CN115160005A - Preparation method of two-dimensional silicon carbide/silicon carbide composite material nut - Google Patents
Preparation method of two-dimensional silicon carbide/silicon carbide composite material nut Download PDFInfo
- Publication number
- CN115160005A CN115160005A CN202210713475.XA CN202210713475A CN115160005A CN 115160005 A CN115160005 A CN 115160005A CN 202210713475 A CN202210713475 A CN 202210713475A CN 115160005 A CN115160005 A CN 115160005A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- deposition
- nut
- depositing
- gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 222
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 218
- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000000151 deposition Methods 0.000 claims description 228
- 230000008021 deposition Effects 0.000 claims description 151
- 239000010410 layer Substances 0.000 claims description 89
- 239000007789 gas Substances 0.000 claims description 77
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 74
- 239000004744 fabric Substances 0.000 claims description 73
- 229910052786 argon Inorganic materials 0.000 claims description 37
- 239000000758 substrate Substances 0.000 claims description 36
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 32
- 239000011159 matrix material Substances 0.000 claims description 31
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 claims description 30
- 239000001257 hydrogen Substances 0.000 claims description 28
- 229910052739 hydrogen Inorganic materials 0.000 claims description 28
- 238000009958 sewing Methods 0.000 claims description 28
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 230000001681 protective effect Effects 0.000 claims description 20
- 238000003754 machining Methods 0.000 claims description 18
- 239000012495 reaction gas Substances 0.000 claims description 16
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 15
- 239000004917 carbon fiber Substances 0.000 claims description 15
- 239000002356 single layer Substances 0.000 claims description 15
- 230000003197 catalytic effect Effects 0.000 claims description 14
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000010030 laminating Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 238000003475 lamination Methods 0.000 claims description 3
- 230000001154 acute effect Effects 0.000 claims description 2
- 230000003064 anti-oxidating effect Effects 0.000 claims description 2
- 238000004364 calculation method Methods 0.000 claims description 2
- 230000002093 peripheral effect Effects 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000009964 serging Methods 0.000 claims description 2
- 238000007493 shaping process Methods 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 14
- 239000000835 fiber Substances 0.000 description 13
- 239000011153 ceramic matrix composite Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 6
- 238000010079 rubber tapping Methods 0.000 description 6
- 150000002431 hydrogen Chemical class 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000007585 pull-off test Methods 0.000 description 5
- 230000037303 wrinkles Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000011265 semifinished product Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000011162 core material Substances 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Images
Classifications
-
- 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
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
-
- 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
-
- 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
- F16B33/00—Features common to bolt and nut
-
- 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
- F16B33/00—Features common to bolt and nut
- F16B33/008—Corrosion preventing means
-
- 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
- F16B33/00—Features common to bolt and nut
- F16B33/06—Surface treatment of parts furnished with screw-thread, e.g. for preventing seizure or fretting
-
- 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
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3821—Boron carbides
-
- 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
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/386—Boron nitrides
-
- 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
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/614—Gas infiltration of green bodies or pre-forms
-
- 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The invention relates to a preparation method of a composite fastener, in particular to a preparation method of a two-dimensional silicon carbide/silicon carbide composite nut. By means of optimizing the type, shaping and preparation process of the prefabricated part, introducing B4C self-healing components and the like, the density uniformity and mechanical property of the product are obviously improved, the service life of the product in a high-temperature environment is obviously prolonged, the preparation period is shortened, and the cost is saved. The method can be applied to the connection and assembly of composite material products under the conditions of ultrahigh temperature, oxidation environment and high bearing capacity.
Description
Technical Field
The invention relates to the field of composite fastener preparation, in particular to a preparation method of a two-dimensional silicon carbide/silicon carbide composite nut.
Background
The ceramic matrix composite material is a novel strategy material integrating the thermal structure/function and having the advantages of metal material, ceramic material and carbon material, has the characteristics of high temperature resistance, low density, high specific strength, high specific modulus, oxidation resistance, ablation resistance, insensitivity to cracks, no catastrophic damage and the like, and is widely applied to the fields of aviation, aerospace, satellite aerospace, nuclear energy, photovoltaic and the like.
Due to the limitation of the prior composite material weaving and forming process technology, the integral preparation of large-size, precise and complex product components by using the ceramic matrix composite material is difficult. Therefore, in order to meet the requirements of higher service temperature and mechanical property of the connecting piece provided by the aircraft in the future aerospace field, the composite connecting piece with high performance and low cost is prepared, and the composite connecting piece has important significance for composite materials, particularly ceramic matrix composite engineering application.
At present, the composite material nut is mostly prepared by adopting a three-dimensional needling carbon/silicon carbide composite material; the invention patent with publication number CN 1111699038A discloses a fiber reinforced resin matrix composite nut, which comprises an inner core material and a composite winding layer wound outside the inner core material, and the preparation method is complex in process, low in preparation efficiency, poor in high temperature resistance and not beneficial to industrial production.
The preparation method of the traditional three-dimensional needling carbon/silicon carbide composite material nut is briefly as follows: selecting a three-dimensional needled carbon felt preform, and alternately and circularly superposing a tire mesh, single-layer 0-degree laid cloth, single-layer tire mesh, single-layer 90-degree laid cloth and single-layer tire mesh to the designed thickness. Wherein the net tire is prepared by adopting a T700SC/12K chopped carbon fiber (with the length of 70-90 mm) air spinning process, and the non-woven cloth is prepared by adopting T700SC/6K carbon fiber. The net tire and the non-woven cloth are subjected to relay needling by using crochet hooks so as to improve interlayer combination. Preparing a pyrolytic carbon interface layer and a silicon carbide substrate by adopting a CVI (chemical vapor infiltration) process, and processing the size of the nut when the densification is carried out to a certain density. The nuts prepared by the preparation method have uneven density, so that the performance difference of the nuts in the same batch is large, and meanwhile, the preparation method has complex process and long production period, and is not beneficial to industrial production.
Disclosure of Invention
In order to further improve the strength of the ceramic matrix composite connecting piece, meet the requirements of a new generation of aircraft in the field of aerospace on the performance of the connecting piece in a severer service environment and overcome the defects of long production cycle, large performance difference and the like of the conventional three-dimensional needled carbon/silicon carbide composite nut, the invention provides a preparation method of a two-dimensional silicon carbide/silicon carbide composite nut.
The technical scheme of the invention provides a preparation method of a two-dimensional silicon carbide/silicon carbide composite material nut, which is characterized by comprising the following steps:
step 1, preparation of two-dimensional silicon carbide/silicon carbide layering plate preform
Step 1.1, laminating multiple layers of silicon carbide cloth, wherein the included angle between every two layers of silicon carbide cloth is a right angle or an acute angle;
step 1.2, laminating multiple layers of silicon carbide cloth to a designed thickness, wherein the designed thickness is the thickness of the nut plus 0.5 mm-1 mm;
step 1.3, puncturing and sewing the laminated silicon carbide cloth by using carbon fibers;
step 2, depositing a BN interface layer
Carrying out BN interface layer deposition on the two-dimensional silicon carbide/silicon carbide layering plate preform prepared in the step 1 to obtain a preform with a BN interface layer;
step 3, depositing SiC matrix
Carrying out silicon carbide matrix deposition on the prefabricated body with the BN interface layer prepared in the step 2; forming a single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate;
step 4, depositing B 4 C base
Monolayer two prepared in step 3Deposition B on Vickers silicon carbide/silicon carbide composite material blank flat plate 4 C, a substrate;
step 5, semi-finishing
For the deposition of B in the step 4 4 C, performing semi-finishing on the blank of the base body to prepare a semi-finished nut blank with a threaded bottom hole in the center;
step 6, depositing the SiC matrix
Depositing a silicon carbide substrate on the semi-finished nut blank after semi-finishing to obtain a nut preform;
step 7, finish machining
Performing finish machining on the nut preform prepared in the step 6 to prepare threads; wherein, can select the mode preparation screw thread that adopts diamond tap tapping, the screw tap rotational speed: 50-100 r/min, wherein the feed quantity of the screw tap is = rotating speed multiplied by screw pitch;
step 8, depositing the SiC coating
And 7, depositing the silicon carbide anti-oxidation coating on the appearance of the nut subjected to finish machining in the step 7, wherein the deposition time is 40-60 hours, the deposition temperature is 800-1200 ℃, and the reaction gas is trichloromethyl silane, argon and/or hydrogen.
Further, in the step 1.3, the step of using the carbon fiber to pierce and sew the silicon carbide cloth after being vertically laminated specifically comprises: firstly, pressing a multilayer silicon carbide cloth lamination layer by using a flat plate die which is subjected to high-temperature treatment and is provided with sewing holes, fixing by using an arch clamp, cutting off the silicon carbide cloth on the peripheral edge of the die after fixing, and reserving at least 2mm for serging during cutting; after cutting, sewing by adopting an in-situ sewing method, wherein the head of the carbon fiber is dipped in water during sewing, and one needle is arranged at each hole; and after the sewing is finished, the carbon fiber dipped with water at the head part is utilized to lock the silicon carbide cloth reserved with the lock edge.
Further, in the step 1.1, in the multilayer silicon carbide cloth laminated layer, the number N of layers of the silicon carbide cloth laminated layer should satisfy: n = h o H +4, wherein h 0 : represents the nut thickness; h: the single-layer thickness of the silicon carbide cloth is represented; h is a total of o And the digits of the/h calculation result are taken as integers after the decimal point is cut off.
Further, in the step 1.1, the relative rotation angle of the adjacent laminated silicon carbide cloths is 90 °, 60 °, 45 ° or 30 °.
Further, in the step 5, the plate blank prepared in the step 4 is semi-finished to form a semi-finished nut blank with a shape of a regular hexagon (but not limited to a regular hexagon) and a bottom hole in the center, wherein the bottom hole = nominal diameter-1.15 × pitch.
Further, the step 2 of depositing the BN interface layer specifically includes:
and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide laying plate preform by using an interface layer deposition furnace, wherein the vacuum degree of a furnace cavity before deposition is 200-320 Pa, the deposition temperature is 590-680 ℃, ammonia gas, boron trichloride gas and/or hydrogen gas are/is used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.5L/min, 0.1-0.2L/min argon gas is used as reaction protective gas for deposition, and the deposition time is 40-55 h, so that the plate-shaped or strip-shaped preform with the BN interface layer is obtained.
Further, the step 3 of depositing the SiC matrix is specifically:
depositing a silicon carbide substrate on the prefabricated body prepared in the step 2 by a CVI deposition furnace, wherein the deposition temperature is 800-1200 ℃, the vacuum degree is less than 600-1000Pa, argon with the flow rate of 0.2-0.5L/min is used as reaction protective gas, and H with the flow rate of 0.25-0.5L/min is used as H 2 The trichloromethylsilane is used as carrier gas and is sent into a deposition furnace to react with hydrogen, the deposition time is 40 to 60 hours, and a silicon carbide substrate is generated.
Further, the step 4 deposits B 4 The matrix C is specifically:
deposition of SiC/B on bar stock blanks by CVI deposition furnace 4 And C, a substrate, wherein the vacuum degree of a furnace chamber before deposition is 200Pa-550Pa, the deposition temperature is 750-850 ℃, trichloromethylsilane, methane, boron trichloride gas and/or hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.2-0.7L/min, 0.4-1.2L/min argon gas is used as reaction protective gas, and the deposition time is 60-85 h.
Further, the step 6 of depositing the SiC matrix is specifically: and (5) placing the semi-finished nut blank prepared in the step (5) in a CVI deposition furnace, and depositing a silicon carbide substrate for 42-50h at 850-1100 ℃ under the reaction gas of trichloromethylsilane, argon and hydrogen.
Further, the step 8 of depositing the SiC coating is specifically: and (3) placing the nut prepared in the step (7) in a CVI deposition furnace, and depositing a silicon carbide substrate on the finished nut after finish machining, wherein the deposition time is 45-60h, the deposition temperature is 900-1200 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
The beneficial effects of the invention are:
1. the blank of the plate has high density uniformity and the tensile strength of the nut is high;
the prefabricated body for processing the nut is formed by overlapping a plurality of layers of two-dimensional silicon carbide/silicon carbide cloth, so that the density of each part can be kept consistent when a SiC matrix is deposited, and finally a composite material blank flat plate with uniform density is obtained; meanwhile, siC/B is adopted in the nut deposition process in the invention 4 The C matrix can further improve the density uniformity of the nut blank; meanwhile, compared with the existing preparation method of the three-dimensional needling composite material nut, the tensile strength of the nut is obviously improved by adopting the preparation method of the silicon carbide/silicon carbide composite material nut.
2. The invention has short production period and is suitable for industrial production;
compared with the prior art, the two-dimensional silicon carbide/silicon carbide composite material blank flat plate has the advantages that when a silicon carbide substrate is deposited by using a chemical vapor deposition method, the density is more uniform, the densification period is shortened, the blank flat plate is formed by laminating silicon carbide cloth woven by silicon carbide fibers, the nut blank deposition period is obviously shortened, the production cost is reduced, the problem that the technical difficulty of weaving a thick-size three-dimensional prefabricated body by using the silicon carbide fibers is high is solved, and the two-dimensional silicon carbide/silicon carbide composite material blank flat plate is suitable for industrial application.
3. Compared with the existing technology for preparing the ceramic matrix composite nut by the CVI, the material matrix prepared by the conventional CVI technology is difficult to avoid micropores in the deposition generation process, the surface open porosity of the ceramic matrix composite prepared by the CVI is 10-15%, and the nut deposition process in the inventionProposed SiC/B 4 The technological process can raise the thermal oxidation life of ceramic base composite material obviously, and the self-healing components of BC, siB, si-B-C, etc. are made to react with corrosive oxidizing medium in environment to produce B 2 O 3 、SiO 2 、B 2 O 3 +SiO 2 When the glass packing phase and a small amount of high-viscosity liquid phase are used, the oxidizing medium is consumed and invaded in situ to pack the microcracks and holes of the material, so that the corrosive oxidizing medium is prevented from entering the material, and the long-life self-healing is realized.
4. The invention provides the technological parameters for the thread processing of the ceramic matrix composite nut, and is more suitable for the preparation of the nuts of various specifications of the ceramic matrix composite.
The traditional three-dimensional needling preform nut is difficult to prepare a large-size nut due to the limitation of the vapor deposition and permeation thickness of the preform.
Drawings
FIG. 1 is a flow chart of the production process of the present invention;
FIG. 2 is a schematic structural view of a two-dimensional silicon carbide/silicon carbide laminate slab preform;
FIG. 3 is a schematic view of a silicon carbide fiber cloth layup;
fig. 4 is an isometric view of an M8 nut made by the method of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, specific embodiments accompanied with figures are described in detail below, and it is apparent that the described embodiments are a part of the embodiments of the present invention, not all of the 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, shall fall within the protection scope of the present invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Furthermore, the present invention is described in detail with reference to the drawings, and in the detailed description of the embodiments of the present invention, the drawings are only examples for convenience of illustration, and should not be construed as limiting the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in the actual fabrication.
Example 1
With reference to fig. 1, in this embodiment, an M8 two-dimensional silicon carbide/silicon carbide composite flat plate with a thickness of 8mm is prepared through the following steps 1 to 8, and various connecting members, such as nuts in this embodiment, may be processed by using the plate material, and of course, other connecting members may also be processed:
step 1, preparing a two-dimensional silicon carbide/silicon carbide layer plate material prefabricated body;
the multilayer silicon carbide cloth is laminated to the designed thickness, as shown in figure 2, the designed thickness is equal to the thickness of the nut, 0.5mm of machining allowance is reserved on each single side, T300-3K carbon fibers are used for being perpendicular to the silicon carbide cloth for puncture sewing, and a metal flat plate tool is used for assisting in flattening before sewing, so that the silicon carbide cloth is guaranteed to be free of wrinkles. Wherein, the thickness of the silicon carbide cloth layer is =8/0.25+4=36 layers (0.25 is the thickness of single-layer silicon carbide cloth), the silicon carbide cloth is cut according to the size of the needed prefabricated body, the edge of the cloth and the fiber layer direction of the silicon carbide cloth form a =0 degree or 90 degrees, and the cutting quantity is 36; and laying the cut cloth layer by layer, and then forming and sewing the cloth by using a mould to form the required prefabricated body.
Step 2, depositing a BN interface layer;
and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide layer plate preform by using an interface layer deposition furnace, wherein the vacuum degree of a furnace chamber before deposition is 240Pa, the deposition temperature is 600 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.35L/min, 0.15L/min argon gas is used as reaction protective gas, and the deposition time is 45h, so that the plate-shaped or strip-shaped preform with the BN interface layer is obtained.
Step 3, depositing a SiC matrix;
depositing a silicon carbide substrate on the prefabricated body prepared in the step 2 through a CVI deposition furnace, wherein the deposition temperature is 860 ℃, the vacuum degree is 800Pa, argon gas of 0.30L/min is used as reaction protective gas, and H with the flow rate of 0.45L/min 2 And (3) as a carrier gas, delivering trichloromethylsilane into a deposition furnace to react with hydrogen for 60 hours to generate a silicon carbide substrate.
Step 4, depositing B 4 C；
Deposition of B on the blank by a CVI deposition furnace 4 And C, the vacuum degree of a deposition forehearth is less than 450Pa, the deposition temperature is 950 ℃, trichloromethyl silane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.4L/min, 0.6L/min argon is used as reaction protection gas, and the deposition time is 80h.
Step 5, semi-finishing the shape and the threaded bottom hole of the nut;
and (3) processing the blank flat plate prepared in the multi-layer step (4) into a 8mm thick plate, wherein the thickness of the processed plate is 8mm of the thickness of the required M8 nut, then processing the shape and the threaded bottom hole of the nut according to the size requirement of the required nut, wherein the diameter of the bottom hole is required to be 6.5mm, the verticality requirement between the bottom hole and the end surface of the nut is not more than 0.1, and the thickness of the blank flat plate is 0.5-1 mm greater than the thickness of the finished nut product.
Step 6, depositing a SiC matrix;
and (3) placing the nut blank prepared in the step (5) in a CVI deposition furnace, and depositing a silicon carbide substrate on the nut semi-finished product after the semi-finishing, wherein the deposition time is 50h, the deposition temperature is 1100 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
Step 7, fine processing;
preparing M8 threads on the nut preform prepared in the step 6 through a thread tapping machine, wherein the rotating speed of a screw tap is as follows: 60r/min, the screw tap feed rate is 75mm/r, and then the step 8 is executed.
Step 8, depositing a SiC matrix;
and (4) placing the nut prepared in the step (7) in a CVI deposition furnace, and depositing a silicon carbide substrate on the finished nut after finish machining, wherein the deposition time is 60 hours, the deposition temperature is 1200 ℃, and the reaction gas is trichloromethyl silane, argon and hydrogen.
The ceramic matrix composite nut is usually matched with a screw for use, and CVI deposition rivet welding is carried out after the nut and the screw are installed, so that the ceramic matrix composite nut currently takes 'screw thread pull-off' as a performance judgment standard, the nut to be tested is matched with the screw in a screwing manner, and after the 'rivet welding' is deposited, the performance of the threaded connection part of the nut is tested by axially stretching the screw. In the M8 nut screw thread pull-off test prepared in the embodiment, the failure strength of the nut screw thread is 162.4MPa.
Example 2
With reference to fig. 1, in this embodiment, an M6 two-dimensional silicon carbide/silicon carbide composite flat plate with a thickness of 6mm is prepared through the following steps 1 to 8, and various connecting members, such as nuts in this embodiment, may be processed by using the plate material, and of course, other connecting members may also be processed:
step 1, preparing a two-dimensional silicon carbide/silicon carbide layering plate material prefabricated body;
the multilayer silicon carbide cloth is laminated to the designed thickness, 1-2 layers of fiber cloth processing allowance are reserved on the single side of the designed thickness equal to the thickness of the nut, T300-1K/3K carbon fibers are used for being perpendicular to the silicon carbide cloth for puncture sewing, and a metal flat plate tool is used for assisting in flattening before sewing, so that the silicon carbide cloth is guaranteed to be free of wrinkles. In the embodiment, the laying angle of each layer of silicon carbide cloth is specially limited, the fiber directions of each layer of the laid layer are different by a =45 degrees, and the layers are alternately laid.
Silicon carbide cloth layer thickness =6/0.25+4=28 layers (0.25 is single-layer silicon carbide cloth thickness)
Alternately laying the cut cloth during laying, and forming a required prefabricated body after shaping and sewing by using a mould, namely step 2, depositing a BN interface layer;
and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide layer plate preform by using an interface layer deposition furnace, wherein the vacuum degree of a furnace chamber before deposition is 300Pa, the deposition temperature is 670 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1L/min, 0.12L/min argon gas is used as reaction protective gas, and the deposition time is 52 hours, so that the plate-shaped or strip-shaped preform with the BN interface layer is obtained.
Step 3, depositing a SiC matrix;
and (3) depositing a silicon carbide substrate on the preform prepared in the step (2) through a CVI deposition furnace, wherein the deposition temperature is 1100 ℃, the vacuum degree is 900Pa, argon gas of 0.35L/min is used as reaction protective gas, H2 with the flow rate of 0.40L/min is used as carrier gas, trichloromethyl silane is fed into the deposition furnace to react with hydrogen, and the deposition time is 50H, so that the silicon carbide substrate is generated.
Step 4, depositing B4C;
B4C is deposited on the blank through a CVI deposition furnace, the vacuum degree of a furnace cavity before deposition is 400Pa, the deposition temperature is 800 ℃, trichloromethylsilane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.5L/min, 0.5L/min argon is used as reaction protective gas, and the deposition time is 70 hours.
Step 5, semi-finishing the shape and the threaded bottom hole of the nut;
processing the blank flat plate prepared in the multilayer step 3 into a 6mm thick plate, wherein the thickness of the processed plate is 6mm of the thickness of the required M6 nut, and then processing the shape of the nut and the threaded bottom hole according to the size requirement of the required nut, wherein the diameter of the bottom hole is required: 4.85mm, the requirement of the verticality of the bottom hole and the end surface of the nut is as follows: less than or equal to 0.1, and the designed thickness of the plate is larger than that of the nut. The thickness of the blank flat plate is 0.5-1 mm greater than the thickness of the finished nut product.
Step 6, depositing a SiC matrix;
and (3) placing the nut blank prepared in the step (5) in a CVI deposition furnace, and depositing a silicon carbide substrate on the nut semi-finished product after the semi-finishing, wherein the deposition time is 50h, the deposition temperature is 1100 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
Step 7, fine machining;
preparing M6 threads on the nut preform prepared in the step 6 through a thread tapping machine, wherein the rotating speed of a screw tap is as follows: 50r/min, the screw tap feed rate is 50mm/r, and then the step 8 is executed.
Step 8, depositing a SiC matrix;
and (3) placing the nut prepared in the step (7) in a CVI deposition furnace, and depositing a silicon carbide substrate on the finished nut after finish machining, wherein the deposition time is 50 hours, the deposition temperature is 1100 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
In the M6 nut screw thread pull-off test prepared in the embodiment, the failure strength of the nut screw thread is 151.2MPa.
Example 3
With reference to fig. 1, in this embodiment, an M8 two-dimensional silicon carbide/silicon carbide composite flat plate with a thickness of 6mm is prepared through the following steps 1 to 8, and various connecting members, such as an M8 nut in this embodiment, may be processed by using the plate material, and of course, other connecting members may also be processed:
step 1, preparing a two-dimensional silicon carbide/silicon carbide layer plate material prefabricated body;
the multilayer silicon carbide cloth is laminated to the designed thickness, 1-2 layers of fiber cloth processing allowance are reserved on the single surface of the designed thickness equal to the thickness of the nut, T300-1K/3K carbon fibers are perpendicular to the silicon carbide cloth for puncture sewing, a metal flat plate tool is used for assisting in flattening before sewing, and the silicon carbide cloth is guaranteed to be free of wrinkles. In the embodiment, the laying angle of each layer of silicon carbide cloth is specially limited, the fiber directions of each layer of the silicon carbide cloth are different by a =30 degrees, and the silicon carbide cloth is alternately layered.
Silicon carbide cloth layer thickness =6/0.25+4=28 layers (0.25 is single-layer silicon carbide cloth thickness)
Alternately laying the cut cloth during laying, and forming a required prefabricated body after shaping and sewing by using a mould, namely step 2, depositing a BN interface layer;
and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide layering plate preform by using an interface layer deposition furnace, wherein the vacuum degree of a furnace chamber before deposition is 300Pa, the deposition temperature is 670 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1L/min, 0.12L/min argon gas is used as reaction protective gas for assistance, and the deposition time is 52h, so that the plate-shaped or strip-shaped preform with the BN interface layer is obtained.
Step 3, depositing a SiC matrix;
and (3) depositing a silicon carbide substrate on the preform prepared in the step (2) through a CVI deposition furnace, wherein the deposition temperature is 950 ℃, the vacuum degree is 900Pa, argon gas of 0.35L/min is used as reaction protective gas, H2 with the flow rate of 0.40L/min is used as carrier gas, trichloromethyl silane is fed into the deposition furnace to react with hydrogen, and the deposition time is 45 hours, so that the silicon carbide substrate is generated.
Step 4, depositing B4C;
B4C is deposited on the blank through a CVI deposition furnace, the vacuum degree of a furnace cavity before deposition is 400Pa, the deposition temperature is 800 ℃, trichloromethyl silane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.5L/min, 0.5L/min argon is used as reaction protective gas, and the deposition time is 70h.
Step 5, semi-finishing the shape and the threaded bottom hole of the nut;
processing the blank flat plate prepared in the multilayer step 3 into a 6mm thick plate, wherein the thickness of the processed plate is 6mm of the thickness of the required M8 nut, and then processing the shape and the threaded bottom hole of the nut according to the size requirement of the required nut, wherein the diameter of the bottom hole is required: 6.5mm, the straightness requirement that hangs down of bottom outlet and nut terminal surface: less than or equal to 0.1, and the thickness of the blank flat plate is 0.5-1 mm greater than the thickness of the finished nut product.
Step 6, depositing a SiC matrix;
and (3) placing the nut blank prepared in the step (5) in a CVI deposition furnace, and depositing a silicon carbide substrate on the semi-finished nut after the semi-finishing, wherein the deposition time is 42h, the deposition temperature is 850 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
Step 7, fine machining;
preparing M6 threads on the nut preform prepared in the step 6 through a thread tapping machine, wherein the rotating speed of a screw tap is as follows: 60r/min, the screw tap feed rate is 75mm/r, and then the step 8 is executed.
Step 8, depositing a SiC matrix;
and (3) placing the nut prepared in the step (7) in a CVI deposition furnace, and depositing a silicon carbide substrate on the finished nut after finish machining, wherein the deposition time is 45 hours, the deposition temperature is 900 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
In the M8 nut screw thread pull-off test prepared in the embodiment, the nut thread failure strength is 154.3MPa.
Example 4
With reference to fig. 1, in this embodiment, an M10 two-dimensional silicon carbide/silicon carbide composite flat plate with a thickness of 10mm is prepared through the following steps 1 to 8, and various connecting members, such as nuts in this embodiment, can be processed by using the plate, and of course, other connecting members can also be processed:
step 1, preparing a two-dimensional silicon carbide/silicon carbide layer plate material prefabricated body;
the multilayer silicon carbide cloth is laminated to the designed thickness, 1-2 layers of fiber cloth processing allowance are reserved on the single surface of the designed thickness equal to the thickness of the nut, T300-1K/3K carbon fibers are perpendicular to the silicon carbide cloth for puncture sewing, a metal flat plate tool is used for assisting in flattening before sewing, and the silicon carbide cloth is guaranteed to be free of wrinkles. In the embodiment, the laying angle of each layer of silicon carbide cloth is specially limited, the fiber directions of each layer of the laid layer are different by a =30 degrees, and the layers are alternately laid.
Silicon carbide cloth layer thickness =10/0.25+4=44 layers (0.25 is single-layer silicon carbide cloth thickness)
Alternately laying the cut cloth during laying, and forming a required prefabricated body after shaping and sewing by using a mould, namely step 2, depositing a BN interface layer;
and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide layer plate preform by using an interface layer deposition furnace, wherein the vacuum degree of a furnace chamber before deposition is 300Pa, the deposition temperature is 670 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1L/min, 0.12L/min argon gas is used as reaction protective gas, and the deposition time is 52 hours, so that the plate-shaped or strip-shaped preform with the BN interface layer is obtained.
Step 3, depositing a SiC matrix;
and (3) depositing a silicon carbide substrate on the prefabricated body prepared in the step (2) through a CVI deposition furnace, wherein the deposition temperature is 1000 ℃, the vacuum degree is 900Pa, argon gas of 0.35L/min is used as reaction protective gas, H2 with the flow rate of 0.40L/min is used as carrier gas, trichloromethylsilane is fed into the deposition furnace to react with hydrogen, and the deposition time is 60 hours, so that the silicon carbide substrate is generated.
Step 4, depositing B4C;
B4C is deposited on the blank through a CVI deposition furnace, the vacuum degree of a furnace cavity before deposition is 400Pa, the deposition temperature is 850 ℃, trichloromethylsilane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.5L/min, 0.5L/min argon is used as reaction protective gas, and the deposition time is 60 hours.
Step 5, semi-finishing the shape and the threaded bottom hole of the nut;
processing the blank flat plate prepared in the multilayer step 3 into a 10mm thick plate, wherein the thickness of the processed plate is 10mm of the thickness of the required M10 nut, and then processing the shape of the nut and the threaded bottom hole according to the size requirement of the required nut, wherein the diameter of the bottom hole is required: 8.3mm, the straightness requirement that hangs down of bottom outlet and nut terminal surface: less than or equal to 0.1, and the thickness of the blank flat plate is 0.5-1 mm greater than the thickness of the finished nut product.
Step 6, depositing a SiC matrix;
and (3) placing the nut blank prepared in the step (5) in a CVI deposition furnace, and depositing a silicon carbide substrate on the nut semi-finished product after the semi-finishing, wherein the deposition time is 50h, the deposition temperature is 950 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
Step 7, fine processing;
preparing M10 threads on the nut preform prepared in the step 6 by using a thread tapping machine, wherein the rotating speed of a screw tap is as follows: 70r/min, the screw tap feed rate is 105mm/r, and then the step 8 is executed.
Step 8, depositing a SiC matrix;
and (4) placing the nut prepared in the step (7) in a CVI deposition furnace, and depositing a silicon carbide substrate on the finished nut after finish machining, wherein the deposition time is 50 hours, the deposition temperature is 960 ℃, and the reaction gas is trichloromethyl silane, argon and hydrogen.
In the M10 nut screw thread pull-off test prepared in the embodiment, the nut thread failure strength is 170.5MPa.
Example 5
With reference to fig. 1, in this embodiment, an M12 two-dimensional silicon carbide/silicon carbide composite flat plate with a thickness of 12mm is prepared through the following steps 1 to 8, and various connecting members, such as nuts in this embodiment, may be processed by using the plate, and of course, other connecting members may also be processed:
step 1, preparing a two-dimensional silicon carbide/silicon carbide layer plate material prefabricated body;
the multilayer silicon carbide cloth is laminated to the designed thickness, 1-2 layers of fiber cloth processing allowance are reserved on the single surface of the designed thickness equal to the thickness of the nut, T300-1K/3K carbon fibers are perpendicular to the silicon carbide cloth for puncture sewing, a metal flat plate tool is used for assisting in flattening before sewing, and the silicon carbide cloth is guaranteed to be free of wrinkles. In the embodiment, the laying angle of each layer of silicon carbide cloth is specially limited, the fiber directions of each layer of the laid layer are different by a =30 degrees, and the layers are alternately laid.
Silicon carbide cloth layer thickness =12/0.25+4=52 layers (0.25 is single-layer silicon carbide cloth thickness)
Alternately laying the cut cloth during layering, and forming a required prefabricated body after shaping and sewing by using a mould, namely step 2, depositing a BN interface layer;
and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide layering plate preform by using an interface layer deposition furnace, wherein the vacuum degree of a furnace chamber before deposition is 300Pa, the deposition temperature is 700 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1L/min, 0.12L/min argon gas is used as reaction protective gas for assistance, and the deposition time is 56h, so that the plate-shaped or strip-shaped preform with the BN interface layer is obtained.
Step 3, depositing a SiC matrix;
and (3) depositing a silicon carbide substrate on the prefabricated body prepared in the step (2) through a CVI (chemical vapor infiltration) deposition furnace, wherein the deposition temperature is 1050 ℃, the vacuum degree is 900Pa, argon gas of 0.35L/min is used as reaction protective gas, H2 with the flow rate of 0.40L/min is used as carrier gas, trichloromethyl silane is fed into the deposition furnace to react with hydrogen, and the deposition time is 63H, so that the silicon carbide substrate is generated.
Step 4, depositing B4C;
depositing B4C on the blank by a CVI deposition furnace, wherein the vacuum degree of a furnace cavity before deposition is 400Pa, the deposition temperature is 880 ℃, trichloromethylsilane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.5L/min, 0.5L/min argon is used as reaction protective gas, and the deposition time is 63 hours.
Step 5, finish machining the shape and the threaded bottom hole of the nut;
processing the blank flat plate prepared in the multilayer step 3 into a 12mm thick plate, wherein the thickness of the processed plate is 12mm of the thickness of the required M12 nut, and then processing the shape of the nut and the threaded bottom hole according to the size requirement of the required nut, wherein the diameter requirement of the bottom hole is as follows: 10mm, the verticality requirement of the bottom hole and the end surface of the nut is as follows: less than or equal to 0.1, and the thickness of the blank flat plate is 0.5-1 mm greater than the thickness of the finished nut product.
Step 6, depositing a SiC matrix;
and (5) placing the nut blank prepared in the step (5) in a CVI deposition furnace, and depositing a silicon carbide substrate on the nut semi-finished product after the semi-finishing, wherein the deposition time is 50h, the deposition temperature is 1000 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
Step 7, fine machining;
preparing M12 threads on the nut preform prepared in the step 6 by using a thread tapping machine, wherein the rotating speed of a screw tap is as follows: 80r/min, the screw tap feeding amount is 140mm/r, and then the step 7 is executed.
Step 8, depositing a SiC matrix;
and (4) placing the nut prepared in the step (7) in a CVI deposition furnace, and depositing a silicon carbide substrate on the finished nut after finish machining, wherein the deposition time is 55 hours, the deposition temperature is 1000 ℃, and the reaction gas is trichloromethyl silane, argon and hydrogen.
In the M12 nut screw thread pull-off test prepared in the embodiment, the nut thread failure strength is 182.3MPa.
Claims (10)
1. A preparation method of a two-dimensional silicon carbide/silicon carbide composite material nut is characterized by comprising the following steps:
step 1, preparation of two-dimensional silicon carbide/silicon carbide layering plate preform
Step 1.1, laminating a plurality of layers of silicon carbide cloth, wherein the included angle between each layer of silicon carbide cloth is a right angle or an acute angle;
step 1.2, laminating multiple layers of silicon carbide cloth to a designed thickness, wherein the designed thickness is the thickness of the nut plus 0.5 mm-1 mm;
step 1.3, puncturing and sewing the laminated silicon carbide cloth by using carbon fibers;
step 2, depositing a BN interface layer
Carrying out BN interface layer deposition on the two-dimensional silicon carbide/silicon carbide layering plate preform prepared in the step 1 to obtain a preform with a BN interface layer;
step 3, depositing SiC matrix
Carrying out silicon carbide matrix deposition on the prefabricated body with the BN interface layer prepared in the step 2; forming a single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate;
step 4, depositing B 4 C base
Depositing B on the single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate prepared in the step 3 4 A C substrate;
step 5, semi-finishing
For the deposition of B in the step 4 4 C, performing semi-finishing on the blank of the base body to manufacture a semi-finished nut blank with a threaded bottom hole in the center;
step 6, depositing the SiC matrix
Depositing a silicon carbide substrate on the semi-finished nut blank after semi-finishing to obtain a nut preform;
step 7, finish machining
Performing finish machining on the nut preform prepared in the step 6 to prepare threads;
step 8, depositing the SiC coating
And 7, depositing a silicon carbide anti-oxidation coating on the appearance of the nut subjected to finish machining in the step 7, wherein the deposition time is 40-60 h, the deposition temperature is 800-1200 ℃, and the reaction gas is trichloromethylsilane, argon and/or hydrogen.
2. The method for preparing the two-dimensional silicon carbide/silicon carbide composite material nut according to claim 1 is characterized in that: in the step 1.3, the carbon fiber vertical to the silicon carbide cloth after lamination is used for puncture sewing, which specifically comprises the following steps:
firstly, pressing a multilayer silicon carbide cloth lamination layer by using a flat plate die which is subjected to high-temperature treatment and is provided with sewing holes, fixing by using an arch clamp, cutting off the silicon carbide cloth on the peripheral edge of the die after fixing, and reserving at least 2mm for serging during cutting;
after cutting, sewing by adopting an in-situ sewing method, wherein the head of the carbon fiber is dipped in water during sewing, and one needle is arranged at each hole;
and after the sewing is finished, the carbon fiber dipped with water at the head part is utilized to lock the silicon carbide cloth reserved with the lock edge.
3. The method for preparing the two-dimensional silicon carbide/silicon carbide composite material nut according to claim 1, which is characterized in that: in the step 1.1, in the multiple silicon carbide cloth laminated layers, the number N of the silicon carbide cloth laminated layers should satisfy: n = h o H +4, wherein h 0 : represents the nut thickness; h: the single-layer thickness of the silicon carbide cloth is represented; h is o And the digits of the/h calculation result are taken as integers after decimal points are cut off.
4. A method for preparing a two-dimensional silicon carbide/silicon carbide composite nut as claimed in any one of claims 1 to 3, wherein in step 1.1, the relative rotation angle of the adjacent laminated silicon carbide cloths is 90 °, 60 °, 45 ° or 30 °.
5. The method for preparing the two-dimensional silicon carbide/silicon carbide composite material nut according to claim 4 is characterized in that: in the step 5, the bottom hole of the semi-finished nut blank with the threaded bottom hole in the center is a through hole, and the diameter of the bottom hole = nominal diameter-1.15 × thread pitch.
6. The method for preparing the two-dimensional silicon carbide/silicon carbide composite material nut according to claim 5 is characterized in that: the step 2 of depositing the BN interface layer is specifically as follows:
and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide layer plate preform by using an interface layer deposition furnace, wherein the vacuum degree of a furnace cavity before deposition is 200 Pa-320 Pa, the deposition temperature is 590-680 ℃, ammonia gas, boron trichloride gas and/or hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.5L/min, 0.1-0.2L/min argon gas is used as reaction protective gas for assistance, and the deposition time is 40-55 h, so that the plate-shaped or strip-shaped preform with the BN interface layer is obtained.
7. The method for preparing the two-dimensional silicon carbide/silicon carbide composite material nut according to claim 6 is characterized in that: the step 3 of depositing the SiC matrix is specifically as follows:
depositing a silicon carbide substrate on the prefabricated body prepared in the step 2 through a CVI deposition furnace, wherein the deposition temperature is 800-1200 ℃, the vacuum degree is less than 600-1000Pa, argon with the flow rate of 0.2L/min-0.5L/min is used as reaction protective gas, and H with the flow rate of 0.25L/min-0.5L/min is used as H 2 Trichloromethylsilane is used as carrier gas and is fed into a deposition furnace to react with hydrogen for 40-60 h to generate the silicon carbide substrate.
8. The method for preparing the two-dimensional silicon carbide/silicon carbide composite nut according to claim 7 is characterized in that: step 4 deposit B 4 The C matrix is specifically:
deposition of B on bar stock blanks by means of a CVI deposition furnace 4 And C, a substrate, wherein the vacuum degree of a furnace chamber before deposition is 200Pa-550Pa, the deposition temperature is 750-850 ℃, trichloromethylsilane, methane, boron trichloride gas and/or hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.2-0.7L/min, 0.4-1.2L/min argon gas is used as reaction protective gas, and the deposition time is 60-85 h.
9. The method for preparing the two-dimensional silicon carbide/silicon carbide composite nut according to claim 8 is characterized in that: the step 6 of depositing the SiC matrix is specifically as follows: and (3) placing the semi-finished nut blank prepared in the step (5) in a CVI deposition furnace, and depositing the silicon carbide substrate for 42-50h at 850-1100 ℃ under the reaction gas of trichloromethylsilane, argon and hydrogen.
10. The method for preparing the two-dimensional silicon carbide/silicon carbide composite material nut according to claim 9, which is characterized in that: the step 8 of depositing the SiC coating specifically comprises the following steps: and (3) placing the nut prepared in the step (7) in a CVI deposition furnace, and depositing a silicon carbide substrate on the finished nut after finish machining, wherein the deposition time is 45-60h, the deposition temperature is 900-1200 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210713475.XA CN115160005A (en) | 2022-06-22 | 2022-06-22 | Preparation method of two-dimensional silicon carbide/silicon carbide composite material nut |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210713475.XA CN115160005A (en) | 2022-06-22 | 2022-06-22 | Preparation method of two-dimensional silicon carbide/silicon carbide composite material nut |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115160005A true CN115160005A (en) | 2022-10-11 |
Family
ID=83486878
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210713475.XA Pending CN115160005A (en) | 2022-06-22 | 2022-06-22 | Preparation method of two-dimensional silicon carbide/silicon carbide composite material nut |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115160005A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116334435A (en) * | 2023-02-17 | 2023-06-27 | 清华大学 | Silicon carbide aluminum-based composite material and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503305A (en) * | 2009-02-03 | 2009-08-12 | 西北工业大学 | Process for preparing self-sealing silicon carbide ceramic based composite material |
| CN106966738A (en) * | 2016-11-25 | 2017-07-21 | 北京航空航天大学 | Self-healing ceramic matric composite combustion chamber flame drum and preparation method and application |
| CN113816755A (en) * | 2021-10-14 | 2021-12-21 | 西安鑫垚陶瓷复合材料有限公司 | Two-dimensional silicon carbide/silicon carbide composite material bar and connecting piece preparation method |
-
2022
- 2022-06-22 CN CN202210713475.XA patent/CN115160005A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503305A (en) * | 2009-02-03 | 2009-08-12 | 西北工业大学 | Process for preparing self-sealing silicon carbide ceramic based composite material |
| CN106966738A (en) * | 2016-11-25 | 2017-07-21 | 北京航空航天大学 | Self-healing ceramic matric composite combustion chamber flame drum and preparation method and application |
| CN113816755A (en) * | 2021-10-14 | 2021-12-21 | 西安鑫垚陶瓷复合材料有限公司 | Two-dimensional silicon carbide/silicon carbide composite material bar and connecting piece preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 刘万辉主编: "《复合材料 第2版》", 哈尔滨工业大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116334435A (en) * | 2023-02-17 | 2023-06-27 | 清华大学 | Silicon carbide aluminum-based composite material and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113816755B (en) | Two-dimensional silicon carbide/silicon carbide composite bar and preparation method of connecting piece | |
| CN101830703B (en) | Carbon fiber reinforced boron carbide composite material and preparation method thereof | |
| CN115160005A (en) | Preparation method of two-dimensional silicon carbide/silicon carbide composite material nut | |
| CN103193497B (en) | Sticky product with silicon erosion resistance of carbon/carbon composite material and preparation method thereof | |
| US5654059A (en) | Fiber-reinforced carbon and graphite articles and method for the production thereof | |
| CN110129992B (en) | Carbon fiber paper for fuel cell and preparation method thereof | |
| CN107285796B (en) | Carbon-based composite material spiral spring and production method thereof | |
| CN113277867A (en) | Preparation method of carbon/silicon carbide composite material crucible | |
| WO2000061518A9 (en) | Chordal preforms for fiber-reinforced articles and method for the production thereof | |
| CN111875401B (en) | Preparation method of high-strength and high-purity carbon/carbon composite material revolving body formed by winding | |
| CN113603495A (en) | Method for preparing ceramic matrix composite bolt and pin based on long rod-shaped prefabricated body structure | |
| EP3768507A1 (en) | Method of making a fibrous preform and a fibrous preform thus obtained | |
| CN101798078B (en) | Quick carbon deposition method of carbon/carbon material member | |
| CN112553779A (en) | Production process of needled carbon crucible support | |
| US3629049A (en) | Shaped pyrolytic graphite articles | |
| CN114656271A (en) | Carbon-carbon crucible and preparation method thereof | |
| CN114407227B (en) | High-layer dense flat carbon fiber gradient suture preform and preparation method thereof | |
| CN115231940A (en) | Production process of carbon thermal insulation cylinder | |
| CN114645462A (en) | High-performance carbon fiber needling preform and preparation method thereof | |
| CN113999034A (en) | Preparation method of long-life carbon crucible side | |
| CN109627031B (en) | SiCw oriented high-toughness ceramic matrix composite and preparation method thereof | |
| CN116675548A (en) | Ceramic matrix composite bolt based on long rod-shaped preform structure | |
| CN114055865A (en) | Forming method of fiber preform of longitudinal corrugated heat shield made of ceramic matrix composite | |
| CN220952180U (en) | Braided crucible preform | |
| EP4183569A1 (en) | Method for making a fibrous preform of carbon and/or fibres of a carbon precursor of pre-set height and preform directly formed |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20221011 |