CN109970460A - A kind of fibre reinforced (carbon -) is silicon carbide-based-ultra-temperature ceramic-based composite material and preparation method thereof - Google Patents
A kind of fibre reinforced (carbon -) is silicon carbide-based-ultra-temperature ceramic-based composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of fibre reinforced (carbon -) it is silicon carbide-based-ultra-temperature ceramic-based composite material and preparation method thereof, belong to ultra-temperature ceramic-based composite material technical field.The composite material is combined into four functional areas according to the characteristics of carbon fiber, pyrolytic carbon (PyC), silicon carbide (SiC), superhigh temperature ceramics (UHTC) each constituent element, that is: a kind of composite material with excellent mechanical performance, fire-resistant oxidation resistant performance is prepared using CVI-PIP-CVD combination process in carbon fiber load bearing frame area, PyC boundary layer area, PyC-SiC load~anti-oxidant area, the anti-oxidant resistance to ablated region of superhigh temperature.
Description
Technical field:
The present invention relates to ultra-temperature ceramic-based composite material technical field, specially a kind of fibre reinforced (carbon -) carbonization
Silicon substrate-ultra-temperature ceramic-based composite material and preparation method thereof.
Background technique:
High-speed aircraft will bear superhigh temperature (>=1600 DEG C), high hot-fluid, mechanical stress and thermal force etc. during reentering
Effect, therefore it is required that heat insulation material has good mechanical property, antioxygenic property, anti-thermal shock and Burning corrosion resistance energy.Currently, C/
C composite has excellent mechanics and thermal property under high temperature anaerobic environment, but opens under aerobic conditions more than 450 DEG C
Originate raw oxidation；Develop C/ (C~) SiC ceramic matrix composite material on this basis, significantly improves its mechanical property and inoxidizability
Can, and when temperature is further increased to 1650 DEG C or more, the active oxidation of SiC limits its use scope.
Superhigh temperature ceramics (Ultra~high~temperature ceramic, UHTC) fusing point generally 3000 DEG C with
On, there is excellent anti-oxidant, Burning corrosion resistance energy, a large number of studies show that, the introducing of UHTC is greatly improved C/C and C/SiC material
Anti-oxidant, the Burning corrosion resistance energy of material, to realize superhigh temperature zero ablation.However, the fibre reinforced superhigh temperature pottery prepared at present
Porcelain based composites are using single C or SiC as matrix mostly, and mechanical property is relatively low, and density is relatively high, it is difficult to same
When meet low-density, strong mechanical performance, it is long when the demands such as anti-oxidant and anti-ablation.Therefore, the invention proposes a kind of material knots
Structure design concept provides the preparation method of a kind of short cycle for realizing material, low cost to realize above-mentioned requirement.
Summary of the invention:
The purpose of the present invention is to provide a kind of fibre reinforced (carbon -) it is silicon carbide-based-ultra-temperature ceramic-based composite material
And preparation method thereof, prepared composite material have complex matrix, while meet low-density, strong mechanical performance, it is long when antioxygen
The demands such as change and anti-ablation, the preparation method period is short, at low cost.
To achieve the above object, the technical solution adopted in the present invention is as follows:
A kind of fibre reinforced (carbon -) is silicon carbide-based-ultra-temperature ceramic-based composite material, which is held by carbon fiber
Power skeleton area, boundary layer area, comprehensive performance regulatory region (PyC-SiC functional layer) and anti-oxidant resistance to ablated region composition, in which:
Carbon fiber load bearing frame area: being using carbon fiber as raw material, using the carbon fiber that is prepared into of the methods of needle thorn, braiding
Precast body；
Boundary layer area: as boundary layer and being wrapped in around carbon fiber using PyC, and boundary layer plays the work of crack deflection
With to improve the intensity and toughness of material；
Comprehensive performance regulatory region: the comprehensive performance regulatory region is PyC-SiC functional layer, is by pyrocarbon matrix and carbonization
Silicon substrate composition, the pyrocarbon matrix and silicon carbide substrate are successively coated on boundary layer；The PyC-SiC functional layer can mention
High material mechanical performance and antioxygenic property, by changing wherein pyrocarbon matrix (PyC matrix) and silicon carbide substrate (SiC base
Body) composition and ratio, the composite material of a variety of excellent combination properties can be prepared；
Anti-oxidant resistance to ablated region: by superhigh temperature ceramics (ZrC, ZrB2, HfC) and SiC coating composition, in which: superhigh temperature pottery
Porcelain is covered on the silicon carbide substrate in comprehensive performance regulatory region, and deposits SiC coating in outer surface.
The carbon fiber precast body is with a thickness of 1~20mm, and interfacial layer thickness is 0.1~3 μm, the superhigh temperature ceramics
It (UHTC) is ZrC, ZrB2One or more of with HfC.
The fibre reinforced (carbon -) is silicon carbide-based-ultra-temperature ceramic-based composite material using chemical vapor infiltration (CVI),
Polymer infiltration and pyrolysis (PIP) and chemical vapor deposition (CVD) combination process realize the preparation of material, specifically include following step
It is rapid:
(1) carbon fiber precast body is placed in cvd furnace, with C3H8For carbon source, Ar or N2For carrier gas and protection gas, use
CVI technique deposits PyC boundary layer, passes through sedimentation time control interface thickness degree；
(2) it deposits PyC matrix: the carbon fiber precast body containing interfacial TCO layer obtained by step (1) is placed in chemical vapor deposition
In furnace, with C3H8For carbon source, Ar or N2For carrier gas and protection gas, PyC matrix is deposited on boundary layer using CVI technique, is obtained
?；
(3) SiC matrix is deposited: in chemical vapor deposition stove, with trichloromethyl silane (MTS) for raw material, with hydrogen
(H2) it is carrier gas, Ar or N2For carrier gas and protection gas, using CVI technique, the carbon fiber containing PyC matrix is pre- in step (2)
SiC matrix is deposited on body processed, and PyC-SiC functional layer is obtained in carbon fiber precast body after deposition；
(4) sample obtained by step (3) is successively machined, is cleaned by ultrasonic and low temperature drying；
(5) PIP technique is used, introduces superhigh temperature ceramics (UHTC) in step (4) treated sample, process are as follows: will
Sample is placed in vacuum pressure container, and superhigh temperature ceramics precursor solution is introduced into sample obtained by step (4) using vacuum environment
In product material, then superhigh temperature ceramics successively are obtained through pressure impregnation, low-temperature setting and Pintsch process process；The above-mentioned mistake of iterative cycles
Journey 3~15 times, until material global density reaches 2.0~2.3g/cm3；
(6) CVD technique is used, the sample containing superhigh temperature ceramics is placed in CVD furnace after depositing SiC coating to get arriving
The fibre reinforced (carbon -) is silicon carbide-based-ultra-temperature ceramic-based composite material.
In above-mentioned steps (1), 2D needling structure, 2.5D braiding structure, 3D braiding knot is can be used in the carbon fiber precast body
Structure carefully compiles puncturing structure, and the bulk density of precast body is unlimited.
In above-mentioned steps (1), the technological parameter of PyC boundary layer is deposited are as follows: Ar or N20.05~0.5m of gas flow3/ h,
C3H80.01~0.5m of gas flow3/ h, 700~1000 DEG C of depositing temperature, 1~10h of sedimentation time.
In above-mentioned steps (2), the technological parameter of PyC matrix is deposited are as follows: Ar or N20.05~0.5m of gas flow3/ h, C3H8
0.01~0.5m of gas flow3/ h, 950~1100 DEG C of depositing temperature, sedimentation time 0~300 hour；If sedimentation time is 0 small
When, finally obtained product is carbon fibre reinforced silicon carbide base-ultra-temperature ceramic-based composite material；If sedimentation time is not 0,
Final products be fibre reinforced (carbon -) it is silicon carbide-based-ultra-temperature ceramic-based composite material.
In above-mentioned steps (3), the technological parameter of SiC matrix is deposited are as follows: Ar or N20.02~0.2m of flow3/ h, H2Flow
0.02~0.2m3/ h, MTS 20~200g/h of flow, 1000~1100 DEG C of depositing temperature, the reaction time 100~500 hours.
In above-mentioned steps (5), the PIP impregnating cracking technology process are as follows: the first step is made pottery superhigh temperature using vacuum environment
The mixed liquor of porcelain presoma and Polycarbosilane is introduced into intrinsic silicon, and vacuum degree≤3000Pa keeps 2~4h；Second step is passed through
Ar or N2And it is forced into 3~6MPa, keep 2~4h；Third step, 100~150 DEG C of 5~10h of crosslinking curing；4th step, with 2 DEG C/
The heating rate of min is warming up to 1500 DEG C, 1500 DEG C of heat preservation 2h；The superhigh temperature ceramics presoma is the organic of superhigh temperature ceramics
Presoma, such presoma obtain corresponding superhigh temperature ceramics after Pintsch process.
In above-mentioned steps (6), the technological parameter of SiC coating is deposited are as follows: Ar or N20.02~0.2m of flow3/ h, H2Flow
0.02~0.2m3/ h, MTS 20~200g/h of flow, depositing temperature is at 1100~1200 DEG C, the reaction time 10~50 hours.
This method can prepare Cf/SiC-ZrC、Cf/SiC-ZrB2-ZrC、Cf/SiC-HfB2-HfC、Cf/SiC-HfC、Cf/
C-SiC-ZrC、Cf/C-SiC-ZrB2、Cf/C-SiC-ZrB2-ZrC、Cf/C-SiC-HfB2Or CfThe composite woods such as/C-SiC-HfC
Material.
The present invention has the following advantages and beneficial effects:
1, material has designability, and PyC-SiC functional layer has variable element abundant, can be carried out according to use demand
Adjustment, can both meet mechanical property requirements, can also meet resistance to ablation, antioxygenic property demand.
2, the composite material of this method preparation can meet the needs of space flight loss of weight well.
3, material ultra-temperature ceramics constituent element diversification can carry out the selection of superhigh temperature ceramics constituent element according to use demand, can
Prepare Cf/SiC-ZrC、Cf/SiC-ZrB2-ZrC、Cf/SiC-HfB2-HfC、Cf/SiC-HfC、Cf/C-SiC-ZrC、Cf/C-SiC-
ZrB2、Cf/C-SiC-ZrB2-ZrC、Cf/C-SiC-HfB2、CfA variety of composite materials such as/C-SiC-HfC.
4, material has mechanical property outstanding, and composite material final densities are greater than 2.0g/cm3, bending strength is greater than
320MPa。
5, this method can realize the mass of material, batch, the production of trade mark metaplasia.
Detailed description of the invention:
Fig. 1 is that the structure design of material and different preparatory phases accordingly form figure.
Fig. 2 is U~ZCS0.12 composite material microstructure.
Fig. 3 is U~ZCS0.12, U~ZCS0.91 and U~ZCS3.28 composite material bending stress and displacement curve.
Fig. 4 is U~ZCS0.91 composite material microstructure.
Fig. 5 is U~ZCS3.28 composite material microstructure.
Specific embodiment:
Technical solution in order to enable those skilled in the art to better understand the present invention makees the present invention below with reference to embodiment
It is described in further detail.
The present invention provide fibre reinforced (carbon -) it is silicon carbide-based-mentality of designing of ultra-temperature ceramic-based composite material, such as scheme
Shown in 1, composite material is made of four kinds of carbon fiber, pyrolytic carbon (PyC), silicon carbide (SiC), superhigh temperature ceramics (UHTC) constituent elements.
They are combined into four functional areas according to the characteristics of each constituent element, it may be assumed that carbon fiber load bearing frame area is adopted based on carbon fiber
With the methods of needle thorn, braiding, it is prepared into the carbon fiber precast body skeleton with certain shapes and function；Boundary layer area, using PyC
It is wrapped in around carbon fiber as boundary layer, mainly plays the role of crack deflection, to improve the intensity and toughness of material；It is comprehensive
It closes property regulation area (PyC-SiC functional layer), which is mainly made of pyrocarbon matrix and silicon carbide substrate, is wrapped in interface
Layer outer layer, by changing the composition and ratio of PyC and SiC, can be designed synthesis to improve material mechanical performance and antioxygenic property
The composite material haveing excellent performance；Anti-oxidant resistance to ablated region, the part is mainly by SiC and superhigh temperature ceramics (ZrC, ZrB2, HfC etc.
Substance or their mixture) composition.
2 the present invention also provides the preparation method of above-mentioned composite material, soaks by using chemical vapor infiltration (CVI)-presoma
Stain cracks the preparation that (PIP)-chemical vapor deposition (CVD) combination process realizes material.
Embodiment 1
The trade mark is U~ZCS0.12 composite material and preparation method thereof and material property:
Select 380 × 80 × 10mm, density 0.5g/cm32D needled carbon fiber preform；It is prepared using ICVI technique
Pyrolysis carbon boundary layer, 900 DEG C of temperature, argon flow 0.1m3/ h, propane 0.1m3/ h, sedimentation time 5 hours；PyC-SiC functional layer
In the PyC matrix deposition time be 0h；SiC matrix needed for preparing PyC-SiC functional layer using ICVI technique, 1000 DEG C of temperature,
Hydrogen, argon gas and trichloromethyl silane, volume ratio 5:5:1, sedimentation time 500 hours, density of material 1.8g/cm3；Take number
After controlling machine-shaping, ultrasonic cleaning；ZrC-SiC superhigh temperature ceramics phase is introduced using PIP technique, by 7 period infiltration pyrolysis,
Specific process parameter are as follows: vacuum degree 2000Pa, impregnation pressure 6MPa, 130 DEG C of solidification temperature, 1500 DEG C of heat treatment temperature, heat at
Manage time 2h；Using CVD prepare SiC coating, 1200 DEG C of temperature, hydrogen, argon gas and trichloromethyl silane, volume ratio 5:5:1,
Time 25 hours, material final densities 2.1g/cm3, bending strength 336MPa.Fig. 2 is material microstructure；Fig. 3 is that bending is answered
Power and displacement curve.
Embodiment 2
The trade mark is U~ZCS0.91 composite material and preparation method thereof and material property:
Select 380 × 80 × 10mm, density 0.5g/cm32D needled carbon fiber preform；It is prepared using ICVI technique
Pyrolysis carbon boundary layer, 900 DEG C of temperature, argon flow 0.1m3/ h, propane 0.1m3/ h, sedimentation time 5 hours；Using ICVI technique
PyC matrix needed for preparing PyC-SiC functional layer, 950 DEG C of temperature, argon flow 0.15m3/ h, propane 0.15m3/ h, sedimentation time
200 hours；SiC matrix needed for preparing PyC-SiC functional layer using ICVI technique, 1000 DEG C of temperature, hydrogen, argon gas and three chloromethanes
Base silane, volume ratio 5:5:1, sedimentation time 300 hours, density of material 1.65g/cm3；It is anti-using ICVI technique preparation SiC
SiC matrix needed for oxide layer, 1050 DEG C of temperature, hydrogen, argon gas and trichloromethyl silane, volume ratio 5:5:1, sedimentation time
200 hours, density of material 1.8g/cm3；After taking numerical control machine-shaping, ultrasonic cleaning；ZrC superhigh temperature is introduced using PIP technique
Ceramic phase, by 7 period infiltration pyrolysis, specific process parameter are as follows: vacuum degree 2000Pa, impregnation pressure 6MPa, solidification temperature
130 DEG C, 1500 DEG C of heat treatment temperature, heat treatment time 2h；Using CVD prepare SiC coating, 1200 DEG C of temperature, hydrogen, argon gas and
Trichloromethyl silane, volume ratio 5:5:1, the time 25 hours, material final densities 2.1g/cm3, bending strength 353MPa.Fig. 3
For bending stress and displacement curve；Fig. 4 is material microstructure.
Embodiment 3
The trade mark is U~ZCS3.28 composite material and preparation method thereof and material property:
Select 380 × 80 × 10mm, density 0.5g/cm32D needled carbon fiber preform；It is prepared using ICVI technique
Pyrolysis carbon boundary layer, 900 DEG C of temperature, argon flow 0.1m3/ h, propane 0.1m3/ h, sedimentation time 5 hours；Using ICVI technique
PyC matrix needed for preparing PyC-SiC functional layer, 950 DEG C of temperature, argon flow 0.15m3/ h, propane 0.15m3/ h, sedimentation time
400 hours；SiC matrix needed for preparing PyC-SiC functional layer using ICVI technique, 1000 DEG C of temperature, hydrogen, argon gas and three chloromethanes
Base silane, volume ratio 5:5:1, sedimentation time 200 hours, density of material 1.8g/cm3；After taking numerical control machine-shaping, ultrasound
Cleaning；ZrC superhigh temperature ceramics phase is introduced using PIP technique, by 7 period infiltration pyrolysis, specific process parameter are as follows: vacuum degree
2000Pa, impregnation pressure 6MPa, 130 DEG C of solidification temperature, 1500 DEG C of heat treatment temperature, heat treatment time 2h；It is prepared using CVD
SiC coating, 1200 DEG C of temperature, hydrogen, argon gas and trichloromethyl silane, volume ratio 5:5:1, the time 25 hours, material was final
Density 2.1g/cm3, bending strength 321MPa.Fig. 3 is bending stress and displacement curve；Fig. 5 is material microstructure.
Claims (10)
1. a kind of fibre reinforced (carbon -) is silicon carbide-based-ultra-temperature ceramic-based composite material, it is characterised in that: the composite material
It is made of carbon fiber load bearing frame area, boundary layer area, comprehensive performance regulatory region and anti-oxidant resistance to ablated region, in which:
Carbon fiber load bearing frame area: being using carbon fiber as raw material, using the prefabricated carbon fiber that is prepared into of the methods of needle thorn, braiding
Body；
Boundary layer area: as boundary layer and being wrapped in around carbon fiber using PyC, and boundary layer plays the role of crack deflection, with
Improve the intensity and toughness of material；
Comprehensive performance regulatory region: the comprehensive performance regulatory region is PyC-SiC functional layer, is by pyrocarbon matrix and silicon carbide-based
Body composition, the pyrocarbon matrix and silicon carbide substrate are successively coated on boundary layer；The PyC-SiC functional layer can improve material
Mechanical property and antioxygenic property are expected, by changing wherein pyrocarbon matrix (PyC matrix) and silicon carbide substrate (SiC matrix)
Composition and ratio can prepare the composite material of a variety of excellent combination properties；
Anti-oxidant resistance to ablated region: it is made of superhigh temperature ceramics and SiC coating, in which: superhigh temperature ceramics are covered on comprehensive performance tune
It saves on the silicon carbide substrate in area, and deposits SiC coating in outer surface.
2. fibre reinforced (carbon -) according to claim 1 is silicon carbide-based-ultra-temperature ceramic-based composite material, feature
Be: for the carbon fiber precast body with a thickness of 1~20mm, interfacial layer thickness is 0.1~3 μm, the superhigh temperature ceramics be ZrC,
ZrB2One or more of with HfC.
3. fibre reinforced (carbon -) according to claim 1 is silicon carbide-based-the preparation side of ultra-temperature ceramic-based composite material
Method, it is characterised in that: this method is using chemical vapor infiltration (CVI), polymer infiltration and pyrolysis (PIP) and chemical vapor deposition
(CVD) combination process realizes the preparation of material, specifically comprises the following steps:
(1) carbon fiber precast body is placed in cvd furnace, with C3H8For carbon source, Ar or N2For carrier gas and gas is protected, using CVI
Technique deposits PyC boundary layer, passes through sedimentation time control interface thickness degree；
(2) it deposits PyC matrix: the carbon fiber precast body containing interfacial TCO layer obtained by step (1) is placed in chemical vapor deposition stove,
With C3H8For carbon source, Ar or N2For carrier gas and protection gas, PyC matrix is deposited on boundary layer using CVI technique, is obtained；
(3) SiC matrix is deposited: in chemical vapor deposition stove, with trichloromethyl silane (MTS) for raw material, with hydrogen (H2) it is to carry
Gas, Ar or N2For carrier gas and gas is protected, using CVI technique, in step (2) in the carbon fiber precast body containing PyC matrix
SiC matrix is deposited, obtains PyC-SiC functional layer in carbon fiber precast body after deposition；
(4) sample obtained by step (3) is successively machined, is cleaned by ultrasonic and low temperature drying；
(5) PIP technique is used, introduces superhigh temperature ceramics, process in step (4) treated sample are as follows: be placed in sample very
In pneumatics force container, superhigh temperature ceramics precursor solution is introduced into specimen material obtained by step (4) using vacuum environment, then
Successively superhigh temperature ceramics are obtained through pressure impregnation, low-temperature setting and Pintsch process process；The iterative cycles above process 3~15 times,
Reach 2.0~2.3g/cm to material global density3；
(6) CVD technique is used, the sample containing superhigh temperature ceramics is placed in CVD furnace after depositing SiC coating to get described in
Fibre reinforced (carbon -) is silicon carbide-based-ultra-temperature ceramic-based composite material.
4. fibre reinforced (carbon -) according to claim 3 is silicon carbide-based-the preparation side of ultra-temperature ceramic-based composite material
Method, it is characterised in that: in step (1), 2D needling structure, 2.5D braiding structure, 3D braiding is can be used in the carbon fiber precast body
Structure carefully compiles puncturing structure, and the bulk density of precast body is unlimited.
5. fibre reinforced (carbon -) according to claim 3 is silicon carbide-based-the preparation side of ultra-temperature ceramic-based composite material
Method, it is characterised in that: in step (1), deposit the technological parameter of PyC boundary layer are as follows: Ar or N20.05~0.5m of gas flow3/ h,
C3H80.01~0.5m of gas flow3/ h, 700~1000 DEG C of depositing temperature, 1~10h of sedimentation time.
6. fibre reinforced (carbon -) according to claim 3 is silicon carbide-based-the preparation side of ultra-temperature ceramic-based composite material
Method, it is characterised in that: in step (2), deposit the technological parameter of PyC matrix are as follows: Ar or N20.05~0.5m of gas flow3/ h,
C3H80.01~0.5m of gas flow3/ h, 950~1100 DEG C of depositing temperature, sedimentation time 0~300 hour；If sedimentation time is 0
Hour, finally obtained product is carbon fibre reinforced silicon carbide base-ultra-temperature ceramic-based composite material；If sedimentation time is not 0,
Then final products be fibre reinforced (carbon -) it is silicon carbide-based-ultra-temperature ceramic-based composite material.
7. fibre reinforced (carbon -) according to claim 3 is silicon carbide-based-the preparation side of ultra-temperature ceramic-based composite material
Method, it is characterised in that: in step (3), deposit the technological parameter of SiC matrix are as follows: Ar or N20.02~0.2m of flow3/ h, H2Flow
0.02~0.2m3/ h, MTS 20~200g/h of flow, 1000~1100 DEG C of depositing temperature, the reaction time 100~500 hours.
8. fibre reinforced (carbon -) according to claim 3 is silicon carbide-based-the preparation side of ultra-temperature ceramic-based composite material
Method, it is characterised in that: in step (5), the PIP impregnating cracking technology process are as follows: the first step, using vacuum environment by superhigh temperature
The mixed liquor of ceramic forerunner and Polycarbosilane is introduced into intrinsic silicon, and vacuum degree≤3000Pa keeps 2~4h；Second step leads to
Enter Ar or N2And it is forced into 3~6MPa, keep 2~4h；Third step, 100~150 DEG C of 5~10h of crosslinking curing；4th step, with 2
DEG C/heating rate of min is warming up to 1500 DEG C, 1500 DEG C of heat preservation 2h；The superhigh temperature ceramics presoma is superhigh temperature ceramics
Organic precursor, such presoma obtain corresponding superhigh temperature ceramics after Pintsch process.
9. fibre reinforced (carbon -) according to claim 3 is silicon carbide-based-the preparation side of ultra-temperature ceramic-based composite material
Method, it is characterised in that: in step (6), deposit the technological parameter of SiC coating are as follows: Ar or N20.02~0.2m of flow3/ h, H2Flow
0.02~0.2m3/ h, MTS 20~200g/h of flow, depositing temperature is at 1100~1200 DEG C, the reaction time 10~50 hours.
10. fibre reinforced (carbon -) according to claim 3 is silicon carbide-based-preparation of ultra-temperature ceramic-based composite material
Method, it is characterised in that: this method can prepare Cf/SiC-ZrC、Cf/SiC-ZrB2-ZrC、Cf/SiC-HfB2-HfC、Cf/
SiC-HfC、Cf/C-SiC-ZrC、Cf/C-SiC-ZrB2、Cf/C-SiC-ZrB2-ZrC、Cf/C-SiC-HfB2Or Cf/C-SiC-HfC
Equal composite materials.
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