CN115650750B - Composite material containing high-low modulus lamellar matrix and preparation method thereof - Google Patents
Composite material containing high-low modulus lamellar matrix and preparation method thereof Download PDFInfo
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- 239000011159 matrix material Substances 0.000 title claims abstract description 93
- 239000002131 composite material Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000835 fiber Substances 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 31
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 26
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005336 cracking Methods 0.000 claims abstract description 18
- 238000000151 deposition Methods 0.000 claims abstract description 15
- 238000005452 bending Methods 0.000 claims abstract description 9
- 238000011065 in-situ storage Methods 0.000 claims abstract description 8
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 12
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 12
- 229920002554 vinyl polymer Polymers 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 230000008021 deposition Effects 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- 239000003292 glue Substances 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 208
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 133
- 238000007598 dipping method Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000008096 xylene Substances 0.000 abstract description 4
- 230000008595 infiltration Effects 0.000 abstract description 2
- 238000001764 infiltration Methods 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000003776 cleavage reaction Methods 0.000 description 3
- 230000007017 scission Effects 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
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- 238000007654 immersion Methods 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
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Abstract
The invention relates to SiC containing high-low modulus lamellar matrix f /((C‑SiC) m ‑SiC) n Composite material, preparation method thereof and SiC f /((C‑SiC) m ‑SiC) n The composite material consists of SiC fibers, BN interfaces and a layered matrix with high and low moduli alternately distributed, wherein the low modulus matrix layer is a C-SiC layer prepared by a precursor dipping cracking method, and the high modulus matrix layer is a SiC layer prepared by a chemical vapor deposition method. The technical method of the invention comprises the following steps: pretreating a silicon carbide fiber preform, depositing a BN interface phase, adopting a low-concentration polycarbosilane xylene solution to generate a low-modulus C-SiC lamellar matrix in situ, adopting a chemical vapor infiltration technology to deposit a high-modulus SiC matrix, alternately preparing the high-modulus matrix and the low-modulus matrix, and finally obtaining compact SiC f /((C‑SiC) m ‑SiC) n A composite material. The composite material prepared by the method has extremely excellent mechanical property, the bending strength can reach 1507+/-122 MPa, and the fracture toughness can reach 58+/-3.5 MPa.m 1/2 The highest tensile strength can reach 889+/-71 MPa.
Description
Technical Field
The invention belongs to SiC f The technical field of preparation of/SiC, relates to a composite material containing a high-low modulus lamellar matrix and a preparation method thereof, in particular to SiC containing a high-low modulus lamellar matrix f /((C-SiC) m -SiC) n Composite materials and methods of making the same.
Background
As aircraft speeds increase, the thrust-to-weight ratio of the aircraft engines increases, and the service conditions of hot-end components of the aircraft engines become increasingly stringent. When the thrust-weight ratio of the aero-engine is further increased to 12-15The average temperature of the turbine inlet of an aeroengine will be as high as 1800 ℃, and high temperature alloys will be difficult to meet operating temperature requirements. Continuous SiC fiber reinforced SiC matrix (SiC f The SiC) composite material has excellent performances of high temperature resistance, high strength, high modulus, oxidation resistance, creep resistance and the like, and is expected to become an ideal thermal structure material of the next generation of high thrust-weight ratio engine.
SiC f The SiC composite material mainly comprises three parts of SiC fibers, an interface phase and a SiC matrix, wherein the SiC fibers play a bearing role; the interface phase has the functions of adjusting interface bonding strength, deflecting cracks, transmitting load, relieving stress and the like, and realizes SiC f The key of non-brittle fracture and high strength and toughness of the SiC composite material; the SiC matrix mainly plays roles of material forming, fiber and interface protection, load transmission and the like.
At present SiC f The SiC composite material mainly realizes lower interface bonding strength by preparing weak interface phases with low breaking energy such as BN, pyC and the like between the fiber and the matrix, so that cracks deflect at interfaces (F/I) between the fiber and the interface phases, interfaces (I/M) between the interface phases and the matrix or inside the interface phases, and the crack propagation path is prolonged, thereby improving the strength and toughness of the composite material and avoiding brittle fracture. Research has demonstrated that crack deflection is SiC f Core stiffening mechanism of SiC composite.
Although by introducing interfacial phase, siC f The SiC composite material has better mechanical property, but is oriented to the future high thrust-weight ratio engine hot end part, especially the application of the rotating part, and the current SiC f The strength and toughness of the SiC composite remain significantly inadequate. For example, new generation engine rotor blades are subjected to centrifugal forces greater than 250MPa, i.e., require material ratio limits of at least greater than 250MPa, while 2D SiC produced by CVI processes f The room temperature tensile strength of the SiC composite material is generally about 350MPa, the proportion limit is about 150-180 MPa, and the mechanical property is improved by 50%.
SiC matrix on SiC f The volume fraction in the SiC composite material is high, if the structural design of the matrix is adopted, cracks can deflect in the matrix, the stress of crack tips is released, the crack propagation path is prolonged, and the crack is startedThe strengthening mechanism of the dynamic matrix is expected to further improve the SiC f Mechanical properties of SiC composite material. SiC (SiC) f The conditions for realizing crack deflection of the SiC matrix in the SiC composite material are as follows: (1) the substrate has a layered structure; (2) there is a difference in high and low modulus between the layers of the matrix. Accordingly, the invention provides SiC containing high-low modulus lamellar matrix f Low cost, short cycle, convenient preparation technique of the SiC composite material.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides SiC containing a high-low modulus lamellar matrix f /((C-SiC) m -SiC) n Composite material and preparation method thereof, simple and reliable process, and the prepared composite material is similar to traditional SiC containing single-phase homogeneous SiC matrix f Compared with the SiC composite material, the strength and toughness are improved by more than 50 percent.
Technical proposal
SiC containing high-low modulus lamellar matrix f /((C-SiC) m -SiC) n The composite material is characterized by comprising SiC fibers, BN interfaces and a layered matrix with high and low moduli alternately distributed; depositing a high modulus SiC substrate on a low modulus C-SiC layered substrate, followed by alternating high modulus and low modulus substrates; the C-SiC matrix layer is matched with the high-low modulus of the high-modulus SiC matrix layer, so that cracks deflect at the interface of the two matrixes.
The thickness of the C layer in the low-modulus C-SiC layered matrix is about 50-100 nm, the thickness of the SiC layer is about 300-500 nm, and the overall modulus of the C-SiC layered matrix layer is 200-250Gpa.
The high-modulus SiC matrix is a high-crystallinity SiC matrix, the thickness of the SiC matrix layer is 1 mu m, and the modulus is 400-450 Gpa.
The SiC is provided with f /((C-SiC) m -SiC) n The density of the composite material is more than 2.5g/cm 3 The open porosity is less than 10%; the bending strength of the material is up to 1507+/-122 MPa, and the fracture toughness is up to 58+/-3.5 MPa.m 1/2 The tensile strength is 889+/-71 MPa at most.
A kind of instituteSiC comprising a high and low modulus layered matrix f /((C-SiC) m -SiC) n The preparation method of the composite material is characterized by comprising the following steps:
step 1: for SiC f Performing glue removal pretreatment on the fiber preform, and preparing a layer of BN interface phase on the surface of the fiber;
step 2: immersing the preform with the BN interface phase deposited in a low-concentration polycarbosilane solution, taking out the preform, and removing redundant solution; then putting the mixture into a cracking furnace, cracking the mixture in Ar atmosphere, and converting the mixture into a low-modulus lamellar C-SiC matrix in situ by polycarbosilane; repeating the process for m times to prepare (C-SiC) inside the composite material m A multicycle low modulus matrix;
the polycarbosilane in the low-concentration polycarbosilane solution is vinyl-containing polycarbosilane, the solvent is dimethylbenzene, and the mass ratio of dimethylbenzene to vinyl-containing polycarbosilane is 15:1-40:1;
step 3: will be prepared (C-SiC) m Placing the intermediate of the multicycle low-modulus matrix into a SiC deposition furnace to deposit a high-modulus layered SiC matrix;
alternately repeating the step 2 and the step 3 to obtain the SiC containing the high-low modulus lamellar matrix f /((C-SiC) m -SiC) n A composite material; n in the material is the number of repetitions.
The step of glue discharging pretreatment in the step 1 is as follows: after soaking the SiC fiber preform with boiling water, washing the SiC fiber preform with deionized water, and then putting the SiC fiber preform into an oven for drying.
The cracking process in the step 2 is as follows: ar gas flow is 200ml/min, heating program is 10 ℃/min, heating from room temperature to 220 ℃, preserving heat for 2h, heating from 220 ℃ to 1000-1300 ℃ at 10 ℃/min, preserving heat for 2h, cooling from 1000-1300 ℃ to 600 ℃ at 5 ℃/min, and naturally cooling.
The preparation process of the BN interface phase in the step 1 is chemical vapor deposition, and the BN thickness is 150-250nm.
The preform in the step 1 is one of a unidirectional SiC fiber preform, a 2D SiC fiber preform, a 2.5DSiC fiber preform or a 3DSiC fiber preform, wherein the fiber volume fraction is 30-50%.
M in the step 2 is repeated for 1-3 times; the repetition number n in the step 3 is 6-10.
Advantageous effects
The invention provides SiC containing high-low modulus lamellar matrix f /((C-SiC) m -SiC) n Composite material, preparation method thereof and SiC f /((C-SiC) m -SiC) n The composite material consists of SiC fibers, BN interfaces and a layered matrix with high and low moduli alternately distributed, wherein the low modulus matrix layer is a C-SiC layer prepared by a precursor dipping cracking method, and the high modulus matrix layer is a SiC layer prepared by a chemical vapor deposition method. The technical method of the invention comprises the following steps: pretreating a silicon carbide fiber preform, depositing a BN interface phase, adopting a low-concentration polycarbosilane xylene solution to generate a low-modulus C-SiC lamellar matrix in situ, adopting a chemical vapor infiltration technology to deposit a high-modulus SiC matrix, alternately preparing the high-modulus matrix and the low-modulus matrix, and finally obtaining compact SiC f /((C-SiC) m -SiC) n A composite material. The composite material prepared by the method has extremely excellent mechanical property, the bending strength can reach 1507+/-122 MPa, and the fracture toughness can reach 58+/-3.5 MPa.m 1/2 The highest tensile strength can reach 889+/-71 MPa.
The beneficial effects of the invention are as follows:
(1) The matrix prepared by the invention is of a layered structure, and the high and low modulus difference exists between different matrix layers. The modulus difference between the low modulus C-SiC matrix layer and the high modulus SiC matrix layer is up to 250GPa, and the obvious difference makes cracks more easily deflect between the two matrixes, prolongs the crack propagation path, and makes the composite material performance more excellent. With SiC containing a single-phase homogeneous SiC matrix f Compared with the SiC composite material, the SiC prepared by the invention f The mechanical property of the SiC composite material is improved by more than 50 percent.
(2) The preparation method of the low-modulus C-SiC matrix layer is a PIP method, and the C layer and the SiC layer can be prepared simultaneously by one-time immersion cracking, wherein the thickness of the C layer is about 50-100 nm, and the thickness of the SiC layer is about 300-500 nm. Compared with the prior reported method for preparing the C-SiC layer by alternating deposition by adopting a chemical vapor deposition method, the method for preparing the C-SiC layer has the advantages of simple process, short period, better matching property of the prepared C-SiC matrix layer and the high-modulus SiC layer and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 SiC prepared in example 1 of the present invention f /((C-SiC) 3 -SiC) 6 TEM image of C-SiC layer in composite material.
FIG. 3 SiC prepared in example 1 of the present invention f /((C-SiC) 3 -SiC) 6 Bending stress-displacement curve of the composite material.
FIG. 4 SiC prepared in example 1 of the present invention f /((C-SiC) 3 -SiC) 6 Tensile stress-strain curve of the composite material.
Detailed Description
The invention will now be further described with reference to examples, figures:
SiC containing high-low modulus lamellar matrix f /((C-SiC) m -SiC) n The preparation method of the composite material is characterized by comprising the following steps:
(1) For SiC f Performing glue removal pretreatment on the fiber preform, and preparing a layer of BN interface phase on the surface of the fiber;
(2) Immersing the preform with the BN interface phase deposited in a low-concentration polycarbosilane solution, taking out the preform, placing the preform on a dried sponge for 5min, absorbing the redundant solution, directly placing the preform into a cracking furnace, and cracking in Ar atmosphere to prepare the low-modulus lamellar C-SiC matrix. Repeating the steps m times to prepare (C-SiC) inside the composite material m A multicycle low modulus matrix. M in the material is 1-3 times;
(3) Placing the intermediate obtained in the step (2) into a SiC chemical vapor deposition furnace to deposit a high-modulus SiC matrix;
(4) Alternately repeating the steps (2) and (3) to finally obtain the SiC containing the high-low modulus lamellar matrix f /((C-SiC) m -SiC) n A composite material. N in the material is 6-10 times.
Preferably, the step of pre-treating the adhesive discharge in the step (1) is as follows: soaking the SiC fiber preform with boiling water at 100 ℃ for 10min for three times, then flushing the SiC fiber preform with deionized water for three times, and finally placing the SiC fiber preform into an oven to keep the temperature at 150 ℃ for 2h for drying.
Preferably, the preform in step (1) may be one of a unidirectional (1D) SiC fiber preform, a two-dimensional (2D) SiC fiber preform, a two-dimensional half (2.5D) SiC fiber preform, and a three-dimensional (3D) SiC fiber preform.
Preferably, the preparation process of the BN interface phase in the step (1) is a chemical vapor deposition method, and the thickness of the BN interface phase is 150-250nm.
Preferably, the low modulus C-SiC substrate layer in step (2) is converted in situ from polycarbosilane without separate preparation.
Preferably, in the low-concentration polycarbosilane solution in the step (2), the polycarbosilane is vinyl-containing polycarbosilane, the solvent is xylene, and the mass ratio of the xylene to the vinyl-containing polycarbosilane is 15:1-40:1.
Preferably, the cleavage process in step (2) is: ar gas flow is 200ml/min, heating program is 10 ℃/min, heating from room temperature to 220 ℃, preserving heat for 2h, heating from 220 ℃ to 1000-1300 ℃ at 10 ℃/min, preserving heat for 2h, cooling from 1000-1300 ℃ to 600 ℃ at 5 ℃/min, and then naturally cooling.
Preferably, the matrix prepared in the step (2) is a layered C-SiC matrix, the thickness of the C layer in one cycle (i.e. m=1) is 50 to 100nm, the thickness of the SiC layer is 300 to 500nm, and the overall modulus of the C-SiC matrix layer is about 200 to 250GPa.
Preferably, the matrix prepared in step (3) is a high crystallinity (99.8%) SiC matrix, the SiC matrix layer having a thickness of about 1 μm and a modulus of about 400 to 450GPa.
Preferably, the low-modulus C-SiC matrix layer prepared in the step (2) and the high-modulus SiC matrix layer prepared in the step (3) can realize the high-low modulus matching design of the composite material matrix, so that cracks deflect at the interface of the two matrixes, and the mechanical property of the composite material is further improved.
Technical solutions in specific embodiments of the present invention will be clearly described below, and it is obvious that the described embodiments are only some of the embodiments of the present invention. Based on the embodiments of the present invention, those of ordinary skill in the art may obtain other embodiments without making any inventive effort and without departing from the methods provided by the present invention.
Example 1
(1) Performing glue removal pretreatment on the 1D SiC fiber preform: the fiber volume fraction of the preform is 40%, the SiC fiber preform is soaked in boiling water at 100 ℃ for 10min for three times, then the SiC fiber preform is rinsed with deionized water for three times, and then the fiber preform is put into an oven for heat preservation at 150 ℃ for 2h and dried.
(2) Depositing BN interface phase: and (3) putting the dried SiC fiber preform into a BN deposition furnace to deposit BN with the thickness of about 200 nm.
(3) Preparing a low-modulus lamellar C-SiC matrix: vacuum dipping the preform deposited with BN interface phase into a low-concentration vinyl-containing polycarbosilane solution for 1 hour, wherein the mass ratio of the solution concentration of dimethylbenzene to the vinyl-containing polycarbosilane is 20:1; taking out the preform, placing on a dried sponge for 5min, and absorbing excessive solution; placing the preform into a cracking furnace, vacuumizing, and then cracking in Ar atmosphere, wherein Ar gas flow is 200ml/min; heating to a temperature of 220 ℃ from room temperature at a speed of 10 ℃/min, preserving heat for 2 hours, heating to 1300 ℃ from 220 ℃ at a speed of 10 ℃/min, preserving heat for 2 hours, cooling to 600 ℃ from 1300 ℃ at a speed of 5 ℃/min, and naturally cooling to prepare the C-SiC layer in situ, wherein the thickness of the C layer is about 100nm, and the thickness of the SiC layer is about 500 nm. Repeated dipping and cracking for 3 times to prepare (C-SiC) 3 Low modulus matrix to obtain SiC f /(C-SiC) 3 An intermediate.
(4) Preparing a high-modulus lamellar SiC matrix: and (3) placing the intermediate obtained in the step (3) into a SiC deposition furnace to deposit a high-modulus layered SiC matrix, wherein the thickness of the matrix is about 1 mu m.
(5) Alternately repeating the step (3) and the step (4) for 6 times to obtain SiC f /((C-SiC) 3 -SiC) 6 The open porosity of the composite material is reduced to 9.3 percent, and the density of the obtained material is 2.57g/cm 3 The bending strength can reach 1507MPa, and the fracture toughness can reach 58 MPa.m 1/2 The tensile strength can reach 889MPa, and the proportion limitMore than 600MPa, and mechanical property is compared with that of 1D SiC prepared by pure PIP technology f The SiC composite material is improved by more than 50 percent (1D SiC prepared by pure PIP technology) f The bending strength of the SiC composite material is 900MPa, and the fracture toughness is 37 MPa.m 1/2 The tensile strength is 550MPa, and the proportion limit is 200 MPa).
Example 2
(1) Performing glue removal pretreatment on the 2D SiC fiber preform: the fiber volume fraction of the preform is 40%, the SiC fiber preform is soaked in boiling water at 100 ℃ for 10min for three times, then the SiC fiber preform is rinsed with deionized water for three times, and then the fiber preform is put into an oven for heat preservation at 150 ℃ for 2h and dried.
(2) Depositing BN interface phase: and (3) putting the dried SiC fiber preform into a BN deposition furnace to deposit BN with the thickness of about 200 nm.
(3) Preparing a low-modulus lamellar C-SiC matrix: vacuum dipping the preform deposited with BN interface phase into a low-concentration vinyl-containing polycarbosilane solution for 1 hour, wherein the mass ratio of the solution concentration of dimethylbenzene to the vinyl-containing polycarbosilane is 20:1; taking out the preform, placing on a dried sponge for 5min, and absorbing excessive solution; placing the preform into a cracking furnace, vacuumizing, and then cracking in Ar atmosphere, wherein Ar gas flow is 200ml/min; heating to a temperature of 220 ℃ from room temperature at a speed of 10 ℃/min, preserving heat for 2 hours, heating to 1300 ℃ from 220 ℃ at a speed of 10 ℃/min, preserving heat for 2 hours, cooling to 600 ℃ from 1300 ℃ at a speed of 5 ℃/min, and naturally cooling to prepare the C-SiC layer in situ, wherein the thickness of the C layer is about 100nm, and the thickness of the SiC layer is about 500 nm. Repeated impregnation cleavage 3 times, low modulus (C-SiC) was prepared 3 A substrate to obtain SiC f /(C-SiC) 3 An intermediate.
(4) Preparing a high-modulus lamellar SiC matrix: and (3) placing the intermediate obtained in the step (3) into a SiC deposition furnace to deposit a high-modulus layered SiC matrix, wherein the thickness of the matrix is about 1 mu m.
(5) Alternately repeating the step (3) and the step (4) for 7 times to obtain SiC f /((C-SiC) 3 -SiC) 7 The open porosity of the composite material is reduced to 9.8 percent, and the density of the obtained material is 2.53g/cm 3 The bending strength can reach 921MPa, and the fracture toughness can reach 36.3 MPa.m 1/2 The tensile strength can reach 450MPa.
Example 3
(1) Performing glue removal pretreatment on the 2.5D SiC fiber preform: the fiber volume fraction of the preform is 40%, the SiC fiber preform is soaked in boiling water at 100 ℃ for 10min for three times, then the SiC fiber preform is rinsed with deionized water for three times, and then the fiber preform is put into an oven for heat preservation at 150 ℃ for 2h and dried.
(2) Depositing BN interface phase: and (3) putting the dried SiC fiber preform into a BN deposition furnace to deposit BN with the thickness of about 200 nm.
(6) Preparing a low-modulus lamellar C-SiC matrix: vacuum dipping the preform deposited with BN interface phase into a low-concentration vinyl-containing polycarbosilane solution for 1 hour, wherein the mass ratio of the solution concentration of dimethylbenzene to the vinyl-containing polycarbosilane is 20:1; taking out the preform, placing on a dried sponge for 5min, and absorbing excessive solution; placing the preform into a cracking furnace, vacuumizing, and then cracking in Ar atmosphere, wherein Ar gas flow is 200ml/min; heating to a temperature of 220 ℃ from room temperature at a speed of 10 ℃/min, preserving heat for 2 hours, heating to 1300 ℃ from 220 ℃ at a speed of 10 ℃/min, preserving heat for 2 hours, cooling to 600 ℃ from 1300 ℃ at a speed of 5 ℃/min, and naturally cooling to prepare the C-SiC layer in situ, wherein the thickness of the C layer is about 100nm, and the thickness of the SiC layer is about 500 nm. Repeated impregnation cleavage 3 times, low modulus (C-SiC) was prepared 3 A substrate to obtain SiC f /(C-SiC) 3 An intermediate.
(7) Preparing a high-modulus lamellar SiC matrix: and (3) placing the intermediate obtained in the step (3) into a SiC deposition furnace to deposit a high-modulus layered SiC matrix, wherein the thickness of the matrix is about 1 mu m.
Alternately repeating the step (3) and the step (4) for 7 times to obtain SiC f /((C-SiC) 3 -SiC) 7 The open porosity of the composite material is reduced to 9.1 percent, and the density of the obtained material is 2.55g/cm 3 The bending strength can reach 1320MPa, and the fracture toughness can reach 47 MPa.m 1/2 The tensile strength can reach 727MPa.
Claims (7)
1. SiC containing high-low modulus lamellar matrix f /((C-SiC) m -SiC) n The preparation method of the composite material is characterized by comprising the following steps:
step 1: for SiC f Performing glue removal pretreatment on the fiber preform, and preparing a layer of BN interface phase on the surface of the fiber;
step 2: immersing the preform with the BN interface phase deposited in a low-concentration polycarbosilane solution, taking out the preform, and removing redundant solution; then putting the mixture into a cracking furnace, cracking the mixture in Ar atmosphere, and converting the mixture into a low-modulus lamellar C-SiC matrix in situ by polycarbosilane; repeating the process for m times to prepare (C-SiC) inside the composite material m A multicycle low modulus matrix;
the cracking process comprises the following steps: ar gas flow is 200ml/min, heating program is 10 ℃/min, heating from room temperature to 220 ℃, heat preservation is carried out for 2h,10 ℃/min is heated from 220 ℃ to 1000-1300 ℃, heat preservation is carried out for 2h,5 ℃/min is cooled from 1000-1300 ℃ to 600 ℃ and then natural cooling is carried out;
the polycarbosilane in the low-concentration polycarbosilane solution is vinyl-containing polycarbosilane, the solvent is dimethylbenzene, and the mass ratio of dimethylbenzene to vinyl-containing polycarbosilane is 15:1-40:1;
the thickness of a C layer in the low-modulus C-SiC layered substrate is 50-100 nm, the thickness of a SiC layer is 300-500 nm, and the overall modulus of the C-SiC substrate layer is 200-250 Gpa; step 3: will be prepared (C-SiC) m Placing the intermediate of the multicycle low-modulus matrix into a SiC deposition furnace to deposit a high-modulus layered SiC matrix; alternately repeating the step 2 and the step 3 to obtain the SiC containing the high-low modulus lamellar matrix f /((C-SiC) m -SiC) n A composite material; n in the material is the repetition number; the modulus of the SiC matrix is 400-450 Gpa.
2. The method according to claim 1, characterized in that: the step of glue discharging pretreatment in the step 1 is as follows: after soaking the SiC fiber preform with boiling water, washing the SiC fiber preform with deionized water, and then putting the SiC fiber preform into an oven for drying.
3. The method according to claim 1, characterized in that: the preparation process of the BN interface phase in the step 1 is chemical vapor deposition, and the BN thickness is 150-250nm.
4. The method according to claim 1, characterized in that: the preform in the step 1 is one of a unidirectional SiC fiber preform, a 2D SiC fiber preform, a 2.5DSiC fiber preform or a 3DSiC fiber preform, wherein the fiber volume fraction is 30-50%.
5. The method according to claim 1, characterized in that: m in the step 2 is repeated 1-3 times; the repetition number n in the step 3 is 6-10.
6. The method according to claim 1, characterized in that: the high modulus SiC matrix is a high crystallinity SiC matrix, and the thickness of the SiC matrix layer is 1 mu m.
7. The method according to claim 1, characterized in that: the SiC is provided with f /((C-SiC) m -SiC) n The density of the composite material is more than 2.5g/cm 3 The open porosity is less than 10%; the bending strength of the material is up to 1507+/-122 MPa, and the fracture toughness is up to 58+/-3.5 MPa.m 1/2 The tensile strength is 889+/-71 MPa at most.
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|---|---|---|---|---|
| US5156912A (en) * | 1989-12-20 | 1992-10-20 | The Standard Oil Company | Multi-layer coatings for reinforcements in high temperature composites |
| JPH10194856A (en) * | 1997-01-14 | 1998-07-28 | Toshiba Corp | Ceramic composite material and its parts |
| CN109553430A (en) * | 2019-01-16 | 2019-04-02 | 苏州宏久航空防热材料科技有限公司 | A kind of SiC with compound interfacef/ SiC ceramic based composites and preparation method thereof |
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|---|---|---|---|---|
| US5156912A (en) * | 1989-12-20 | 1992-10-20 | The Standard Oil Company | Multi-layer coatings for reinforcements in high temperature composites |
| JPH10194856A (en) * | 1997-01-14 | 1998-07-28 | Toshiba Corp | Ceramic composite material and its parts |
| CN109553430A (en) * | 2019-01-16 | 2019-04-02 | 苏州宏久航空防热材料科技有限公司 | A kind of SiC with compound interfacef/ SiC ceramic based composites and preparation method thereof |
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| 先驱体浸渍裂解结合化学气相渗透工艺下二维半和三维织构SiC/SiC复合材料的结构与性能;赵爽;杨自春;周新贵;;材料导报(16);第10-13页 * |
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