CN115677366A - Carbon nanosheet toughened PyC/SiC composite interface and preparation method thereof - Google Patents
Carbon nanosheet toughened PyC/SiC composite interface and preparation method thereof Download PDFInfo
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- CN115677366A CN115677366A CN202211366219.4A CN202211366219A CN115677366A CN 115677366 A CN115677366 A CN 115677366A CN 202211366219 A CN202211366219 A CN 202211366219A CN 115677366 A CN115677366 A CN 115677366A
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Abstract
The present invention relates to SiC f The method comprises the steps of sequentially depositing a PyC interface, a CNS (central nervous system) interface and a SiC interface on the surface of a fiber preform by a chemical vapor deposition process, making up the defects of a single PyC weak interface and a single SiC strong interface, enhancing the combination of the SiC interface and the PyC interface by utilizing the pinning effect of the CNS, improving the brittleness of the SiC interface, and improving the SiC by interface modification f The strength and toughness of the/SiC composite material effectively avoid the brittle fracture of the ceramic composite material, so that the safety and reliability of the ceramic composite material part are improved, and the service life of the part is prolonged by 30 percent.
Description
Technical Field
The present invention relates to SiC f a/SiC composite material, in particular to a carbon nano sheet toughened PyC/SiC composite interface and a preparation method thereof.
Background
SiC f/ SiC composite materialThe material is a complex phase material which is formed by introducing SiC continuous fibers into a SiC ceramic matrix and taking the SiC fibers as a dispersed reinforcing phase and the SiC ceramic as a continuous phase. The ceramic composite material has lower density (only 1/4~1/3 of high-temperature alloy), excellent high-temperature performance (the higher-temperature alloy is improved by 200 ℃), specific strength and specific modulus, oxidation resistance and the like, and has wide application prospect in the field of aerospace.
The direct contact of the ceramic fiber and the matrix can form strong fiber-matrix combination, so that the reinforcing and toughening effects of the fiber cannot be exerted, and meanwhile, the preparation process can cause severe damage to the fiber. The introduction of the interface layer between the fiber and the matrix is an effective means for solving the problem of fiber-matrix combination and avoiding fiber damage, and is particularly critical for adjusting the comprehensive performance of the ceramic composite material, so the design and preparation process of the interface layer are very important.
SiC at present f The interface material of the/SiC composite material mainly comprises pyrolytic carbon (PyC), boron Nitride (BN), silicon carbide (SiC) and a multilayer composite interface. The special layered crystal structure is beneficial to toughening the ceramic composite material, so that PyC becomes a common interface phase of the ceramic composite material, but the characteristic of easy oxidation limits the application of the composite material in the service environment of a hot end part of an aircraft engine. Compared with the prior art, siC has better oxidation resistance, but has large brittleness and poor high-temperature performance, and cannot meet the bearing requirement of a hot end part of an engine. Considering that the fracture failure behavior of the ceramic composite material is directly influenced by the interface composition and the interface property, the invention provides a Carbon Nanosheet (CNS) -modified PyC/SiC composite interface layer, the damage tolerance and the thermophysical property of the ceramic composite material are improved by the PyC interface, the oxidation resistance of the ceramic composite material is improved by the SiC interface, and meanwhile, the brittleness of the SiC interface layer is improved by utilizing the induced deflection of the CNS to an interface crack, the bridging and the debonding of the CNS.
Disclosure of Invention
For the above SiC f The invention discloses a PyC/SiC composite interface toughened by carbon nano sheets and a preparation method thereof, and relates to the problem of material selection of a/SiC composite interface.
The technical scheme of the invention is as follows:
carbon Nanosheet (CNS) -toughened PyC/SThe preparation method of the iC composite interface comprises the steps of sequentially depositing a PyC interface, a CNS (central nervous system) and a SiC interface on the surface of a fiber preform by a chemical vapor deposition process, making up the defects of a single PyC weak interface and a single SiC strong interface, enhancing the combination of the SiC interface and the PyC interface by utilizing the pinning effect of the CNS, and improving the brittleness of the SiC interface, so that the SiC is improved by interface modification f Strength and toughness of the/SiC composite material.
Further, the preparation method of the Carbon Nanosheet (CNS) -toughened PyC/SiC composite interface comprises the following specific steps:
step 1) weaving of fiber preform
Adopts second-generation SiC fiber and 2.5D weaving structure, the density of warp yarn is 8 plus or minus 0.2 pieces/cm, the density of weft yarn is 3.5 plus or minus 0.2 pieces/cm, and the size of the weaving body is 200 multiplied by 100 multiplied by 3.5mm 3 ；
Step 2) PyC interfacial deposition
Depositing a PyC interface layer on the surface of the fiber by adopting a chemical vapor deposition process, placing the fiber preform in a PyC deposition furnace, and performing chemical vapor deposition with propylene 3 H 6 As a carbon source, high-purity argon Ar is used as a diluting and protecting gas, and the deposition parameters are as follows: c 3 H 6 The flow rate is 100 to 200mL/min, the Ar flow rate is 120 to 200mL/min, the deposition temperature is 800 to 1500 ℃, the heating rate is 8 ℃ per min, the deposition pressure is 1 to 2kPa, the deposition time is 1 to 3h, and the thickness of the obtained PyC interface layer is 200 to 300nm;
step 3) CNS deposition
Depositing CNS by chemical vapor deposition, heating methanol in water bath by taking methanol as a precursor, and keeping the temperature of the water bath at 20-30 ℃; regulating the flow of methanol to keep the pressure in a deposition chamber at 10 to 20kPa; the deposition temperature is 1000 to 1300 ℃, and the deposition time is 1 to 3h;
step 4) SiC interface deposition
Depositing SiC interface layer by chemical vapor deposition process, taking Methyl Trichlorosilane (MTS) as precursor, and obtaining high-purity H 2 As carrier gas, high-purity Ar as diluent gas, deposition parameters are as follows: h 2 The flow rate is 1.5 to 3L/min, the Ar flow rate is 300 to 800mL/min, the deposition temperature is 900 to 1500 ℃, the heating rate is 7 ℃ per min, the deposition pressure is 0.5 to 3kPa, the deposition time is 2 to 10h, and the obtained SiC interface layerThe thickness is 0.5 to 1 mu m;
step 5) SiC matrix deposition
Adopts chemical vapor deposition process to realize SiC matrix densification, uses methyl trichlorosilane MTS as a precursor, and has high purity H 2 As carrier gas, high-purity Ar as diluent gas, deposition parameters are as follows: h 2 The flow rate is 1.5 to 3L/min, the Ar flow rate is 200 to 600mL/min, the deposition temperature is 900 to 1500 ℃, the heating rate is 7 ℃ per min, the deposition pressure is 1 to 3kPa, the deposition time is 100 to 200h, and the obtained SiC f The density of the/SiC composite material is 1.9 to 2.1g/cm 2 。
The carbon nanosheet toughened PyC/SiC composite interface prepared by the preparation method is provided.
The invention has the advantages and beneficial effects that:
compared with the existing PyC/SiC composite interface, the carbon nanosheet toughened PyC/SiC composite interface provided by the invention has the advantages that the interlayer combination of the PyC interface and the SiC interface is strengthened by introducing the nanocarbon, the crack propagation resistance is increased, the bridging and debonding effects of the nanophase are exerted, the interface brittleness is obviously improved, and the SiC is further improved f The strength and the toughness of the/SiC composite material effectively avoid the brittle fracture of the ceramic composite material, so that the safety and the reliability of the ceramic composite material part are improved, and the service life of the part is prolonged by 30 percent.
Drawings
FIG. 1 is a surface CNS topography of a PyC interface layer according to the invention;
FIG. 2 shows SiC prepared by the present invention f Bending strength-displacement curve diagram of the/SiC composite material.
Detailed Description
The invention is described in further detail below with reference to the drawings and the detailed description.
A carbon nanosheet toughened PyC/SiC composite interface is prepared according to the following steps:
step 1) weaving of fiber preform
Adopts second-generation SiC fiber and 2.5D weaving structure, the density of warp yarn is 8 plus or minus 0.2 pieces/cm, the density of weft yarn is 3.5 plus or minus 0.2 pieces/cm, and the size of the weaving body is 200 multiplied by 100 multiplied by 3.5mm 3 ；
Step 2) PyC interfacial deposition
Depositing a PyC interface layer on the surface of the fiber by adopting a chemical vapor deposition process, placing the fiber preform in a PyC deposition furnace, and performing chemical vapor deposition on the fiber preform by using propylene 3 H 6 As a carbon source, high-purity argon Ar is used as a diluting and protecting gas, and the deposition parameters are as follows: c 3 H 6 The flow rate is 120mL/min, the Ar flow rate is 120mL/min, the deposition temperature is 1050 ℃, the heating rate is 8 ℃ per min, the deposition pressure is 1.2kPa, the deposition time is 1h, and the thickness of the obtained PyC interface layer is 200nm;
step 3) CNS deposition
Depositing CNS by chemical vapor deposition, heating methanol in water bath at 28 deg.C by using methanol as precursor; regulating the flow of the methanol to keep the pressure in the deposition chamber at 10kPa; the deposition temperature is 1200 ℃, and the deposition time is 1.5h;
step 4) SiC interface deposition
Depositing SiC interface layer by chemical vapor deposition process, taking Methyl Trichlorosilane (MTS) as precursor, and obtaining high-purity H 2 As carrier gas, high-purity Ar as diluent gas, deposition parameters are as follows: h 2 The flow rate is 1.8L/min, the Ar flow rate is 400mL/min, the deposition temperature is 980 ℃, the heating rate is 7 ℃/min, the deposition pressure is 1.2kPa, the deposition time is 4h, and the thickness of the obtained SiC interface layer is 0.8 mu m;
step 5) SiC matrix deposition
Adopts chemical vapor deposition process to realize SiC matrix densification, uses methyl trichlorosilane MTS as a precursor, and has high purity H 2 As carrier gas, high-purity Ar as diluent gas, deposition parameters are as follows: h 2 The flow rate is 2.4L/min, the Ar flow rate is 600mL/min, the deposition temperature is 980 ℃, the heating rate is 7 ℃ per min, the deposition pressure is 1-3kPa, the deposition time is 180 hours, and the obtained SiC f The density of the/SiC composite material is 2.0g/cm 2 。
As shown in fig. 1, the surface CNS topography of the PyC interface layer of the present invention shows the presence of a large number of nanophase on the PyC layer.
The bending properties of the SiCf/SiC composites were tested using a universal tester (CMT 5304-30 kN). The test parameters are: the sample size was 40X 5X 3mm 3 AcrossThe distance is 30mm, the loading direction is vertical to the in-plane direction of the fiber, and the loading speed is 0.5mm/min. The bending strength-displacement curve is shown in FIG. 2, and when no CNS is introduced at the interface, the bending strength of the composite material is 335MPa; after the CNS modified composite interface is introduced, the bending strength of the composite material is 352MPa. In addition, the fracture toughness of the composite material is improved after the CNS is introduced, and the pseudoplastic characteristic of the corresponding curve is more obvious. This indicates the introduction of CNS to SiC at the composite interface f the/SiC composite material has double functions of strengthening and toughening.
Claims (3)
1. A preparation method of a carbon nanosheet toughened PyC/SiC composite interface is characterized in that a PyC interface, a CNS (central nervous system) interface and a SiC interface are sequentially deposited on the surface of a fiber preform through a chemical vapor deposition process, the defects of a single PyC weak interface and a single SiC strong interface are overcome, the combination of the SiC interface and the PyC interface is enhanced by utilizing the pinning effect of the CNS, the brittleness of the SiC interface is improved, and therefore the interface modification is used for improving the brittleness of the SiC interface f Strength and toughness of the/SiC composite material.
2. The method for preparing the carbon nanosheet-toughened PyC/SiC composite interface according to claim 1, comprising the following specific steps:
step 1) weaving of fiber preform
Adopts second-generation SiC fiber and 2.5D weaving structure, the density of warp yarn is 8 plus or minus 0.2 pieces/cm, the density of weft yarn is 3.5 plus or minus 0.2 pieces/cm, and the size of the weaving body is 200 multiplied by 100 multiplied by 3.5mm 3 ；
Step 2) PyC interfacial deposition
Depositing a PyC interface layer on the surface of the fiber by adopting a chemical vapor deposition process, placing the fiber preform in a PyC deposition furnace, and performing chemical vapor deposition on the fiber preform by using propylene 3 H 6 As a carbon source, high-purity argon Ar is used as a diluting and protecting gas, and the deposition parameters are as follows: c 3 H 6 The flow rate is 100 to 200mL/min, the Ar flow rate is 120 to 200mL/min, the deposition temperature is 800 to 1500 ℃, the heating rate is 8 ℃ per min, the deposition pressure is 1 to 2kPa, the deposition time is 1 to 3h, and the thickness of the obtained PyC interface layer is 200 to 300nm;
step 3) CNS deposition
Depositing CNS by chemical vapor deposition, heating methanol in water bath by taking methanol as a precursor, and keeping the temperature of the water bath at 20-30 ℃; regulating the flow of the methanol to keep the pressure in the deposition chamber within 10 to 20kPa; the deposition temperature is 1000 to 1300 ℃, and the deposition time is 1 to 3h;
step 4) SiC interface deposition
Depositing SiC interface layer by chemical vapor deposition process, taking Methyl Trichlorosilane (MTS) as precursor, and obtaining high-purity H 2 As carrier gas, high-purity Ar as diluent gas, and the deposition parameters are as follows: h 2 The flow rate is 1.5 to 3L/min, the Ar flow rate is 300 to 800mL/min, the deposition temperature is 900 to 1500 ℃, the heating rate is 7 ℃ per min, the deposition pressure is 0.5 to 3kPa, the deposition time is 2 to 10h, and the thickness of the obtained SiC interface layer is 0.5 to 1 mu m;
step 5) SiC matrix deposition
Adopts chemical vapor deposition process to realize SiC matrix densification, uses methyl trichlorosilane MTS as a precursor, and has high purity H 2 As carrier gas, high-purity Ar as diluent gas, deposition parameters are as follows: h 2 The flow rate is 1.5 to 3L/min, the Ar flow rate is 200 to 600mL/min, the deposition temperature is 900 to 1500 ℃, the heating rate is 7 ℃ per min, the deposition pressure is 1 to 3kPa, the deposition time is 100 to 200h, and the obtained SiC f The density of the/SiC composite material is 1.9 to 2.1g/cm 2 。
3. A carbon nanoplate toughened PyC/SiC composite interface prepared by the method of preparing a carbon nanoplate toughened PyC/SiC composite interface of claim 2.
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| CN116283324A (en) * | 2023-02-13 | 2023-06-23 | 杭州英希捷科技有限责任公司 | Method for improving carbon fiber ceramic interface, preparation method and application |
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