CN112552063A - Preparation method of carbon fiber reinforced silicon carbide composite material - Google Patents
Preparation method of carbon fiber reinforced silicon carbide composite material Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 130
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 70
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 238000011282 treatment Methods 0.000 claims abstract description 72
- 239000000203 mixture Substances 0.000 claims abstract description 56
- 239000000835 fiber Substances 0.000 claims abstract description 48
- 239000002002 slurry Substances 0.000 claims abstract description 42
- 238000001723 curing Methods 0.000 claims abstract description 40
- 238000010438 heat treatment Methods 0.000 claims abstract description 38
- 235000015895 biscuits Nutrition 0.000 claims abstract description 36
- 238000002425 crystallisation Methods 0.000 claims abstract description 34
- 230000008025 crystallization Effects 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 239000004744 fabric Substances 0.000 claims abstract description 22
- 238000003825 pressing Methods 0.000 claims abstract description 15
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- 238000003754 machining Methods 0.000 claims abstract description 13
- 208000037998 chronic venous disease Diseases 0.000 claims abstract 6
- 238000007723 die pressing method Methods 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 51
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 30
- 239000002243 precursor Substances 0.000 claims description 28
- 239000011347 resin Substances 0.000 claims description 28
- 229920005989 resin Polymers 0.000 claims description 28
- 229910052799 carbon Inorganic materials 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000005229 chemical vapour deposition Methods 0.000 claims description 24
- 239000003795 chemical substances by application Substances 0.000 claims description 23
- 238000005245 sintering Methods 0.000 claims description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 21
- 238000000151 deposition Methods 0.000 claims description 21
- 230000008021 deposition Effects 0.000 claims description 20
- 239000003995 emulsifying agent Substances 0.000 claims description 18
- 230000002787 reinforcement Effects 0.000 claims description 18
- 239000011863 silicon-based powder Substances 0.000 claims description 18
- 239000000725 suspension Substances 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 239000000919 ceramic Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 238000007599 discharging Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000013461 design Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 8
- 239000003085 diluting agent Substances 0.000 claims description 6
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical group CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 6
- 229920003257 polycarbosilane Polymers 0.000 claims description 6
- 239000001294 propane Substances 0.000 claims description 5
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 5
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 26
- 239000010410 layer Substances 0.000 description 22
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 239000011812 mixed powder Substances 0.000 description 9
- 238000003892 spreading Methods 0.000 description 9
- 238000005452 bending Methods 0.000 description 8
- 230000008595 infiltration Effects 0.000 description 5
- 238000001764 infiltration Methods 0.000 description 5
- 238000002679 ablation Methods 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000011153 ceramic matrix composite Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
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- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002296 pyrolytic carbon Substances 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000002490 spark plasma sintering Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 239000012153 distilled water Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
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- 238000007676 flexural strength test Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- NCWQJOGVLLNWEO-UHFFFAOYSA-N methylsilicon Chemical compound [Si]C NCWQJOGVLLNWEO-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
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- C—CHEMISTRY; METALLURGY
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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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
- C04B2235/5248—Carbon, e.g. graphite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/614—Gas infiltration of green bodies or pre-forms
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
A preparation method of a carbon fiber reinforced silicon carbide composite material comprises the following steps: (1) CVD treatment: carrying out CVD treatment on the carbon fiber filaments; (2) cutting into short fibers: cutting the carbon fiber filaments subjected to the CVD treatment into short fibers; (3) mixing short fibers with silicon carbide slurry: mechanically stirring the short fibers and the silicon carbide slurry uniformly to obtain a mixture; (4) die pressing and curing: flatly paving the carbon fiber mesh cloth and the mixture in a mold until the thickness reaches a designed thickness, pressurizing and pressing into a biscuit body; heating the mould to solidify the biscuit; (5) machining; (6) crystallization treatment: placing the biscuit body in a high-temperature furnace for crystallization treatment; and (5) obtaining the carbon fiber reinforced silicon carbide composite material product after the crystallization treatment is finished. The preparation method provided by the invention has the characteristics of short preparation period, environment-friendly preparation process, isotropic product performance, easiness in processing and the like, and is suitable for large-scale production.
Description
Technical Field
The invention relates to a preparation method of a ceramic matrix composite, in particular to carbon fiber reinforced silicon carbide (C)fA preparation method of the/SiC) composite material.
Background
Carbon fiber reinforced silicon carbide (C)fthe/SiC) composite material has the excellent performances of low density, small thermal expansion coefficient, high temperature resistance, corrosion resistance and the like, has more excellent high temperature resistance and oxidation resistance than a carbon/carbon (C/C) composite material, and has wide application in the fields of aerospace, energy, machinery, chemical industry and the like. The most common and technically mature preparation method of the carbon fiber reinforced silicon carbide composite material mainly comprises the following steps: firstly, useThe displacement in volume (PIP) method, the Chemical Vapor Infiltration (CVI) method, the reactive solution infiltration (RMI) method.
The precursor conversion process (PIP) suffers from the following disadvantages: (1) in the process of ceramic precursor, gas escapes all the time, so that the composite material has higher porosity; (2) the volume shrinkage in the precursor ceramic process can cause a large amount of micro-cracks, internal stress and other defects, (3) the manufacturing process needs to go through a repeated 'dipping cracking' process; thereby causing the performance of the material to be reduced, the production period to be long and the production cost to be high.
Chemical Vapor Infiltration (CVI) suffers from the following disadvantages: (1) the prepared composite material product has a density gradient, wherein the density of the surface layer is higher than that of the inner part; (2) a large amount of corrosive byproducts are released in the deposition process, so that the environment is seriously polluted; (3) the manufacturing period is long (more than 100 h), the production cost is high, and the manufacturing process is dangerous.
The reaction solution infiltration (RMI) method suffers from the following disadvantages: (1) in the infiltration process, liquid silicon reacts with carbon fibers to cause the performance of the material to be reduced; (2) the silicon-rich property of the composite material seriously leads to poor high-temperature performance.
CN 201610611979.5 discloses a method for rapidly preparing a C/SiC composite material, which comprises the steps of acid cleaning, impurity removal, SiC modification, SiC slurry preparation and slip casting sintering. According to the method, pure SiC is used as a ceramic source, high-solid-phase SiC slurry can smoothly enter the interior of the three-dimensional carbon fiber through modified SiC, and then the C/SiC composite material is prepared through high-temperature sintering at 2200-2400 ℃, no elemental silicon and other organic matters are introduced in the preparation process, the preparation period is short, and the cost is low. But the product has large porosity and poor performance.
CN 201610470960.3 discloses a method for rapidly preparing a C/SiC ceramic composite material by introducing a matrix in advance, which creatively provides a method for mould pressing and introducing the matrix in advance by improving a braided body structure, greatly shortens the period for preparing the C/SiC ceramic composite material by a PIP process, and achieves the purpose of reducing the preparation cost. The method comprises the steps of processing a braided body, pretreating the braided body, impregnating a precursor, curing, molding, pyrolyzing at high temperature, repeating the steps of impregnating, curing and pyrolyzing, and stopping impregnating and pyrolyzing when the weight gain is less than 1% of the original weight to finish the preparation of the material. The method reduces the time of subsequent polycarbosilane PIP impregnation, cracking and densification by adding SiC matrix powder in the preparation process of the preform, shortens the period of preparing the C/SiC ceramic composite material by the process, and achieves the aim of reducing the preparation cost. Wherein the maximum bending high strength can reach 325MPa, and the maximum tensile strength can reach 180 MPa. However, in this method, the SiC powder is large in dust when introduced, and easily leaks from the fiber body, and the amount of powder introduced is limited; PIP impregnation times are multiple, particularly, the subsequent densification speed is very slow, and the problems of long preparation period and high preparation cost of the C/SiC ceramic matrix composite are not fundamentally solved.
CN 201510377418.9 discloses a rapid preparation method of a C/SiC composite material, which comprises the following steps: 1. depositing a pyrolytic carbon (PyC) interface on the surface of the thin-layer carbon fiber preform by adopting a chemical vapor deposition process; 2. impregnating a thin-layer carbon fiber preform deposited with a PyC interface with a polycarbosilane mixed solution, and then sequentially crosslinking, curing and cracking under a protective atmosphere to obtain a thin-layer C/SiC composite material; 3. repeating the previous step for 2-3 times; 4. and (3) placing a plurality of single-layer composite materials in a graphite mould in a laminated manner for spark plasma sintering, and finally quickly preparing the compact C/SiC composite material. The method fully utilizes the characteristics of short time for dipping the thin layer by the PIP method and rapid sintering by the SPS method, thereby realizing the preparation of the C/SiC composite material, but the method is only suitable for the compaction of small components and is difficult to manufacture large complex parts.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art, and provides the carbon fiber reinforced silicon carbide (C) with the performances of short manufacturing period, environment-friendly manufacturing process, isotropic material performance and the likefA preparation method of the/SiC) composite material.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a carbon fiber reinforced silicon carbide composite material comprises the following steps:
(1) CVD treatment: loading the carbon fiber filaments into a chemical vapor deposition furnace for CVD (chemical vapor deposition) treatment;
(2) cutting into short fibers: cutting the carbon fiber filaments treated in the step (1) into short fibers of 6-20 mm;
(3) mixing short fibers with silicon carbide slurry: mixing the short fibers treated in the step (2) with the silicon carbide slurry, and mechanically stirring uniformly to obtain a mixture of the short fibers and the silicon carbide slurry;
(4) and (3) mould pressing and curing treatment: flatly paving the carbon fiber mesh cloth and the mixture obtained in the step (3) in a mould, applying pressure to the mould after flatly paving the carbon fiber mesh cloth and the mixture to a designed thickness according to a mode of one layer of carbon fiber mesh cloth and one layer of mixture, and pressing the carbon fiber mesh cloth and the mixture to a biscuit body; heating the mould to solidify the biscuit body in the mould to obtain a solidified biscuit body;
(5) and (3) machining treatment: machining the biscuit body obtained in the step (4) according to a design size to obtain a biscuit body meeting the design size requirement;
(6) crystallization treatment: placing the biscuit body obtained in the step (5) in a high-temperature furnace for crystallization treatment; and (5) obtaining the carbon fiber reinforced silicon carbide composite material product after the crystallization treatment is finished.
Further, in the step (1), the CVD treatment process includes: one of methane, propane and propylene is used as a carbon source gas, nitrogen is used as a diluent gas, and the flow ratio of the carbon source gas to the nitrogen is 1 (1-8); and controlling the air pressure in the furnace to be 1-5 KPa during deposition, controlling the deposition temperature to be 970-1150 ℃ and controlling the deposition time to be 5-20 h.
Further, in the step (2), the length of the short fiber is at least one of 6mm, 9mm, 15mm and 20 mm.
Further, in the step (3), the components of the silicon carbide slurry comprise silicon carbide precursor resin and a curing agent thereof, a reinforcement, a suspension emulsifier and a sintering aid; the weight ratio of the silicon carbide precursor resin to the curing agent is 50-100 parts, the reinforcement is 100-200 parts, the suspension emulsifier is 1-10 parts, and the sintering aid is 1-10 parts; and (3) mechanically stirring and blending all the components of the silicon carbide slurry for 1-3 hours to achieve full stirring and uniform dispersion.
Further, in the step (3), the silicon carbide precursor resin is at least one of polycarbosilane, polymethylsilane and methylsilicone resin, and the curing agent is vinyltriethoxysilane (A151); the weight ratio of the curing agent to the silicon carbide precursor resin ranges from 1 per mill to 5 per mill; the reinforcement is at least one of 2000-mesh silicon carbide powder, 1500-mesh silicon carbide powder, 800-mesh silicon carbide powder, 200nm silicon carbide powder, 150nm silicon carbide powder and 100nm silicon carbide powder; the suspension emulsifier is at least one of 200nm white carbon black, 100nm white carbon black, 200nm silicon powder and 100nm silicon powder; the sintering aid is at least one of 2000-mesh silicon powder, 1000-mesh silicon powder, 800-mesh silicon powder and 2000-mesh graphite powder.
Further, in the step (3), the weight ratio of the short fibers to the silicon carbide slurry is 1 (3-5); the mechanical stirring time is 3-5 h.
Further, in the step (4), the pressure of the pressed green body is 5-10 MPa.
Further, in the step (4), the curing process comprises: heating the mixture from room temperature to 80-100 ℃, and keeping the temperature for 6-8 h; then heating to 145-155 ℃ (preferably 150 ℃), and keeping the temperature for 2-4 h; then heating to 215-225 ℃ (preferably 220 ℃), and preserving heat for 2-4 h; cooling to below 60 ℃ along with the furnace, and discharging.
Further, in the step (6), the crystallization treatment process is as follows: under the protection of inert atmosphere, heating to 850-910 ℃ (900 ℃ is preferred) at the speed of 5-10 ℃/min, carrying out ceramic treatment, and preserving heat for 1-2 h at 850-910 ℃ (900 ℃ is preferred); heating to 1600-1650 ℃ at the speed of 1.5-2.5 ℃/min (preferably 2 ℃/min) for crystallization treatment, and keeping the temperature at 1600-1650 ℃ for 1-2 h; then cooling the mixture with the furnace to below 200 ℃ and discharging the mixture.
Further, in the step (6), the density of the carbon fiber reinforced silicon carbide composite material product is 1.75-2.0 g/cm3。
Further, in the step (6), the inert atmosphere is an argon atmosphere or a nitrogen atmosphere.
According to the invention, the carbon fiber wire is subjected to CVD carbon deposition treatment, so that a thin carbon deposition interface protective coating (about 50-100 mu m) is obtained on the surface of the carbon fiber wire, and the coating can prevent later introductionThe interface bonding between the silicon carbide and the carbon fiber wire is too strong, so that the strength of the carbon fiber is greatly reduced, and the mechanical property of a final product is further ensured. The cut short fibers are uniformly dispersed in the SiC slurry, the SiC slurry is used as a binder of the short fibers and a source of SiC ceramic, the bonding strength between the short fibers and silicon carbide is improved, and the short fibers are randomly dispersed in all directions in the mixing process, so that the orientation of the fibers in the layering process tends to be balanced, the final performance of the material tends to be isotropic, the strength and the rigidity of the material are kept unchanged no matter the loading direction of the material, and the difficulty of post-processing is greatly reduced. Finally, a series of sintering treatments such as curing and shaping, ceramic treatment, SiC crystallization and the like are carried out to obtain the product with the density of 1.75-2.0 g/cm3Carbon fiber reinforced silicon carbide (C)fThe introduction of SiC ceramic crystal grains greatly improves the mechanical property and the oxidation resistance of the product.
The carbon fiber reinforced silicon carbide (C) prepared by the method of the inventionfThe manufacturing period of the/SiC) composite material product is about 15 days, the bending strength of the product reaches 30-40 MPa, and is several times higher than that of a graphite material (the bending strength of common graphite is 6-20 MPa).
Compared with the prior art, the invention has the following beneficial effects:
carbon fiber reinforced silicon carbide (C) prepared by the method of the inventionfthe/SiC) composite material product has the excellent characteristics of easy processing, short manufacturing period, high mechanical property, isotropic material property and the like, and is suitable for the large-scale production of the ceramic matrix composite material.
Detailed Description
The present invention will be described in further detail with reference to examples.
The starting materials used in the examples were obtained by conventional commercial means.
The detection method of the product performance of each embodiment is as follows:
the porosity is detected by adopting a soaking medium method: the radius r and the height h of the sample (from which the total volume of the sample can be calculated) are first measured with a vernier caliper, the weight m1 of the dried sample in air is weighed out and then saturated by immersion in distilled water, i.e. the medium is filled up to the pores of the porous material by the heat bubbling method. After the sample is fully saturated in a certain period of time, taking out the sample, slightly wiping off the medium on the surface of the sample, weighing the total mass m2 of the sample in the air at the moment by using an electronic scale, and calculating the porosity of the porous material by using the following formula.
Θ＝[(m2-m1)/ρWater (W)]/π·r2·h。
The bending strength is detected by a three-point bending method: the flexural strength test was performed on a universal material testing machine. The test bar used for the test is 3X 4X 35 mm. The span was 30mm and the loading rate was 0.5mm/min as measured by three-point bending. Each data was tested on 5 bars and then averaged.
The thermal conductivity is detected by a thermal flowmeter method: the instrument is used to add a stable hot surface temperature to one surface of the sample, the heat is transferred to the cold surface (room temperature) through the sample, and the heat transfer is measured to calculate the thermal conductivity.
Oxidation resistance: and (3) placing the sample in a tube furnace, opening a tube cover, heating to 1000 ℃, preserving heat for 10 hours, and testing the weight loss rate of the sample.
Example 1
The preparation method of the carbon fiber reinforced silicon carbide composite material comprises the following steps:
(1) CVD treatment: putting the carbon fiber filaments into a chemical vapor deposition furnace for CVD treatment; the CVD treatment process comprises the following steps: taking methane as a carbon source gas and nitrogen as a diluent gas, wherein the flow ratio of the methane to the nitrogen is 1:1, and the flow of the methane is 10L/min; and during deposition, controlling the air pressure in the furnace to be 5KPa, the deposition temperature to be 1150 ℃ and the deposition time to be 5 h.
(2) Cutting into short fibers: cutting the carbon fiber filaments treated in the step (1) into short fibers with the length of 20 mm;
(3) mixing short fibers with silicon carbide slurry: mixing the short fibers obtained in the step (2) with the silicon carbide slurry, wherein the weight ratio of the short fibers to the silicon carbide slurry is 1:3, mechanically stirring for 5 hours, and uniformly mixing to obtain a mixture of the short fibers and the silicon carbide slurry; the components of the silicon carbide slurry comprise silicon carbide precursor resin and a curing agent thereof, a reinforcement body, a suspension emulsifier and a sintering aid; the weight ratio is that, silicon carbide precursor resin and curing agent 50 shares, reinforcement 200 shares, suspension emulsifier 10 shares, sintering auxiliary agent 10 shares; mixing the components of the silicon carbide slurry, mechanically stirring for 1 hour, and uniformly mixing; the silicon carbide precursor resin is polycarbosilane, and the curing agent is vinyl triethoxysilane (A151); the weight ratio of the curing agent to the silicon carbide precursor resin is 5 per mill; the reinforcement is mixed powder of 2000-mesh silicon carbide powder, 1500-mesh silicon carbide powder and 800-mesh silicon carbide powder (the weight ratio of the three is 5:3: 2); the suspension emulsifier is mixed powder of 200nm white carbon black and 100nm silicon powder (the weight ratio is 1: 1); the sintering aid is mixed powder of 2000-mesh silicon powder and 2000-mesh graphite powder (the weight ratio is 1: 1);
(4) and (3) mould pressing and curing treatment: flatly paving the carbon fiber mesh cloth and the mixture obtained in the step (3) in a mould, flatly paving the carbon fiber mesh cloth and the mixture to a designed thickness in a mode of one layer of carbon fiber mesh cloth and one layer of mixture, wherein the flatly paving thickness of each layer of carbon fiber mesh cloth and one layer of mixture is about 5mm, applying certain pressure to the mould, and pressing the mixture into a biscuit body; heating the mould to solidify the biscuit in the mould; the green compact was pressed to a pressure of 5 Mpa. The curing process comprises the following steps: heating the mixture from room temperature to 80 ℃, and keeping the temperature for 8 hours; then heating to 150 ℃, and preserving heat for 3 hours; then heating to 220 ℃, and preserving heat for 3 hours; cooling to 60 ℃ along with the furnace, discharging, and demolding to obtain a solidified biscuit body;
(5) and (3) machining treatment: machining the biscuit body processed in the step (4) according to the design size to obtain a solidified biscuit body conforming to the design size;
(6) crystallization treatment: placing the biscuit body obtained in the step (5) in a high-temperature furnace for crystallization treatment; after the crystallization treatment is finished, the carbon fiber reinforced silicon carbide (C) is obtainedf/SiC) composite products. The crystallization treatment process comprises the following steps: under the protection of argon atmosphere, heating to 900 ℃ at the speed of 10 ℃/min for ceramic treatment, and preserving heat at 900 ℃ for 2 h; then heating to 1650 ℃ at the speed of 2 ℃/min for crystallization treatment, and preserving heat at 1650 ℃ for 1 h; then cooling along with the furnaceCooling to below 200 ℃ and discharging. The carbon fiber-reinforced silicon carbide (C)f/SiC) composite product having a density of 1.85g/cm3. The preparation period of the product of this example was 15 days.
The detection shows that the performance of the obtained product is as follows: porosity: 10.5 percent; bending strength: 35.25 MPa; thermal conductivity: 89W (m.K); ablation rate in an aerobic environment at 1000 ℃ (10 h): 5.25 wt%.
Example 2
This example carbon fiber reinforced silicon carbide (C)fThe preparation method of the/SiC) composite material comprises the following steps:
(1) CVD treatment: putting the carbon fiber filaments into a chemical vapor deposition furnace for CVD treatment; the CVD treatment process comprises the following steps: propane is used as a carbon source gas, nitrogen is used as a diluent gas, the flow ratio of propane to nitrogen is 1:6, and the flow of propane is 3L/min; controlling the air pressure in the furnace to be 3KPa during deposition, the deposition temperature to be 970 ℃, and the deposition time to be 10 h;
(2) cutting into short fibers: cutting the carbon fiber filaments treated in the step (1) into short fibers of 6 mm;
(3) mixing short fibers with silicon carbide slurry: and (3) mixing the short fibers treated in the step (2) with the silicon carbide slurry, wherein the weight ratio of the short fibers to the silicon carbide slurry is 1:5, mechanically stirring for 3 hours, and uniformly mixing to obtain a mixture of the short fibers and the silicon carbide slurry. The components of the silicon carbide slurry comprise silicon carbide precursor resin and a curing agent thereof, a reinforcement body, a suspension emulsifier and a sintering aid; the weight ratio of the silicon carbide precursor resin to the curing agent is 100 parts, the reinforcement is 100 parts, the suspending emulsifier is 1 part, and the sintering aid is 1 part; and (3) mechanically stirring and blending all the components of the silicon carbide slurry for 3 hours to achieve full stirring and uniform dispersion. The silicon carbide precursor resin is a mixture of polymethyl silane and methyl silicon resin (the weight ratio is 1:1), and the curing agent is vinyl triethoxysilane (A151); the weight ratio of the curing agent to the silicon carbide precursor resin ranges from 1 per mill; the reinforcement is mixed powder of 200nm silicon carbide powder, 150nm silicon carbide powder and 100nm silicon carbide powder (the weight ratio is 2:3: 5); the suspension emulsifier is mixed powder of 100nm white carbon black and 200nm silicon powder (the weight ratio is 1: 1); the sintering aid is mixed powder of 1000-mesh silicon powder and 800-mesh silicon powder (the weight ratio is 1: 1).
(4) And (3) mould pressing and curing treatment: spreading the carbon fiber mesh cloth and the mixture processed in the step (3) in a mold, spreading the mixture to a designed thickness in a manner of one layer of carbon fiber mesh cloth and one layer of mixture, spreading the mixture to a thickness of about 5mm in a manner of one layer of carbon fiber mesh cloth and one layer of mixture, applying a certain pressure to the mold, and pressing the mixture into a biscuit body; heating the mould to cure the biscuit body in the mould; the green compact was pressed to a pressure of 10 MPa. The curing treatment process comprises the following steps: heating the mixture from room temperature to 100 ℃, and keeping the temperature for 6 hours; then heating to 150 ℃, and preserving heat for 2 h; then heating to 220 ℃, and preserving the heat for 2 hours; cooling to 60 ℃ along with the furnace, discharging, and demolding to obtain a solidified biscuit body; .
(5) And (3) machining treatment: machining the biscuit body processed in the step (4) according to the design size;
(6) crystallization treatment: placing the biscuit processed in the step (5) in a high-temperature furnace for crystallization; after the crystallization treatment is finished, the carbon fiber reinforced silicon carbide (C) can be obtainedf/SiC) composite products. The crystallization treatment process comprises the following steps: under the protection of nitrogen atmosphere, heating to 900 ℃ at the speed of 5 ℃/min for ceramic treatment, and preserving heat at 900 ℃ for 1 h; then heating to 1600 ℃ at the speed of 2 ℃/min for crystallization treatment, and preserving heat at 1600 ℃ for 2 h; then cooling the mixture with the furnace to below 200 ℃ and discharging the mixture. The carbon fiber-reinforced silicon carbide (C)f/SiC) composite product having a density of 1.75g/cm3. The preparation period of the product of this example was 15 days.
The properties of the finished product obtained are: porosity: 15.3 percent; bending strength: 30.95 MPa; thermal conductivity: 65W (m.K); ablation rate in an aerobic environment at 1000 ℃ (10 h): 10.65 wt%.
Example 3
This example carbon fiber reinforced silicon carbide (C)fThe preparation method of the/SiC) composite material comprises the following steps:
(1) CVD treatment: putting the carbon fiber filaments into a chemical vapor deposition furnace for CVD treatment; the CVD treatment process comprises the following steps: taking propylene as a carbon source gas and nitrogen as a diluent gas, wherein the flow ratio of the propylene to the nitrogen is 1:8, and the flow of the propylene is 5L/min; during deposition, the air pressure in the furnace is controlled to be 1KPa, the deposition temperature is 1020 ℃, and the deposition time is 20 h;
(2) cutting into short fibers: cutting the carbon fiber filaments treated in the step (1) into short fibers of 15 mm;
(3) mixing short fibers with silicon carbide slurry: and (3) mixing the short fibers treated in the step (2) with the silicon carbide slurry, wherein the weight ratio of the short fibers to the silicon carbide slurry is 1:4, mechanically stirring for 4 hours, and uniformly mixing to obtain a mixture of the short fibers and the silicon carbide slurry. The components of the silicon carbide slurry comprise silicon carbide precursor resin and a curing agent thereof, a reinforcement body, a suspension emulsifier and a sintering aid; the weight proportion of the silicon carbide precursor resin is 75 parts of silicon carbide precursor resin and curing agent thereof, 150 parts of reinforcement, 5 parts of suspension emulsifier and 5 parts of sintering aid; and (3) blending the components of the silicon carbide slurry for 2 hours under mechanical stirring to achieve full stirring and uniform dispersion. The silicon carbide precursor resin is polymethyl silane, and the curing agent is vinyl triethoxysilane (A151); the weight ratio range of the curing agent to the silicon carbide precursor resin is 3 per mill; the reinforcement is 200nm silicon carbide powder; the suspension emulsifier is 100nm white carbon black; the sintering aid is 1000-mesh silicon powder.
(4) And (3) mould pressing and curing treatment: spreading the carbon fiber mesh cloth and the mixture processed in the step (3) in a mold, spreading the mixture to a designed thickness in a manner of one layer of carbon fiber mesh cloth and one layer of mixture, spreading the mixture to a thickness of about 5mm in a manner of one layer of carbon fiber mesh cloth and one layer of mixture, applying a certain pressure to the mold, and pressing the mixture into a biscuit body; heating the mould to cure the biscuit body in the mould; the pressure of the green compact was 8 MPa. The curing treatment process comprises the following steps: heating the mixture from room temperature to 90 ℃, and preserving the heat for 7 hours; then heating to 150 ℃, and preserving heat for 4 hours; then heating to 220 ℃, and preserving the heat for 4 hours; cooling to 60 ℃ along with the furnace, discharging, and demolding to obtain a solidified biscuit body;
(5) and (3) machining treatment: machining the biscuit body processed in the step (4) according to the design size;
(6) crystallization treatment: placing the biscuit processed in the step (5) in a high-temperature furnace for crystallization; after the crystallization treatment is finished, the carbon fiber reinforced silicon carbide (C) can be obtainedf/SiC) composite products. The crystallization treatment process comprises the following steps: under the protection of argon atmosphere, heating to 900 ℃ at the speed of 8 ℃/min for ceramic treatment, and preserving heat at 900 ℃ for 1.5 h; then heating to 1630 ℃ at the speed of 2 ℃/min for crystallization treatment, and preserving heat at 1630 ℃ for 1.5 h; then cooling the mixture with the furnace to below 200 ℃ and discharging the mixture. The carbon fiber-reinforced silicon carbide (C)f/SiC) composite product having a density of 2.0g/cm3. The preparation period of the product of this example was 15 days.
The properties of the finished product obtained are: porosity: 4.2 percent; bending strength: 38.23 MPa; thermal conductivity: 102W (m.K); ablation rate in an aerobic environment at 1000 ℃ (10 h): 0.83 wt%.
Example 4
The preparation method of the carbon fiber reinforced silicon carbide (Cf/SiC) composite material comprises the following steps:
(1) CVD treatment: putting the carbon fiber filaments into a chemical vapor deposition furnace for CVD treatment; the CVD treatment process comprises the following steps: taking methane as a carbon source gas and nitrogen as a diluent gas, wherein the flow ratio of the methane to the nitrogen is 1:2, and the flow of the methane is 15L/min; and during deposition, controlling the air pressure in the furnace to be 4KPa, the deposition temperature to be 1100 ℃, and the deposition time to be 12 h.
(2) Cutting into short fibers: cutting the carbon fiber filaments treated in the step (1) into 9mm short fibers;
(3) mixing short fibers with silicon carbide slurry: and (3) mixing the short fibers treated in the step (2) with the silicon carbide slurry, wherein the weight ratio of the short fibers to the silicon carbide slurry is 1:3, mechanically stirring for 4 hours, and uniformly mixing to obtain a mixture of the short fibers and the silicon carbide slurry. The components of the silicon carbide slurry comprise silicon carbide precursor resin and a curing agent thereof, a reinforcement body, a suspension emulsifier and a sintering aid; the weight proportion of the silicon carbide precursor resin is 80 parts of silicon carbide precursor resin and curing agent thereof, 120 parts of reinforcement, 8 parts of suspension emulsifier and 8 parts of sintering aid; and (3) blending the components of the silicon carbide slurry for 2 hours under mechanical stirring to achieve full stirring and uniform dispersion. The silicon carbide precursor resin is polycarbosilane (molecular weight is 1500), and the curing agent is vinyl triethoxysilane (A151); the weight ratio of the curing agent to the silicon carbide precursor resin ranges from 4 per mill; the reinforcement is mixed powder of 2000-mesh silicon carbide powder and 800-mesh silicon carbide powder (the weight ratio is 1: 1); the suspension emulsifier is mixed powder of 100nm white carbon black and 100nm silicon powder (the weight ratio is 2: 1); the sintering aid is mixed powder of 2000-mesh silicon powder and 2000-mesh graphite powder (the weight ratio is 1: 2);
(4) and (3) mould pressing and curing treatment: spreading the carbon fiber mesh cloth and the mixture processed in the step (3) in a mold, spreading the mixture to a designed thickness in a manner of one layer of carbon fiber mesh cloth and one layer of mixture, spreading the mixture to a thickness of about 5mm in a manner of one layer of carbon fiber mesh cloth and one layer of mixture, applying a certain pressure to the mold, and pressing the mixture into a biscuit body; heating the mould to cure the biscuit body in the mould; the green compact was pressed to a pressure of 8 Mpa. The curing treatment process comprises the following steps: heating the mixture from room temperature to 90 ℃, and keeping the temperature for 6 hours; then heating to 150 ℃, and preserving heat for 4 hours; then heating to 220 ℃, and preserving the heat for 4 hours; cooling to 60 ℃ along with the furnace, discharging, and demolding to obtain a solidified biscuit body;
(5) and (3) machining treatment: machining the biscuit body processed in the step (4) according to the design size;
(6) crystallization treatment: placing the biscuit processed in the step (5) in a high-temperature furnace for crystallization; after the crystallization treatment is finished, the carbon fiber reinforced silicon carbide (C) can be obtainedf/SiC) composite products. The crystallization treatment process comprises the following steps: under the protection of argon atmosphere, heating to 900 ℃ at the speed of 6 ℃/min for ceramic treatment, and preserving heat at 900 ℃ for 2 h; then heating to 1640 ℃ at the speed of 2 ℃/min for crystallization treatment, and keeping the temperature at 1640 ℃ for 2 h; then cooling the mixture with the furnace to below 200 ℃ and discharging the mixture. The carbon fiber-reinforced silicon carbide (C)f/SiC) composite product having a density of 1.9g/cm3. The preparation period of the product of this example was 15 days.
The properties of the finished product obtained are: porosity: 8.2 percent; bending strength: 36.86 MPa; thermal conductivity: 92W (m.K); ablation rate in an aerobic environment at 1000 ℃ (10 h): 1.96 wt%.
The parts are all parts by weight.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all modifications, variations and equivalents of the above described embodiment, which are made according to the technical spirit of the present invention, are still within the scope of the claims of the present patent application.
Claims (10)
1. The preparation method of the carbon fiber reinforced silicon carbide composite material is characterized by comprising the following steps of:
(1) CVD treatment: putting the carbon fiber filaments into a chemical vapor deposition furnace for CVD treatment;
(2) cutting into short fibers: cutting the carbon fiber filaments processed in the step (1) into short fibers with the length of 6-20 mm;
(3) mixing short fibers with silicon carbide slurry: mixing the short fibers cut in the step (2) with silicon carbide slurry, and mechanically stirring uniformly to obtain a mixture of the short fibers and the silicon carbide slurry;
(4) die pressing and curing: flatly paving the carbon fiber mesh cloth and the mixture obtained in the step (3) in a mould, applying pressure to the mould after flatly paving the carbon fiber mesh cloth and the mixture to a designed thickness according to a mode of one layer of carbon fiber mesh cloth and one layer of mixture, and pressing the carbon fiber mesh cloth and the mixture to a biscuit body; heating the mould to solidify the biscuit body in the mould to obtain a solidified biscuit body;
(5) and (3) machining: machining the biscuit body obtained in the step (4) according to a design size to obtain a biscuit body meeting the design size requirement;
(6) crystallization treatment: placing the biscuit body obtained in the step (5) in a high-temperature furnace for crystallization treatment; and (5) obtaining the carbon fiber reinforced silicon carbide composite material product after the crystallization treatment is finished.
2. The method for producing a carbon fiber-reinforced silicon carbide composite material according to claim 1, wherein in the step (1), the CVD treatment is performed by: taking one of methane, propane and propylene as a carbon source gas, taking nitrogen as a diluent gas, wherein the flow ratio of the carbon source gas to the nitrogen is 1 (1-8); and controlling the air pressure in the furnace to be 1-5 KPa during deposition, controlling the deposition temperature to be 970-1150 ℃ and controlling the deposition time to be 5-20 h.
3. The method for producing a carbon fiber-reinforced silicon carbide composite material according to claim 1 or 2, wherein in the step (2), the length of the short fiber is at least one of 6mm, 9mm, 15mm, and 20 mm.
4. The method for preparing a carbon fiber-reinforced silicon carbide composite material according to any one of claims 1 to 3, wherein in the step (3), the silicon carbide slurry comprises a silicon carbide precursor resin and a curing agent thereof, a reinforcement, a suspending emulsifier and a sintering aid; the weight proportion is that the silicon carbide precursor resin and the curing agent thereof are 50 to 100 weight portions, the reinforcement is 100 weight portions, the suspension emulsifier is 1 to 10 weight portions, and the sintering auxiliary agent is 1 to 10 weight portions; and mixing the components of the silicon carbide slurry, mechanically stirring for 1-6 hours, and uniformly mixing.
5. The method for preparing a carbon fiber-reinforced silicon carbide composite material according to claim 4, wherein in the step (3), the silicon carbide precursor resin is at least one of polycarbosilane, polymethylsilane and methylsilicone resin, and the curing agent is vinyltriethoxysilane;
the reinforcement is at least one of 2000-mesh silicon carbide powder, 1500-mesh silicon carbide powder, 800-mesh silicon carbide powder, 200nm silicon carbide powder, 150nm silicon carbide powder and 100nm silicon carbide powder;
the suspension emulsifier is at least one of 200nm white carbon black, 100nm white carbon black, 200nm silicon powder and 100nm silicon powder;
the sintering aid is at least one of 2000-mesh silicon powder, 1000-mesh silicon powder, 800-mesh silicon powder and 2000-mesh graphite powder.
6. The method for preparing the carbon fiber reinforced silicon carbide composite material according to any one of claims 1 to 5, wherein in the step (3), the weight ratio of the short fibers to the silicon carbide slurry is 1 (3-5); the mechanical stirring time is preferably 3-5 h.
7. The method for preparing a carbon fiber-reinforced silicon carbide composite material according to any one of claims 1 to 6, wherein in the step (4), the pressure of the green compact is 5 to 10 MPa.
8. The method for producing a carbon fiber-reinforced silicon carbide composite material according to any one of claims 1 to 7, wherein in the step (4), the curing is performed by: heating the mixture from room temperature to 80-100 ℃, and keeping the temperature for 6-8 h; then heating to 145-155 ℃, and preserving heat for 2-4 h; then heating to 215-225 ℃, and preserving heat for 2-4 h; cooling to below 60 ℃ along with the furnace, and discharging.
9. The preparation method of the carbon fiber reinforced silicon carbide composite material according to any one of claims 1 to 8, wherein in the step (6), the crystallization process comprises: under the protection of inert atmosphere, heating to 850-910 ℃ at the speed of 5-10 ℃/min, carrying out ceramic treatment, and keeping the temperature at 850-910 ℃ for 1-2 h; then heating to 1600-1650 ℃ at the speed of 1.5-2.5 ℃/min for crystallization treatment, and preserving heat at 1600-1650 ℃ for 1-2 h; then cooling the mixture with the furnace to below 200 ℃ and discharging the mixture.
10. The method for producing a carbon fiber-reinforced silicon carbide composite material according to any one of claims 1 to 9, wherein in the step (6), the density of the carbon fiber-reinforced silicon carbide composite material product is 1.75 to 2.0g/cm3。
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| CN114773066A (en) * | 2022-05-19 | 2022-07-22 | 醴陵市凯德特种陶瓷有限公司 | Manufacturing method of toughened silicon carbide ceramic kiln furniture flat plate |
| CN114907144A (en) * | 2022-06-06 | 2022-08-16 | 吉林联科特种石墨材料有限公司 | Method for preparing SiC-C composite high-temperature coating by one-step method |
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| CN117125995A (en) * | 2023-09-13 | 2023-11-28 | 浙江星辉新材料科技有限公司 | Soft carbon fiber ceramic brake pad and preparation method thereof |
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