CN113816755A - Two-dimensional silicon carbide/silicon carbide composite material bar and connecting piece preparation method - Google Patents
Two-dimensional silicon carbide/silicon carbide composite material bar and connecting piece preparation method Download PDFInfo
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- CN113816755A CN113816755A CN202111198015.XA CN202111198015A CN113816755A CN 113816755 A CN113816755 A CN 113816755A CN 202111198015 A CN202111198015 A CN 202111198015A CN 113816755 A CN113816755 A CN 113816755A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 363
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 363
- 239000002131 composite material Substances 0.000 title claims abstract description 120
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000010410 layer Substances 0.000 claims abstract description 88
- 239000002356 single layer Substances 0.000 claims abstract description 32
- 238000012545 processing Methods 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 26
- 239000011159 matrix material Substances 0.000 claims abstract description 24
- 238000000151 deposition Methods 0.000 claims description 243
- 230000008021 deposition Effects 0.000 claims description 179
- 239000007789 gas Substances 0.000 claims description 122
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 82
- 238000000034 method Methods 0.000 claims description 54
- 229910052786 argon Inorganic materials 0.000 claims description 41
- 238000006243 chemical reaction Methods 0.000 claims description 37
- 230000001681 protective effect Effects 0.000 claims description 36
- 239000004744 fabric Substances 0.000 claims description 34
- 239000000463 material Substances 0.000 claims description 29
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 28
- 239000001257 hydrogen Substances 0.000 claims description 26
- 229910052739 hydrogen Inorganic materials 0.000 claims description 26
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 claims description 26
- 238000013461 design Methods 0.000 claims description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 21
- 230000003197 catalytic effect Effects 0.000 claims description 20
- 238000003754 machining Methods 0.000 claims description 20
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims description 20
- 238000009958 sewing Methods 0.000 claims description 19
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 15
- 239000004917 carbon fiber Substances 0.000 claims description 15
- 238000010030 laminating Methods 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 12
- 238000005520 cutting process Methods 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 239000012159 carrier gas Substances 0.000 claims description 10
- 230000003647 oxidation Effects 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- 239000011153 ceramic matrix composite Substances 0.000 claims description 9
- 150000002431 hydrogen Chemical class 0.000 claims description 8
- 238000003475 lamination Methods 0.000 claims description 7
- 230000003064 anti-oxidating effect Effects 0.000 claims description 6
- 239000012495 reaction gas Substances 0.000 claims description 6
- 238000009434 installation Methods 0.000 claims description 4
- WZDGZWOAQTVYBX-XOINTXKNSA-N tibolone Chemical compound C([C@@H]12)C[C@]3(C)[C@@](C#C)(O)CC[C@H]3[C@@H]1[C@H](C)CC1=C2CCC(=O)C1 WZDGZWOAQTVYBX-XOINTXKNSA-N 0.000 claims 1
- 238000005137 deposition process Methods 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 239000003963 antioxidant agent Substances 0.000 abstract description 2
- 230000003078 antioxidant effect Effects 0.000 abstract description 2
- 239000002184 metal Substances 0.000 description 5
- 230000001590 oxidative effect Effects 0.000 description 5
- 230000037303 wrinkles Effects 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003575 carbonaceous material 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
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000007514 turning Methods 0.000 description 1
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Abstract
The invention relates to a preparation method of a composite material fastener, in particular to a preparation method of a two-dimensional silicon carbide/silicon carbide composite material bar and a connecting piece, which are mainly applied to the connection assembly of ultrahigh-temperature, high-strength and antioxidant composite material products. The prefabricated body for processing the bar stock blank is formed by riveting a plurality of layers of two-dimensional silicon carbide/silicon carbide composite material blank flat plates, and the thickness of the single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate is largeIs positioned in the range of 3-6 mm, so that the density of each part can be kept consistent when the SiC matrix is deposited, and simultaneously, SiC/B is adopted in the deposition process of the bar blank4The C substrate can further improve the density uniformity of the bar blank; compared with the existing preparation method of the carbon/silicon carbide composite material bolt, the shear strength of the bolt is obviously improved to 240-320 MPa after the preparation method of the silicon carbide/silicon carbide composite material bolt is adopted.
Description
Technical Field
The invention relates to a preparation method of a composite material fastener, in particular to a preparation method of a two-dimensional silicon carbide/silicon carbide composite material bar and a connecting piece, which are mainly applied to the connection assembly of ultrahigh-temperature, high-strength and antioxidant composite material products.
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.
Because of the limitation of the current composite material weaving and forming process technology, the integral preparation of large-size, precise and complex product components is difficult to develop by using the ceramic matrix composite material. Therefore, in order to meet the requirements of higher service temperature and mechanical property of connecting pieces provided by aircrafts in the field of aerospace in the future, the development of the composite connecting piece with high performance and low cost has important significance for composite materials, particularly ceramic-based composite material engineering application.
The invention patent with the publication number of CN102775176B discloses a preparation method of a three-dimensional needle-punched carbon/silicon carbide composite material bolt. This three-dimensional needled carbon felt preform: the 12K T700 carbon fiber is made into a tire mesh, single-layer 0-degree laid cloth, single-layer tire mesh, single-layer 90-degree laid cloth and single-layer tire mesh are alternately and circularly superposed to the designed thickness, and then the single-layer 0-degree laid cloth, the single-layer tire mesh, the single-layer 90-degree laid cloth and the single-layer tire mesh are vertically penetrated into the space between the laid cloths in a relay needling mode along the thickness. And (5) processing the bolt into the required bolt size by supplementing a pyrolytic carbon interface layer and a silicon carbide substrate. The tensile strength of the bolt prepared by the method is about 180-200 MPa at room temperature, and the shear strength is about 80-100 MPa. However, the density of the bolts prepared by the preparation method is not uniform, so that the performance difference of the bolts in the same batch is large, and meanwhile, the preparation method is complex in process, long in production period and 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 caused by uneven density and the like of the conventional three-dimensional needled carbon/silicon carbide composite bolt, the invention provides a two-dimensional silicon carbide/silicon carbide composite bar and a preparation method of the connecting piece, wherein the room-temperature tensile strength of the two-dimensional silicon carbide/silicon carbide bolt is about 190-230 MPa, and the shear strength is improved to 240-320 MPa.
The technical scheme of the invention provides a preparation method of a two-dimensional silicon carbide/silicon carbide composite material connecting piece, which is characterized in that the connecting piece is a pin, and comprises the following steps:
step 1, preparing a two-dimensional silicon carbide/silicon carbide layer plate material prefabricated body;
step 1.1, laminating the layersLaminating the silicon carbide cloth to the designed thickness, and when the diameter of the pin is more than or equal to the designed thickness
When the design thickness is smaller than the diameter of the pin, the diameter of the pin is smaller than that of the pin
When the pin is used, the designed thickness is larger than the diameter xmm of the pin, so that the density uniformity of the final pin is improved conveniently;
step 1.2, using carbon fibers to be vertical to the silicon carbide cloth after lamination for puncture sewing;
step 2, depositing a BN interface layer;
placing the two-dimensional silicon carbide/silicon carbide layer plate preform prepared in the step 1 in an interface layer deposition furnace, and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide layer plate preform to obtain a preform with the BN interface layer;
step 3, depositing a SiC matrix;
placing the prefabricated body with the BN interface layer prepared in the step 2 in a CVI deposition furnace, and depositing a silicon carbide substrate on the prefabricated body with the BN interface layer; forming a single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate; the thickness of the single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate is more than 6 mm;
step 4, riveting, combining and processing a blank;
step 4.1, when the diameter of the pin is smaller than that of the pin
Cutting the blank flat plate preform prepared in the single-layer step 3 into strips along the shape length or width direction, and then processing the strips into a bar blank;
step 4.2, when the diameter of the pin is more than or equal to the diameter of the pin
Laminating a plurality of layers of blank plates prepared in the step 3 to a designed thickness, and riveting by using a two-dimensional silicon carbide/silicon carbide composite material pin with a smaller specification to obtain a riveting prefabricated body; on the upper partThe design thickness after lamination is larger than the diameter of the pin, so that a bar blank can be conveniently processed;
4.3, cutting the riveting prefabricated body prepared in the step 4.2 into strips along the shape length or width direction, and then processing a bar blank;
step 5, depositing SiC/B4C, a substrate;
placing the bar stock blank prepared in the step 4 in a CVI deposition furnace, and depositing SiC/B on the bar stock blank4The base C can obviously prolong the thermal oxidation life of the ceramic matrix composite;
step 6, fine machining;
finish machining the shape of the bar blank prepared in the step 5 to form a finished pin;
step 7, depositing a SiC coating;
and (3) placing the pin prepared in the step (6) in a CVI deposition furnace, and depositing a silicon carbide anti-oxidation coating on the appearance of the finished pin after finish machining, wherein the deposition time is 35-40 h, the deposition temperature is 850-950 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
Further, in order to ensure the deposition efficiency and economy of single prefabricated plate or strip, and improve the density uniformity of single plate or strip, the diameter of the pin in step 1.1 is more than or equal to that of the pin
And when the pin is used, the design thickness of the laying layer of the single two-dimensional silicon carbide/silicon carbide laying plate preform is more than or equal to one third of the diameter of the pin.
Further, in order to improve the riveting and thermal adaptation performance of the pin, in step 4.2, the two-dimensional silicon carbide/silicon carbide composite pin with the smaller specification is prepared by a two-dimensional silicon carbide/silicon carbide composite pin preparation method.
Further, in order to enhance the high-temperature mechanical property of the pin and improve the micro-crack bridging and plugging capability in the high-temperature service environment, step 5 is to deposit SiC/B4The specific process parameters of the C matrix are as follows: the vacuum degree of the furnace chamber is required to be less than 500Pa before deposition, the deposition temperature is 850-950 ℃, and trichloromethylsilane, methane and boron trichloride gas are usedThe hydrogen is used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.5-1L/min argon is used as reaction protective gas, and the deposition time is 60-80 h.
Furthermore, in order to meet the use requirements under the conditions of ultrahigh temperature and long service life and enable the material to resist a high-temperature oxidation stress environment for a long time, the deposition temperature is 900 ℃, the gas flow is 0.3L/min, 0.7L/min argon is used as a reaction protective gas for assistance, and the deposition time is 65 hours.
Further, the specific process parameters for depositing the BN interface layer in the step 2 are as follows: the vacuum degree of a furnace cavity before deposition is required to be less than 300Pa, the deposition temperature is 620-670 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.2-0.3L/min argon gas is used as reaction protective gas, and the deposition time is 35-40 h.
Further, the specific process parameters of the SiC matrix deposited in the step 3 are as follows: deposition temperature is 800-1000 ℃, vacuum degree is required to be less than 1000Pa, argon gas with the flow rate of 0.2L/min-0.5L/min is used as reaction protective gas, and H with the flow rate of 0.15L/min-0.4L/min is used2And (3) introducing trichloromethylsilane into a deposition furnace as carrier gas to react with hydrogen, wherein the deposition time is 40-60 h.
Further, in order to improve the deposition efficiency and economy and ensure the density uniformity of the pins, the diameter of the two-dimensional silicon carbide/silicon carbide composite material pins with smaller specifications for riveting is not more than
Further, in order to give consideration to mechanical properties and deposition uniformity of the finished pin, the small-size two-dimensional silicon carbide/silicon carbide composite pin for riveting is positioned as follows: the pin holes are uniformly distributed along the length direction of the bar stock, and the distance between the pin holes is not less than 8 mm.
Further, in the step 1.2, T300-3K carbon fibers are perpendicular to the silicon carbide cloth for puncture sewing, and a metal tool is used for assisting in flattening before sewing, so that the silicon carbide cloth is enabled not to have wrinkles; step 1.1 x equals 1.
The invention also provides a preparation method of the two-dimensional silicon carbide/silicon carbide composite material bar, which is characterized by comprising the following steps of:
step 1, preparing a two-dimensional silicon carbide/silicon carbide layer plate material prefabricated body;
step 1.1, laminating multiple layers of silicon carbide cloth to a designed thickness, and when the diameter of the bar stock is more than or equal to the designed thickness
When the design thickness of the plate is smaller than the diameter of the bar; when the diameter of the bar stock is smaller than
When the design thickness of the plate is larger than the diameter xmm of the bar stock, the density uniformity of the final bar stock is improved conveniently;
step 1.2, using carbon fibers to be vertical to the silicon carbide cloth after lamination for puncture sewing;
step 2, depositing a BN interface layer;
placing the two-dimensional silicon carbide/silicon carbide layer plate preform prepared in the step 1 in an interface layer deposition furnace, and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide layer plate preform to obtain a preform with the BN interface layer;
step 3, depositing a SiC matrix;
placing the prefabricated body with the BN interface layer prepared in the step 2 in a CVI deposition furnace, and depositing a silicon carbide substrate on the prefabricated body with the BN interface layer; forming a single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate; the thickness of the single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate is more than 6 mm;
step 4, riveting, combining and processing a blank;
step 4.1, when the diameter of the bar stock is smaller than that
Cutting and processing the blank flat plate prefabricated body prepared in the single-layer step 3 into a strip material along the shape length or width direction, and then processing the strip material into a bar material blank;
step 4.2, when the diameter of the bar stock is more than or equal to the diameter of the bar stock
Laminating a plurality of layers of blank plates prepared in the step 3 to a designed thickness, and riveting by using a two-dimensional silicon carbide/silicon carbide composite material pin with a smaller specification to obtain a riveting prefabricated body; the designed thickness is larger than the diameter of the bar stock, so that the bar stock is convenient to process;
4.3, cutting the riveting prefabricated body prepared in the step 4.2 into strips along the shape length or width direction, and then processing a bar blank;
step 5, depositing SiC/B4C, a substrate;
placing the bar stock blank prepared in the step 4 in a CVI deposition furnace, and depositing SiC/B on the bar stock blank4The base C can obviously prolong the thermal oxidation life of the ceramic matrix composite;
step 6, fine machining;
and (5) finishing the shape of the bar blank prepared in the step 5 to form a target bar.
Further, in order to ensure the deposition efficiency and economy of single prefabricated plate or strip, and improve the density uniformity of single plate or strip, step 1.1 is carried out when the diameter of the rod is greater than or equal to that of the rod
When the thickness of the layer of the single prefabricated body is more than or equal to one third of the diameter of the bar stock.
Further, in order to enhance the capability of blocking microcracks in a high-temperature service environment, the two-dimensional silicon carbide/silicon carbide composite pin with a smaller specification is prepared by the same preparation method of the two-dimensional silicon carbide/silicon carbide composite bar.
Further, in order to meet the use requirements under the conditions of ultrahigh temperature and long service life and enable the SiC/B to resist the high-temperature oxidation stress environment for a long time, step 5 is to deposit SiC/B4The specific process parameters of the C matrix are as follows: the vacuum degree of a furnace chamber before deposition is required to be less than 500Pa, the deposition temperature is 850-950 ℃, trichloromethyl silane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, and auxiliary materials are addedArgon gas of 0.5L/min-1L/min is used as reaction protective gas, and the deposition time is 60-80 h.
Furthermore, in order to generate a glass sealing phase by the rapid reaction of each micro structural unit of the composite material and the oxidizing medium when the oxidizing medium invades, the multi-layer sealing line of the fiber, the interface and the matrix is realized, the long-life self-healing is better realized, the deposition temperature is 900 ℃, the gas flow is 0.3L/min, 0.7L/min argon is used as a reaction protective gas, and the deposition time is 65 hours.
Further, the specific process parameters for depositing the BN interface layer in the step 2 are as follows: the vacuum degree of a furnace cavity before deposition is required to be less than 300Pa, the deposition temperature is 620-670 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.2-0.3L/min argon gas is used as reaction protective gas, and the deposition time is 35-40 h.
Further, the specific process parameters of the SiC matrix deposited in the step 3 are as follows: deposition temperature is 800-1000 ℃, vacuum degree is required to be less than 1000Pa, argon gas with the flow rate of 0.2L/min-0.5L/min is used as reaction protective gas, and H with the flow rate of 0.15L/min-0.4L/min is used2And (3) introducing trichloromethylsilane into a deposition furnace as carrier gas to react with hydrogen, wherein the deposition time is 40-60 h.
Further, in order to improve the deposition efficiency and economy and ensure the density uniformity of the bar stock, the diameter size of the two-dimensional silicon carbide/silicon carbide composite material pin for riveting is not more than
Further, in order to give consideration to the mechanical property and the deposition uniformity of the finished bar stock, the two-dimensional silicon carbide/silicon carbide composite material pin is positioned as follows: the pin holes are uniformly distributed along the length direction of the bar stock, and the distance between the pin holes is not less than 8 mm.
Further, in the step 1.2, T300-3K carbon fibers are perpendicular to the silicon carbide cloth for puncture sewing, and a metal tool is used for assisting in flattening before sewing, so that the silicon carbide cloth is enabled not to have wrinkles; step 1.1 x equals 1.
The invention also provides a preparation method of the two-dimensional silicon carbide/silicon carbide composite material connecting piece, which is characterized in that the connecting piece is a bolt and comprises the following steps:
step 1, preparing a two-dimensional silicon carbide/silicon carbide layer plate material prefabricated body;
step 1.1, laminating multiple layers of silicon carbide cloth to the designed thickness, and when the diameter of the bolt is more than or equal to the designed thickness
When the design thickness is smaller than the diameter of the bolt, the density uniformity of the final bar stock is improved conveniently, and when the diameter of the bolt is smaller than the diameter of the bolt
When the design thickness is larger than the diameter of the bolt by at least xmm;
step 1.2, using carbon fibers to be vertical to the silicon carbide cloth after lamination for puncture sewing;
step 2, depositing a BN interface layer;
placing the two-dimensional silicon carbide/silicon carbide layer plate preform prepared in the step 1 in an interface layer deposition furnace, and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide layer plate preform to obtain a preform with the BN interface layer;
step 3, depositing a SiC matrix;
placing the prefabricated body with the BN interface layer prepared in the step 2 in a CVI deposition furnace, and depositing a silicon carbide substrate on the prefabricated body with the BN interface layer; forming a single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate; the thickness of the single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate is more than 6 mm;
step 4, riveting, combining and processing a blank;
step 4.1, when the diameter of the bolt is smaller than
Cutting and processing the blank flat plate prefabricated body prepared in the single-layer step 3 into a strip material along the shape length or width direction, and then processing the strip material into a bar material blank;
step 4.2, when the diameter of the bolt is more than or equal to the diameter of the bolt
Laminating a plurality of layers of blank plates prepared in the step 3 to a designed thickness, and riveting by using a two-dimensional silicon carbide/silicon carbide composite material pin with a smaller specification to obtain a riveting prefabricated body; the design thickness is larger than the diameter of the bolt, so that bars can be conveniently processed;
4.3, cutting the prefabricated body prepared in the step 4.2 into strips along the shape length or width direction, and then processing a bar blank;
step 5, depositing SiC/B4C, a substrate;
placing the bar stock blank prepared in the step 4 in a CVI deposition furnace, and depositing SiC/B on the bar stock blank4The base C can obviously prolong the thermal oxidation life of the ceramic matrix composite;
step 6, fine machining;
finish machining the shape of the bar blank prepared in the step 5 to form a finished bolt;
step 7, depositing a SiC coating;
and (3) placing the finished bolt prepared in the step (6) in a CVI deposition furnace, and depositing a silicon carbide anti-oxidation coating on the appearance of the finished bolt after finish machining, wherein the deposition time is 35-40 h, the deposition temperature is 850-950 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
Further, in order to ensure the deposition efficiency and economy of single prefabricated body plate materials or strip materials and improve the density uniformity of the single prefabricated body plate materials or strip materials, the diameter of the bolt is more than or equal to that of the bolt in the step 1.1
And when the thickness of the single prefabricated body laying plate is more than or equal to one third of the diameter of the bar.
Further, in order to improve the high-temperature mechanical property of the pin and meet the requirement of microcrack closure under a high-temperature oxidation environment, namely, self-healing is realized, and step 5, SiC/B is deposited4The specific process parameters of the C matrix are as follows: the vacuum degree of the furnace chamber before deposition is required to be less than 500Pa, the deposition temperature is 850-950 ℃, and trichloromethylsilane, methane, boron trichloride gas and hydrogen are usedThe gas is used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.5-1L/min argon is used as reaction protective gas, and the deposition time is 60-80 h.
Furthermore, in order to meet the use requirements under the conditions of ultrahigh temperature and long service life and enable the material to resist a high-temperature oxidation stress environment for a long time, the deposition temperature is 900 ℃, the gas flow is 0.3L/min, 0.7L/min argon is used as a reaction protective gas for assistance, and the deposition time is 65 hours.
Further, the specific process parameters for depositing the BN interface layer in the step 2 are as follows: the vacuum degree of a furnace cavity before deposition is required to be less than 300Pa, the deposition temperature is 620-670 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.2-0.3L/min argon gas is used as reaction protective gas, and the deposition time is 35-40 h.
Further, the specific process parameters of the SiC matrix deposited in the step 3 are as follows: deposition temperature is 800-1000 ℃, vacuum degree is required to be less than 1000Pa, argon gas with the flow rate of 0.2L/min-0.5L/min is used as reaction protective gas, and H with the flow rate of 0.15L/min-0.4L/min is used2And (3) introducing trichloromethylsilane into a deposition furnace as carrier gas to react with hydrogen, wherein the deposition time is 40-60 h.
Further, in order to improve the deposition efficiency and economy and ensure the density uniformity of the bolt, the diameter size of the pin made of the two-dimensional silicon carbide/silicon carbide composite material is not more than
Further, in order to give consideration to mechanical properties and deposition uniformity of the finished bolt, the positions of the two-dimensional silicon carbide/silicon carbide composite pin are as follows: along bolt length direction equipartition, the pin hole interval is not less than 8mm, when for further improving bolt performance, can be close to or arrange the nut installation stirrup position with the riveting position.
Further, in the step 1.2, T300-3K carbon fibers are perpendicular to the silicon carbide cloth for puncture sewing, and before sewing, the silicon carbide cloth is flattened in an auxiliary mode through a metal tool, so that the silicon carbide cloth is enabled not to be wrinkled.
The invention has the beneficial effects that:
1. the blank of the bar stock has high density uniformity and high shearing strength of the bolt;
the prefabricated body for processing the bar blank is a single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate or is formed by riveting a plurality of layers of two-dimensional silicon carbide/silicon carbide composite material blank flat plates, and the thickness of the single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate is 3-6 mm, so that the density of each part can be kept consistent when a SiC matrix is deposited, and if riveting is carried out, the composite material blank flat plate with uniform density can be finally obtained; the composite material pin prepared by the same processing procedure is adopted to combine and rivet a plurality of layers of two-dimensional silicon carbide/silicon carbide composite material blank plates with uniform density, compared with a three-dimensional needling blank, the density uniformity of the blank is improved, and no obvious density gradient exists along the radial direction of a bolt or the pin; meanwhile, SiC/B is adopted in the deposition process of the bar blank in the invention4The C substrate can further improve the density uniformity of the bar blank; compared with the existing preparation method of the carbon/silicon carbide composite material bolt, the shear strength of the bolt is obviously improved to 240-320 MPa after the preparation method of the silicon carbide/silicon carbide composite material bolt is adopted.
2. The invention has short production period and is suitable for industrial production;
compared with the prior art, the single-layer two-dimensional silicon carbide/silicon carbide composite material blank has the advantages that the thickness of the flat plate wall is thin, when the silicon carbide substrate is deposited by using a chemical vapor deposition method, the density is more uniform, the densification period is also shortened, after the blank flat plate is combined and riveted, the bolt 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 silicon carbide fibers is high is solved, and the method is suitable for industrial application.
3. The silicon carbide/silicon carbide composite material pin is adopted to realize the riveting of blank plates, and the size specification of the pin is less than or equal to
The riveting position can be adjusted according to the installation position of the nut, so that the riveting part is close to or arranged at the nut installation stirrup part,the tensile strength of the bolt is further improved in a targeted manner;
4. compared with the existing technology for preparing the ceramic matrix composite bolt 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 SiC/B adopted in the bolt deposition process provided by the invention4The 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 used to react with corrosive oxidizing medium in environment to produce B2O3、SiO2、B2O3+SiO2When the glass sealing and filling phase and a small amount of high-viscosity liquid phase are used, the oxidizing medium is consumed and invaded in situ, the microcracks and holes of the material are sealed and filled, the corrosive oxidizing medium is prevented from entering the material, and the long-life self-healing is realized.
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 multi-layer two-dimensional silicon carbide/silicon carbide composite blank flat plate riveting;
FIG. 4 is a pictorial view of a M8 bolt prepared by the method of the present invention;
fig. 5 is an SEM photograph of the M8 bolt thread profile prepared 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 creative efforts based on the embodiments of 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
Referring to FIG. 1, this example prepares a two-dimensional silicon carbide/silicon carbide composite material by the following steps 1 to 6
Bar stock from which various connectors can be machined, such as the pin in this example and the bolt in example 2, although other connectors can be machined:
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 one third of the diameter of a bolt, 1mm of processing allowance is reserved in the thickness, T300-3K carbon fibers are used for being 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 this embodiment, the laying angle of each layer of silicon carbide cloth is not particularly limited, and may be, for example, a forward laying at 0 °/90 °, or an oblique laying at more than 0 ° and less than 90 °, or alternatively a forward laying and an oblique laying. In other embodiments, if a two-dimensional silicon carbide/silicon carbide composite is prepared
The designed thickness of the bar stock can be designed to be 6 mm.
Step 2, depositing a BN interface layer;
and (2) 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 270Pa, the deposition temperature is 630 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.25L/min, 0.25L/min argon gas is used as reaction protective gas for assistance, and the deposition time is 35h, so that the plate-shaped or strip-shaped preform with the BN interface layer is obtained. In other embodiments, the deposition process parameters may satisfy the following conditions: the vacuum degree of a furnace cavity before deposition is required to be less than 300Pa, the deposition temperature is 620-670 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.2-0.3L/min argon gas is used as reaction protective gas, and the deposition time is 35-40 h.
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 850 ℃, the vacuum degree is less than 950Pa, 0.35L/min argon is used as reaction protective gas, and the flow rate is 0.4L/min H2And (3) as carrier gas, trichloromethylsilane is fed into a deposition furnace to react with hydrogen for 40h to generate the silicon carbide substrate. In other embodiments, the deposition process parameters satisfy the following conditions: deposition temperature is 800-1000 ℃, vacuum degree is required to be less than 1000Pa, argon gas with the flow rate of 0.2L/min-0.5L/min is used as reaction protective gas, and H with the flow rate of 0.15L/min-0.4L/min is used2And (3) introducing trichloromethylsilane into a deposition furnace as carrier gas to react with hydrogen, wherein the deposition time is 40-60 h.
Step 4, riveting, combining and processing a blank;
laminating the multiple layers of the blank plates prepared in step 3 to a designed thickness, and riveting the laminated blank plates by using two-dimensional silicon carbide/silicon carbide composite pins, wherein the diameter size of each pin is shown in figure 3
The design thickness should be greater than the diameter of the product pin. And processing a bar blank on the prefabricated plate or strip along the shape length or width direction. In other embodiments, if a two-dimensional silicon carbide/silicon carbide composite is prepared
The bar stock is directly cut into bar stock along the length direction or the width direction of the blank flat plate prefabricated body prepared in the single-layer step 3, and then the bar stock is processed into a bar stock blank.
The two-dimensional silicon carbide/silicon carbide composite material pin preferably can be a pin prepared by the two-dimensional silicon carbide/silicon carbide composite material pin preparation method, and in other embodiments, a silicon carbide/silicon carbide composite material pin prepared by other methods can also be adopted.
Step 5, depositing SiC/B4C, a substrate;
deposition of SiC/B on bar stock blanks by CVI deposition furnace4And C, a substrate, wherein the vacuum degree of a furnace chamber before deposition is less than 500Pa, the deposition temperature is 900 ℃, trichloromethyl silane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.3L/min, 0.7L/min argon is used as reaction protective gas, and the deposition time is 65 hours. In other embodiments, the following process parameters may be satisfied: the vacuum degree of a furnace chamber before deposition is required to be less than 500Pa, the deposition temperature is 850-950 ℃, trichloromethyl silane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.5-1L/min argon is used as reaction protective gas, and the deposition time is 60-80 h.
Step 6, fine machining;
and (7) finish machining the bar blank through a numerical control lathe to form a target bar, if the target product is the pin, finish machining the bar blank through the numerical control lathe to form a target pin, and executing the step 7.
Step 7, depositing a SiC coating;
and (3) placing the pin prepared in the step (6) in a CVI deposition furnace, and depositing a silicon carbide anti-oxidation coating on the appearance of the finished pin after finish machining, wherein the deposition time is 35-40 h, the deposition temperature is 850-950 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
The two-dimensional silicon carbide/silicon carbide composite material prepared in this example
The pins, after room temperature shear strength testing,
pin shear strength 312.3 MPa.
Example 2
Referring to FIG. 1, this example prepares a two-dimensional silicon carbide/silicon carbide composite by the following procedure
Bolt:
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 one third of the diameter of a bolt, 1mm of processing allowance is reserved in the thickness, T300-3K carbon fibers are used for being 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 this embodiment, the laying angle of each layer of silicon carbide cloth is not particularly limited, and may be, for example, a forward laying at 0 °/90 °, or an oblique laying at more than 0 ° and less than 90 °, or alternatively a forward laying and an oblique laying. In other embodiments, if a two-dimensional silicon carbide/silicon carbide composite is prepared
The design thickness of the bolt of (2) can be designed to be 7 mm.
Step 2, depositing a BN interface layer;
and (2) 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 270Pa, the deposition temperature is 630 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.25L/min, 0.25L/min argon gas is used as reaction protective gas for assistance, and the deposition time is 35h, so that the plate-shaped or strip-shaped preform with the BN interface layer is obtained. In other embodiments, the deposition process parameters may satisfy the following conditions: the vacuum degree of a furnace cavity before deposition is required to be less than 300Pa, the deposition temperature is 620-670 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.2-0.3L/min argon gas is used as reaction protective gas, and the deposition time is 35-40 h.
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 850 ℃, the vacuum degree is less than 950Pa, 0.35L/min argon is used as reaction protective gas, and the flow rate is 0.4L/min H2And (3) as carrier gas, trichloromethylsilane is fed into a deposition furnace to react with hydrogen for 40h to generate the silicon carbide substrate. In other embodiments, the deposition process parameters satisfy the following conditions: deposition temperature is 800-1000 ℃, vacuum degree is required to be less than 1000Pa, argon gas with the flow rate of 0.2L/min-0.5L/min is used as reaction protective gas, and H with the flow rate of 0.15L/min-0.4L/min is used2And (3) introducing trichloromethylsilane into a deposition furnace as carrier gas to react with hydrogen, wherein the deposition time is 40-60 h.
Step 4, riveting, combining and processing a blank;
laminating the multiple layers of the blank plates prepared in step 3 to a designed thickness, and riveting the laminated blank plates by using two-dimensional silicon carbide/silicon carbide composite pins, wherein the diameter size of each pin is shown in figure 3
The design thickness should be greater than the diameter of the product bolt. And processing a bar blank on the prefabricated plate or strip along the shape length or width direction. In other embodiments, if a two-dimensional silicon carbide/silicon carbide composite is prepared
Where the blank plate preform prepared in the single-layer step 3 is directly put alongCutting into strips in the length or width direction, and processing into bar blanks.
The two-dimensional silicon carbide/silicon carbide composite pin can be preferably the pin prepared in example 1, and the two-dimensional silicon carbide/silicon carbide composite pin prepared in other manners can be also adopted in other examples.
Step 5, depositing SiC/B4C, a substrate;
deposition of SiC/B on bar stock blanks by CVI deposition furnace4And C, a substrate, wherein the vacuum degree of a furnace chamber before deposition is less than 500Pa, the deposition temperature is 900 ℃, trichloromethyl silane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.3L/min, 0.7L/min argon is used as reaction protective gas, and the deposition time is 65 hours. In other embodiments, the following process parameters may be satisfied: the vacuum degree of a furnace chamber before deposition is required to be less than 500Pa, the deposition temperature is 850-950 ℃, trichloromethyl silane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.5-1L/min argon is used as reaction protective gas, and the deposition time is 60-80 h.
Step 6, fine machining;
and (3) finish machining the profile of the bar blank screw by using a numerical control lathe and turning threads by using a special diamond thread sheet cutter.
Step 7, depositing a SiC coating;
and depositing the silicon carbide anti-oxidation coating on the appearance of the finished bolt by using a CVI deposition furnace, wherein the deposition time is 40 hours, the deposition temperature is 920 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen. Finally forming the two-dimensional silicon carbide/silicon carbide composite material bolt. In other embodiments, the following process parameters may be satisfied: the deposition time is 35-40 h, and the deposition temperature is 850-950 ℃.
As shown in fig. 4 and 5, when the thread height of the two-dimensional silicon carbide/silicon carbide composite material bolt prepared in this example is observed under a Scanning Electron Microscope (SEM), the thread shape is complete, the thread height meets the requirement, and the tensile strength test at room temperature shows that the tensile strength of the bolt M8 is 196.4 MPa.
Claims (29)
1. A preparation method of a two-dimensional silicon carbide/silicon carbide composite connecting piece is characterized in that the connecting piece is a pin, and comprises the following steps:
step 1, preparing a two-dimensional silicon carbide/silicon carbide layer plate material prefabricated body;
step 1.1, laminating multiple layers of silicon carbide cloth to a designed thickness, wherein when the diameter of the pin is larger than or equal to the diameter of the pin
When the design thickness is smaller than the pin diameter, the design thickness is smaller than the pin diameter when the pin diameter is smaller than the pin diameter
When the design thickness is larger than the pin diameter by at least xmm;
step 1.2, using carbon fibers to be vertical to the silicon carbide cloth after lamination for puncture sewing;
step 2, depositing a BN interface layer;
placing the two-dimensional silicon carbide/silicon carbide layer plate preform prepared in the step 1 in an interface layer deposition furnace, and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide layer plate preform to obtain a preform with the BN interface layer;
step 3, depositing a SiC matrix;
placing the prefabricated body with the BN interface layer prepared in the step 2 in a CVI deposition furnace, and depositing a silicon carbide substrate on the prefabricated body with the BN interface layer; forming a single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate; the thickness of the single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate is more than 6 mm;
step 4, riveting, combining and processing a blank;
step 4.1, when the diameter of the pin is smaller than that of the pin
Cutting the blank flat plate prepared in the single-layer step 3 into strips along the shape length or width direction, and then processing the strips into bar blanks;
step 4.2, when the pin is usedNail diameter greater than or equal to
Laminating a plurality of layers of blank plates prepared in the step 3 to a designed thickness, and riveting by using a two-dimensional silicon carbide/silicon carbide composite material pin with a smaller specification to obtain a riveting prefabricated body; the design thickness is greater than the pin diameter;
4.3, cutting the riveting prefabricated body prepared in the step 4.2 into strips along the shape length or width direction, and then processing a bar blank;
step 5, depositing SiC/B4C, a substrate;
placing the bar stock blank prepared in the step 4 in a CVI deposition furnace, and depositing SiC/B on the bar stock blank4C, a substrate;
step 6, fine machining;
finish machining the shape of the bar blank prepared in the step 5 to form a finished pin;
step 7, depositing a SiC coating;
and (3) placing the pin prepared in the step (6) in a CVI deposition furnace, and depositing a silicon carbide anti-oxidation coating on the appearance of the finished pin after finish machining, wherein the deposition time is 35-40 h, the deposition temperature is 850-950 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
2. The method for preparing a two-dimensional silicon carbide/silicon carbide composite material connecting piece according to claim 1, wherein: step 1.1 when the diameter of the pin is larger than or equal to the diameter of the pin
When the design thickness is more than or equal to one third of the pin diameter.
3. The method for preparing a two-dimensional silicon carbide/silicon carbide composite material connector according to claim 1 or 2, wherein: in step 4.2, the two-dimensional silicon carbide/silicon carbide composite pin with the smaller specification is prepared by a two-dimensional silicon carbide/silicon carbide composite pin preparation method.
4. The method for preparing a two-dimensional silicon carbide/silicon carbide composite material connector according to claim 1 or 2, wherein: step 5 deposition of SiC/B4The specific process parameters of the C matrix are as follows: the vacuum degree of a furnace chamber before deposition is required to be less than 500Pa, the deposition temperature is 850-950 ℃, trichloromethyl silane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.5-1L/min argon is used as reaction protective gas, and the deposition time is 60-80 h.
5. The method for preparing a two-dimensional silicon carbide/silicon carbide composite material connecting piece according to claim 4, wherein: the deposition temperature is 900 ℃, the gas flow is 0.3L/min, 0.7L/min of argon is used as the reaction protective gas, and the deposition time is 65 hours.
6. The method for preparing a two-dimensional silicon carbide/silicon carbide composite material connecting piece according to claim 4, wherein: the specific process parameters for depositing the BN interface layer in the step 2 are as follows: the vacuum degree of a furnace cavity before deposition is required to be less than 300Pa, the deposition temperature is 620-670 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.2-0.3L/min argon gas is used as reaction protective gas, and the deposition time is 35-40 h.
7. The method for preparing a two-dimensional silicon carbide/silicon carbide composite material connecting piece according to claim 6, wherein: the specific process parameters of the SiC matrix deposited in the step 3 are as follows: deposition temperature is 800-1000 ℃, vacuum degree is required to be less than 1000Pa, argon gas with the flow rate of 0.2L/min-0.5L/min is used as reaction protective gas, and H with the flow rate of 0.15L/min-0.4L/min is used2And (3) introducing trichloromethylsilane into a deposition furnace as carrier gas to react with hydrogen, wherein the deposition time is 40-60 h.
8. The method of claim 7, wherein the two-dimensional silicon carbide/silicon carbide composite material connector is prepared by: the diameter size of the two-dimensional silicon carbide/silicon carbide composite material pin with smaller specification in step 4.2 is not more than
9. The method of preparing a two-dimensional silicon carbide/silicon carbide composite connector according to claim 8, wherein: the two-dimensional silicon carbide/silicon carbide composite material pins with small specifications are uniformly distributed along the length direction of the bar, and the distance between riveting pin holes is not less than 8 mm.
10. The method of preparing a two-dimensional silicon carbide/silicon carbide composite connector according to claim 9, wherein: in the step 1.2, T300-3K carbon fibers are used for perpendicular to silicon carbide cloth for puncture sewing; step 1.1 x equals 1.
11. A preparation method of a two-dimensional silicon carbide/silicon carbide composite bar is characterized by comprising the following steps:
step 1, preparing a two-dimensional silicon carbide/silicon carbide layer plate material prefabricated body;
step 1.1, laminating multiple layers of silicon carbide cloth to a designed thickness, wherein when the diameter of a bar stock is larger than 6mm, the designed thickness is smaller than the diameter of the bar stock; when the diameter of the bar stock is smaller than
When the design thickness of the silicon carbide/silicon carbide plate is larger than the diameter of the bar stock by at least xmm;
step 1.2, using carbon fibers to be vertical to the silicon carbide cloth after lamination for puncture sewing;
step 2, depositing a BN interface layer;
placing the two-dimensional silicon carbide/silicon carbide layer plate preform prepared in the step 1 in an interface layer deposition furnace, and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide layer plate preform to obtain a preform with the BN interface layer;
step 3, depositing a SiC matrix;
placing the prefabricated body with the BN interface layer prepared in the step 2 in a CVI deposition furnace, and depositing a silicon carbide substrate on the prefabricated body with the BN interface layer; forming a single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate; the thickness of the single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate is more than 6 mm;
step 4, riveting, combining and processing a blank;
step 4.1, when the diameter of the bar stock is less than 6mm, cutting the blank flat plate prefabricated body prepared in the single-layer step 3 into strip materials along the length direction or the width direction, and then processing the strip materials into bar stock;
step 4.2, when the diameter of the bar stock is larger than or equal to 6mm, laminating a plurality of layers of blank flat plates prepared in the step 3 to a designed thickness, and riveting through a two-dimensional silicon carbide/silicon carbide composite material pin with a smaller specification to obtain a riveting prefabricated body; the design thickness is larger than the diameter of the bar stock;
4.3, cutting the riveting prefabricated body prepared in the step 4.2 into strips along the shape length or width direction, and then processing a bar blank;
step 5, depositing SiC/B4C, a substrate;
placing the bar stock blank prepared in the step 4 in a CVI deposition furnace, and depositing SiC/B on the bar stock blank4C, a substrate;
step 6, fine machining;
and (5) finishing the shape of the bar blank prepared in the step 5 to form a target bar.
12. The method for preparing a two-dimensional silicon carbide/silicon carbide composite bar stock as recited in claim 11, wherein the design thickness is equal to or greater than one third of the diameter of the bar stock when the diameter of the bar stock is greater than 6mm in step 1.1.
13. The method for preparing the two-dimensional silicon carbide/silicon carbide composite bar stock according to claim 11 or 12, wherein: in step 4.2, the smaller gauge two-dimensional silicon carbide/silicon carbide composite pin is prepared by the method of any of claims 1 or 10.
14. The method of preparing a two-dimensional silicon carbide/silicon carbide composite bar stock as recited in claim 13, wherein step 5 deposits SiC/B4The specific process parameters of the C matrix are as follows: the vacuum degree of a furnace chamber before deposition is required to be less than 500Pa, the deposition temperature is 850-950 ℃, trichloromethyl silane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.5-1L/min argon is used as reaction protective gas, and the deposition time is 60-80 h.
15. The method for preparing a two-dimensional silicon carbide/silicon carbide composite bar stock as recited in claim 14, wherein: the deposition temperature is 900 ℃, the gas flow is 0.3L/min, 0.7L/min of argon is used as the reaction protective gas, and the deposition time is 65 hours.
16. The method for preparing the two-dimensional silicon carbide/silicon carbide composite bar stock as recited in claim 15, wherein: the specific process parameters for depositing the BN interface layer in the step 2 are as follows: the vacuum degree of a furnace cavity before deposition is required to be less than 300Pa, the deposition temperature is 620-670 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.2-0.3L/min argon gas is used as reaction protective gas, and the deposition time is 35-40 h.
17. The method for preparing a two-dimensional silicon carbide/silicon carbide composite bar stock as recited in claim 16, wherein: the specific process parameters of the SiC matrix deposited in the step 3 are as follows: deposition temperature is 800-1000 ℃, vacuum degree is required to be less than 1000Pa, argon gas with the flow rate of 0.2L/min-0.5L/min is used as reaction protective gas, and H with the flow rate of 0.15L/min-0.4L/min is used2And (3) introducing trichloromethylsilane into a deposition furnace as carrier gas to react with hydrogen, wherein the deposition time is 40-60 h.
18. The method for preparing the two-dimensional silicon carbide/silicon carbide composite bar stock as recited in claim 17, wherein: when the diameter of the bar stock is more than or equal to 6mmThe diameter size of the two-dimensional silicon carbide/silicon carbide composite pin with smaller specification is not more than
19. The method for preparing a two-dimensional silicon carbide/silicon carbide composite bar stock as recited in claim 18, wherein: the two-dimensional silicon carbide/silicon carbide composite material pin for riveting the silicon carbide/silicon carbide composite material flat plate is positioned as follows: the pin holes are uniformly distributed along the length direction of the bar stock, and the distance between the pin holes is not less than 8 mm.
20. The method for preparing a two-dimensional silicon carbide/silicon carbide composite bar stock as recited in claim 19, wherein: in the step 1.2, T300-3K carbon fibers are used for perpendicular to silicon carbide cloth for puncture sewing; step 1.1 x equals 1.
21. A preparation method of a two-dimensional silicon carbide/silicon carbide composite material connecting piece is characterized in that the connecting piece is a bolt and comprises the following steps:
step 1, preparing a two-dimensional silicon carbide/silicon carbide layer plate material prefabricated body;
step 1.1, laminating multiple layers of silicon carbide cloth to a designed thickness: when the diameter of the bolt is more than or equal to
When the design thickness is smaller than the diameter of the bolt; when the diameter of the bolt is smaller than
When the design thickness is larger than the diameter of the bolt by at least xmm;
step 1.2, using carbon fibers to be vertical to the silicon carbide cloth after lamination for puncture sewing;
step 2, depositing a BN interface layer;
placing the two-dimensional silicon carbide/silicon carbide layer plate preform prepared in the step 1 in an interface layer deposition furnace, and depositing a BN interface layer on the two-dimensional silicon carbide/silicon carbide layer plate preform to obtain a preform with the BN interface layer;
step 3, depositing a SiC matrix;
placing the prefabricated body with the BN interface layer prepared in the step 2 in a CVI deposition furnace, and depositing a silicon carbide substrate on the prefabricated body with the BN interface layer; forming a single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate; the thickness of the single-layer two-dimensional silicon carbide/silicon carbide composite material blank flat plate is more than 6 mm;
step 4, riveting, combining and processing a blank;
step 4.1, when the diameter of the bolt is smaller than
Cutting the blank flat plate preform prepared in the single-layer step 3 into strips along the shape length or width direction, and then processing the bar blank;
step 4.2, when the diameter of the bolt is more than or equal to the diameter of the bolt
Laminating a plurality of layers of blank plates prepared in the step 3 to a designed thickness, and riveting by using a two-dimensional silicon carbide/silicon carbide composite material pin with a smaller specification to obtain a riveting prefabricated body; when the diameter of the bolt is more than or equal to
When the design thickness of the blank flat plate is larger than the diameter of the bolt;
4.3, cutting the prefabricated body prepared in the step 4.2 into strips along the shape length or width direction, and then processing a bar blank;
step 5, depositing SiC/B4C, a substrate;
placing the bar stock blank prepared in the step 4 in a CVI deposition furnace, and depositing SiC/B on the bar stock blank4The base C can obviously prolong the thermal oxidation life of the ceramic matrix composite;
step 6, fine machining;
finish machining the shape of the bar blank prepared in the step 5 to form a finished bolt;
step 7, depositing a SiC coating;
and (3) placing the finished bolt prepared in the step (6) in a CVI deposition furnace, and depositing a silicon carbide anti-oxidation coating on the appearance of the finished bolt after finish machining, wherein the deposition time is 35-40 h, the deposition temperature is 850-950 ℃, and the reaction gas is trichloromethylsilane, argon and hydrogen.
22. A method of making a two-dimensional silicon carbide/silicon carbide composite connector according to claim 21, wherein: step 1.1 when the diameter of the bolt is more than or equal to the diameter of the bolt
When the bolt is used, the design thickness of the prefabricated body is more than or equal to one third of the diameter of the bolt; in step 4.2, the two-dimensional silicon carbide/silicon carbide composite pin with the smaller specification is prepared by a two-dimensional silicon carbide/silicon carbide composite pin preparation method.
23. A method of making a two-dimensional silicon carbide/silicon carbide composite connector according to claim 21 or 22, wherein: step 5 deposition of SiC/B4The specific process parameters of the C matrix are as follows: the vacuum degree of a furnace chamber before deposition is required to be less than 500Pa, the deposition temperature is 850-950 ℃, trichloromethyl silane, methane, boron trichloride gas and hydrogen are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.5-1L/min argon is used as reaction protective gas, and the deposition time is 60-80 h.
24. A method of making a two-dimensional silicon carbide/silicon carbide composite connector according to claim 23, wherein: the deposition temperature is 900 ℃, the gas flow is 0.3L/min, 0.7L/min of argon is used as the reaction protective gas, and the deposition time is 65 hours.
25. A method of making a two-dimensional silicon carbide/silicon carbide composite connector according to claim 21 or 22, wherein: the specific process parameters for depositing the BN interface layer in the step 2 are as follows: the vacuum degree of a furnace cavity before deposition is required to be less than 300Pa, the deposition temperature is 620-670 ℃, ammonia gas, boron trichloride gas and hydrogen gas are used as deposition gas and a catalytic carrier, the gas flow is 0.1-0.6L/min, 0.2-0.3L/min argon gas is used as reaction protective gas, and the deposition time is 35-40 h.
26. A method of making a two-dimensional silicon carbide/silicon carbide composite connector according to claim 25, wherein: the specific process parameters of the SiC matrix deposited in the step 3 are as follows: deposition temperature is 800-1000 ℃, vacuum degree is required to be less than 1000Pa, argon gas with the flow rate of 0.2L/min-0.5L/min is used as reaction protective gas, and H with the flow rate of 0.15L/min-0.4L/min is used2And (3) introducing trichloromethylsilane into a deposition furnace as carrier gas to react with hydrogen, wherein the deposition time is 40-60 h.
27. A method of making a two-dimensional silicon carbide/silicon carbide composite connector according to claim 26, wherein: when the diameter of the bolt is more than or equal to the diameter of the bolt
In the process, the diameter size of the two-dimensional silicon carbide/silicon carbide composite pin for riveting the silicon carbide/silicon carbide flat plate is not more than
28. A method of making a two-dimensional silicon carbide/silicon carbide composite connector according to claim 27, wherein: the position of the two-dimensional silicon carbide/silicon carbide composite pin with the smaller specification is as follows: the bolts are uniformly distributed along the length direction of the bolts, the distance between the pin holes is not less than 8mm, and the riveting part is close to or arranged at the nut installation stirrup part.
29. A method of making a two-dimensional silicon carbide/silicon carbide composite connector according to claim 28, wherein: in the step 1.2, T300-3K carbon fibers are used for perpendicular to silicon carbide cloth for puncture sewing; step 1.1 x equals 1.
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