 to obtain the high-strength silicon carbide composite ceramic.
According to an embodiment of the present invention, in step S5, the densification process includes: a precursor polymer solution impregnation treatment and/or a precursor polymer chemical vapor infiltration treatment.
According to one embodiment of the invention, the precursor Polymer solution is a high carbon residue carbon precursor solution or a high Si-based ceramic precursor PDCs (Polymer-derived ceramics) solution; the carbon precursor with high carbon residue content can be one or more of phenolic resin, pitch resin, sucrose and furan resin; the precursor PDCs of the Gao Can Si-based ceramic can be one or more of polycarbosilane, polysiloxane and polysilazane.
According to one embodiment of the invention, the precursor polymer solution impregnation treatment process comprises the following steps: placing the degreased silicon carbide ceramic biscuit sample into a precursor polymer solution for dipping, crosslinking and curing; converting the precursor polymer into cracked carbon or SiC ceramic through high-temperature cracking; and repeating the dipping-curing-cracking process to obtain the densified ceramic sample.
Wherein, the time of impregnation and crosslinking curing is 4-12h, preferably 10h;
each impregnation is followed by a high temperature degreasing, and the impregnation-curing-cracking process is repeated 1-3 times.
According to one embodiment of the invention, the chemical vapor infiltration treatment process 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 pyrolysis and polycondensation, the hydrocarbon and silicon-based gases are converted into carbon or silicon-based ceramic and deposited in the porous degreasing biscuit to obtain a biscuit sample after carburization or silicon-based ceramic treatment;
wherein the chemical vapor infiltration treatment is performed in a chemical vapor deposition apparatus;
according to one embodiment of the invention, the flow rate of the hydrocarbon or silicon-based gas is 200-300mL/min; the pressure is 100-300 torr, the temperature of high temperature decomposition polycondensation is 1000-1300 ℃, and the time is 1-10 days;
the hydrocarbon is one or more of methane, ethylene and propylene;
the silicon-based gas is one or more of silicon halides (SiX) and trichlorosilane (MTS).
According to one embodiment of the present invention, in step S6, the high temperature sintering is performed at 1450 to 2200 ℃ for 60 to 120 minutes.
According to an embodiment of the present invention, in step S6, the specific steps of siliconizing sintering are: burying the obtained product in silicon powder, and sintering at 1450-2200 ℃ for 60-120 minutes.
The invention also aims to provide the silicon carbide composite ceramic prepared by the preparation method.
According to one embodiment of the invention, the properties of the obtained silicon carbide composite ceramic are as follows: the relative density is 90-99%; silicon content 0-55 vol%; density of 2.72-3.15 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The three-point bending strength is 200-500 MPa; the elastic modulus is 200-460 GPa; fracture toughness of 2.0-4.0 MPam 1/2 The method comprises the steps of carrying out a first treatment on the surface of the The heat conductivity is 40-200W/m.K; the thermal expansion coefficient (RT-400 ℃) is 2.0 to 4.0X10 -6 。
The beneficial effects are that:
compared with the prior art, the invention has the advantages that:
in the prior art, the density of the silicon carbide ceramic material biscuit prepared by 3D printing is low, and the silicon carbide composite ceramic material with ideal bulk density can be prepared by subsequent densification or sintering treatment for multiple times. The invention realizes the high-density silicon carbide ceramic material biscuit by taking silicon carbide powder with specific parameters (particle size, angular coefficient and bulk density) as raw materials and combining the operations of pumping air and vibrating at low frequency on the layered powder in the 3D printing process, and the density of the prepared silicon carbide ceramic material biscuit can reach 1.90g/cm 3 . The silicon carbide composite ceramic material with the same biscuit density is prepared, the subsequent densification times are reduced, the process is simplified, and the energy is saved.
Detailed Description
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.
Example 1
Taking silicon carbide powder with the particle size d50=200 um as a raw material, wherein the angular coefficient of the powder is=1.63; washing the powder with acid, and washing with clear water to neutral 7, wherein the acid consumption value of the powder is 4.0, and the bulk density of the powder is 1.35g cm -3 The method comprises the steps of carrying out a first treatment on the surface of the Mixing the raw materials with p-benzenesulfonic acid serving as a curing agent for 30 seconds, wherein the content of the curing agent is 40wt% of the binder; adopting a binder jet printing method, selecting a phenolic resin binder, controlling the jet quantity of the binder to be 1.0% of the mass of powder, controlling the printing temperature to be 20 ℃, controlling the humidity to be 50%, controlling the jet scanning speed to be 0.4m/s, controlling the scanning interval to be 0.1mm, and controlling the thickness of a printed layer to be 0.15mm; pumping powder during printingPerforming gas treatment, controlling the air suction vacuum degree at 1000Pa, and simultaneously performing low-frequency vibration on the powder layer, wherein the vibration frequency is 30Hz/120s, so as to obtain a silicon carbide ceramic material biscuit with the density of 1.50 g.cm -3 The method comprises the steps of carrying out a first treatment on the surface of the High-temperature degreasing is carried out on the ceramic material biscuit at the degreasing temperature of 900 ℃/12h, and a defatted biscuit sample is obtained; immersing the degreased biscuit sample in furan resin solution for densification treatment, wherein the cross-linking curing time is 12h, degreasing the densified ceramic biscuit at 1000 ℃/24h, and then further carrying out siliconizing reaction sintering at 1600 ℃ for 120 minutes to obtain silicon carbide composite ceramic with the density of 2.72g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Three-point bending strength 200MPa; the elastic modulus is 220GPa; fracture toughness 2.0MPam 1/2 The method comprises the steps of carrying out a first treatment on the surface of the Thermal conductivity 125W/mK; coefficient of thermal expansion (RT-400) 4.0X10 -6 。
Example 2
Taking silicon carbide powder with the particle size d50=30um as a raw material, wherein the angular coefficient of the powder is=1.15; washing the powder with acid, and washing with clear water to neutral 7, wherein the acid consumption value of the powder is 5.0, and the bulk density of the powder is 1.65 g.cm -3 The method comprises the steps of carrying out a first treatment on the surface of the Mixing the raw materials with p-benzenesulfonic acid curing agent for 60s, wherein the content of the curing agent is 50wt% of the binder; adopting a binder jet printing method, selecting a furan resin binder, controlling the jet quantity of the binder to be 1.5% of the mass of powder, controlling the printing temperature to be 25 ℃, controlling the humidity to be 60%, controlling the jet scanning speed to be 1m/s, controlling the scanning interval to be 0.2mm, and controlling the thickness of a printed layer to be 0.30mm; during printing, the powder is subjected to air extraction treatment, the air extraction vacuum degree is controlled to be 1000Pa, meanwhile, the powder layer is subjected to low-frequency vibration, the vibration frequency is 30Hz/120s, and a silicon carbide ceramic material biscuit with the density of 1.72 g.cm is obtained -3 The method comprises the steps of carrying out a first treatment on the surface of the High-temperature degreasing is carried out on the ceramic material biscuit at the degreasing temperature of 1000 ℃/24h, and a defatted biscuit sample is obtained; immersing the defatted biscuit sample in polycarbosilane resin solution for densification treatment, wherein the crosslinking curing time is 10h, and sintering the densified ceramic biscuit at a high temperature of 1500 ℃/1h to obtain silicon carbide composite ceramic with the density of 2.94g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Three-point bending strength 295MPa; the elastic modulus is 300GPa; fracture toughness 2.0MPam 1/2 The method comprises the steps of carrying out a first treatment on the surface of the Thermal conductivity 40W/mK; coefficient of thermal expansion (RT-400) 3.7X10 -6 。
Example 3
Taking silicon carbide powder with the particle size d50=100 um as a raw material, wherein the angular coefficient of the powder is=1.20; washing the powder with acid, washing with clear water to neutral 7, wherein the acid consumption value of the powder is=4.5, and the bulk density of the powder is 1.70 g.cm -3 The method comprises the steps of carrying out a first treatment on the surface of the Mixing the raw materials with p-benzenesulfonic acid serving as a curing agent for 120 seconds, wherein the content of the curing agent is 50wt% of that of the binder; adopting a binder jet printing method, selecting a furan resin binder, controlling the jet quantity of the binder to be 1.0% of the mass of powder, controlling the printing temperature to be 23 ℃, controlling the humidity to be 65%, controlling the jet scanning speed to be 0.4m/s, controlling the scanning interval to be 0.5mm, and controlling the thickness of a printed layer to be 0.3mm; during printing, the powder is subjected to air extraction treatment, the air extraction vacuum degree is controlled to be 1000Pa, meanwhile, the powder layer is subjected to low-frequency vibration, the vibration frequency is 30Hz/120s, and a silicon carbide ceramic material biscuit with the density of 1.90 g.cm is obtained -3 The method comprises the steps of carrying out a first treatment on the surface of the High-temperature degreasing is carried out on the ceramic material biscuit at a speed of 1200 ℃/48h, and a defatted biscuit sample is obtained; carrying out phenolic resin solution impregnation densification treatment on a degreased biscuit sample, wherein the cross-linking curing time is 10h, carrying out phenolic resin solution impregnation densification treatment on the ceramic biscuit subjected to the first densification treatment after being degreased at 1200 ℃/48h, wherein the cross-linking curing time is 10h, carrying out siliconizing reaction sintering on the ceramic biscuit subjected to the densification treatment after being degreased at 1200 ℃/48h, wherein the sintering temperature is 1800 ℃ and the time is 120 min, so as to obtain the high-density silicon carbide composite ceramic with the density of 3.13g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The three-point bending strength is 500MPa; the elastic modulus is 450GPa; fracture toughness 4.0MPam 1/2 The method comprises the steps of carrying out a first treatment on the surface of the Thermal conductivity 120W/mK; coefficient of thermal expansion (RT-400 ℃ C.) 4.0X10 -6 。
Comparative example 1
Other conditions are the same as in example 1, except that the powder is not subjected to air extraction and low-frequency vibration treatment in the 3D printing process, and the density of the obtained silicon carbide ceramic material biscuit is 1.35 g.cm -3 。
Comparative example 2
The other conditions were the same as in example 1, except that the raw material silicon carbide powder had a particle diameter of 0.5 μm, an angular coefficient of 1.7 and a bulk density of 1.12 g.cm -3 The obtained carbonized productThe density of the biscuit of the silicon ceramic material is 1.21 g.cm -3 。
As can be seen from analysis of examples 1-3 and comparative examples 1-2, the technical scheme of the application uses silicon carbide powder with specific parameters (particle size, angular coefficient and bulk density) as raw materials, and combines the operations of air extraction and low-frequency vibration on the layered powder in the 3D printing process to realize the preparation of the high-density silicon carbide ceramic material biscuit.
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 (12)
1. The preparation method of the silicon carbide composite ceramic is characterized by comprising the following steps of:
s1, taking silicon carbide powder as a raw material, pickling the silicon carbide powder, and then cleaning the silicon carbide powder to be neutral by using clear water to obtain a silicon carbide powder raw material;
s2, uniformly mixing the silicon carbide powder raw material obtained in the step S1 with a curing agent to obtain a silicon carbide-curing agent mixture;
and S3, performing 3D printing on the silicon carbide-curing agent mixture obtained in the step S2 to obtain a silicon carbide ceramic material biscuit.
2. The method of manufacturing according to claim 1, further comprising the steps of:
s4, degreasing the silicon carbide ceramic material biscuit obtained in the step S3 at a high temperature to obtain a degreased silicon carbide ceramic biscuit;
s5, densifying the degreased silicon carbide ceramic biscuit obtained in the step S4 to obtain a densified silicon carbide composite ceramic biscuit;
s6, performing high-temperature sintering or siliconizing sintering on the densified silicon carbide composite ceramic biscuit obtained in the step S5 to obtain the high-strength silicon carbide composite ceramic.
3. The method according to claim 1, wherein in step S1, the silicon carbide powder has a particle size of 1 to 600 μm, preferably 10 to 300 μm, more preferably 100to 150 μm.
4. The method according to claim 1, wherein in the step S2, the curing agent is: one or more of dilute sulfuric acid, hydrochloric acid, phosphoric acid, boric acid, oxalic acid, maleic anhydride, citric acid, malic acid, p-toluenesulfonic acid, benzenesulfonic acid or phenolsulfonic acid, preferably p-toluenesulfonic acid, benzenesulfonic acid or phenolsulfonic acid, more preferably p-toluenesulfonic acid.
5. The preparation method according to claim 1, wherein in the step S3, the specific operation steps are selecting a proper binder, setting printing parameters, performing 3D printing according to a CAD design structure, simultaneously pumping air from the layed powder during the printing process, and vibrating at a low frequency to obtain a biscuit of silicon carbide ceramic material;
preferably, the binder comprises one or more of phenolic resin, furan resin, polyvinyl alcohol (PVA), polyvinyl butyral (PVB), polymethyl methacrylate (PMMA), or epoxy resin.
6. The method according to claim 2, characterized in that in step S4, the degreasing temperature is not higher than 1200 ℃, preferably 900-1100 ℃; degreasing time is 12-48 h.
7. The method according to claim 2, wherein in the step S5, the densification process includes: a precursor polymer solution impregnation treatment and/or a precursor polymer chemical vapor infiltration treatment.
8. The method of claim 7, wherein the precursor polymer solution impregnation process comprises: placing the degreased silicon carbide ceramic biscuit sample into the precursor polymer solution for dipping, crosslinking and curing; converting the precursor polymer to a cracked carbon or SiC ceramic via pyrolysis; and repeating the dipping-curing-cracking process to obtain the ceramic sample after densification treatment.
9. The method of claim 8, wherein the precursor Polymer solution is a high carbon residue carbon precursor solution or a high Si residue ceramic precursor PDCs (Polymer-derived ceramics) solution; the carbon precursor with high carbon residue content can be one or more of phenolic resin, pitch resin, sucrose and furan resin; the precursor PDCs of the Gao Can Si-based ceramic are one or more of polycarbosilane, polysiloxane and polysilazane.
10. The method according to claim 7, wherein the 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 and silicon-based gases are converted into carbon or silicon-based ceramic and deposited in the porous degreasing biscuit to obtain a biscuit sample after carburization or silicon-based ceramic treatment.
11. The silicon carbide composite ceramic prepared by the preparation method according to any one of claims 1 to 10.
12. The silicon carbide composite ceramic according to claim 11, having a relative density of 90 to 99%; silicon content 0-55 vol%; density of 2.72-3.15 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The three-point bending strength is 200-500 MPa; the elastic modulus is 200-460 GPa; fracture toughness of 2.0-4.0 MPam 1/2 The method comprises the steps of carrying out a first treatment on the surface of the The heat conductivity is 40-200W/m.K; the thermal expansion coefficient (RT-400 ℃) is 2.0 to 4.0X10 -6 。
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