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CN112552065A - Fiber-reinforced ceramic matrix composite bolt and preparation method thereof - Google Patents

Fiber-reinforced ceramic matrix composite bolt and preparation method thereof Download PDF

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Publication number
CN112552065A
CN112552065A CN202110108175.4A CN202110108175A CN112552065A CN 112552065 A CN112552065 A CN 112552065A CN 202110108175 A CN202110108175 A CN 202110108175A CN 112552065 A CN112552065 A CN 112552065A
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Prior art keywords
screw
temperature
cracking
head
fiber
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Granted
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CN202110108175.4A
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CN112552065B (en
Inventor
张东生
吴恒
马美霞
潘广镇
刘毫豪
刘帅
王琰
魏庆勃
李江涛
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Gongyi Fanrui Yihui Composite Materials Co.,Ltd.
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Gongyi Van Research Yihui Composite Material Co Ltd
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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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Ceramic Products (AREA)

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 and 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; repeating the steps of dipping, curing and pyrolysis for 1-2 times; (7) adopting CVI technology to densify SiC matrix; (8) and depositing the SiC coating on the surface of the product by using a CVD (chemical vapor deposition) 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

Fiber-reinforced ceramic matrix composite bolt and preparation method thereof
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 SiC/SiC composite material pins 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.
Disclosure of invention patent CN107021770BA preparation method of the 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 a continuous screw, depositing a SiC matrix through a chemical vapor deposition process, performing finish machining to a size, introducing ultrahigh-temperature ceramic through multiple dipping-cracking of an ultrahigh-temperature ceramic precursor, processing the continuous screw into a single screw, depositing a SiC coating on the surface of the screw, and finally processing threads by adopting a diamond cutter to obtain a screw product. 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. However, the method is used for preparing the ultrahigh temperature matrix with the density of 1.9g/cm on a CVD-SiC matrix and PIP3The 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/cm3The head and the screw;
(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 low-temperature cracking the product obtained in the step (5) with the mould for 2-4 times, and then repeatedly dipping, curing and high-temperature cracking for 1-2 times, wherein the low-temperature cracking is the low-temperature cracking with the cracking temperature of 950-; the high-temperature cracking is high-temperature cracking at the cracking temperature of 1300 ℃ and 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 thread 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.
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/cm3。
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 0.5-20 kPa.
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, 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: the product is put into a blast drying box, heated to 120 ℃ and 250 ℃ at the heating rate of 5-10 ℃/min, and the heat preservation time is 3-10h, and is naturally cooled to the room temperature along with the furnace and then taken out.
Further, the cracking in the step (3) and the step (6) is: putting the product into a sintering furnace, heating to the 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 the heat for 2-10h, and naturally cooling to the 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, B4C、HfC、TaC、WC、Si3N4、ZrN、BN、HfN、SiBCN、SiB4、ZrB2、HfB2And TaB2One 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 rotating 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 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 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 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.
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 process threads when the threads have certain density so as to realize threaded connection, compared with the mode that the threads are not processed, the screw rod and the head are directly connected through filling the SiC matrix, the bonding strength of the screw rod and the head is better, the adhesive force of the SiC matrix on the surfaces of the screw rod and the head is higher, and the connection strength of the screw rod 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, the nano-fiber is added into the ceramic precursor slurry before the screw is connected with the internal thread of the groove 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 any inventive step based on the embodiments of the present invention, are within the 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 65 mm; the diameter of the screw is 18 mm.
The preparation method of the carbon fiber reinforced ceramic matrix composite bolt comprises the following steps:
(1) preparing a prefabricated body: according to the method for selecting 0/90 degrees 2.5D needle-punching forming of a carbon fiber (12K) weftless fabric-mesh tire of the component, a head fiber preform and a screw fiber preform are prepared, wherein the diameter of the head fiber preform is 32mm, the height of the head fiber preform is 40mm, and the density of the head fiber preform is 0.5g/cm3(ii) a The screw rod fiber preform has a diameter of 20mm, a height of 68mm and a density of 0.5g/cm3。
(2) CVI deposition of a pyrolytic carbon interface layer: fixing the fiber preform obtained in the step (1) by using a graphite tool, introducing methane gas at a gas flow rate 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 the vacuum is maintained for 1h, keeping the vacuum for 1h, breaking the vacuum and taking out the preform to obtain a preform containing the precursor slurry; the ceramic precursor slurry is prepared by uniformly mixing polycarbosilane and xylene according to a mass ratio of 10:5 through mechanical stirring, and stirring for 5 hours at a rotating speed of 50r/min in a 70 ℃ water bath kettle 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 below 200Pa, preserving the temperature for 2h, and then naturally cooling to room temperature in an argon or nitrogen atmosphere;
(3e) high-temperature cracking: 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) to (3 e) on the product obtained in the step (3 e), and repeating the steps 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.
(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 dipping-curing-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/cm3。
(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 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 is 850 ℃, the deposition time is 100 hours, the deposition pressure is 15kPa, the molar ratio of the reducing gas to trichlorosilane is 15:1, the flow rate of the precursor is 4g/min, the flow rate of the diluting gas is 10L/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 mL/min.
(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 a screw rod extending out of a 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 diluting gas, setting the deposition temperature of the chemical vapor deposition to 950 ℃, the deposition time to 30 hours, the deposition pressure to 20kPa, the molar ratio of the reducing hydrogen to the trichlorosilane to be 8:1, the flow rate of the precursor to be 15g/min, the flow rate of the diluting gas to be 20L/min, the flow rate of the reducing gas to be determined by the molar ratio of the reducing gas to the silicon source, the flow rate of the carrier gas to be 100mL/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, the density of the obtained product is 1.99g/cm3。
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 70 mm; the diameter of the screw is 24 mm.
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 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 44mm, the height of the head fiber preform is 28mm, and the head fiber preform is denseThe degree is 0.45 g/cm3(ii) a The screw rod fiber preform has a diameter of 26mm, a height of 72mm and a density of 0.45 g/cm3。
(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 10 kPa. 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 at the vacuum degree of below 200Pa for 0.5h, injecting ceramic precursor slurry, vacuumizing for 5h, and taking out the preform after vacuum breaking to obtain a preform containing the precursor slurry; the ceramic precursor slurry is prepared by uniformly mixing polymethyl silane and divinyl benzene in a mass ratio of 10:5 through mechanical stirring, and stirring for 10 hours at a rotating speed of 60r/min in a water bath kettle at 50 ℃ 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 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 ℃ 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: 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 at the vacuum degree of below 200Pa for 0.5h, injecting ceramic precursor slurry, vacuumizing for 5h, and taking out after vacuum breaking to obtain a prefabricated body containing the precursor slurry; the ceramic precursor is formed by uniformly mixing polymethyl silicane and divinyl benzene according to the mass ratio of 10:5 through mechanical stirring, and the ceramic precursor is stirred for 10 hours at the rotating speed of 60r/min in a water bath kettle at the temperature of 50 ℃ through mechanical stirring.
(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: 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;
(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.
(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 dipping-curing-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, 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 a carrier gas and a reducing gas, argon is used as a diluting 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 trichlorosilane is 10:1, 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 flow rate of the carrier gas is 150 mL/min.
(8) CVD deposition of SiC coating: ultrasonically cleaning and drying the product obtained in the step (7) by using ethanol, coating the screw rod extending out of the groove by using carbon paper, then 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 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 12:1, 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 the silicon source, the flow rate of the carrier gas is 120mL/min, a SiC coating is prepared on the surface of the product through chemical vapor deposition, the oxidation resistance and the wear resistance of the member are improved, then the carbon paper is removed to obtain the fiber reinforced ceramic matrix composite bolt, and the density of the obtained product is 1.98 g/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 55 mm; the diameter of the screw is 20 mm.
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/cm3(ii) a The screw rod fiber preform has a diameter of 25mm, a height of 60mm and a density of 0.5g/cm3。
(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 5 kPa. 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 divinyl benzene is prepared by uniformly mixing divinyl benzene with mechanical stirring according to the mass ratio of 10:8, and stirring for 10 hours at the rotating speed of 60r/min in a water bath kettle at the temperature of 50 ℃ with 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 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: putting 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 with the pressure of 100kPa, preserving the temperature for 2h, 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 the temperature of 70 ℃ for 1 hour at the rotating speed of 50r/min by mechanical stirring.
(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) High-temperature cracking: 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 in a micro-positive pressure state with the pressure in the furnace being 200kPa, 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.
(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: 1. The ball milling time is 4 hours, and the ball milling speed is 350 r/min.
(6) Repeating dipping-curing-cracking: firstly, low-temperature cracking is carried out, the product obtained in the step (5) is subjected to the steps (3 a) to (3 d), and the steps are repeated 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 trichlorosilane is 10:1, the flow rate of the precursor is 7g/min, the flow rate of the diluting 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 flow rate of the carrier gas is 100 mL/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, and argon as a diluent gas, wherein the deposition temperature of the chemical vapor deposition is 1100 ℃, the deposition time is 80 hours, the deposition pressure is 1kPa, the molar ratio of the reducing hydrogen to the trichlorosilane is 15:1, the flow rate of the precursor is 1g/min, the flow rate of the diluent gas is 15L/min, and the flow rate of the reducing gas is determined by the reducing gas and the silicon source of the silicon sourceThe mol ratio is determined, the carrier gas flow is 150mL/min, a SiC coating is prepared on the surface of the product through chemical vapor deposition, the oxidation resistance and the wear resistance of the member are improved, then the carbon paper is removed to obtain the fiber reinforced ceramic matrix composite bolt, and the density of the obtained product is 2.0g/cm3。
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 (4) not processing internal threads in the groove, not processing external threads on the part of the screw matched with the groove, directly matching the screw with the groove of the head part, fixing 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 integrated prefabricated body by the head part and the screw rod, wherein the size of the prefabricated body is the same as that of the prefabricated body in the example 1; in the step (4), machining is carried out, grooves are not machined, and external threads are only machined on the screw; step (5) is not carried out; otherwise, the same procedure as in example 1 was repeated. The tensile strength and the compressive strength of the ceramic matrix composite bolts obtained in examples 1 to 3 and comparative examples 1 to 3 were directly tested, the samples of the screw portions of the ceramic matrix composite bolts obtained in examples 1 to 3 and comparative examples 1 to 3 were cut out, and the density and the open porosity of the cut-out samples were tested by a drainage method, and the results are shown in table 1.
TABLE 1 Properties of the product samples
Figure DEST_PATH_IMAGE001

Claims (10)

1.一种纤维增强陶瓷基复合材料螺栓，其特征在于：所述螺栓由头部和螺杆组成，所述头部设有凹槽，凹槽设有内螺纹，螺杆设有外螺纹，头部与螺杆通过螺纹连接，所述螺杆长度大于头部凹槽深度；所述头部和螺杆之间螺纹缝隙内填充有陶瓷基体。1. A fiber-reinforced ceramic matrix composite material bolt, characterized in that: the bolt is composed of a head and a screw, the head is provided with a groove, the groove is provided with an internal thread, the screw is provided with an external thread, and the head is provided with an external thread. The screw is connected with the screw through a thread, and the length of the screw is greater than the depth of the groove of the head; the thread gap between the head and the screw is filled with a ceramic matrix. 2.一种制备如权利要求1所述纤维增强陶瓷基复合材料螺栓的方法，其特征在于：包括如下步骤：2. A method for preparing fiber-reinforced ceramic matrix composite material bolts as claimed in claim 1, characterized in that: comprising the steps of: 制备预制体：将连续碳纤维或碳化硅纤维制备成与设计尺寸形状一致、尺寸富有余量的头部纤维预制体和螺杆纤维预制体；Preparation of preforms: the continuous carbon fibers or silicon carbide fibers are prepared into head fiber preforms and screw fiber preforms that are consistent with the design size and shape and have a size margin; 制备界面层：将步骤（1）所得的纤维预制体采用模具固定，经CVI沉积热解炭界面层；Preparation of the interface layer: the fiber preform obtained in step (1) is fixed with a mold, and the pyrolytic carbon interface layer is deposited by CVI; 浸渍-固化-裂解：将步骤（2）所得的预制体坯体使用模具固定，重复浸渍-固化-裂解2-4次；所述裂解包括低温裂解和/或高温裂解，所述低温裂解的裂解温度为950℃-1300℃，高温裂解的裂解温度为1300-1500℃，获得密度为1.45-1.55g/cm3的头部和螺杆；Impregnation-curing-cracking: the preform body obtained in step (2) is fixed with a mold, and the dipping-curing-cracking is repeated 2-4 times; the cracking includes low-temperature cracking and/or high-temperature cracking, and the cracking of the low-temperature cracking The temperature is 950°C-1300°C, and the pyrolysis temperature of high-temperature pyrolysis is 1300-1500°C, to obtain a head and a screw with a density of 1.45-1.55g/ cm3 ; 机械加工：将步骤（3）所得头部按照设计尺寸加工凹槽，并在凹槽内加工内螺纹，按照设计尺寸对螺杆加工外螺纹，所述外螺纹与头部凹槽的内螺纹螺纹配合；Machining: The head obtained in step (3) is processed into grooves according to the design size, and internal threads are processed in the grooves, and external threads are processed on the screw according to the design size, and the external threads are matched with the internal threads of the head groove. ; 安装：将螺杆的外螺纹与头部凹槽的内螺纹螺纹连接，采用模具固定，保证头部与螺杆同轴配合；Installation: Connect the external thread of the screw with the internal thread of the groove of the head, and fix it with a mold to ensure that the head and the screw are coaxially matched; 重复浸渍-固化-裂解：将步骤（5）所得制品连带模具重复浸渍-固化-低温裂解2-4次，再重复浸渍-固化-高温裂解1-2次，所述低温裂解为裂解温度950-1300℃的低温裂解；所述高温裂解为裂解温度1300-1500℃的高温裂解；Repeated dipping-curing-pyrolysis: repeat dipping-curing-low-temperature cracking 2-4 times for the product obtained in step (5) together with the mold, and then repeat dipping-curing-high-temperature cracking 1-2 times, and the low-temperature cracking is a cracking temperature of 950- Low temperature cracking at 1300 °C; the high temperature cracking is high temperature cracking with a cracking temperature of 1300-1500 °C; CVI技术增密SiC基体：将步骤（6）所得制品采用CVI技术制备SiC基体，封填螺纹配合处微小孔隙；CVI technology to densify the SiC matrix: the product obtained in step (6) is prepared by the CVI technology to prepare the SiC matrix, and the tiny pores at the thread fitting are filled; CVD沉积SiC涂层：将第二部件伸出凹槽的外螺纹用碳纸包覆，然后放入化学气相沉积炉中，在步骤（7）所得制品表面化学气相沉积一层SiC涂层，然后拆除碳纸，即得到纤维增强陶瓷基复合材料螺杆。CVD deposition of SiC coating: the outer thread of the second part extending out of the groove is covered with carbon paper, and then placed in a chemical vapor deposition furnace, a layer of SiC coating is deposited on the surface of the product obtained in step (7), and then The fiber-reinforced ceramic matrix composite screw is obtained by removing the carbon paper. 3.根据权利要求2所述的制备纤维增强陶瓷基复合材料螺栓的方法，其特征在于：步骤（1）中，所述纤维为碳纤维或碳化硅纤维；所述纤维预制体为通过1-12K纤维以2.5D针刺、2.5D穿刺的成型方式制备而成，纤维预制体的密度为0.4-0.6g/cm3。3. The method for preparing fiber-reinforced ceramic matrix composite bolts according to claim 2, characterized in that: in step (1), the fibers are carbon fibers or silicon carbide fibers; The fibers are prepared by 2.5D needling and 2.5D puncturing, and the density of the fiber preform is 0.4-0.6 g/cm 3 . 4.根据权利要求2所述的制备纤维增强陶瓷基复合材料螺栓的方法，其特征在于：步骤（2）所述CVI沉积热解炭界面层具体为：将纤维预制体用石墨工装固定，以5-15L/min的流量通入碳源气体，采用等温CVI在纤维预制体表面沉积一层热解炭界面层，在氩气或氮气气氛下自然降温至室温；所述碳源气体选自天然气、甲烷、丙烷、丙烯中的任一种或多种；所述CVI的沉积温度为800-1300℃，沉积时间为1-60h，炉内压力为0.5-20kP。4. The method for preparing fiber-reinforced ceramic matrix composite material bolts according to claim 2, characterized in that: in step (2), the CVI deposition of the pyrolytic carbon interface layer is specifically: fixing the fiber preform with a graphite tool to The carbon source gas was introduced at a flow rate of 5-15L/min, a layer of pyrolytic carbon interface layer was deposited on the surface of the fiber preform by isothermal CVI, and the temperature was naturally cooled to room temperature under an argon or nitrogen atmosphere; the carbon source gas was selected from natural gas , any one or more of methane, propane and propylene; the deposition temperature of the CVI is 800-1300° C., the deposition time is 1-60h, and the pressure in the furnace is 0.5-20kP. 5.根据权利要求2所述的制备纤维增强陶瓷基复合材料螺栓的方法，其特征在于：步骤（3）和步骤（6）中所述浸渍包括真空浸渍和压力浸渍；所述真空浸渍为：将制品放入真空浸渍桶中，抽真空至200Pa以下，保真空0.5-1h后，注入陶瓷先驱体浆料或含有纳米陶瓷粉的陶瓷先驱体浆料，再保真空1-5h，破真空取出；所述压力浸渍为：将制品放入压力浸渍罐中，压力浸渍罐内压力为1-6MPa，缓慢升温至50-70℃，保温1-5h，随炉降温至室温后取出；所述陶瓷先驱体浆料是由陶瓷先驱体与溶剂按照10:（3-8）的质量比通过机械搅拌均匀混合而成；所述含有纳米陶瓷粉的陶瓷先驱体浆料是由陶瓷先驱体、溶剂、纳米陶瓷粉按照10：（3-8）：（0.5-2）的质量比通过机械搅拌均匀混合而成；陶瓷先驱体为聚甲基硅烷、聚碳硅烷、聚碳硅氮烷、聚硅氮烷、聚硅氧烷、聚硼硅氮烷中的一种或多种；溶剂为二乙烯基苯、二甲苯、甲苯中的一种或多种；纳米陶瓷粉选自硅、锆以及其它过渡金属元素的碳化物、氮化物和硼化物中的任一种或多种，例如：SiC、ZrC、B4C、HfC、TaC、WC、Si3N4、ZrN、BN、HfN、SiBCN、SiB4、ZrB2、HfB2和TaB2中的一种或多种；机械搅拌在50-70℃水浴锅中进行，以50-60r/min转速搅拌1-10h。5. The method for preparing fiber-reinforced ceramic matrix composite bolts according to claim 2, wherein the impregnation in steps (3) and (6) includes vacuum impregnation and pressure impregnation; the vacuum impregnation is: Put the product into the vacuum impregnation barrel, vacuum to below 200Pa, keep the vacuum for 0.5-1h, inject the ceramic precursor slurry or the ceramic precursor slurry containing nano-ceramic powder, keep the vacuum for 1-5h, break the vacuum and take out The pressure impregnation is as follows: put the product into the pressure impregnation tank, the pressure in the pressure impregnation tank is 1-6MPa, slowly heat up to 50-70 ℃, keep the temperature for 1-5h, and take out after cooling down to room temperature with the furnace; the ceramic The precursor slurry is uniformly mixed by the ceramic precursor and the solvent according to the mass ratio of 10:(3-8) through mechanical stirring; the ceramic precursor slurry containing the nano-ceramic powder is composed of the ceramic precursor, the solvent, the The nano ceramic powder is uniformly mixed by mechanical stirring according to the mass ratio of 10:(3-8):(0.5-2); the ceramic precursors are polymethylsilane, polycarbosilane, polycarbosilazane, polysilicon nitride One or more of alkane, polysiloxane, and polyborosilazane; solvent is one or more of divinylbenzene, xylene, and toluene; nano-ceramic powder is selected from silicon, zirconium and other transition Any one or more of carbides, nitrides and borides of metal elements, such as: SiC, ZrC, B4C, HfC, TaC, WC, Si3N4, ZrN , BN, HfN, SiBCN , SiB 4. One or more of ZrB 2 , HfB 2 and TaB 2 ; mechanical stirring is carried out in a water bath at 50-70° C., and stirring is carried out at a speed of 50-60 r/min for 1-10 hours. 6.根据权利要求2所述的制备纤维增强陶瓷基复合材料螺栓的方法，其特征在于：步骤（3）和步骤（6）中所述裂解为：将制品放入烧结炉中，炉内为200Pa以下的真空状态或炉内压力为100-200kPa的微正压状态，以5-10℃/min的升温速率升温至裂解温度，保温2-10h，然后在氩气或氮气氛围下自然冷却至室温。6. The method for preparing fiber-reinforced ceramic matrix composite bolts according to claim 2, wherein the cracking in steps (3) and (6) is: placing the product in a sintering furnace, and the furnace is In a vacuum state below 200Pa or a slightly positive pressure state with a pressure of 100-200kPa in the furnace, heat up to the cracking temperature at a heating rate of 5-10℃/min, keep it for 2-10h, and then naturally cool it to a room temperature. 7.根据权利要求2所述的制备纤维增强陶瓷基复合材料螺栓的方法，其特征在于：步骤（5）安装螺杆时，先在螺杆表面涂抹含纳米纤维的陶瓷先驱体浆料，在头部凹槽的内螺纹表面涂抹含纳米纤维的陶瓷先驱体浆料，然后再将螺杆与头部凹槽的内螺纹螺纹连接。7. The method for preparing fiber-reinforced ceramic matrix composite bolts according to claim 2, characterized in that: when installing the screw in step (5), first apply the ceramic precursor slurry containing nanofibers on the surface of the screw, and then apply the nanofiber-containing ceramic precursor slurry on the head of the screw. The surface of the inner thread of the groove is coated with ceramic precursor slurry containing nanofibers, and then the screw is connected with the inner thread of the head groove. 8.根据权利要求7所述的制备纤维增强陶瓷基复合材料螺栓的方法，其特征在于：所述的含纳米纤维的陶瓷先驱体浆料是由陶瓷先驱体、溶剂、纳米纤维按照10：（6-12）：（1-3）的质量比通过球磨均匀混合而成；所述的纳米纤维为纳米碳纤维、碳纳米管、纳米SiC纤维、纳米ZrC纤维；所述的球磨时间为3-5h，球磨转速为300-400转/分钟。8. The method for preparing fiber-reinforced ceramic matrix composite bolts according to claim 7, wherein the nanofiber-containing ceramic precursor slurry is composed of ceramic precursors, solvents, and nanofibers according to 10: ( 6-12): The mass ratio of (1-3) is uniformly mixed by ball milling; the nanofibers are carbon nanofibers, carbon nanotubes, nano-SiC fibers, and nano-ZrC fibers; the ball-milling time is 3-5h , the ball milling speed is 300-400 rpm. 9.根据权利要求2所述的制备纤维增强陶瓷基复合材料螺栓的方法，其特征在于：步骤（7）所述的CVI制备增密SiC基体具体为：将制品放入化学气相渗透炉中，以三氯甲硅烷为先驱体，氢气为载气和还原气体，氩气为稀释气体，沉积温度为850℃-1200℃，沉积时间为5h-100h，沉积压力为5kPa-15kPa，所述的还原气体与三氯甲硅烷的摩尔比为（5-20）:1，先驱体流量为1g/min-15g/min，稀释气体流量为5L/min-20L/min，还原气体的流量由还原气体与硅源的摩尔比来确定，载气流量为100mL/min -200mL/min。9 . The method for preparing fiber-reinforced ceramic matrix composite material bolts according to claim 2 , wherein the preparation of the densified SiC matrix by CVI in step (7) is specifically: placing the product in a chemical vapor infiltration furnace, Using trichlorosilane as the precursor, hydrogen as the carrier gas and reducing gas, argon as the diluent gas, the deposition temperature is 850 ℃-1200 ℃, the deposition time is 5h-100h, and the deposition pressure is 5kPa-15kPa. The molar ratio of gas to trichlorosilane is (5-20): 1, the flow rate of precursor is 1g/min-15g/min, the flow rate of dilution gas is 5L/min-20L/min, and the flow rate of reducing gas is determined by reducing gas and reducing gas. The molar ratio of the silicon source is determined, and the flow rate of the carrier gas is 100mL/min-200mL/min. 10.根据权利要求2所述的制备纤维增强陶瓷基复合材料螺栓的方法，其特征在于：步骤（8）所述CVD沉积SiC涂层具体为：将制品放入化学气相沉积炉中，以三氯甲硅烷为先驱体，氢气为载气和还原气体，氩气为稀释气体，化学气相沉积的沉积温度为950℃-1500℃，沉积时间为5h-80h，沉积压力为1kPa-20kPa，所述还原气体与三氯甲硅烷的摩尔比为（8-20）:1，先驱体流量为1g/min-15g/min，稀释气体流量为2L/min-20L/min，还原气体的流量由还原气体与硅源的摩尔比来确定，载气流量为100mL/min-300mL/min。10. The method for preparing fiber-reinforced ceramic matrix composite bolts according to claim 2, characterized in that: the CVD deposition of the SiC coating in step (8) is specifically: placing the product in a chemical vapor deposition furnace, using three Chlorosilane is the precursor, hydrogen is the carrier gas and reducing gas, argon is the diluent gas, the deposition temperature of chemical vapor deposition is 950℃-1500℃, the deposition time is 5h-80h, and the deposition pressure is 1kPa-20kPa. The molar ratio of reducing gas to trichlorosilane is (8-20): 1, the flow rate of precursor is 1g/min-15g/min, the flow rate of diluent gas is 2L/min-20L/min, and the flow rate of reducing gas is determined by reducing gas. Determined by the molar ratio with the silicon source, the flow rate of the carrier gas is 100mL/min-300mL/min.
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CN116947519A (en) * 2023-07-28 2023-10-27 内蒙古栢特新材料科技有限公司 Preparation method of carbon ceramic brake block for passenger car
CN117534474A (en) * 2023-12-26 2024-02-09 中国航空制造技术研究院 Preparation method of matrix boron modified SiC/SiC composite material
RU231746U1 (en) * 2024-12-13 2025-02-07 Владимир Васильевич Галайко CARBON COMPOSITE SELF-TAPPING SCREW
CN119775017A (en) * 2025-03-07 2025-04-08 西北工业大学 Production and processing technology of high-strength ceramic matrix composite bolt
CN119775017B (en) * 2025-03-07 2025-06-13 西北工业大学 A production and processing technology for high-strength ceramic-based composite bolts

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