CN112552065B - Fiber-reinforced ceramic matrix composite bolt and preparation method thereof - Google Patents
Fiber-reinforced ceramic matrix composite bolt and preparation method thereof Download PDFInfo
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- CN112552065B CN112552065B CN202110108175.4A CN202110108175A CN112552065B CN 112552065 B CN112552065 B CN 112552065B CN 202110108175 A CN202110108175 A CN 202110108175A CN 112552065 B CN112552065 B CN 112552065B
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- 239000011159 matrix material Substances 0.000 title claims abstract description 59
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000011226 reinforced ceramic Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000005336 cracking Methods 0.000 claims abstract description 86
- 239000000835 fiber Substances 0.000 claims abstract description 81
- 238000000151 deposition Methods 0.000 claims abstract description 64
- 239000011248 coating agent Substances 0.000 claims abstract description 25
- 238000000576 coating method Methods 0.000 claims abstract description 25
- 238000001723 curing Methods 0.000 claims abstract description 25
- 238000005516 engineering process Methods 0.000 claims abstract description 15
- 238000007598 dipping method Methods 0.000 claims abstract description 14
- 238000013461 design Methods 0.000 claims abstract description 13
- 238000000197 pyrolysis Methods 0.000 claims abstract description 11
- 238000003754 machining Methods 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims description 61
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 52
- 230000008021 deposition Effects 0.000 claims description 49
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 48
- 239000012700 ceramic precursor Substances 0.000 claims description 46
- 238000005470 impregnation Methods 0.000 claims description 42
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 38
- 239000002002 slurry Substances 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 34
- 238000001816 cooling Methods 0.000 claims description 26
- 239000002243 precursor Substances 0.000 claims description 25
- 229910052786 argon Inorganic materials 0.000 claims description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- 238000012545 processing Methods 0.000 claims description 22
- 239000002121 nanofiber Substances 0.000 claims description 21
- 239000000919 ceramic Substances 0.000 claims description 20
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 20
- 239000005052 trichlorosilane Substances 0.000 claims description 20
- 238000005229 chemical vapour deposition Methods 0.000 claims description 19
- 239000012159 carrier gas Substances 0.000 claims description 18
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 17
- 239000004917 carbon fiber Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 14
- 239000002296 pyrolytic carbon Substances 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- 238000000498 ball milling Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- 230000008595 infiltration Effects 0.000 claims description 10
- 238000001764 infiltration Methods 0.000 claims description 10
- 239000010703 silicon Substances 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 238000007865 diluting Methods 0.000 claims description 9
- 239000003085 diluting agent Substances 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 9
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000012300 argon atmosphere Substances 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 238000010907 mechanical stirring Methods 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- -1 polycarbosilazane Polymers 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000280 densification Methods 0.000 claims description 4
- 238000009434 installation Methods 0.000 claims description 4
- 239000001294 propane Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 3
- 229910021392 nanocarbon Inorganic materials 0.000 claims description 3
- 229920003257 polycarbosilane Polymers 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 239000003345 natural gas Substances 0.000 claims description 2
- 229920001709 polysilazane Polymers 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 9
- 230000035939 shock Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 45
- 239000010410 layer Substances 0.000 description 11
- 238000001035 drying Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000011153 ceramic matrix composite Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 239000011215 ultra-high-temperature ceramic Substances 0.000 description 3
- 238000009941 weaving Methods 0.000 description 3
- 239000011184 SiC–SiC matrix composite Substances 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229920002943 EPDM rubber Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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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
-
- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
- C04B41/5059—Silicon carbide
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
- F16B35/00—Screw-bolts; Stay-bolts; Screw-threaded studs; Screws; Set screws
- F16B35/04—Screw-bolts; Stay-bolts; Screw-threaded studs; Screws; Set screws with specially-shaped head or shaft in order to fix the bolt on or in an object
- F16B35/041—Specially-shaped shafts
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
- F16B35/00—Screw-bolts; Stay-bolts; Screw-threaded studs; Screws; Set screws
- F16B35/04—Screw-bolts; Stay-bolts; Screw-threaded studs; Screws; Set screws with specially-shaped head or shaft in order to fix the bolt on or in an object
- F16B35/06—Specially-shaped heads
-
- 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
- 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
- C04B2235/5244—Silicon carbide
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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
- 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
Abstract
The invention relates to a fiber reinforced ceramic matrix composite bolt and a preparation method thereof, wherein (1) a fiber preform is processed according to a design size; (2) preparing an interface layer; (3) repeating the dipping-curing-cracking for 2-4 times; (4) Machining grooves of the head part and the head part of the bolt and external threads of the screw according to the designed size; (5) connecting the screw rod with the head groove in a threaded manner; (6) repeating the steps of dipping, curing and low-temperature cracking for 2-4 times; then repeating the dipping, curing and pyrolysis for 1-2 times; (7) densifying the SiC matrix by adopting a CVI technology; and (8) depositing the SiC coating on the surface of the product by adopting a CVD technology. The invention can produce large-size bolts, and the produced bolts have compact core parts, high core part strength and good mechanical strength and thermal shock resistance.
Description
Technical Field
The invention belongs to the technical field of fasteners, and particularly relates to a fiber reinforced ceramic matrix composite bolt and a preparation method thereof.
Background
The continuous fiber reinforced ceramic matrix composite as a structural member has the advantages of low density (about 1/4 of steel), high specific strength, high specific modulus, high fracture toughness, high temperature resistance, low thermal expansion coefficient, thermal shock resistance, strong structural designability and the like, can be applied to the harsh environment of aerospace, can be used for a long time at about 1650 ℃, and can reach 2000 ℃ in a short time.
At present, ceramic matrix composite materials are used for preparing connecting members such as studs, pins, bolts and the like, but the types of connecting pieces are still few, and the prior art can only prepare small-size connecting pieces. With the development of science and technology, the application environment of the connecting component is more and more complex and harsh, and the requirements on the connecting component gradually tend to be larger in size range, higher in strength, more uniform in performance and excellent in comprehensive performance.
The invention patent CN106565261A discloses a method for preparing a SiC/SiC composite material pin by precursor impregnation and cracking. The method includes weaving a pin fiber preform by a 1K SiC fiber bundle, depositing a PyC/SiC composite interface layer on the preform through a chemical vapor deposition method, then carrying out immersion-solidification-cracking steps on the preform by using a liquid phase SiC precursor to prepare a SiC matrix, and repeating the steps for 7-8 times to complete the preparation of the SiC/SiC composite material pin. The pin prepared by the method has high shearing strength, high connection fastening strength and small strength dispersion, and can realize net size forming. But the prefabricated body of the method is formed by weaving, the diameter of the prepared pin is only 3mm-4mm, and the diameter size range is smaller.
The invention patent CN107021770B discloses a preparation method of a high-temperature-resistant ceramic matrix composite screw. The method comprises the steps of preparing a prefabricated body by adopting fiber non-woven fabric and mesh tire continuous needling forming, 2.5D weaving forming or fiber cloth laminated integral puncturing, depositing pyrolytic carbon in the fiber prefabricated body, processing a semi-finished prefabricated body into continuous screws, depositing a SiC matrix through a chemical vapor deposition process, performing finish machining to a size, introducing ultrahigh-temperature ceramics through multiple dipping-cracking of the ultrahigh-temperature ceramic precursor, processing the continuous screws into single screws, depositing a SiC coating on the surfaces of the screws, and finally processing threads by adopting a diamond cutter to obtain screw products. The method introduces ultrahigh-temperature ceramic, improves the temperature resistance of the screw to 2000 ℃, improves the mechanical property and the oxidation resistance of the ceramic matrix composite screw, combines the preparation method and the processing of the screw, and has the advantages of complete screw teeth, high precision and high yield. But the method is applied to CVD-SiC substrates andPIP (Poly-ethylene-propylene-diene monomer) prepared ultrahigh-temperature substrate with density of 1.9g/cm 3 The SiC coating is deposited on the surface through CVD, then threads are machined on the screw, and due to the fact that the hardness of the material is high and is second to that of diamond, abrasion of a diamond cutter is increased, cost is improved, threads are prone to cracking, and product reject ratio is improved. The diameter of the screw product prepared by the method is only 4-15mm, and the method is not suitable for preparing the connecting piece with larger diameter size.
The prior preparation technology has limited infiltration depth for the large-size connecting piece, and the surface layer is easy to form closed pores, so that the porosity of the core part of the product is large, the density is uneven, and the strength of the core part is low, thus the preparation requirement of the large-size connecting piece can not be met.
Disclosure of Invention
Aiming at the problems that the core part of the large-size connecting piece is difficult to compact, the core part has low strength and the mechanical strength and the thermal shock resistance are poor, the invention provides the fiber reinforced ceramic matrix composite bolt to solve the problems in the prior art.
The invention also provides a preparation method of the fiber reinforced ceramic matrix composite bolt.
In order to achieve the purpose, the invention adopts the following technical scheme:
a fiber reinforced ceramic matrix composite bolt is composed of a head and a screw, wherein the head is provided with a groove, the groove is provided with an internal thread, the screw is provided with an external thread, the head is in threaded connection with the screw, and the length of the screw is larger than the depth of the groove of the head; and a ceramic matrix is filled in a thread gap between the head and the screw rod.
The invention provides a preparation method of the fiber reinforced ceramic matrix composite bolt, which comprises the following steps:
(1) Preparing a prefabricated body: preparing continuous carbon fibers or silicon carbide fibers into a head fiber preform and a screw fiber preform which are consistent with the designed size and shape and have allowance in size;
(2) Preparing an interface layer: fixing the fiber preform obtained in the step (1) by adopting a mold, and depositing a pyrolytic carbon interface layer by CVI;
(3) Dipping-curing-cracking: fixing the preform body obtained in the step (2) by using a mould, and repeating the steps of dipping, curing and cracking for 2-4 times; the cracking comprises low-temperature cracking and/or high-temperature cracking, wherein the cracking temperature of the low-temperature cracking is 950-1300 ℃, the cracking temperature of the high-temperature cracking is 1300-1500 ℃, and the obtained density is 1.45-1.55g/cm 3 The head and the screw of (a);
(4) And (3) machining: processing a groove on the head obtained in the step (3) according to a design size, processing an internal thread in the groove, processing an external thread on the screw rod according to the design size, wherein the external thread is in threaded fit with the internal thread of the groove on the head;
(5) Installation: connecting the external thread of the screw with the internal thread of the head groove in a threaded manner, and fixing by adopting a mold to ensure that the head is coaxially matched with the screw;
(6) Repeating dipping-curing-cracking: repeatedly dipping, curing and cracking at low temperature for 2-4 times, and then repeatedly dipping, curing and cracking at high temperature for 1-2 times, wherein the low temperature cracking is the low temperature cracking with the cracking temperature of 950-1300 ℃; the high-temperature cracking is high-temperature cracking at the cracking temperature of 1300-1500 ℃;
(7) Preparing a densified SiC matrix by CVI: in order to improve the matching strength of the head and the screw rod and the strength of the head and the screw rod, the product obtained in the step (6) is used for preparing a SiC matrix by adopting a CVI technology, and tiny pores at the matching part of the threads are sealed and filled;
(8) CVD deposition of SiC coating: and (4) coating the external threads of the second part extending out of the groove with carbon paper, then placing the second part into a chemical vapor deposition furnace, performing chemical vapor deposition on the surface of the product obtained in the step (7) to form a SiC coating, and then removing the carbon paper to obtain the fiber reinforced ceramic matrix composite screw.
Further, in the step (1), the fiber is carbon fiber or silicon carbide fiber; the fiber preform is prepared by molding 1-12K fibers by 2.5D needling and 2.5D puncturing, and the density of the fiber preform is 0.4-0.6g/cm 3 。
Further, the CVI deposited pyrolytic carbon interface layer in step (2) is specifically: fixing the fiber preform by using a graphite tool, introducing a carbon source gas at the flow rate of 5-15L/min, depositing a pyrolytic carbon interface layer on the surface of the fiber preform by adopting isothermal CVI (chemical vapor infiltration), and naturally cooling to room temperature in the atmosphere of argon or nitrogen; the carbon source gas is selected from any one or more of natural gas, methane, propane and propylene; the deposition temperature of the CVI is 800-1300 ℃, the deposition time is 1-60h, and the pressure in the furnace is 0.5-20kPa.
Further, the impregnation in the step (3) and the step (6) comprises vacuum impregnation and pressure impregnation;
the vacuum impregnation comprises the following steps: putting the product into a vacuum impregnation barrel, vacuumizing to below 200Pa, keeping the vacuum for 0.5-1h, injecting ceramic precursor slurry or ceramic precursor slurry containing nano ceramic powder, keeping the vacuum for 1-5h, breaking the vacuum and taking out;
the pressure impregnation comprises the following steps: putting the product into a pressure impregnation tank, slowly heating to 50-70 ℃ under the pressure of 1-6MPa in the pressure impregnation tank, preserving heat for 1-5h, cooling to room temperature along with a furnace, and taking out.
Further, the curing in the step (3) and the step (6) is: putting the product into a blast drying oven, heating to 120-250 ℃ at the heating rate of 5-10 ℃/min, keeping the temperature for 3-10h, naturally cooling to room temperature along with the furnace, and taking out.
Further, the cracking in the step (3) and the step (6) is: putting the product into a sintering furnace, heating to a cracking temperature at a heating rate of 5-10 ℃/min under a vacuum state below 200Pa or a micro-positive pressure state with the pressure in the furnace of 100-200kPa, preserving heat for 2-10h, and naturally cooling to room temperature under the atmosphere of argon or nitrogen. The purpose of cracking is to break down the ceramic precursor into ceramic.
Further, the ceramic precursor slurry is prepared by mechanically stirring and uniformly mixing a ceramic precursor and a solvent according to the mass ratio of 10 (3-8);
the ceramic precursor slurry containing the nano ceramic powder is prepared from a ceramic precursor, a solvent and the nano ceramic powder according to the weight ratio of 10: (3-8): (0.5-2) by mechanical stirring and mixing;
the ceramic precursor is one or more of polymethylsilane, polycarbosilane, polycarbosilazane, polysilazane, polysiloxane and polyborosilazane;
the solvent is one or more of divinylbenzene, xylene and toluene;
the nano ceramic powder is selected from any one or more of carbides, nitrides and borides of silicon, zirconium and other transition metal elements, such as: siC, zrC, B 4 C、HfC、TaC、WC、Si 3 N 4 、ZrN、BN、HfN、SiBCN、SiB 4 、ZrB 2 、HfB 2 And TaB 2 One or more of (a). The mechanical stirring is carried out in a water bath kettle at the temperature of 50-70 ℃, and the stirring is carried out for 1-10h at the rotating speed of 50-60 r/min.
Further, when the screw is installed in the step (5), firstly ceramic precursor slurry containing nano-fibers is coated on the surface of the screw, then ceramic precursor slurry containing nano-fibers is coated on the surface of the internal thread of the head groove, and then the screw is in threaded connection with the internal thread of the head groove.
The ceramic precursor slurry containing the nano-fibers is prepared from a ceramic precursor, a solvent and the nano-fibers according to the weight ratio of 10: (6-12): the mass ratio of (1-3) is formed by ball milling and even mixing.
The nano-fiber is nano-carbon fiber, carbon nano-tube, nano-SiC fiber, nano-ZrC fiber. The ball milling time is 3-5h, and the ball milling speed is 300-400 r/min.
Further, the CVI preparation of the densified SiC matrix in the step (7) specifically comprises the following steps: the product is put into a chemical vapor infiltration furnace, trichlorosilane is taken as a precursor, hydrogen is taken as carrier gas and reducing gas, argon is taken as diluent gas, the deposition temperature is 850-1200 ℃, the deposition time is 5-100 h, the deposition pressure is 5-15 kPa, the molar ratio of the reducing gas to the trichlorosilane is (5-20): 1, the flow rate of the precursor is 1-15 g/min, the flow rate of the diluting gas is 5-20L/min, the flow rate of the reducing gas is determined by the molar ratio of the reducing gas to a silicon source, and the flow rate of the carrier gas is 100-200 mL/min.
Further, the CVD deposited SiC coating in step (8) is specifically: the product is placed in a chemical vapor deposition furnace, trichlorosilane is used as a precursor, hydrogen is used as carrier gas and reducing gas, argon is used as diluent gas, the deposition temperature of chemical vapor deposition is 950-1500 ℃, the deposition time is 5-80 h, the deposition pressure is 1-20 kPa, the molar ratio of the reducing gas to trichlorosilane is (8-20): 1, the flow rate of the precursor is 1-15 g/min, the flow rate of the diluting gas is 2-20L/min, the flow rate of the reducing gas is determined by the molar ratio of the reducing gas to a silicon source, and the flow rate of the carrier gas is 100-300 mL/min.
Compared with the prior art, the invention has the following beneficial effects:
(1) The bolt prepared by the invention comprises a head part and a screw rod, wherein the head part is provided with a groove, the groove is provided with an internal thread, the screw rod is provided with an external thread, the head part is connected with the screw rod through the thread, a ceramic matrix is filled at the joint part to improve the connection strength, and the length of the screw rod is greater than the depth of the groove of the head part. The prepared bolt can effectively reduce the height and thickness of integral preparation and molding, avoids the problems of incompact core part, low strength and the like of a product, has unlimited diameter and size of the product, can expand the application range of the ceramic matrix composite connecting piece, and promotes the development of aerospace industry.
(2) According to the invention, the two parts are prepared to be processed with threads when certain density so as to realize threaded connection, compared with the mode that the threads are not processed, the screw and the head are directly connected by filling the SiC matrix, the bonding strength of the screw and the head is better, the adhesive force of the SiC matrix on the surfaces of the screw and the head is higher, and the connection strength of the screw and the head is further improved.
(3) In the preparation process, after the screw is connected with the screw, the ceramic matrix is filled in a gap between the screw and the thread of the head part through the repeated impregnation-solidification-cracking step (6) and the SiC matrix densification step (7) of CVI preparation, and the head part and the screw are fixedly connected into a whole to form a structure with certain bonding strength and a connecting effect;
(4) According to the invention, before the screw is connected with the internal thread of the groove, the nano fiber is added into the ceramic precursor slurry to serve as a reinforcing phase, so that the binding force between SiC matrixes can be improved, and the connection strength between the screw and the head is improved;
(5) According to the invention, a densification process of preparing the SiC matrix by CVI is added after the impregnation-solidification-cracking process, the gas-phase ceramic precursor is convenient to permeate into micro pores, and the SiC matrix is cracked to fill the micro pores, so that the joint is more dense, and the connection strength between the screw and the head is further improved;
(6) The thread is processed when the density is relatively low, so that the situation that the thread is cracked and fallen in the preparation process can be effectively avoided, the finished product rate of the thread is ensured, and the product percent of pass is improved;
(7) The invention deposits a SiC coating on the surface of the product by chemical vapor deposition, thereby improving the oxidation resistance and the wear resistance of the component and prolonging the service life of the bolt.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below in conjunction with the implementation of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
A carbon fiber reinforced ceramic matrix composite bolt is composed of a head and a screw, wherein the head is provided with a groove, the groove is provided with an internal thread, the screw is provided with an external thread, the head is in threaded connection with the screw, and the length of the screw is larger than the depth of the groove of the head; a ceramic matrix is filled in a thread gap between the head and the screw rod; the depth of the groove of the head part is 30mm, the diameter of the head part is 30mm, and the length of the screw rod is 65mm; the diameter of the screw is 18mm.
The preparation method of the carbon fiber reinforced ceramic matrix composite bolt comprises the following steps:
(1) Preparing a prefabricated body: according to the component selection, a head fiber preform and a screw fiber preform are prepared in a 0/90 DEG 2.5D needling forming mode of a carbon fiber (12K) laid fabric-mesh tire, wherein the diameter of the head fiber preform is 32mm, height of 40mm, density of 0.5g/cm 3 (ii) a The screw rod fiber preform has a diameter of 20mm, a height of 68mm and a density of 0.5g/cm 3 。
(2) CVI deposition of a pyrolytic carbon interface layer: fixing the fiber preform obtained in the step (1) by using a graphite tool, then introducing methane gas at a gas flow of 10L/min, depositing a pyrolytic carbon interface layer on the surfaces of the head fiber preform and the screw fiber preform by adopting an isothermal CVI technology, wherein the deposition temperature is 1150 ℃, the deposition time is 30h, the pressure in a furnace is 10kPa, and then naturally cooling to room temperature in an argon or nitrogen atmosphere to obtain a preform body.
(3) Dipping-curing-cracking:
(3a) Vacuum impregnation: putting the preform blank obtained in the step (2) into a vacuum impregnation barrel, firstly vacuumizing for 1h, keeping the vacuum degree below 100Pa, injecting ceramic precursor slurry after keeping the vacuum for 1h, breaking the vacuum and taking out to obtain a preform containing the precursor slurry; the ceramic precursor slurry is prepared by uniformly mixing polycarbosilane and xylene according to the mass ratio of 10 to 5 through mechanical stirring, and stirring for 5 hours at the rotating speed of 50r/min in a water bath kettle at the temperature of 70 ℃ through mechanical stirring.
(3b) Pressure impregnation: and (4) putting the prefabricated body obtained in the step (3 a) into a pressure impregnation tank, slowly heating to 50 ℃ under the pressure of 1MPa in the impregnation tank, preserving heat for 2 hours, cooling to room temperature along with a furnace, and taking out.
(3c) And (3) curing: curing the preform obtained in step (3 b): putting into a blast drying oven, heating to 120 ℃ at a heating rate of 10 ℃/min, preserving heat for 10h, naturally cooling to room temperature along with the furnace, and taking out.
(3d) Low-temperature cracking: subjecting the preform obtained in step (3 c) to cryogenic cracking: putting the prefabricated body into a sintering furnace, heating the furnace to a low-temperature cracking temperature of 1000 ℃ at a heating rate of 10 ℃/min in a vacuum state of less than 200Pa, preserving heat for 2 hours, and then naturally cooling to room temperature in an argon or nitrogen atmosphere;
(3e) Pyrolysis: carrying out pyrolysis on the preform obtained in the step (3 d): putting the prefabricated body into a sintering furnace, heating the furnace to the high-temperature cracking temperature of 1400 ℃ at the heating rate of 10 ℃/min in a vacuum state below 200Pa, preserving the heat for 2 hours, and then naturally cooling the prefabricated body to the room temperature in the argon or nitrogen atmosphere;
(3f) Performing the steps (3 a) - (3 e) on the product obtained in the step (3 e), and repeating for 4 times;
(4) And (3) machining: and (4) processing a groove on the head product obtained in the step (3) according to a design size, processing an internal thread on the groove, processing an external thread on the screw rod according to the design size, and matching the external thread with the internal thread of the head groove in a threaded manner.
(5) Installation: and the external thread of the screw is in threaded connection with the internal thread of the head groove, and the head is ensured to be coaxially matched with the screw by adopting the die for fixation.
(6) Repeating the steps of dipping, curing and cracking: firstly, carrying out low-temperature cracking, namely, carrying out steps (3 a) - (3 d) on the product obtained in the step (5), and repeating for 2 times; then pyrolysis, i.e., continuing steps (3 a) - (3 c) and step (3 e), was repeated 2 times, and the density of the obtained product was 1.9g/cm 3 。
(7) Preparing a densified SiC matrix by CVI: in order to improve the matching strength of the screw and the head, preparing a SiC matrix from the product obtained in the step (6) by adopting a CVI (chemical vapor infiltration) technology, and sealing and filling micro pores at the matching part of the threads; the product is placed in a chemical vapor infiltration furnace, trichlorosilane is used as a precursor, hydrogen is used as carrier gas and reducing gas, argon is used as diluent gas, the deposition temperature is 850 ℃, the deposition time is 100 hours, the deposition pressure is 15kPa, the molar ratio of the reducing gas to trichlorosilane is 15.
(8) CVD deposition of SiC coating: ultrasonically cleaning and drying the product obtained in the step (7) by using ethanol, coating the external thread of the screw rod extending out of the groove by using carbon paper, then putting the product into a chemical vapor deposition furnace, taking silicon source trichlorosilane as a precursor, hydrogen as carrier gas and reducing gas, argon as diluent gas, depositing at 950 ℃ for 30h for deposition pressureThe force is 20kPa, the molar ratio of the reducing hydrogen to the trichlorosilane is 8, the flow rate of a precursor is 15g/min, the flow rate of a diluent gas is 20L/min, the flow rate of the reducing gas is determined by the molar ratio of the reducing gas to a silicon source, the flow rate of a carrier gas is 100mL/min, a SiC coating is prepared on the surface of a product through chemical vapor deposition, the oxidation resistance and the wear resistance of the component are improved, then carbon paper is removed to obtain the fiber reinforced ceramic matrix composite bolt, and the density of the obtained product is 1.99g/cm 3 。
Example 2
A carbon fiber reinforced ceramic matrix composite bolt is composed of a head and a screw, wherein the head is provided with a groove, the groove is provided with an internal thread, the screw is provided with an external thread, the head is in threaded connection with the screw, and the length of the screw is larger than the depth of the groove of the head; a ceramic matrix is filled in a thread gap between the head and the screw rod; the depth of the groove of the head part is 25mm, the diameter of the head part is 40mm, and the length of the screw rod is 70mm; the diameter of the screw is 24mm.
The preparation method of the carbon fiber reinforced ceramic matrix composite bolt comprises the following steps:
(1) Preparing a prefabricated body: selecting carbon fiber (12K) cloth laminated whole according to the components to be subjected to 2.5D puncture to prepare a head fiber preform and a screw fiber preform, wherein the diameter of the head fiber preform is 44mm, the height of the head fiber preform is 28mm, and the density of the head fiber preform is 0.45 g/cm 3 (ii) a The screw fiber preform has a diameter of 26mm, a height of 72mm and a density of 0.45 g/cm 3 。
(2) CVI deposition of a pyrolytic carbon interface layer: and (2) fixing the preform obtained in the step (1) by using a graphite tool, then introducing propane gas at a gas flow rate of 15L/min, and depositing a pyrolytic carbon interface layer on the surface of the preform by adopting an isothermal CVI technology, wherein the deposition temperature is 800 ℃, the deposition time is 60 hours, and the pressure in the furnace is 10kPa. And then naturally cooling to room temperature in the argon or nitrogen atmosphere to obtain a head fiber preform body and a screw fiber preform body.
(3) Cyclic impregnation-curing-cracking:
(3a) Vacuum impregnation: putting the preform blank obtained in the step (2) into a vacuum impregnation barrel, vacuumizing for 1h, keeping the vacuum degree below 200Pa, injecting ceramic precursor slurry after keeping the vacuum for 0.5h, keeping the vacuum for 5h, breaking the vacuum and taking out to obtain a preform containing the precursor slurry; the ceramic precursor slurry is prepared by uniformly mixing polymethyl silane and divinyl benzene according to the mass ratio of 10.
(3b) Pressure impregnation: and (4) putting the prefabricated body obtained in the step (3 a) into a pressure impregnation tank, slowly heating to 70 ℃ under the pressure of 6MPa in the impregnation tank, preserving heat for 1h, cooling to room temperature along with a furnace, and taking out.
(3c) And (3) curing: curing the preform obtained in step (3 b): putting into a blast drying oven, heating to 250 deg.C at a heating rate of 5 deg.C/min, maintaining for 3 hr, naturally cooling to room temperature, and taking out.
(3d) Low-temperature cracking: subjecting the preform obtained in step (3 c) to cryogenic cracking: putting the prefabricated body into a sintering furnace, heating to a low-temperature cracking temperature of 1000 ℃ at a heating rate of 5 ℃/min under a micro-positive pressure state with the pressure of 100kPa, preserving heat for 2h, and then naturally cooling to room temperature under the atmosphere of argon or nitrogen;
(3e) Vacuum impregnation: putting the blank prefabricated body obtained in the step (3 d) into a vacuum impregnation barrel, vacuumizing for 1h, keeping the vacuum degree below 200Pa, injecting ceramic precursor slurry after keeping the vacuum for 0.5h, keeping the vacuum for 5h, breaking the vacuum and taking out to obtain a prefabricated body containing the precursor slurry; the ceramic precursor is prepared by uniformly mixing polymethyl silane and divinyl benzene according to the mass ratio of 10.
(3f) Pressure impregnation: and (4) putting the prefabricated body obtained in the step (3 e) into a pressure impregnation tank, slowly heating to 70 ℃ under the pressure of 6MPa in the impregnation tank, preserving heat for 1h, cooling to room temperature along with a furnace, and taking out.
(3g) And (3) curing: curing the preform obtained in step (3 f): putting into a blast drying oven, heating to 250 ℃ at the heating rate of 5 ℃/min, preserving heat for 3h, naturally cooling to room temperature along with the furnace, and taking out.
(3h) High-temperature cracking: subjecting the preform obtained in step (3 g) to pyrolysis: placing the prefabricated body into a sintering furnace, heating to the high-temperature cracking temperature of 1400 ℃ at the heating rate of 10 ℃/min under the vacuum state of less than 200Pa in the furnace, preserving heat for 2 hours, and then naturally cooling to the room temperature under the argon or nitrogen atmosphere;
(3i) And (4) carrying out steps (3 a) - (3 h) on the product obtained in the step (3 h), and repeating for 3 times.
(4) And (3) machining: and (4) processing a groove on the head product obtained in the step (3) according to a design size, processing an internal thread on the groove, processing an external thread on the screw rod according to the design size, and matching the external thread with the internal thread of the head groove in a threaded manner.
(5) Installing a screw: firstly, smearing ceramic precursor slurry containing nano fibers on the surface of a screw, smearing the ceramic precursor slurry containing the nano fibers on the surface of the internal thread of the groove, and then connecting the screw with the internal thread of the groove in a threaded manner; the ceramic precursor slurry containing the nano-fibers is prepared from a ceramic precursor, a solvent and the nano-fibers according to the weight ratio of 10: 6:1 is prepared by ball milling and even mixing; the nano-fiber is nano-carbon fiber; the ball milling time is 3h, and the ball milling speed is 300 r/min.
(6) Repeating the steps of dipping, curing and cracking: firstly, carrying out low-temperature cracking, namely, carrying out steps (3 a) - (3 d) on the product obtained in the step (5), and repeating for 2 times; then pyrolysis, i.e. continuing steps (3 e) - (3 h), repeated 2 times.
(7) Preparing a densified SiC matrix by CVI: in order to improve the matching strength of the screw and the groove, the product obtained in the step (6) is used for preparing a SiC matrix by adopting a CVI (chemical vapor infiltration) technology, and tiny pores at the matching part of the threads are sealed; the product is placed in a chemical vapor infiltration furnace, trichlorosilane is used as a precursor, hydrogen is used as carrier gas and reducing gas, argon is used as diluent gas, the deposition temperature is 1100 ℃, the deposition time is 10 hours, the deposition pressure is 10kPa, the molar ratio of the reducing gas to the trichlorosilane is 10, the flow rate of the precursor is 12g/min, the flow rate of the diluting gas is 8L/min, the flow rate of the reducing gas is determined by the molar ratio of the reducing gas to a silicon source, and the carrier gas flow rate is 150mL/min.
(8) CVD deposition of SiC coating: ultrasonically cleaning and drying the product obtained in the step (7) by using ethanol, coating a screw rod extending out of a groove by using carbon paper, then putting the product into a chemical vapor deposition furnace, taking trichlorosilane as a precursor, hydrogen as a carrier gas and a reducing gas, argon as a diluting gas, wherein the deposition temperature of the chemical vapor deposition is 1500 ℃, the deposition time is 5h, the deposition pressure is 10kPa, the molar ratio of the reducing hydrogen to the trichlorosilane is 12, the flow rate of the precursor is 5g/min, the flow rate of the diluting gas is 8L/min, the flow rate of the reducing gas is determined by the molar ratio of the reducing gas to a silicon source, the flow rate of the carrier gas is 120mL/min, preparing a SiC coating on the surface of the product by chemical vapor deposition, improving the oxidation resistance and the wear resistance of the component, and then removing the carbon paper to obtain the fiber reinforced ceramic matrix composite bolt, wherein the density of the obtained product is 1.98g/cm 3 。
Example 3
A carbon fiber reinforced ceramic matrix composite bolt is composed of a head and a screw, wherein the head is provided with a groove, the groove is provided with an internal thread, the screw is provided with an external thread, the head is in threaded connection with the screw, and the length of the screw is larger than the depth of the groove of the head; a ceramic matrix is filled in a thread gap between the head and the screw rod; the depth of the groove of the head part is 20mm, the diameter of the head part is 30mm, and the length of the screw rod is 55mm; the diameter of the screw is 20mm.
The preparation method of the carbon fiber reinforced ceramic matrix composite bolt comprises the following steps:
(1) Preparing a prefabricated body: selecting a carbon fiber cloth laminated whole body according to components to be manufactured into a head fiber preform and a screw fiber preform by 2.5D puncture, wherein the diameter of the head fiber preform is 36mm, the height of the head fiber preform is 30mm, and the density of the head fiber preform is 0.55g/cm 3 (ii) a The screw rod fiber preform has a diameter of 25mm, a height of 60mm and a density of 0.5g/cm 3 。
(2) CVI deposition of a pyrolytic carbon interface layer: and (2) fixing the preform obtained in the step (1) by using a graphite tool, then introducing propane gas at a gas flow rate of 5L/min, and depositing a pyrolytic carbon interface layer on the surface of the preform by adopting an isothermal CVI technology, wherein the deposition temperature is 1300 ℃, the deposition time is 5 hours, and the pressure in the furnace is 5kPa. And then naturally cooling to room temperature in the argon or nitrogen atmosphere to obtain a preform body.
(3) Cyclic impregnation-curing-cracking:
(3a) Vacuum impregnation: putting the preform blank obtained in the step (2) into a vacuum impregnation barrel, vacuumizing for 1h, keeping the vacuum degree below 200Pa, injecting ceramic precursor slurry after keeping the vacuum for 0.8h, keeping the vacuum for 3h, breaking the vacuum and taking out to obtain a preform containing the precursor slurry; the ceramic precursor slurry is prepared from polycarbosilazane: the divinylbenzene is prepared by uniformly mixing the divinylbenzene by mechanical stirring according to the mass ratio of 10 to 8, and the divinylbenzene is stirred for 10 hours at the rotating speed of 60r/min in a water bath kettle at the temperature of 50 ℃.
(3b) Pressure impregnation: and (4) putting the prefabricated body obtained in the step (3 a) into a pressure impregnation tank, slowly heating to 70 ℃ under the pressure of 4MPa in the impregnation tank, preserving heat for 1h, cooling to room temperature along with a furnace, and taking out.
(3c) And (3) curing: curing the preform obtained in step (3 b): putting into a blast drying oven, heating to 250 ℃ at the heating rate of 5 ℃/min, preserving heat for 3h, naturally cooling to room temperature along with the furnace, and taking out.
(3d) Low-temperature cracking: subjecting the preform obtained in step (3 c) to cryogenic cracking: placing the prefabricated body into a sintering furnace, heating to a low-temperature cracking temperature of 950 ℃ at a heating rate of 5 ℃/min under a micro-positive pressure state of 100kPa, preserving heat for 2 hours, and then naturally cooling to room temperature under the atmosphere of argon or nitrogen;
(3e) Repeating the steps (3 a) - (3 d) for 3 times on the product obtained in the step (3 d);
(3f) Vacuum impregnation: putting the prefabricated body obtained in the step (3 e) into a vacuum impregnation barrel, vacuumizing for 1h, keeping the vacuum degree below 200Pa, keeping the vacuum for 0.5h, injecting ceramic precursor slurry containing the nano ceramic powder, keeping the vacuum for 5h, breaking the vacuum and taking out to obtain the prefabricated body of the ceramic precursor containing the nano ceramic powder; the ceramic precursor slurry containing the nano ceramic powder is prepared from polymethyl silane, dimethylbenzene and silicon carbide according to the weight ratio of 10:5:2, and stirring the mixture in a water bath kettle at 70 ℃ for 1 hour at a rotating speed of 50 r/min.
(3g) Pressure impregnation: and (4) putting the prefabricated body obtained in the step (3 f) into a pressure impregnation tank, injecting the ceramic precursor slurry containing the nano ceramic powder in the step (3 f) into the impregnation tank, slowly heating to 60 ℃ under the pressure of 6MPa in the impregnation tank, preserving heat for 3h, cooling to room temperature along with a furnace, and taking out.
(3h) And (3) curing: curing the preform obtained in step (3 f): putting into a forced air drying oven, heating to 200 ℃ at a heating rate of 8 ℃/min, keeping the temperature for 5h, naturally cooling to room temperature along with the furnace, and taking out.
(3i) Pyrolysis: performing high-temperature cracking on the preform obtained in the step (3 g), raising the temperature to 1450 ℃ at a heating rate of 10 ℃/min under a micro-positive pressure state of 200kPa in a furnace, preserving the temperature for 10h, and then naturally cooling to room temperature in an argon or nitrogen atmosphere;
(3j) And (4) carrying out steps (3 f) - (3 i) on the product obtained in the step (3 i), and repeating for 3 times.
(4) And (3) machining: and (4) processing a groove on the head product obtained in the step (3) according to a design size, processing an internal thread on the groove, processing an external thread on the screw rod according to the design size, and matching the external thread with the internal thread of the head groove in a threaded manner.
(5) Installing a screw: smearing ceramic precursor slurry containing nano-fibers on the surface of the internal thread of the groove at the head part, smearing ceramic precursor slurry containing nano-fibers on the surface of a screw rod matched with the internal thread of the groove in a threaded manner, and connecting the screw rod with the internal thread of the groove in a threaded manner. The ceramic precursor slurry containing the nano-fibers is prepared from a ceramic precursor, a solvent and the nano-fibers according to the weight ratio of 10:8:1.2 by ball milling and mixing evenly. The nano-fibers are nano-SiC fibers and nano-ZrC fibers with the mass ratio of 1. The ball milling time is 4 hours, and the ball milling speed is 350 r/min.
(6) Repeating the steps of dipping, curing and cracking: firstly, carrying out low-temperature cracking, and carrying out steps (3 a) - (3 d) on the product obtained in the step (5) for 4 times; then pyrolysis, i.e. continuing steps (3 f) - (3 i), is repeated 1 time.
(7) Preparing a densified SiC matrix by CVI: in order to improve the matching strength of the screw and the groove, preparing a SiC matrix from the product obtained in the step (6) by adopting a CVI (chemical vapor infiltration) technology, and sealing and filling micro pores at the matching part of the threads; the product is placed in a chemical vapor infiltration furnace, trichlorosilane is used as a precursor, hydrogen is used as carrier gas and reducing gas, argon is used as diluent gas, the deposition temperature is 1200 ℃, the deposition time is 50h, the deposition pressure is 6kPa, the molar ratio of the reducing gas to the trichlorosilane is 10, the flow rate of the precursor is 7g/min, the flow rate of the diluent gas is 13L/min, the flow rate of the reducing gas is determined by the molar ratio of the reducing gas to a silicon source, and the carrier gas flow rate is 100mL/min.
(8) CVD deposition of SiC coating: ultrasonically cleaning and drying the product obtained in the step (7) by using ethanol, coating a screw rod extending out of a groove by using carbon paper, then putting the product into a chemical vapor deposition furnace, taking trichlorosilane as a precursor, hydrogen as a carrier gas and a reducing gas, argon as a diluting gas, wherein the deposition temperature of the chemical vapor deposition is 1100 ℃, the deposition time is 80h, the deposition pressure is 1kPa, the molar ratio of the reducing hydrogen to the trichlorosilane is 15 3 。
Comparative example 1
The difference from example 1 is that: the ceramic precursor slurry described in the step (3 a) was applied to the inner thread surface of the head groove in the step (5), and the others were the same as in example 1.
Comparative example 2
The difference from example 1 is that: and (5) in the step (4), internal threads are not processed in the groove, external threads are not processed in the part where the screw is matched with the groove, the screw is directly matched with the head groove and is fixed by adopting a tool, and the rest parts are the same as those in the embodiment 1.
Comparative example 3
The difference from example 1 is that: in the step (1), preparing an integral prefabricated body by the head part and the screw, wherein the size of the prefabricated body is the same as that of the prefabricated body in the embodiment 1; in the step (4), machining is carried out without machining grooves, and only external threads are machined on the screw; step (5) is not carried out; otherwise, the same procedure as in example 1 was repeated. Tensile strength and compressive strength performance tests were directly performed on the ceramic matrix composite bolts obtained in examples 1 to 3 and comparative examples 1 to 3, samples of the screw portions of the ceramic matrix composite bolts obtained in examples 1 to 3 and comparative examples 1 to 3 were obtained, and the density and the open porosity of the samples were measured by a drainage method, and the results are shown in table 1.
TABLE 1 Properties of the product samples
Claims (10)
1. A fiber reinforced ceramic matrix composite bolt is characterized in that: the bolt consists of a head part and a screw rod, wherein the head part is provided with a groove, the groove is provided with an internal thread, the screw rod is provided with an external thread, the head part is connected with the screw rod through the thread, and the length of the screw rod is greater than the depth of the groove of the head part; a ceramic matrix is filled in a thread gap between the head and the screw rod;
the preparation method comprises the following steps:
(1) Preparing a prefabricated body: preparing continuous carbon fibers or silicon carbide fibers into a head fiber preform and a screw fiber preform which are consistent with the designed size and shape and have allowance in size;
(2) Preparing an interface layer: fixing the fiber preform obtained in the step (1) by adopting a mold, and depositing a pyrolytic carbon interface layer by CVI;
(3) Dipping-curing-cracking: fixing the preform body obtained in the step (2) by using a mould, and repeating the steps of dipping, curing and cracking for 2-4 times; the cracking comprises low temperature cracking and/or high temperature cracking,the cracking temperature of the low-temperature cracking is 950-1300 ℃, the cracking temperature of the high-temperature cracking is 1300-1500 ℃, and the obtained density is 1.45-1.55g/cm 3 The head and the screw;
(4) And (3) machining: processing a groove in the head obtained in the step (3) according to a design size, processing an internal thread in the groove, processing an external thread on the screw rod according to the design size, wherein the external thread is in threaded fit with the internal thread of the groove in the head;
(5) Installation: connecting the external thread of the screw with the internal thread of the head groove in a threaded manner, and fixing by adopting a mold to ensure that the head is coaxially matched with the screw;
(6) Repeating dipping-curing-cracking: repeatedly dipping, curing and cracking at low temperature for 2-4 times, and then repeatedly dipping, curing and cracking at high temperature for 1-2 times, wherein the low temperature cracking is the low temperature cracking with the cracking temperature of 950-1300 ℃; the high-temperature cracking is high-temperature cracking at the cracking temperature of 1300-1500 ℃;
(7) Densification of SiC matrix by CVI technology: preparing a SiC matrix for the product obtained in the step (6) by adopting a CVI technology, and sealing and filling micro pores at the matching part of the threads;
(8) CVD deposition of SiC coating: and (4) coating the external threads of the second part extending out of the groove with carbon paper, then placing the second part into a chemical vapor deposition furnace, performing chemical vapor deposition on the surface of the product obtained in the step (7) to form a SiC coating, and then removing the carbon paper to obtain the fiber reinforced ceramic matrix composite screw.
2. A method of making a fiber reinforced ceramic matrix composite bolt according to claim 1, wherein: the method comprises the following steps:
(1) Preparing a prefabricated body: preparing continuous carbon fibers or silicon carbide fibers into a head fiber preform and a screw fiber preform which are consistent with the designed size and shape and have allowance in size;
(2) Preparing an interface layer: fixing the fiber preform obtained in the step (1) by adopting a mold, and depositing a pyrolytic carbon interface layer by CVI;
(3) Dipping-curing-cracking: using a die for the preform blank obtained in the step (2)Fixing, repeating dipping, curing and cracking for 2-4 times; the cracking comprises low-temperature cracking and/or high-temperature cracking, wherein the cracking temperature of the low-temperature cracking is 950-1300 ℃, the cracking temperature of the high-temperature cracking is 1300-1500 ℃, and the obtained density is 1.45-1.55g/cm 3 The head and the screw;
(4) And (3) machining: processing a groove in the head obtained in the step (3) according to a design size, processing an internal thread in the groove, processing an external thread on the screw rod according to the design size, wherein the external thread is in threaded fit with the internal thread of the groove in the head;
(5) Installation: connecting the external thread of the screw with the internal thread of the head groove in a threaded manner, and fixing by adopting a mold to ensure that the head is coaxially matched with the screw;
(6) Repeating dipping-curing-cracking: repeatedly dipping, curing and cracking at low temperature for 2-4 times, and then repeatedly dipping, curing and cracking at high temperature for 1-2 times, wherein the low temperature cracking is the low temperature cracking with the cracking temperature of 950-1300 ℃; the pyrolysis is pyrolysis at the pyrolysis temperature of 1300-1500 ℃;
(7) Densification of SiC matrix by CVI technology: preparing a SiC matrix for the product obtained in the step (6) by adopting a CVI technology, and sealing and filling micro pores at the matching part of the threads;
(8) CVD deposition of SiC coating: and (4) coating the external threads of the second part extending out of the groove with carbon paper, then placing the second part into a chemical vapor deposition furnace, chemically vapor depositing a SiC coating on the surface of the product obtained in the step (7), and then removing the carbon paper to obtain the fiber reinforced ceramic matrix composite screw.
3. The method of making a fiber reinforced ceramic matrix composite bolt according to claim 2, wherein: in the step (1), the fiber is carbon fiber or silicon carbide fiber; the fiber preform is prepared by molding 1-12K fibers in a manner of 2.5D needling and 2.5D puncturing, and the density of the fiber preform is 0.4-0.6g/cm 3 。
4. The method of making a fiber reinforced ceramic matrix composite bolt according to claim 2, wherein: the CVI deposition pyrolytic carbon interface layer in the step (2) is specifically as follows: fixing the fiber preform by using a graphite tool, introducing carbon source gas at the flow rate of 5-15L/min, depositing a pyrolytic carbon interface layer on the surface of the fiber preform by adopting isothermal CVI (chemical vapor infiltration), and naturally cooling to room temperature in the argon or nitrogen atmosphere; the carbon source gas is selected from any one or more of natural gas, methane, propane and propylene; the deposition temperature of the CVI is 800-1300 ℃, the deposition time is 1-60h, and the pressure in the furnace is 0.5-20kPa.
5. The method of manufacturing a fiber reinforced ceramic matrix composite bolt according to claim 2, wherein: the impregnation in the step (3) and the step (6) comprises vacuum impregnation and pressure impregnation; the vacuum impregnation comprises the following steps: putting the product into a vacuum impregnation barrel, vacuumizing to below 200Pa, keeping the vacuum for 0.5-1h, injecting ceramic precursor slurry or ceramic precursor slurry containing nano ceramic powder, keeping the vacuum for 1-5h, breaking the vacuum and taking out; the pressure impregnation comprises the following steps: putting the product into a pressure impregnation tank, slowly heating to 50-70 ℃ under the pressure of 1-6MPa, preserving heat for 1-5h, cooling to room temperature along with a furnace, and taking out; the ceramic precursor slurry is prepared by mechanically stirring and uniformly mixing a ceramic precursor and a solvent according to the mass ratio of 10 (3-8); the ceramic precursor slurry containing the nano ceramic powder is prepared from a ceramic precursor, a solvent and the nano ceramic powder according to the weight ratio of 10: (3-8): (0.5-2) by mechanical stirring and mixing; the ceramic precursor is one or more of polymethylsilane, polycarbosilane, polycarbosilazane, polysilazane, polysiloxane and polyborosilazane; the solvent is one or more of divinylbenzene, xylene and toluene; the nano ceramic powder is selected from SiC, zrC and B 4 C、HfC、TaC、WC、Si 3 N 4 、ZrN、BN、HfN、SiBCN、SiB 4 、ZrB 2 、HfB 2 And TaB 2 One or more of (a); the mechanical stirring is carried out in a water bath kettle at the temperature of 50-70 ℃, and the stirring is carried out for 1-10h at the rotating speed of 50-60 r/min.
6. The method of manufacturing a fiber reinforced ceramic matrix composite bolt according to claim 2, wherein: the cracking in the step (3) and the step (6) is as follows: putting the product into a sintering furnace, heating to a cracking temperature at a heating rate of 5-10 ℃/min under a vacuum state below 200Pa or a micro-positive pressure state with the pressure in the furnace of 100-200kPa, preserving heat for 2-10h, and naturally cooling to room temperature under the atmosphere of argon or nitrogen.
7. The method of making a fiber reinforced ceramic matrix composite bolt according to claim 2, wherein: and (5) when the screw is installed, firstly coating ceramic precursor slurry containing nano fibers on the surface of the screw, coating ceramic precursor slurry containing nano fibers on the surface of the internal thread of the head groove, and then connecting the screw and the internal thread of the head groove in a threaded manner.
8. The method of making a fiber reinforced ceramic matrix composite bolt according to claim 7, wherein: the ceramic precursor slurry containing the nano-fibers is prepared from a ceramic precursor, a solvent and the nano-fibers according to the weight ratio of 10: (6-12): the mass ratio of (1-3) is formed by ball milling and uniform mixing; the nano-fibers are nano-carbon fibers, carbon nano-tubes, nano-SiC fibers and nano-ZrC fibers; the ball milling time is 3-5h, and the ball milling speed is 300-400 r/min.
9. The method of making a fiber reinforced ceramic matrix composite bolt according to claim 2, wherein: the CVI prepared densified SiC matrix in the step (7) specifically comprises the following steps: the product is placed in a chemical gas-phase permeation furnace, trichlorosilane is taken as a precursor, hydrogen is taken as carrier gas and reducing gas, argon is taken as diluent gas, the deposition temperature is 850-1200 ℃, the deposition time is 5-100 h, the deposition pressure is 5-15 kPa, the molar ratio of the reducing gas to the trichlorosilane is (5-20): 1, the flow rate of the precursor is 1-15 g/min, the flow rate of the diluting gas is 5-20L/min, the flow rate of the reducing gas is determined by the molar ratio of the reducing gas to a silicon source, and the flow rate of the carrier gas is 100-200 mL/min.
10. The method of manufacturing a fiber reinforced ceramic matrix composite bolt according to claim 2, wherein: the CVD deposition SiC coating in the step (8) is specifically as follows: the product is put into a chemical vapor deposition furnace, trichlorosilane is taken as a precursor, hydrogen is taken as a carrier gas and a reducing gas, argon is taken as a diluting gas, the deposition temperature of chemical vapor deposition is 950-1500 ℃, the deposition time is 5-80 h, the deposition pressure is 1-20 kPa, the molar ratio of the reducing gas to the trichlorosilane is (8-20): 1, the flow rate of the precursor is 1-15 g/min, the flow rate of the diluting gas is 2-20L/min, the flow rate of the reducing gas is determined by the molar ratio of the reducing gas to a silicon source, and the flow rate of the carrier gas is 100-300 mL/min.
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| CN113582729A (en) * | 2021-08-11 | 2021-11-02 | 上海大学绍兴研究院 | Ceramic matrix composite material and preparation method and application thereof |
| CN113816755B (en) * | 2021-10-14 | 2023-09-01 | 西安鑫垚陶瓷复合材料有限公司 | Two-dimensional silicon carbide/silicon carbide composite bar and preparation method of connecting piece |
| CN113956061B (en) * | 2021-11-12 | 2023-08-22 | 中国航空制造技术研究院 | Preparation method of continuous fiber reinforced ceramic matrix composite screw |
| CN114874031B (en) * | 2022-05-09 | 2023-04-18 | 西安鑫垚陶瓷复合材料有限公司 | Ceramic matrix composite material thread machining method |
| CN115198253A (en) * | 2022-07-05 | 2022-10-18 | 苏州步科斯新材料科技有限公司 | Preparation method of graphite matrix surface tantalum carbide coating |
| CN115894048B (en) * | 2022-10-12 | 2023-09-26 | 安徽精亘机械科技有限公司 | Carbon fiber and ceramic structured composite reinforced bolt |
| CN115716757B (en) * | 2022-11-21 | 2023-11-17 | 西安鑫垚陶瓷复合材料股份有限公司 | Ceramic matrix composite high-strength bolt and preparation method thereof |
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