CN117285362A - SiC/SiC composite material high temperature resistant and oxidation resistant interface layer and preparation method thereof - Google Patents
SiC/SiC composite material high temperature resistant and oxidation resistant interface layer and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 61
- 239000011184 SiC–SiC matrix composite Substances 0.000 title claims abstract description 52
- 230000003647 oxidation Effects 0.000 title claims abstract description 45
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000010410 layer Substances 0.000 claims abstract description 200
- 239000000835 fiber Substances 0.000 claims abstract description 134
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 84
- 238000000034 method Methods 0.000 claims abstract description 58
- 230000005501 phase interface Effects 0.000 claims abstract description 51
- 230000008569 process Effects 0.000 claims abstract description 28
- 239000011241 protective layer Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims description 202
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 132
- 239000007789 gas Substances 0.000 claims description 97
- 229910052786 argon Inorganic materials 0.000 claims description 66
- 238000001035 drying Methods 0.000 claims description 27
- 238000004804 winding Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 238000006467 substitution reaction Methods 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 146
- 229910010271 silicon carbide Inorganic materials 0.000 description 143
- 239000010936 titanium Substances 0.000 description 17
- 229910052582 BN Inorganic materials 0.000 description 11
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 11
- 238000000576 coating method Methods 0.000 description 9
- 239000002296 pyrolytic carbon Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 7
- 239000002131 composite material Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 108010066057 cabin-1 Proteins 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- 239000005388 borosilicate glass Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- DXZIFGZIQQRESB-UHFFFAOYSA-N [C].[Ti].[Si] Chemical compound [C].[Ti].[Si] DXZIFGZIQQRESB-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical class OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
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Abstract
The invention discloses a high-temperature-resistant and oxidation-resistant interface layer of a SiC/SiC composite material and a preparation method thereof, wherein the interface layer is Ta 4 C 3 B x MXene interface layer, where x = 0.1-0.5. The preparation method comprises the following steps: designing a continuous chemical vapor deposition device and a continuous ultrasonic device to ensure that the device is normally used in the continuous chemical vapor deposition and continuous ultrasonic process; sequentially preparing TaC on the outer surface of SiC fiber bundle filaments by adopting a continuous chemical vapor deposition device x Protective layer and Ta 4 SiC 3 MAX phase interface layer; ta on outer surface of SiC fiber bundle filaments by adopting continuous ultrasonic device 4 SiC 3 Conversion of MAX phase interface layer to Ta 4 C 3 F x An MXene interfacial layer; adopting a continuous chemical vapor deposition device to perform chemical vapor deposition on the outer surface Ta of the SiC fiber bundle filaments 4 C 3 F x F element in the MXene interface layer is removed, and B element is doped at the same time, so that the product can be preparedObtain the high-temperature-resistant and oxidation-resistant Ta of the SiC/SiC composite material 4 C 3 B x MXene interface layer. According to the invention, the service performance and service life of the SiC/SiC composite material in a high-temperature oxidation environment are improved by introducing a new interface layer material system, so that the application field of the SiC/SiC composite material is further expanded.
Description
Technical Field
The invention belongs to the technical field of preparation of ceramic matrix composite interface layers, and particularly relates to a high-temperature-resistant and oxidation-resistant interface layer of a SiC/SiC composite material and a preparation method thereof.
Background
The silicon carbide-based composite material (SiC/SiC composite material) toughened by the continuous filament-spun silicon carbide fibers has the advantages of high temperature resistance, oxidation resistance, low density, high thermal conductivity, low thermal expansion coefficient and the like of the silicon carbide ceramic, and has the characteristics of no catastrophic damage and the like due to the introduction of the toughening fibers, so that the silicon carbide-based composite material has wide application in the fields of aeroengines and the like. The SiC/SiC composite material uses continuous filament silicon carbide fibers as a toughening phase and silicon carbide ceramics as a matrix phase, and a weak interface phase is also required for avoiding strong combination between the fibers and the matrix, and is usually pyrolytic carbon (PyC) or hexagonal boron nitride (h-BN). The interfacial phase is often prepared at the surface of the fibers and is ultimately between the fibers and the matrix of the composite, and is therefore referred to as a fiber coating relative to the fibers and as an interfacial phase or interface layer relative to the composite as a whole. A layer of boron nitride or pyrolytic carbon coating is prepared on the surface of the bundle silk silicon carbide fiber by adopting a Chemical Vapor Deposition (CVD) or Chemical Vapor Infiltration (CVI) process, and a layer of silicon carbide or silicon nitride coating can be prepared outside the boron nitride and pyrolytic carbon coating to form a composite interface layer. The boron nitride and the pyrolytic carbon coating are both lamellar materials, and play a role in toughening; silicon carbide and silicon nitride coatings protect the fiber, boron nitride or pyrolytic carbon coatings.
The service temperature of the SiC/SiC composite material adopted by the hot end component of the aeroengine is usually 1200 ℃ or even higher. The pyrolytic carbon interface layer is oxidized in an oxygen-containing environment with the temperature of more than 400 ℃, and the pyrolytic carbon interface layer is not selected. While boron nitride interfacial layers can form borosilicate glass phases at 800 ℃ to inhibit oxidation, this mechanism is no longer effective at 1000 ℃ and above. In the presence of water vapor, boron nitride can oxidize to form volatizable boric acid compounds at even lower temperatures, resulting in loss of interfacial layer material.
Doping can improve oxidation resistance at the expense of some toughening properties of the boron nitride interface layer, for example, doped aluminum can further inhibit degradation of the interface layer by forming alumina and borosilicate glass (Carminati P.et al Journal of the European Ceramic Society, 2021, 41 (5): 3120-3131). The silicon carbide, silicon nitride or aluminum nitride protective layer is prepared outside the boron nitride interface layer, so that oxidation of the inner boron nitride interface layer can be slowed down, but the oxidation resistance of the interface layer cannot be fundamentally improved by the method, and damage mechanisms such as terminal oxidation and the like are not enough, so that people never abandon the exploration of novel high-temperature-resistant and oxidation-resistant interface layer materials.
There are reports of using MAX phase as the interface layer of SiC/SiC composite. however,thetraditionalpyrolyticcarbonandboronnitrideinterfacelayerhasalamellarstructure,thelayersarecombinedbycovalentbonds,thelayersarecombinedbyVanderWaalsforce,M-AbondsbetweenMAXphaselayershavemetalbondcharacteristics,MAXistakenasaweakinterfacelayer,andthetougheningeffectisnotideal. For example, the invention patent with application publication number CN112479718A discloses a Ti 3 SiC 2 MAX phase interface layer modified SiC/SiC composite material and preparation method thereof, wherein Ti 3 SiC 2 The thickness of the interface layer is 200-1200nm, and the thickness of the SiC interface layer is 3-5 mu m. The invention patent with publication number CN111592371A discloses a titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material and a preparation method thereof, and Ti is deposited on a SiC fiber preform by adopting a CVD method 3 SiC 2 The interface coating, however, the precursor used has no Si source and C source, si and C can only be derived from SiC fiber or matrix, so that the thickness of the coating can be limited, and only the interface transition function is achieved.
If the A atoms in the MAX phase are selectively etched, a layered MXene material M can be obtained n+1 X n T x T represents a surface functional group, which mayOH, F, O, H, the closer the atomic ratio of M to X, i.e., the larger the n value, the more stable the MXene material. The MXene material has weak interlayer bonding force and can be mechanically peeled, and the bonding force is similar to the properties of graphite and hexagonal boron nitride. The reported MXene materials include Ti 3 C 2 、Ti 2 C、Nb 2 C、V 2 C、Ta 4 C 3 、Nb 4 C 3 、(Ti 0.5 Nb 0.5 ) 2 C、(V 0.5 Cr 0.5 ) 3 C 2 、Ti 3 CN, etc. Currently, X is pure N MXene, e.g. Ti 2 N or Ti 4 N 3 And the like are rarely reported. Theoretical calculation results show that Ti n+1 N n Binding energy ratio of Ti n+1 C n Low from Ti n+1 AlN n To Ti (Ti) n+1 N n But the energy of formation of (C) is greater than that of Ti n+1 SiC n To Ti (Ti) n+1 C n The production energy of (C) is higher, and thus the MXene material of the mixture in which X is C or C, N is more stable than the MXene material in which X is N.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a high-temperature-resistant and oxidation-resistant interface layer of a SiC/SiC composite material, wherein the interface layer is Ta 4 C 3 B x MXene interface layer, where x = 0.1-0.5.
The invention also provides a preparation method of the high-temperature-resistant and oxidation-resistant interface layer of the SiC/SiC composite material, which is used for preparing the high-temperature-resistant and oxidation-resistant interface layer of the SiC/SiC composite material, and comprises the following steps in sequence:
step one: designing and assembling a continuous chemical vapor deposition device and a continuous ultrasonic device, so that the device can be normally used in the continuous chemical vapor deposition process and the continuous ultrasonic process;
step two: sequentially preparing TaC on the outer surface of SiC fiber bundle filaments by adopting a continuous chemical vapor deposition device x Protective layer and Ta 4 SiC 3 MAX phase interface layer;
step three: ta on outer surface of SiC fiber bundle filaments by adopting continuous ultrasonic device 4 SiC 3 Conversion of MAX phase interface layer to Ta 4 C 3 F x An MXene interfacial layer;
step four: adopting a continuous chemical vapor deposition device to perform chemical vapor deposition on the outer surface Ta of the SiC fiber bundle filaments 4 C 3 F x F element in the MXene interface layer is removed, and meanwhile B element is doped, so that the high-temperature-resistant and oxidation-resistant Ta of the SiC/SiC composite material can be prepared 4 C 3 B x MXene interface layer.
Preferably, the continuous chemical vapor deposition device comprises a wire unwinding cabin, a furnace tube and a wire winding cabin which are sequentially connected from left to right; a silk placing roller and a silk placing guide wheel are arranged in the silk placing cabin, and a fifth air inlet pipe is arranged outside the silk placing cabin; a wire collecting roller and a wire collecting guide wheel are arranged in the wire collecting cabin, and a sixth air inlet pipe is arranged outside the wire collecting cabin; a first heating furnace is arranged at one end of the furnace tube, which is close to the wire unwinding cabin, and a second heating furnace is arranged at one end of the furnace tube, which is close to the wire winding cabin; the one end that is close to of first heating furnace put silk cabin sets up first intake pipe and second intake pipe, the second heating furnace is close to the one end of first heating furnace sets up third intake pipe and fourth intake pipe, the second heating furnace is close to the one end of receipts silk cabin sets up the tail gas pipe, the end-to-end connection vacuum pump of tail gas pipe.
In any of the above schemes, preferably, the continuous ultrasonic device comprises a wire unwinding roller, an ultrasonic assembly, a drying furnace and a wire winding roller which are arranged in sequence from left to right; the ultrasonic assembly comprises an ultrasonic groove, an ultrasonic rod, four driving rollers, a heater and a sound-proof cover, wherein the ultrasonic groove is filled with HF solution, the four driving rollers are arranged in the ultrasonic groove and are positioned below the liquid level of the HF solution, the ultrasonic rod is perpendicular to the ultrasonic groove, one end of the ultrasonic rod is inserted into the HF solution, and the heater is arranged at the bottom of the ultrasonic groove; and a plurality of guide rollers are arranged on the continuous ultrasonic device.
In any of the above embodiments, preferably, in the second step, taC is sequentially prepared on the outer surface of the SiC fiber bundle filaments by using a continuous chemical vapor deposition apparatus x Protective layer and Ta 4 SiC 3 The method of the MAX phase interface layer comprises the following steps in sequenceThe method comprises the following steps:
step (1): installing SiC fiber bundle filaments on a filament placing roller in a filament placing cabin, pulling out the head of the SiC fiber bundle filaments to sequentially pass through a first heating furnace, a second heating furnace and a filament collecting cabin, and fixing the SiC fiber bundle filaments on the filament collecting roller in the filament collecting cabin, wherein the central axis of the SiC fiber bundle filaments, the central axis of the first heating furnace and the central axis of the second heating furnace are coincident at the moment;
step (2): closing the fifth air inlet pipe and the sixth air inlet pipe, and simultaneously opening a vacuum pump to vacuumize the interior of the continuous chemical vapor deposition device; opening a fifth air inlet pipe and a sixth air inlet pipe under the state of maintaining vacuumizing, and introducing argon into the continuous chemical vapor deposition device to maintain a certain pressure in the continuous chemical vapor deposition device; simultaneously opening the first heating furnace and the second heating furnace to raise the furnace temperature to a certain temperature;
step (3): starting a wire releasing roller and a wire collecting roller to convey SiC fiber bundle wires, so that the SiC fiber bundle wires continuously move and sequentially pass through a first heating furnace and a second heating furnace; when the SiC fiber bundle wire enters the first heating furnace, the first air inlet pipe and the second air inlet pipe are simultaneously opened, and after the SiC fiber bundle wire continuously passes through the first heating furnace, taC can be prepared on the outer surface of the SiC fiber bundle wire x A protective layer; when the SiC fiber bundle wire enters the second heating furnace, the third air inlet pipe and the fourth air inlet pipe are simultaneously opened, and Ta can be prepared on the outer surface of the SiC fiber bundle wire after continuously passing through the second heating furnace 4 SiC 3 MAX phase interface layer;
step (4): taC for external surface of SiC fiber bundle x Protective layer and Ta 4 SiC 3 And after the preparation of the MAX phase interface layer is finished, sequentially closing the third air inlet pipe, the fourth air inlet pipe, the first air inlet pipe, the second air inlet pipe, the first heating furnace, the second heating furnace, the vacuum pump, the fifth air inlet pipe and the sixth air inlet pipe, and stopping running the continuous chemical vapor deposition device.
In any of the above schemes, preferably, in the step (2), the flow rate of argon gas introduced into the continuous chemical vapor deposition device by the fifth air inlet pipe and the sixth air inlet pipe is 0.1-0.5L/min; the heating area of the first heating furnace is 0.5-0.8m in length, the heating temperature is 600-800 ℃, and the pressure is 60-100Pa; the heating area of the second heating furnace is 0.8-1.2m in length, the heating temperature is 600-800 ℃ and the pressure is 60-100Pa;
in the step (3), the conveying speed of the SiC fiber bundle filaments is 0.1-0.2m/min; the first air inlet pipe is used for introducing TaCl into the first heating furnace 5 Gas and argon, the TaCl 5 The flow rate of the gas is 0.3-0.5L/min, and the flow rate of the argon is 0.5-0.7L/min; the second air inlet pipe is used for introducing CH into the first heating furnace 4 And argon gas, said CH 4 The flow rate of the argon is 0.225-0.375L/min, and the flow rate of the argon is 0.625-0.775L/min; the total flow of the gas introduced into the first heating furnace by the first air inlet pipe and the second air inlet pipe is equal; the TaCl 5 Gas and the CH 4 The molar ratio of (2) is 4:3; the TaC is x X=0.75-1 in the protective layer;
in the step (3), taCl is introduced into the second heating furnace through the third air inlet pipe 5 Gas, siCl 4 Gas and argon, the TaCl 5 The flow rate of the gas is 0.3-0.5L/min, and the SiCl is 4 The flow rate of the gas is 0.075-0.125L/min, and the flow rate of the argon is 0.375-0.625L/min; the fourth air inlet pipe is used for introducing CH into the second heating furnace 4 And argon gas, said CH 4 The flow rate of the argon is 0.225-0.375L/min, and the flow rate of the argon is 0.625-0.775L/min; the total flow of the gas introduced into the second heating furnace by the third air inlet pipe and the fourth air inlet pipe is equal; the TaCl 5 Gas, siCl 4 Gas and the CH 4 The molar ratio of (2) is 4:1:3.
In any of the above embodiments, preferably, in the third step, ta on the outer surface of the SiC fiber bundle filaments is applied by a continuous ultrasonic device 4 SiC 3 Conversion of MAX phase interface layer to Ta 4 C 3 F x The method of the MXene interface layer comprises the following steps in sequence:
step A: will be provided with Ta 4 SiC 3 The SiC fiber bundle wire of the MAX phase interface layer is arranged on a wire releasing roller, and the head part is pulled out to sequentially pass through an ultrasonic groove and a drying furnace and is fixed on a wire collecting deviceA roller; pouring HF solution into an ultrasonic tank to enable four driving rollers and the belt to be Ta 4 SiC 3 The SiC fiber bundle filaments of the MAX phase interface layer are positioned below the liquid level of the HF solution; the heater is opened to heat the HF solution in the ultrasonic tank, and the drying furnace is opened to raise the furnace temperature to a certain temperature;
and (B) step (B): starting the pay-off roller, the driving roller and the take-up roller conveyer belt with Ta 4 SiC 3 SiC fiber bundle filament with MAX phase interface layer, and Ta 4 SiC 3 Continuously moving the SiC fiber bundle filaments of the MAX phase interface layer sequentially through an ultrasonic tank and a drying furnace, and respectively carrying out ultrasonic replacement and drying treatment; with Ta 4 SiC 3 In the process that the SiC fiber bundle filaments of the MAX phase interface layer continuously pass through the ultrasonic tank, the HF solution is used for Ta 4 SiC 3 Substitution of Si element in MAX phase, ta 4 SiC 3 Conversion of MAX phase interface layer to Ta 4 C 3 F x MXene interface layer, i.e. Ta formed on the outer surface of SiC fiber bundle filaments 4 C 3 F x An MXene interfacial layer;
step C: and after the ultrasonic replacement and drying treatment are finished, the heater and the drying furnace are closed, and the continuous ultrasonic device is stopped.
In any of the above schemes, preferably, in step a, the concentration of the HF solution is 10%; the heating temperature of the HF solution is 40-80 ℃; the heating area of the drying furnace is 0.8-1.2m in length and the heating temperature is 100-120 ℃;
in step B, the belt is Ta 4 SiC 3 The travel of the SiC fiber bundle filaments of the MAX phase boundary layer in the ultrasonic groove is 1.5-2.4m, and the conveying speed is 0.03-0.06m/min; the ultrasonic frequency is 40-80kHz, and the ultrasonic power is 1-3kW; the Ta is 4 C 3 F x X=1-2 in the MXene interface layer.
In any of the above embodiments, preferably, in the fourth step, the outer surface Ta of the SiC fiber strand is subjected to a continuous chemical vapor deposition apparatus 4 C 3 F x The method for removing F element in the MXene interface layer and doping B element simultaneously comprises the following steps in sequence:
step a: will be provided withTa 4 C 3 F x The SiC fiber bundle filaments of the MXene interface layer are arranged on a filament releasing roller in a filament releasing cabin, and the head part is pulled out to sequentially pass through a first heating furnace, a second heating furnace and a filament collecting cabin and is fixed on the filament collecting roller in the filament collecting cabin, and the filament collecting cabin is provided with Ta 4 C 3 F x The central axis of the SiC fiber bundle wire of the MXene interface layer, the central axis of the first heating furnace and the central axis of the second heating furnace are overlapped;
step b: closing the fifth air inlet pipe and the sixth air inlet pipe, and simultaneously opening a vacuum pump to vacuumize the interior of the continuous chemical vapor deposition device; opening a fifth air inlet pipe and a sixth air inlet pipe under the state of maintaining vacuumizing, and introducing argon into the continuous chemical vapor deposition device to maintain a certain pressure in the continuous chemical vapor deposition device; simultaneously, a second heating furnace is opened to raise the furnace temperature to a certain temperature;
Step c: starting the godet and godet conveyer belt with Ta 4 C 3 F x SiC fiber bundle filament of MXene interface layer, and Ta is carried 4 C 3 F x The SiC fiber bundle filaments of the MXene interface layer continuously move to pass through the first heating furnace and the second heating furnace in sequence; when carrying Ta 4 C 3 F x When the SiC fiber bundle wire of the MXene interface layer enters the second heating furnace, a third air inlet pipe is opened, and the second air inlet pipe is provided with Ta 4 C 3 F x In the process that SiC fiber bundle filaments of the MXene interface layer continuously pass through the second heating furnace, ta is removed 4 C 3 F x F element in MXene interface layer is doped with B element, and Ta can be prepared on the outer surface of the MXene interface layer 4 C 3 B x An MXene interfacial layer;
step d: and sequentially closing the third air inlet pipe, the second heating furnace, the vacuum pump, the fifth air inlet pipe and the sixth air inlet pipe, and stopping running the continuous chemical vapor deposition device.
In any of the above schemes, preferably, in the step b, the flow rate of argon gas introduced into the continuous chemical vapor deposition device by the fifth air inlet pipe and the sixth air inlet pipe is 0.1-0.5L/min; the heating temperature of the second heating furnace is 1000-1200 ℃ and the pressure is 10-20Pa; the first heating furnace is not started to heat;
in step c, the belt is Ta 4 C 3 F x The conveying speed of the SiC fiber bundle filaments of the MXene interface layer is 0.1-0.2m/min; the third air inlet pipe is led into the second heating furnace with B 2 H 6 And H 2 Mixture of gases, B 2 H 6 Is 5% by volume of said B 2 H 6 And H 2 The flow rate of the mixed gas is 0.6-1L/min; the Ta is 4 C 3 B x X=0.1-0.5 in the MXene interface layer.
In the invention, ta is prepared 4 SiC 3 Before the MAX phase interface layer, taC is prepared on the outer surface of the SiC fiber bundle silk x And a protective layer for protecting the SiC fiber bundle filaments from the attack of the Si source precursor and the HF solution. TaCl is firstly put into 5 Solid, siCl 4 Conversion of liquid to TaCl 5 Gas, siCl 4 And after the gas is fed into the first heating furnace and/or the second heating furnace. The outer surface Ta of the SiC fiber bundle filaments is subjected to continuous chemical vapor deposition 4 C 3 F x The F element in the MXene interface layer is removed, and in the process of doping the B element, the first heating furnace does not start heating, namely, the process only uses the second heating furnace and does not use the first heating furnace.
The invention utilizes the MAX phase with larger n to stabilize the corresponding MXene, the element A is easy to be removed by HF solution when Si is selected, and the element B is doped to improve Ta 4 C 3 Oxidation resistance and four properties of MAX (MAX) are easily formed by three elements of Ta, si and C in a molar ratio of 4:1:3, and Ta is prepared by adopting a continuous Chemical Vapor Deposition (CVD) process firstly 4 SiC 3 MAX phase interface layer, then removing Si element by HF solution with concentration of 10% to form stable Ta 4 C 3 MXene, and finally adopting a continuous Chemical Vapor Deposition (CVD) process to further dope B element to prepare Ta 4 C 3 B x The MXene interface layer improves the high-temperature oxidation resistance of the SiC/SiC composite interface layer, and solves the technical problems that the traditional SiC/SiC composite interface layer, such as PyC, BN and the like, cannot resist high-temperature oxidation, especially water oxidation.
The SiC/SiC composite material high temperature resistant and oxidation resistant interface layer and the preparation method of the invention introduce a new interface layer material system, namely Ta 4 C 3 B x The MXene interface layer can improve the service performance and service life of the SiC/SiC composite material in a high-temperature oxidation environment, thereby further expanding the application field of the SiC/SiC composite material.
Drawings
FIG. 1 is a process flow diagram of a preferred embodiment of a high temperature resistant and oxidation resistant interfacial layer of a SiC/SiC composite material and method of making in accordance with the present invention;
FIG. 2 is a schematic view of a continuous chemical vapor deposition apparatus according to the embodiment shown in FIG. 1;
FIG. 3 is a schematic view of the structure of the continuous ultrasound device of the embodiment shown in FIG. 1;
FIG. 4 shows Ta according to the embodiment of FIG. 1 4 SiC 3 A microstructure photograph of the MAX phase interface layer;
FIG. 5 shows Ta according to the example of FIG. 1 4 C 3 F x A photograph of the microstructure of the MXene interfacial layer;
FIG. 6 shows Ta according to the embodiment of FIG. 1 4 C 3 B x A photograph of the microstructure of the MXene interfacial layer;
FIG. 7 shows the embodiment of FIG. 1 for SiC/SiC composites with BN interface layer and Ta 4 C 3 B x And (3) comparing test result bar graphs obtained by checking the SiC/SiC composite material of the MXene interface layer.
The reference numerals in the drawings indicate:
1-a wire discharge cabin, 11-a wire discharge roller, 12-a wire discharge guide wheel and 13-a fifth air inlet pipe;
2-furnace tubes, 21-first heating furnaces, 22-second heating furnaces, 23-first air inlet pipes, 24-second air inlet pipes, 25-third air inlet pipes, 26-fourth air inlet pipes, 27-tail air pipes and 28-vacuum pumps;
3-wire collecting cabin, 31-wire collecting roller, 32-wire collecting guide wheel and 33-sixth air inlet pipe;
4-a wire releasing roller;
5-ultrasonic components, 51-ultrasonic grooves, 52-ultrasonic rods, 53-driving rollers, 54-heaters, 55-sound insulation covers and 56-HF solution;
6-drying furnace, 7-take-up roller and 8-guide roller.
Detailed Description
For a further understanding of the present invention, the present invention will be described in detail with reference to the following examples.
Embodiment one:
according to a preferred embodiment of the high temperature resistant and oxidation resistant interfacial layer of the SiC/SiC composite material of the invention, the interfacial layer is Ta 4 C 3 B x MXene interface layer, where x=0.5.
As shown in fig. 1, this embodiment also provides a method for preparing a high temperature resistant and oxidation resistant interface layer of a SiC/SiC composite material, which is used for preparing the high temperature resistant and oxidation resistant interface layer of the SiC/SiC composite material, and includes the following steps in order:
step one: designing and assembling a continuous chemical vapor deposition device and a continuous ultrasonic device, so that the device can be normally used in the continuous chemical vapor deposition process and the continuous ultrasonic process;
step two: sequentially preparing TaC on the outer surface of SiC fiber bundle filaments by adopting a continuous chemical vapor deposition device x Protective layer and Ta 4 SiC 3 MAX phase interface layer;
step three: ta on outer surface of SiC fiber bundle filaments by adopting continuous ultrasonic device 4 SiC 3 Conversion of MAX phase interface layer to Ta 4 C 3 F x An MXene interfacial layer;
step four: adopting a continuous chemical vapor deposition device to perform chemical vapor deposition on the outer surface Ta of the SiC fiber bundle filaments 4 C 3 F x F element in the MXene interface layer is removed, and meanwhile B element is doped, so that the high-temperature-resistant and oxidation-resistant Ta of the SiC/SiC composite material can be prepared 4 C 3 B x MXene interface layer.
As shown in fig. 2, the continuous chemical vapor deposition device comprises a wire unwinding cabin 1, a furnace tube 2 and a wire winding cabin 3 which are sequentially connected from left to right; a godet roller 11 and a godet guide wheel 12 are arranged in the godet chamber 1, and a fifth air inlet pipe 13 is arranged outside the godet chamber 1; a wire collecting roller 31 and a wire collecting guide wheel 32 are arranged in the wire collecting cabin 3, and a sixth air inlet pipe 33 is arranged outside the wire collecting cabin 3; a first heating furnace 21 is arranged at one end of the furnace tube 2 close to the wire unwinding cabin 1, and a second heating furnace 22 is arranged at one end of the furnace tube 2 close to the wire winding cabin 3; the first heating furnace 21 is close to one end of the wire unwinding cabin 1 and is provided with a first air inlet pipe 23 and a second air inlet pipe 24, the second heating furnace 22 is close to one end of the first heating furnace 21 and is provided with a third air inlet pipe 25 and a fourth air inlet pipe 26, one end of the second heating furnace 22, which is close to the wire winding cabin 3, is provided with a tail gas pipe 27, and the tail end of the tail gas pipe 27 is connected with a vacuum pump 28.
As shown in fig. 3, the continuous ultrasonic device comprises a paying-off roller 4, an ultrasonic assembly 5, a drying furnace 6 and a wire winding roller 7 which are sequentially arranged from left to right; the ultrasonic assembly 5 comprises an ultrasonic tank 51, an ultrasonic rod 52, four driving rollers 53, a heater 54 and a sound-proof cover 55, wherein the ultrasonic tank 51 is filled with an HF solution 56, the four driving rollers 53 are arranged in the ultrasonic tank 51 and are positioned below the liquid level of the HF solution 56, the ultrasonic rod 52 is perpendicular to the ultrasonic tank 51, one end of the ultrasonic rod 52 is inserted into the HF solution 56, and the heater 54 is arranged at the bottom of the ultrasonic tank 51; a plurality of guide rollers 8 are arranged on the continuous ultrasonic device.
In the second step, adopting a continuous chemical vapor deposition device to sequentially prepare TaC on the outer surface of the SiC fiber bundle filaments x Protective layer and Ta 4 SiC 3 The method of the MAX phase interface layer comprises the following steps in sequence:
step (1): installing SiC fiber bundle filaments on a filament placing roller in a filament placing cabin, pulling out the head of the SiC fiber bundle filaments to sequentially pass through a first heating furnace, a second heating furnace and a filament collecting cabin, and fixing the SiC fiber bundle filaments on the filament collecting roller in the filament collecting cabin, wherein the central axis of the SiC fiber bundle filaments, the central axis of the first heating furnace and the central axis of the second heating furnace are coincident at the moment;
Step (2): closing the fifth air inlet pipe and the sixth air inlet pipe, and simultaneously opening a vacuum pump to vacuumize the interior of the continuous chemical vapor deposition device; opening a fifth air inlet pipe and a sixth air inlet pipe under the state of maintaining vacuumizing, and introducing argon into the continuous chemical vapor deposition device to maintain a certain pressure in the continuous chemical vapor deposition device; simultaneously opening the first heating furnace and the second heating furnace to raise the furnace temperature to a certain temperature;
step (3): starting a wire releasing roller and a wire collecting roller to convey SiC fiber bundle wires, so that the SiC fiber bundle wires continuously move and sequentially pass through a first heating furnace and a second heating furnace; when the SiC fiber bundle wire enters the first heating furnace, the first air inlet pipe and the second air inlet pipe are simultaneously opened, and after the SiC fiber bundle wire continuously passes through the first heating furnace, taC can be prepared on the outer surface of the SiC fiber bundle wire x A protective layer; when the SiC fiber bundle wire enters the second heating furnace, the third air inlet pipe and the fourth air inlet pipe are simultaneously opened, and Ta can be prepared on the outer surface of the SiC fiber bundle wire after continuously passing through the second heating furnace 4 SiC 3 MAX phase interface layer;
step (4): taC for external surface of SiC fiber bundle x Protective layer and Ta 4 SiC 3 And after the preparation of the MAX phase interface layer is finished, sequentially closing the third air inlet pipe, the fourth air inlet pipe, the first air inlet pipe, the second air inlet pipe, the first heating furnace, the second heating furnace, the vacuum pump, the fifth air inlet pipe and the sixth air inlet pipe, and stopping running the continuous chemical vapor deposition device.
In the step (2), the flow rate of argon gas introduced into the continuous chemical vapor deposition device by the fifth air inlet pipe and the sixth air inlet pipe is 0.5L/min; the length of the heating zone of the first heating furnace is 0.8m, the heating temperature is 800 ℃, and the pressure is 100Pa; the heating zone length of the second heating furnace is 1.2m, the heating temperature is 800 ℃, and the pressure is 100Pa.
In the step (3), the conveying speed of the SiC fiber bundle filaments is 0.2m/min; the first air inlet pipe is used for introducing TaCl into the first heating furnace 5 Gas and argon, the TaCl 5 The flow rate of the gas is 0.5L/min, and the flow rate of the argon is 0.5L/min; the second air inlet pipe is used for introducing CH into the first heating furnace 4 And argon gas, said CH 4 The flow rate of the argon is 0.375L/min, and the flow rate of the argon is 0.625L/min; the total flow of the gas introduced into the first heating furnace by the first air inlet pipe and the second air inlet pipe is equalThe method comprises the steps of carrying out a first treatment on the surface of the The TaCl 5 Gas and the CH 4 The molar ratio of (2) is 4:3; the TaC is x X=1 in the protective layer.
In the step (3), taCl is introduced into the second heating furnace through the third air inlet pipe 5 Gas, siCl 4 Gas and argon, the TaCl 5 The flow rate of the gas is 0.5L/min, and the SiCl is 4 The flow rate of the gas is 0.125L/min, and the flow rate of the argon is 0.375L/min; the fourth air inlet pipe is used for introducing CH into the second heating furnace 4 And argon gas, said CH 4 The flow rate of the argon is 0.375L/min, and the flow rate of the argon is 0.625L/min; the total flow of the gas introduced into the second heating furnace by the third air inlet pipe and the fourth air inlet pipe is equal; the TaCl 5 Gas, siCl 4 Gas and the CH 4 The molar ratio of (2) is 4:1:3.
In the third step, a continuous ultrasonic device is adopted to carry out Ta on the outer surface of the SiC fiber bundle filaments 4 SiC 3 Conversion of MAX phase interface layer to Ta 4 C 3 F x The method of the MXene interface layer comprises the following steps in sequence:
step A: will be provided with Ta 4 SiC 3 The SiC fiber bundle filaments of the MAX phase interface layer are arranged on a wire releasing roller, and the head part is pulled out to sequentially pass through an ultrasonic groove and a drying furnace and is fixed on a wire collecting roller; pouring HF solution into an ultrasonic tank to enable four driving rollers and the belt to be Ta 4 SiC 3 The SiC fiber bundle filaments of the MAX phase interface layer are positioned below the liquid level of the HF solution; the heater is opened to heat the HF solution in the ultrasonic tank, and the drying furnace is opened to raise the furnace temperature to a certain temperature;
and (B) step (B): starting the pay-off roller, the driving roller and the take-up roller conveyer belt with Ta 4 SiC 3 SiC fiber bundle filament with MAX phase interface layer, and Ta 4 SiC 3 Continuously moving the SiC fiber bundle filaments of the MAX phase interface layer sequentially through an ultrasonic tank and a drying furnace, and respectively carrying out ultrasonic replacement and drying treatment; with Ta 4 SiC 3 In the process that the SiC fiber bundle filaments of the MAX phase interface layer continuously pass through the ultrasonic tank, the HF solution is used for Ta 4 SiC 3 Substitution of Si element in MAX phase, ta 4 SiC 3 Conversion of MAX phase interface layer to Ta 4 C 3 F x MXene interface layer, i.e. Ta formed on the outer surface of SiC fiber bundle filaments 4 C 3 F x An MXene interfacial layer;
step C: and after the ultrasonic replacement and drying treatment are finished, the heater and the drying furnace are closed, and the continuous ultrasonic device is stopped.
In step a, the concentration of the HF solution is 10%; the heating temperature of the HF solution is 80 ℃; the heating zone length of the drying furnace is 1.2m, and the heating temperature is 120 ℃.
In step B, the belt is Ta 4 SiC 3 The travel of the SiC fiber bundle filaments of the MAX phase interface layer in the ultrasonic groove is 2.4m, and the conveying speed is 0.06m/min; ultrasonic frequency is 80kHz, and ultrasonic power is 3kW; the Ta is 4 C 3 F x X=1.5 in the MXene interface layer.
In the fourth step, a continuous chemical vapor deposition device is adopted to conduct the treatment on the outer surface Ta of the SiC fiber bundle filaments 4 C 3 F x The method for removing F element in the MXene interface layer and doping B element simultaneously comprises the following steps in sequence:
Step a: will be provided with Ta 4 C 3 F x The SiC fiber bundle filaments of the MXene interface layer are arranged on a filament releasing roller in a filament releasing cabin, and the head part is pulled out to sequentially pass through a first heating furnace, a second heating furnace and a filament collecting cabin and is fixed on the filament collecting roller in the filament collecting cabin, and the filament collecting cabin is provided with Ta 4 C 3 F x The central axis of the SiC fiber bundle wire of the MXene interface layer, the central axis of the first heating furnace and the central axis of the second heating furnace are overlapped;
step b: closing the fifth air inlet pipe and the sixth air inlet pipe, and simultaneously opening a vacuum pump to vacuumize the interior of the continuous chemical vapor deposition device; opening a fifth air inlet pipe and a sixth air inlet pipe under the state of maintaining vacuumizing, and introducing argon into the continuous chemical vapor deposition device to maintain a certain pressure in the continuous chemical vapor deposition device; simultaneously, a second heating furnace is opened to raise the furnace temperature to a certain temperature;
step c: starting the yarn feeding roller and the yarn collecting rollerRoller conveyer belt with Ta 4 C 3 F x SiC fiber bundle filament of MXene interface layer, and Ta is carried 4 C 3 F x The SiC fiber bundle filaments of the MXene interface layer continuously move to pass through the first heating furnace and the second heating furnace in sequence; when carrying Ta 4 C 3 F x When the SiC fiber bundle wire of the MXene interface layer enters the second heating furnace, a third air inlet pipe is opened, and the second air inlet pipe is provided with Ta 4 C 3 F x In the process that SiC fiber bundle filaments of the MXene interface layer continuously pass through the second heating furnace, ta is removed 4 C 3 F x F element in MXene interface layer is doped with B element, and Ta can be prepared on the outer surface of the MXene interface layer 4 C 3 B x An MXene interfacial layer;
step d: and sequentially closing the third air inlet pipe, the second heating furnace, the vacuum pump, the fifth air inlet pipe and the sixth air inlet pipe, and stopping running the continuous chemical vapor deposition device.
In the step b, the flow rate of argon gas introduced into the continuous chemical vapor deposition device by the fifth air inlet pipe and the sixth air inlet pipe is 0.5L/min; the heating temperature of the second heating furnace is 1200 ℃ and the pressure is 20Pa; the first heating furnace does not start heating.
In step c, the belt is Ta 4 C 3 F x The conveying speed of the SiC fiber bundle filaments of the MXene interface layer is 0.2m/min; the third air inlet pipe is led into the second heating furnace with B 2 H 6 And H 2 Mixture of gases, B 2 H 6 Is 5% by volume of said B 2 H 6 And H 2 The flow rate of the mixed gas is 1L/min; the Ta is 4 C 3 B x X=0.5 in the MXene interface layer, which is 500nm thick.
In this example, in the preparation of Ta 4 SiC 3 Before the MAX phase interface layer, taC is prepared on the outer surface of the SiC fiber bundle silk x And a protective layer for protecting the SiC fiber bundle filaments from the attack of the Si source precursor and the HF solution. TaCl is firstly put into 5 Solid, siCl 4 Conversion of liquid to TaCl 5 Gas, siCl 4 After the gas is introduced into the first heating furnace and/or the second heating furnace. The outer surface Ta of the SiC fiber bundle filaments is subjected to continuous chemical vapor deposition 4 C 3 F x The F element in the MXene interface layer is removed, and in the process of doping the B element, the first heating furnace does not start heating, namely, the process only uses the second heating furnace and does not use the first heating furnace. Ta produced in step two of this example 4 SiC 3 The microstructure of the MAX phase interface layer is shown in FIG. 4, and Ta is prepared in the third step 4 C 3 F x The microstructure of the MXene interface layer is shown in FIG. 5, and Ta is prepared in the fourth step 4 C 3 B x The microstructure of the MXene interface layer is shown in fig. 6.
With Ta prepared in this example 4 C 3 B x SiC fiber bundle filaments of the MXene interface layer are used as raw materials, and a prepreg-infiltration method (Prep-MI) is adopted to prepare a 0 degree/90 degree layered SiC/SiC composite material; siC fiber bundle filaments with BN interface layers (prepared by adopting a CVD process) are used as raw materials, and the SiC/SiC composite material is prepared by adopting the CVD process. The CVD process and the prepreg-infiltration process used in this embodiment are all conventional methods, and no special requirements are made on the process parameters.
At the temperature of 1200 ℃ under the condition of 1', the atmosphere is 21% O 2 /79%N 2 (v/v), gas flow rate 5cm/s, time 500h "and condition 2" temperature 1200 ℃, atmosphere 100% H 2 O, gas flow rate 5cm/s, time 500 h' for SiC/SiC composite material with BN interface layer and Ta respectively 4 C 3 B x The SiC/SiC composite material of the MXene interface layer was examined, and the change in tensile strength was compared. Three samples are taken for comparison before and after the two SiC/SiC composite materials are checked.
The tensile strength of the SiC/SiC composite material with the BN interface layer before examination is 348+/-52 MPa (wherein 348MPa is the average value of the tensile strengths of three samples, 52MPa is the standard deviation, the interpretation method is applicable to the following data), the tensile strength after examination under the condition 1 is 299+/-53 MPa, the strength retention rate is 86%, the tensile strength after examination under the condition 2 is 211+/-48 MPa, and the strength retention rate is 61%; with Ta 4 C 3 B x Assessment of SiC/SiC composite material of MXene interface layerThe tensile strength before the test is 311+/-49 MPa, the tensile strength after the test under the condition 1 is 277+/-50 MPa, the strength retention rate is 89%, and the tensile strength after the test under the condition 2 is 253+/-42 MPa, and the strength retention rate is 81%. The results of the comparative tests of the two SiC/SiC composites are shown in FIG. 7.
In the embodiment, the corresponding MXene of the MAX phase with larger n is more stable, the element A is easily removed by HF solution when the element A is selected as Si, and the element B is doped to improve Ta 4 C 3 Oxidation resistance and four properties of MAX (MAX) are easily formed by three elements of Ta, si and C in a molar ratio of 4:1:3, and Ta is prepared by adopting a continuous Chemical Vapor Deposition (CVD) process firstly 4 SiC 3 MAX phase interface layer, then removing Si element by HF solution with concentration of 10% to form stable Ta 4 C 3 MXene, and finally adopting a continuous Chemical Vapor Deposition (CVD) process to further dope B element to prepare Ta 4 C 3 B x The MXene interface layer system can improve the service performance and service life of the SiC/SiC composite material in a high-temperature oxidation environment.
Embodiment two:
according to another preferred embodiment of the high temperature resistant and oxidation resistant interface layer of the SiC/SiC composite material and the preparation method, the design principle, the preparation method, the used device and the beneficial effects of the new interface layer material system are basically the same as those of the first embodiment, except that:
the new interface layer material system is Ta 4 C 3 B x MXene interface layer, where x=0.1.
Sequentially preparing TaC on the outer surface of the SiC fiber bundle filaments by adopting a continuous chemical vapor deposition device x Protective layer and Ta 4 SiC 3 In the method of MAX phase interface layer:
in the step (2), the flow rate of argon gas introduced into the continuous chemical vapor deposition device by the fifth air inlet pipe and the sixth air inlet pipe is 0.1L/min; the length of the heating zone of the first heating furnace is 0.5m, the heating temperature is 600 ℃, and the pressure is 60Pa; the heating area length of the second heating furnace is 0.8m, the heating temperature is 600 ℃, and the pressure is 60Pa.
In the step (3), the conveying speed of the SiC fiber bundle filaments is 0.1m/min; the first air inlet pipe is used for introducing TaCl into the first heating furnace 5 Gas and argon, the TaCl 5 The flow rate of the gas is 0.3L/min, and the flow rate of the argon is 0.7L/min; the second air inlet pipe is used for introducing CH into the first heating furnace 4 And argon gas, said CH 4 The flow rate of the argon is 0.225L/min, and the flow rate of the argon is 0.775L/min; the total flow of the gas introduced into the first heating furnace by the first air inlet pipe and the second air inlet pipe is equal; the TaCl 5 Gas and the CH 4 The molar ratio of (2) is 4:3; the TaC is x X=0.75 in the protective layer.
In the step (3), taCl is introduced into the second heating furnace through the third air inlet pipe 5 Gas, siCl 4 Gas and argon, the TaCl 5 The flow rate of the gas is 0.3L/min, and the SiCl is 4 The flow rate of the gas is 0.125L/min, and the flow rate of the argon is 0.575L/min; the fourth air inlet pipe is used for introducing CH into the second heating furnace 4 And argon gas, said CH 4 The flow rate of the argon is 0.225L/min, and the flow rate of the argon is 0.775L/min; the total flow of the gas introduced into the second heating furnace by the third air inlet pipe and the fourth air inlet pipe is equal; the TaCl 5 Gas, siCl 4 Gas and the CH 4 The molar ratio of (2) is 4:1:3.
Ta on the outer surface of SiC fiber bundle filaments by adopting continuous ultrasonic device 4 SiC 3 Conversion of MAX phase interface layer to Ta 4 C 3 F x In the method of the MXene interface layer:
in step a, the concentration of the HF solution is 10%; the heating temperature of the HF solution is 40 ℃; the heating zone length of the drying furnace is 0.8m, and the heating temperature is 100 ℃.
In step B, the belt is Ta 4 SiC 3 The travel of the SiC fiber bundle filaments of the MAX phase interface layer in the ultrasonic groove is 1.5m, and the conveying speed is 0.03m/min; the ultrasonic frequency is 40kHz, and the ultrasonic power is 1kW; the Ta is 4 C 3 F x X=1 in the MXene interface layer.
The outer surface Ta of the SiC fiber bundle filaments is subjected to continuous chemical vapor deposition 4 C 3 F x F element in the MXene interface layer is removed, and meanwhile, B element is doped in the method:
in the step b, the flow rate of argon gas introduced into the continuous chemical vapor deposition device by the fifth air inlet pipe and the sixth air inlet pipe is 0.1L/min; the heating temperature of the second heating furnace is 1000 ℃ and the pressure is 10Pa; the first heating furnace does not start heating.
In step c, the belt is Ta 4 C 3 F x The conveying speed of the SiC fiber bundle filaments of the MXene interface layer is 0.1m/min; the third air inlet pipe is led into the second heating furnace with B 2 H 6 And H 2 Mixture of gases, B 2 H 6 Is 5% by volume of said B 2 H 6 And H 2 The flow rate of the mixed gas is 0.6L/min; the Ta is 4 C 3 B x X=0.1 in the MXene interface layer, which is 200nm thick.
Embodiment III:
according to another preferred embodiment of the high temperature resistant and oxidation resistant interface layer of the SiC/SiC composite material and the preparation method, the design principle, the preparation method, the used device and the beneficial effects of the new interface layer material system are basically the same as those of the first embodiment, except that:
the new interface layer material system is Ta 4 C 3 B x MXene interface layer, where x=0.3.
Sequentially preparing TaC on the outer surface of the SiC fiber bundle filaments by adopting a continuous chemical vapor deposition device x Protective layer and Ta 4 SiC 3 In the method of MAX phase interface layer:
in the step (2), the flow rate of argon gas introduced into the continuous chemical vapor deposition device by the fifth air inlet pipe and the sixth air inlet pipe is 0.3L/min; the heating area of the first heating furnace is 0.6m in length, the heating temperature is 700 ℃, and the pressure is 80Pa; the heating area of the second heating furnace is 1m in length, the heating temperature is 700 ℃, and the pressure is 80Pa.
In step (3), the SiC fiber bundle filamentsThe conveying speed is 0.15m/min; the first air inlet pipe is used for introducing TaCl into the first heating furnace 5 Gas and argon, the TaCl 5 The flow rate of the gas is 0.4L/min, and the flow rate of the argon is 0.6L/min; the second air inlet pipe is used for introducing CH into the first heating furnace 4 And argon gas, said CH 4 The flow of the argon is 0.3L/min, and the flow of the argon is 0.7L/min; the total flow of the gas introduced into the first heating furnace by the first air inlet pipe and the second air inlet pipe is equal; the TaCl 5 Gas and the CH 4 The molar ratio of (2) is 4:3; the TaC is x X=0.85 in the protective layer.
In the step (3), taCl is introduced into the second heating furnace through the third air inlet pipe 5 Gas, siCl 4 Gas and argon, the TaCl 5 The flow rate of the gas is 0.4L/min, and the SiCl is 4 The flow rate of the gas is 0.1L/min, and the flow rate of the argon is 0.5L/min; the fourth air inlet pipe is used for introducing CH into the second heating furnace 4 And argon gas, said CH 4 The flow of the argon is 0.3L/min, and the flow of the argon is 0.7L/min; the total flow of the gas introduced into the second heating furnace by the third air inlet pipe and the fourth air inlet pipe is equal; the TaCl 5 Gas, siCl 4 Gas and the CH 4 The molar ratio of (2) is 4:1:3.
Ta on the outer surface of SiC fiber bundle filaments by adopting continuous ultrasonic device 4 SiC 3 Conversion of MAX phase interface layer to Ta 4 C 3 F x In the method of the MXene interface layer:
in step a, the concentration of the HF solution is 10%; the heating temperature of the HF solution is 60 ℃; the heating zone length of the drying furnace is 1m, and the heating temperature is 110 ℃.
In step B, the belt is Ta 4 SiC 3 The travel of the SiC fiber bundle filaments of the MAX phase interface layer in the ultrasonic groove is 2m, and the conveying speed is 0.045m/min; the ultrasonic frequency is 60kHz, and the ultrasonic power is 2kW; the Ta is 4 C 3 F x X=2 in the MXene interface layer.
The SiC fiber bundle filaments are processed by adopting a continuous chemical vapor deposition deviceOuter surface Ta 4 C 3 F x F element in the MXene interface layer is removed, and meanwhile, B element is doped in the method:
in the step b, the flow rate of argon gas introduced into the continuous chemical vapor deposition device by the fifth air inlet pipe and the sixth air inlet pipe is 0.3L/min; the heating temperature of the second heating furnace is 1100 ℃, and the pressure is 15Pa; the first heating furnace does not start heating.
In step c, the belt is Ta 4 C 3 F x The conveying speed of the SiC fiber bundle filaments of the MXene interface layer is 0.15m/min; the third air inlet pipe is led into the second heating furnace with B 2 H 6 And H 2 Mixture of gases, B 2 H 6 Is 5% by volume of said B 2 H 6 And H 2 The flow rate of the mixed gas is 0.8L/min; the Ta is 4 C 3 B x X=0.3 in the MXene interface layer, which is 300nm thick.
The specific description is as follows: the technical scheme of the invention relates to a plurality of parameters, and the beneficial effects and remarkable progress of the invention can be obtained by comprehensively considering the synergistic effect among the parameters. In addition, the value ranges of all the parameters in the technical scheme are obtained through a large number of tests, and aiming at each parameter and the mutual combination of all the parameters, the inventor records a large number of test data, and the specific test data are not disclosed herein for a long period of time. It will be appreciated by those skilled in the art that the SiC/SiC composite high temperature resistant and oxidation resistant interfacial layer and method of making of the present invention includes any combination of the foregoing summary of the invention and detailed description of the invention and the portions shown in the drawings, is limited in scope and does not describe each of these combinations in one-to-one fashion for simplicity of the description. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A high temperature resistant and oxidation resistant interface layer of SiC/SiC composite material is characterized in that: the interfacial layer is Ta 4 C 3 B x An interfacial layer of MXene,where x=0.1-0.5.
2. A preparation method of a high-temperature-resistant and oxidation-resistant interface layer of a SiC/SiC composite material is characterized by comprising the following steps: the method for preparing the high-temperature-resistant and oxidation-resistant interface layer of the SiC/SiC composite material of claim 1 comprises the following steps in sequence,
Step one: designing and assembling a continuous chemical vapor deposition device and a continuous ultrasonic device, so that the device can be normally used in the continuous chemical vapor deposition process and the continuous ultrasonic process;
step two: sequentially preparing TaC on the outer surface of SiC fiber bundle filaments by adopting a continuous chemical vapor deposition device x Protective layer and Ta 4 SiC 3 MAX phase interface layer;
step three: ta on outer surface of SiC fiber bundle filaments by adopting continuous ultrasonic device 4 SiC 3 Conversion of MAX phase interface layer to Ta 4 C 3 F x An MXene interfacial layer;
step four: adopting a continuous chemical vapor deposition device to perform chemical vapor deposition on the outer surface Ta of the SiC fiber bundle filaments 4 C 3 F x F element in the MXene interface layer is removed, and meanwhile B element is doped, so that the high-temperature-resistant and oxidation-resistant Ta of the SiC/SiC composite material can be prepared 4 C 3 B x MXene interface layer.
3. The method for preparing the high-temperature-resistant and oxidation-resistant interface layer of the SiC/SiC composite material, which is characterized by comprising the following steps of: the continuous chemical vapor deposition device comprises a wire unwinding cabin, a furnace tube and a wire winding cabin which are sequentially connected from left to right; a silk placing roller and a silk placing guide wheel are arranged in the silk placing cabin, and a fifth air inlet pipe is arranged outside the silk placing cabin; a wire collecting roller and a wire collecting guide wheel are arranged in the wire collecting cabin, and a sixth air inlet pipe is arranged outside the wire collecting cabin; a first heating furnace is arranged at one end of the furnace tube, which is close to the wire unwinding cabin, and a second heating furnace is arranged at one end of the furnace tube, which is close to the wire winding cabin; the one end that is close to of first heating furnace put silk cabin sets up first intake pipe and second intake pipe, the second heating furnace is close to the one end of first heating furnace sets up third intake pipe and fourth intake pipe, the second heating furnace is close to the one end of receipts silk cabin sets up the tail gas pipe, the end-to-end connection vacuum pump of tail gas pipe.
4. The method for preparing the high temperature resistant and oxidation resistant interface layer of the SiC/SiC composite material according to claim 3, which is characterized in that: the continuous ultrasonic device comprises a wire unwinding roller, an ultrasonic assembly, a drying furnace and a wire winding roller which are sequentially arranged from left to right; the ultrasonic assembly comprises an ultrasonic groove, an ultrasonic rod, four driving rollers, a heater and a sound-proof cover, wherein the ultrasonic groove is filled with HF solution, the four driving rollers are arranged in the ultrasonic groove and are positioned below the liquid level of the HF solution, the ultrasonic rod is perpendicular to the ultrasonic groove, one end of the ultrasonic rod is inserted into the HF solution, and the heater is arranged at the bottom of the ultrasonic groove; and a plurality of guide rollers are arranged on the continuous ultrasonic device.
5. The method for preparing the high-temperature-resistant and oxidation-resistant interface layer of the SiC/SiC composite material, which is characterized in that: in the second step, adopting a continuous chemical vapor deposition device to sequentially prepare TaC on the outer surface of the SiC fiber bundle filaments x Protective layer and Ta 4 SiC 3 The method of the MAX phase interface layer comprises the following steps according to the sequence,
step (1): installing SiC fiber bundle filaments on a filament placing roller in a filament placing cabin, pulling out the head of the SiC fiber bundle filaments to sequentially pass through a first heating furnace, a second heating furnace and a filament collecting cabin, and fixing the SiC fiber bundle filaments on the filament collecting roller in the filament collecting cabin, wherein the central axis of the SiC fiber bundle filaments, the central axis of the first heating furnace and the central axis of the second heating furnace are coincident at the moment;
Step (2): closing the fifth air inlet pipe and the sixth air inlet pipe, and simultaneously opening a vacuum pump to vacuumize the interior of the continuous chemical vapor deposition device; opening a fifth air inlet pipe and a sixth air inlet pipe under the state of maintaining vacuumizing, and introducing argon into the continuous chemical vapor deposition device to maintain a certain pressure in the continuous chemical vapor deposition device; simultaneously opening the first heating furnace and the second heating furnace to raise the furnace temperature to a certain temperature;
step (3): starting a wire releasing roller and a wire collecting roller to convey SiC fiber bundle wires, so that the SiC fiber bundle wires continuously move and sequentially pass through a first heating furnace and a second heating furnace; when the SiC fiber bundle wire enters the first heating furnace, the first air inlet pipe and the second air inlet pipe are simultaneously opened, and after the SiC fiber bundle wire continuously passes through the first heating furnace, taC can be prepared on the outer surface of the SiC fiber bundle wire x A protective layer; when the SiC fiber bundle wire enters the second heating furnace, the third air inlet pipe and the fourth air inlet pipe are simultaneously opened, and Ta can be prepared on the outer surface of the SiC fiber bundle wire after continuously passing through the second heating furnace 4 SiC 3 MAX phase interface layer;
step (4): taC for external surface of SiC fiber bundle x Protective layer and Ta 4 SiC 3 And after the preparation of the MAX phase interface layer is finished, sequentially closing the third air inlet pipe, the fourth air inlet pipe, the first air inlet pipe, the second air inlet pipe, the first heating furnace, the second heating furnace, the vacuum pump, the fifth air inlet pipe and the sixth air inlet pipe, and stopping running the continuous chemical vapor deposition device.
6. The method for preparing the high-temperature-resistant and oxidation-resistant interface layer of the SiC/SiC composite material, which is characterized in that: in the step (2), the flow rate of argon gas introduced into the continuous chemical vapor deposition device by the fifth air inlet pipe and the sixth air inlet pipe is 0.1-0.5L/min; the heating area of the first heating furnace is 0.5-0.8m in length, the heating temperature is 600-800 ℃, and the pressure is 60-100Pa; the heating area of the second heating furnace is 0.8-1.2m in length, the heating temperature is 600-800 ℃ and the pressure is 60-100Pa;
in the step (3), the conveying speed of the SiC fiber bundle filaments is 0.1-0.2m/min; the first air inlet pipe is used for introducing TaCl into the first heating furnace 5 Gas and argon, the TaCl 5 The flow rate of the gas is 0.3-0.5L/min, and the flow rate of the argon is 0.5-0.7L/min; the second air inlet pipe is used for introducing CH into the first heating furnace 4 And argon gas, said CH 4 The flow rate of the argon is 0.225-0.375L/min, and the flow rate of the argon is 0.625-0.775L/min; the first air inlet pipeThe total flow of the gas introduced into the first heating furnace by the second air inlet pipe is equal; the TaCl 5 Gas and the CH 4 The molar ratio of (2) is 4:3; the TaC is x X=0.75-1 in the protective layer;
In the step (3), taCl is introduced into the second heating furnace through the third air inlet pipe 5 Gas, siCl 4 Gas and argon, the TaCl 5 The flow rate of the gas is 0.3-0.5L/min, and the SiCl is 4 The flow rate of the gas is 0.075-0.125L/min, and the flow rate of the argon is 0.375-0.625L/min; the fourth air inlet pipe is used for introducing CH into the second heating furnace 4 And argon gas, said CH 4 The flow rate of the argon is 0.225-0.375L/min, and the flow rate of the argon is 0.625-0.775L/min; the total flow of the gas introduced into the second heating furnace by the third air inlet pipe and the fourth air inlet pipe is equal; the TaCl 5 Gas, siCl 4 Gas and the CH 4 The molar ratio of (2) is 4:1:3.
7. The method for preparing the high-temperature-resistant and oxidation-resistant interface layer of the SiC/SiC composite material, which is characterized in that: in the third step, a continuous ultrasonic device is adopted to carry out Ta on the outer surface of the SiC fiber bundle filaments 4 SiC 3 Conversion of MAX phase interface layer to Ta 4 C 3 F x The method of the MXene interface layer comprises the following steps in sequence,
step A: will be provided with Ta 4 SiC 3 The SiC fiber bundle filaments of the MAX phase interface layer are arranged on a wire releasing roller, and the head part is pulled out to sequentially pass through an ultrasonic groove and a drying furnace and is fixed on a wire collecting roller; pouring HF solution into an ultrasonic tank to enable four driving rollers and the belt to be Ta 4 SiC 3 The SiC fiber bundle filaments of the MAX phase interface layer are positioned below the liquid level of the HF solution; the heater is opened to heat the HF solution in the ultrasonic tank, and the drying furnace is opened to raise the furnace temperature to a certain temperature;
and (B) step (B): starting the pay-off roller, the driving roller and the take-up roller conveyer belt with Ta 4 SiC 3 SiC fiber bundle filament with MAX phase interface layer, and Ta 4 SiC 3 Continuous transport of SiC fiber bundles of MAX phase boundary layerSequentially passing through an ultrasonic tank and a drying furnace, and respectively performing ultrasonic replacement and drying treatment; with Ta 4 SiC 3 In the process that the SiC fiber bundle filaments of the MAX phase interface layer continuously pass through the ultrasonic tank, the HF solution is used for Ta 4 SiC 3 Substitution of Si element in MAX phase, ta 4 SiC 3 Conversion of MAX phase interface layer to Ta 4 C 3 F x MXene interface layer, i.e. Ta formed on the outer surface of SiC fiber bundle filaments 4 C 3 F x An MXene interfacial layer;
step C: and after the ultrasonic replacement and drying treatment are finished, the heater and the drying furnace are closed, and the continuous ultrasonic device is stopped.
8. The method for preparing the high-temperature-resistant and oxidation-resistant interface layer of the SiC/SiC composite material, which is characterized in that: in step a, the concentration of the HF solution is 10%; the heating temperature of the HF solution is 40-80 ℃; the heating area of the drying furnace is 0.8-1.2m in length and the heating temperature is 100-120 ℃;
In step B, the belt is Ta 4 SiC 3 The travel of the SiC fiber bundle filaments of the MAX phase boundary layer in the ultrasonic groove is 1.5-2.4m, and the conveying speed is 0.03-0.06m/min; the ultrasonic frequency is 40-80kHz, and the ultrasonic power is 1-3kW; the Ta is 4 C 3 F x X=1-2 in the MXene interface layer.
9. The method for preparing the high-temperature-resistant and oxidation-resistant interface layer of the SiC/SiC composite material, which is characterized in that: in the fourth step, a continuous chemical vapor deposition device is adopted to conduct the treatment on the outer surface Ta of the SiC fiber bundle filaments 4 C 3 F x The method for removing F element and doping B element in MXene interface layer comprises the following steps in sequence,
step a: will be provided with Ta 4 C 3 F x The SiC fiber bundle filaments of the MXene interface layer are arranged on a filament releasing roller in a filament releasing cabin, and the head part is pulled out to sequentially pass through a first heating furnace, a second heating furnace and a filament collecting cabin and is fixed on the filament collecting roller in the filament collecting cabin, and the filament collecting cabin is provided with Ta 4 C 3 F x The central axis of the SiC fiber bundle wire of the MXene interface layer, the central axis of the first heating furnace and the central axis of the second heating furnace are overlapped;
step b: closing the fifth air inlet pipe and the sixth air inlet pipe, and simultaneously opening a vacuum pump to vacuumize the interior of the continuous chemical vapor deposition device; opening a fifth air inlet pipe and a sixth air inlet pipe under the state of maintaining vacuumizing, and introducing argon into the continuous chemical vapor deposition device to maintain a certain pressure in the continuous chemical vapor deposition device; simultaneously, a second heating furnace is opened to raise the furnace temperature to a certain temperature;
Step c: starting the godet and godet conveyer belt with Ta 4 C 3 F x SiC fiber bundle filament of MXene interface layer, and Ta is carried 4 C 3 F x The SiC fiber bundle filaments of the MXene interface layer continuously move to pass through the first heating furnace and the second heating furnace in sequence; when carrying Ta 4 C 3 F x When the SiC fiber bundle wire of the MXene interface layer enters the second heating furnace, a third air inlet pipe is opened, and the second air inlet pipe is provided with Ta 4 C 3 F x In the process that SiC fiber bundle filaments of the MXene interface layer continuously pass through the second heating furnace, ta is removed 4 C 3 F x F element in MXene interface layer is doped with B element, and Ta can be prepared on the outer surface of the MXene interface layer 4 C 3 B x An MXene interfacial layer;
step d: and sequentially closing the third air inlet pipe, the second heating furnace, the vacuum pump, the fifth air inlet pipe and the sixth air inlet pipe, and stopping running the continuous chemical vapor deposition device.
10. The method for preparing the high-temperature-resistant and oxidation-resistant interface layer of the SiC/SiC composite material, which is characterized by comprising the following steps of:
in the step b, the flow rate of argon gas introduced into the continuous chemical vapor deposition device by the fifth air inlet pipe and the sixth air inlet pipe is 0.1-0.5L/min; the heating temperature of the second heating furnace is 1000-1200 ℃ and the pressure is 10-20Pa; the first heating furnace is not started to heat;
in step c, the belt is Ta 4 C 3 F x The conveying speed of the SiC fiber bundle filaments of the MXene interface layer is 0.1-0.2m/min; the third air inlet pipe is led into the second heating furnace with B 2 H 6 And H 2 Mixture of gases, B 2 H 6 Is 5% by volume of said B 2 H 6 And H 2 The flow rate of the mixed gas is 0.6-1L/min; the Ta is 4 C 3 B x X=0.1-0.5 in the MXene interface layer.
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