CN113004044A - SiC added with graphenefPreparation method of/SiC composite material - Google Patents
SiC added with graphenefPreparation method of/SiC composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 65
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 45
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000012700 ceramic precursor Substances 0.000 claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 229910052786 argon Inorganic materials 0.000 claims abstract description 12
- 239000000835 fiber Substances 0.000 claims abstract description 10
- 230000008021 deposition Effects 0.000 claims abstract description 8
- 239000002296 pyrolytic carbon Substances 0.000 claims abstract description 8
- 238000005470 impregnation Methods 0.000 claims abstract description 7
- 238000011049 filling Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000280 densification Methods 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims abstract description 3
- 238000007711 solidification Methods 0.000 claims abstract description 3
- 230000008023 solidification Effects 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229920003257 polycarbosilane Polymers 0.000 claims description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 8
- 238000007598 dipping method Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 2
- 238000000527 sonication Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 239000002243 precursor Substances 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C04B35/571—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 obtained from Si-containing polymer precursors or organosilicon monomers
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Abstract
The invention belongs to SiCfThe technical field of preparation of/SiC composite materials, in particular to SiC added with graphenefA preparation method of a/SiC composite material. Mixing the graphene solution and the silicon carbide ceramic precursor, mechanically stirring, and ultrasonically dispersing to obtain a graphene-containing ceramic precursor solution; putting the silicon carbide fiber prefabricated member into a deposition furnace for pyrolytic carbon interface layer deposition, and introducing Ar and C3H6Obtaining a silicon carbide fiber prefabricated part with a pyrolytic carbon interface layer; immersing the prefabricated member with the interface layer into a graphene-containing ceramic precursor solution, and putting the prefabricated member into a pressure impregnation furnace; vacuumizing, and filling argon for impregnation; discharging graphene-containing ceramicsIntroducing argon after the precursor solution is heated and insulated, and then cooling to room temperature along with the furnace to finish solidification; vacuumizing the pressure in the furnace, heating and preserving heat, continuing heating and preserving heat, and cooling along with the furnace; taking out the prefabricated part, and finishing densification treatment to obtain SiC with graphene reinforcementfa/SiC composite material. The invention improves the mechanical property and the thermal conductivity of the material.
Description
Technical Field
The invention belongs to SiCfThe technical field of preparation of/SiC composite materials, in particular to SiC added with graphenefA preparation method of a/SiC composite material.
Background
The SiCf/SiC composite material combines the advantages of high-performance SiC fibers and SiC matrixes, has the characteristics of high strength, low density, high temperature resistance, low chemical activity and the like, is a very promising high-temperature structural material, and has very wide application prospects in the fields of national defense, aerospace, energy sources and the like. However, the SiCf/SiC composite material also has problems such as brittle matrix and poor thermal conductivity. Conventional SiCf/SiC composites must therefore be optimized.
Graphene is a two-dimensional carbon nanomaterial consisting of carbon atoms in sp2 hybridized orbitals forming a hexagonal honeycomb lattice. Besides the honeycomb-type layered structure in which the sigma bonds are linked with other carbon atoms to form hexagonal rings, the PZ orbitals of each carbon atom perpendicular to the plane of the layer can form large pi bonds of multiple atoms throughout the entire layer, with excellent thermal conductivity. Graphene is one of the highest known materials, while also being very tough and bendable. Therefore, the graphene is added into the SiCf/SiC composite material, so that the density and toughness of the SiC matrix can be improved, and the strength and thermal conductivity of the SiCf/SiC composite material are improved.
At present, the main mode of adding graphene into ceramic is a mechanical addition method, but the graphene added in the mode has high dispersion difficulty and is easy to agglomerate, the uniformity of the obtained material is poor, and certain difficulty exists in improving the overall performance of the material.
Disclosure of Invention
The invention aims to provide SiC added with graphenefAccording to the preparation method of the/SiC composite material, the graphene is prepared into the silicon carbide ceramic precursor solution, and then the graphene reinforced SiCf/SiC composite material is obtained through a precursor impregnation cracking process, so that the problem that the graphene is difficult to disperse in a fiber prefabricated part can be effectively solved, and the mechanical property and the thermal conductivity of the material are improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
SiC added with graphenefA preparation method of a/SiC composite material,
the method comprises the following steps: preparing raw materials: the graphene, polyvinylpyrrolidone, ethanol and silicon carbide ceramic precursor is liquid polycarbosilane or polycarbosilane solution prepared by polycarbosilane and xylene solvent;
step two: preparing a dispersion solution by using polyvinylpyrrolidone and ethanol, adding graphene into the dispersion solution, mechanically stirring, and then ultrasonically stirring to obtain a graphene solution;
step three: mixing a graphene solution and a silicon carbide ceramic precursor in a volume ratio of 1: 2, mechanically stirring and then ultrasonically dispersing to obtain a ceramic precursor solution containing graphene;
step four: putting the silicon carbide fiber prefabricated member into a deposition furnace for pyrolytic carbon interface layer deposition, and introducing Ar and C3H6Cooling the mixed gas to room temperature along with the furnace to obtain a silicon carbide fiber prefabricated part with a pyrolytic carbon interface layer;
step five: dipping the prefabricated part with the interface layer in the fourth step into a ceramic precursor solution containing graphene, and putting the prefabricated part into a pressure dipping furnace; vacuumizing, and filling argon for impregnation; after discharging the ceramic precursor solution containing graphene, introducing argon, heating and preserving heat, cooling to room temperature along with the furnace, and finishing solidification;
step six: vacuumizing the pressure in the furnace, heating and preserving heat, continuing heating and preserving heat, and cooling along with the furnace;
step seven: taking out the prefabricated part, repeating the fifth step and the sixth step for 4-7 times to complete densification treatment to obtain SiC with graphene reinforcementfa/SiC composite material.
The second step is that: the polyvinylpyrrolidone concentration was 10 mg/ml.
The second step is that: after 10 minutes by mechanical stirring, stirring was carried out again for 1 hour by sonication.
The third step is that: after mechanical stirring for 1 hour, ultrasonic dispersion was carried out for 2 hours.
The fourth step is that: heating to 1100 deg.C at 10 deg.C/min, introducing Ar and C3H6The flow ratio of the mixed gas is 1: 5, keeping the furnace pressure at 1000Pa, and keeping the temperature for 5 hours.
The fifth step is as follows: and (3) after vacuumizing to less than 1Pa, filling argon until the pressure is 2-4 MPa and the temperature is 80-120 ℃, and dipping for 1 hour.
The fifth step is as follows: after the ceramic precursor solution containing graphene is discharged, argon pressure is introduced into the solution at a pressure of 1 x 105And Pa, heating to 160-220 ℃, keeping the temperature for 1 hour, and cooling to room temperature along with the furnace to finish curing.
The sixth step is as follows: vacuumizing the pressure in the furnace<10-1And Pa, heating to 500 ℃, keeping the temperature for 30min at the heating rate of 5 ℃/min, continuously heating to 1100 ℃, keeping the temperature for 1 hour at the heating rate of 10 ℃/min, and cooling along with the furnace.
The beneficial effects obtained by the invention are as follows:
the invention discloses graphene reinforced SiCfThe preparation method of the/SiC composite material mainly comprises the steps of preparing graphene dispersion liquid to obtain graphene-containing solution, mixing the solution and silicon carbide ceramic precursor solution to obtain graphene-containing ceramic precursor solution, and performing multiple cycles through a precursor impregnation cracking process to obtain graphene-reinforced SiCfa/SiC composite material. The invention effectively solves the problems that the graphene is difficult to be added into the SiC composite material and is not uniformly dispersed, and the added graphene improves the mechanical property and the heat-conducting property of the composite material.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The invention relates to SiC added with graphenefThe preparation method of the/SiC composite material comprises the following steps:
the method comprises the following steps: preparing raw materials: the graphene, polyvinylpyrrolidone, ethanol and silicon carbide ceramic precursor is liquid polycarbosilane or polycarbosilane solution prepared by polycarbosilane and xylene solvent.
Step two: preparing a dispersion solution by using polyvinylpyrrolidone and ethanol, wherein the concentration of the polyvinylpyrrolidone is 10mg/ml, adding graphene into the dispersion solution, mechanically stirring for 10 minutes, and then ultrasonically stirring for 1 hour to obtain a graphene solution.
Step three: mixing a graphene solution and a silicon carbide ceramic precursor in a volume ratio of 1: 2, mechanically stirring for 1 hour, and then ultrasonically dispersing for 2 hours to obtain the ceramic precursor solution containing graphene.
Step four: putting the silicon carbide fiber prefabricated member into a deposition furnace for pyrolytic carbon interface layer deposition, raising the temperature to 1100 ℃ at the rate of 10 ℃/min, and introducing Ar and C3H6The flow ratio of the mixed gas is 1: and 5, keeping the furnace pressure at 1000Pa for 5 hours, and cooling to room temperature along with the furnace to obtain the silicon carbide fiber prefabricated part with the pyrolytic carbon interface layer.
Step five: and (4) immersing the prefabricated member with the interface layer in the fourth step into a graphene-containing ceramic precursor solution, and putting the prefabricated member into a pressure impregnation furnace. Vacuum pumping<And (3) after 1Pa, filling argon to the pressure of 2-4 MPa and the temperature of 80-120 ℃, and dipping for 1 hour. After the ceramic precursor solution containing graphene is discharged, argon pressure is introduced into the solution at a pressure of 1 x 105And Pa, heating to 160-220 ℃, keeping the temperature for 1 hour, and cooling to room temperature along with the furnace to finish curing.
Step six: vacuumizing the pressure in the furnace<10-1And Pa, heating to 500 ℃, keeping the temperature for 30min at the heating rate of 5 ℃/min, continuously heating to 1100 ℃, keeping the temperature for 1 hour at the heating rate of 10 ℃/min, and cooling along with the furnace.
Step seven: taking out the prefabricated part, repeating the fifth step and the sixth step for 4-7 times to complete densification treatment to obtain SiC with graphene reinforcementfa/SiC composite material.
Claims (8)
1. SiC added with graphenefThe preparation method of the/SiC composite material is characterized by comprising the following steps:
the method comprises the following steps: preparing raw materials: the graphene, polyvinylpyrrolidone, ethanol and silicon carbide ceramic precursor is liquid polycarbosilane or polycarbosilane solution prepared by polycarbosilane and xylene solvent;
step two: preparing a dispersion solution by using polyvinylpyrrolidone and ethanol, adding graphene into the dispersion solution, mechanically stirring, and then ultrasonically stirring to obtain a graphene solution;
step three: mixing a graphene solution and a silicon carbide ceramic precursor in a volume ratio of 1: 2, mechanically stirring and then ultrasonically dispersing to obtain a ceramic precursor solution containing graphene;
step four: putting the silicon carbide fiber prefabricated member into a deposition furnace for pyrolytic carbon interface layer deposition, and introducing Ar and C3H6Cooling the mixed gas to room temperature along with the furnace to obtain a silicon carbide fiber prefabricated part with a pyrolytic carbon interface layer;
step five: dipping the prefabricated part with the interface layer in the fourth step into a ceramic precursor solution containing graphene, and putting the prefabricated part into a pressure dipping furnace; vacuumizing, and filling argon for impregnation; after discharging the ceramic precursor solution containing graphene, introducing argon, heating and preserving heat, cooling to room temperature along with the furnace, and finishing solidification;
step six: vacuumizing the pressure in the furnace, heating and preserving heat, continuing heating and preserving heat, and cooling along with the furnace;
step seven: taking out the prefabricated part, repeating the fifth step and the sixth step for 4-7 times to complete densification treatment to obtain SiC with graphene reinforcementfa/SiC composite material.
2. The graphene-added SiC according to claim 1fThe preparation method of the/SiC composite material is characterized by comprising the following steps: the second step is that: the polyvinylpyrrolidone concentration was 10 mg/ml.
3. The graphene-added SiC according to claim 1fThe preparation method of the/SiC composite material is characterized by comprising the following steps: the second step is that: after 10 minutes by mechanical stirring, stirring was carried out again for 1 hour by sonication.
4. The graphene-added SiC according to claim 1fThe preparation method of the/SiC composite material is characterized by comprising the following steps: the third step is that: mechanical stirrerAfter stirring for 1 hour, ultrasonic dispersion is carried out for 2 hours.
5. The graphene-added SiC according to claim 1fThe preparation method of the/SiC composite material is characterized by comprising the following steps: the fourth step is that: heating to 1100 deg.C at 10 deg.C/min, introducing Ar and C3H6The flow ratio of the mixed gas is 1: 5, keeping the furnace pressure at 1000Pa, and keeping the temperature for 5 hours.
6. The graphene-added SiC according to claim 1fThe preparation method of the/SiC composite material is characterized by comprising the following steps: the fifth step is as follows: vacuum pumping<And (3) after 1Pa, filling argon to the pressure of 2-4 MPa and the temperature of 80-120 ℃, and dipping for 1 hour.
7. The graphene-added SiC according to claim 1fThe preparation method of the/SiC composite material is characterized by comprising the following steps: the fifth step is as follows: after the ceramic precursor solution containing graphene is discharged, argon pressure is introduced into the solution at a pressure of 1 x 105And Pa, heating to 160-220 ℃, keeping the temperature for 1 hour, and cooling to room temperature along with the furnace to finish curing.
8. The graphene-added SiC according to claim 1fThe preparation method of the/SiC composite material is characterized by comprising the following steps: the sixth step is as follows: vacuumizing the pressure in the furnace<10-1And Pa, heating to 500 ℃, keeping the temperature for 30min at the heating rate of 5 ℃/min, continuously heating to 1100 ℃, keeping the temperature for 1 hour at the heating rate of 10 ℃/min, and cooling along with the furnace.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114874020A (en) * | 2022-05-13 | 2022-08-09 | 厦门大学 | Carbon fiber reinforced silicon carbide ceramic matrix porous composite material and preparation method thereof |
| CN115611648A (en) * | 2022-07-25 | 2023-01-17 | 中南大学 | Preparation method of high-strength graphene modified SiCf/SiC composite material |
| CN115744908A (en) * | 2022-10-21 | 2023-03-07 | 北京航空航天大学 | Preparation method of ultrathin silicon carbide nanosheet |
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