CN106747671A - The preparation method of superhigh temperature thermostructural composite boundary layer - Google Patents
The preparation method of superhigh temperature thermostructural composite boundary layer Download PDFInfo
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Abstract
The invention provides a kind of preparation method of superhigh temperature thermostructural composite boundary layer, the method is provided with the composite material interface layer of three-decker between the fiber and matrix of superhigh temperature thermostructural composite, and silicon carbide layer, porous mullite layer, silicon carbide layer are outwards respectively from fiber.Silicon carbide layer can prevent elements diffusion, protect matrix not lost with fibre property；Porous mullite layer has excellent high-temperature oxidation resistance, and high-temperature stability is good, loose structure plays a part of induction micro-crack deflection, the performance of the toughening mechanisms such as effective guarantee fiber-bridged, spike protein gene；MULTILAYER COMPOSITE boundary layer is conducive to micro-crack to deflect.Therefore the superhigh temperature thermostructural composite for having the boundary layer has excellent high-temperature oxidation resistance and excellent mechanical behavior under high temperature.
Description
Technical field
The present invention relates to technical field of composite materials, more particularly to a kind of system of superhigh temperature thermostructural composite boundary layer
Preparation Method.
Background technology
Carborundum have excellent elevated temperature strength, high-temperature stability and obtain extensive concern, but monomer silicon carbide ceramics is tough
Property is low, is easily caused material catastrophic failure.Silicon carbide fiber reinforced silicon carbide is prepared with continuous carbofrax fibre toughening silicon carbide
Composite can be obviously improved monomer ceramics toughness, and ripple material is inhaled in high-temperature structural material, frit reaction heap and thermal structure
The fields such as material have broad application prospects.
Interface be mutually silicon carbide fiber reinforced silicon carbide composite material mechanical property and the realization of other performances it is crucial because
One of element, suitable interface phase, appropriate interface phase thickness can effectively induce matrix micro-cracks to deflect, and make fiber-bridged, fibre
The toughening mechanisms such as dimension extraction are played.
Silicon carbide fiber reinforced silicon carbide composite material is generally using pyrolytic carbon and hexagonal boron nitride as interface phase.Its
In, pyrolytic carbon has special layered crystal structure, prepares wide material sources, and the compatibility with fiber and matrix is good, with good
Mechanical property.But pyrolytic carbon is easily aoxidized, at high temperature, after boundary layer is all oxidized, fiber and matrix will be by
Oxidation form silicon oxide layer so that most at last fiber together with bond matrix, the strong combination at interface can prevent the sliding of fiber
And extraction, cause material to show as fragility, have impact on the performance of silicon carbide fiber reinforced silicon carbide composite material mechanical behavior under high temperature.
Additionally, using with the hexagonal boron nitride with pyrolytic carbon similar crystal structure as boundary layer, compared with pyrolytic carbon, its have compared with
Good antioxygenic property, the glassy state boron oxide formed after oxidation can make up the gap between fibrous matrix, hinder the diffusion of oxygen,
Therefore composite material exhibits go out preferable inoxidizability.But there is problems with as boundary layer in hexagonal boron nitride：(1) prepare logical
Frequently with source of the gas (boron trifluoride, ammonia) there is corrosivity to silicon carbide fibre, the damage of fiber can be caused；(2) boron nitride circle
Face phase inside and its combination and fiber between are weaker, generally require subsequent high temperature heat treatment to improve its combination, but warm high
Place is comprehended to silicon carbide fibre, and particularly the silicon carbide fibre of elevated oxygen level can be caused to damage；(3) boron nitride oxidation product oxygen
Change boron in high temperature, particularly readily volatilized loss when higher than 1300 DEG C, its inhibition to oxygen is lost, while the oxygen of liquid
Changing boron can dissolve the silica of Oxidation of SiC formation, form low melting point silicon boron compound, increase the diffusivity of oxygen, promote carbon
The consumption of SiClx；(4) boron oxide of glassy state or silicon boron glass can form strong combination with fiber and matrix, destruction composite
Weak binding interface, reduces the toughness of composite.
Pyrolytic carbon and hexagonal boron nitride boundary layer have that high-temperature oxidation resistance is poor, seriously constrain carborundum fine
The performance of dimension enhancing composite material of silicon carbide mechanical behavior under high temperature, therefore, oxidation resistant interface phase is developed, improve silicon carbide fibre
Enhancing composite material of silicon carbide mechanical behavior under high temperature is significantly.
The content of the invention
It is an object of the invention to provide a kind of preparation method of superhigh temperature thermostructural composite boundary layer, it is intended to solve existing
There is the superhigh temperature thermostructural composite of technology its high-temperature oxidation resistance poor, the problem that restriction mechanical behavior under high temperature is played.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of preparation method of superhigh temperature thermostructural composite boundary layer, including：
Silicon carbide layer is prepared on the surface of initial fiber precast body, one-level fiber preform is prepared；
Porous mullite layer is prepared on the surface of the one-level fiber preform, secondary fiber precast body is prepared；
Silicon carbide layer is prepared on the surface of the secondary fiber precast body.
On this basis, further, porous mullite layer is prepared on the surface of the one-level fiber preform, prepares two
The step of level fiber preform, specially：
Using aluminium secondary butylate as silicon source, tetraethyl orthosilicate as silicon source, ethyl acetoacetate as chelating agent, by quality
It is dissolved in ethanol than the aluminium secondary butylate for the first predetermined ratio, tetraethyl orthosilicate, ethyl acetoacetate, is stirred, is prepared
First mixed liquor；
The water that mass ratio with aluminium secondary butylate is the second predetermined ratio is added in first mixed liquor, stirring is equal
It is even, prepare the second mixed liquor；
The one-level fiber preform is carried out into vacuum impregnation in second mixed liquor, insulation makes its gelation, makes
The fiber preform of standby gelation；
Using the technique of Pintsch process, mullite layer is prepared on the surface of the fiber preform of the gelation, prepare two
Level fiber preform.
On this basis, further, first predetermined ratio is 50:1:26.
Or, further, second predetermined ratio is 1:2.
On the basis of above-mentioned any embodiment, further, the surface in initial fiber precast body prepares carbonization
In the step of silicon layer, preparation one-level fiber preform, long-pending technique is oozed using gas phase and prepares silicon carbide layer.
On this basis, further, during the gas phase oozes long-pending technique, with trichloromethyl silane as silicon source.
Or, further, the gas phase is oozed in long-pending technique, with argon gas as diluent gas.
Or, further, the gas phase is oozed in long-pending technique, oozes accumulated temperature degree for 1000 DEG C.
On the basis of above-mentioned any embodiment, further, prepared by the surface in the secondary fiber precast body
In the step of silicon carbide layer, long-pending technique is oozed using gas phase and prepares silicon carbide layer.
On the basis of above-mentioned any embodiment, further, the initial fiber precast body is Hi-Nicalon fibers
Or Hi-Nicalon type S fibers.
The beneficial effects of the invention are as follows：
The invention provides a kind of preparation method of superhigh temperature thermostructural composite boundary layer, the method is warmed in superelevation
The composite material interface layer of three-decker is provided between the fiber and matrix of structural composite material, is outwards respectively from fiber and is carbonized
Silicon layer, porous mullite layer, silicon carbide layer.Silicon carbide layer can prevent elements diffusion, protect matrix not lost with fibre property；
Porous mullite layer has excellent high-temperature oxidation resistance, and high-temperature stability is good, and loose structure plays induction micro-crack deflection
Effect, the performance of the toughening mechanisms such as effective guarantee fiber-bridged, spike protein gene；MULTILAYER COMPOSITE boundary layer is conducive to micro-crack
Deflection.Therefore the superhigh temperature thermostructural composite for having the boundary layer has excellent high-temperature oxidation resistance and excellent height
Warm mechanical property.
Brief description of the drawings
The present invention is further described with reference to the accompanying drawings and examples.
Fig. 1 shows a kind of preparation method of superhigh temperature thermostructural composite boundary layer provided in an embodiment of the present invention
Flow chart；
Fig. 2 shows the graph of a relation of a kind of composite oxidation quality provided in an embodiment of the present invention and time.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only used to explain the present invention, not
Limit the present invention.
Specific embodiment one
As shown in figure 1, a kind of preparation method of superhigh temperature thermostructural composite boundary layer is the embodiment of the invention provides,
Including：
Step S101, silicon carbide layer is prepared on the surface of initial fiber precast body, prepares one-level fiber preform；
Step S102, porous mullite layer is prepared on the surface of one-level fiber preform, prepares secondary fiber precast body；
Step S103, silicon carbide layer is prepared on the surface of secondary fiber precast body.
The embodiment of the present invention is provided with the compound of three-decker between the fiber and matrix of superhigh temperature thermostructural composite
Material interface layer, silicon carbide layer, porous mullite layer, silicon carbide layer are outwards respectively from fiber.Silicon carbide layer can prevent unit
Element diffusion, protects matrix not lost with fibre property；Porous mullite layer has excellent high-temperature oxidation resistance, high-temperature stable
Property it is good, loose structure plays a part of the toughening mechanisms such as induction micro-crack deflection, effective guarantee fiber-bridged, spike protein gene
Play；MULTILAYER COMPOSITE boundary layer is conducive to micro-crack to deflect.The superhigh temperature thermostructural composite therefore with the boundary layer has
There is excellent high-temperature oxidation resistance and excellent mechanical behavior under high temperature.
The raw material and mode that the embodiment of the present invention prepares porous mullite layer to sol-gal process are not limited, it is preferred that
The mode for preparing porous mullite layer can be specially：Using aluminium secondary butylate as silicon source, tetraethyl orthosilicate is used as silicon source, acetyl
Ethyl acetate is molten by aluminium secondary butylate that mass ratio is the first predetermined ratio, tetraethyl orthosilicate, ethyl acetoacetate as chelating agent
Solution stirs in ethanol, prepares the first mixed liquor；The water that mass ratio with aluminium secondary butylate is the second predetermined ratio is added
To in the first mixed liquor, stir, prepare the second mixed liquor；One-level fiber preform is carried out into vacuum in the second mixed liquor
Dipping, heating makes its gelation, then using the technique of Pintsch process, mullite is prepared on the surface of one-level fiber preform
Layer, prepares secondary fiber precast body.
The embodiment of the present invention to silicon source aluminium secondary butylate, silicon source tetraethyl orthosilicate, chelating agent ethyl acetoacetate mass ratio
Do not limit, it is preferred that aluminium secondary butylate, tetraethyl orthosilicate, the mass ratio of ethyl acetoacetate can be 50:1:26.
The embodiment of the present invention is not limited the quality of the water for preparing the second mixed liquor, it is preferred that water and sec-butyl alcohol
The mass ratio of aluminium can be 1:2.
The embodiment of the present invention is not limited the technique that silicon carbide layer is prepared in step S101 and step S103, it is preferred that
Long-pending technique can be oozed using gas phase and prepare silicon carbide layer.
The embodiment of the present invention is oozed long-pending technological parameter to gas phase and is not limited, it is preferred that can be made using trichloromethyl silane
It is silicon source.It is that the atomicity such as Si and C, is easy to get in trichloromethyl silane molecule as the benefit of silicon source using trichloromethyl silane
To the SiC of chemical molecular metering, and ooze that accumulated temperature degree is wider, technique is easily controllable, therefore oozes long-pending SiC as the most frequently used gas phase
Gas.
The embodiment of the present invention is oozed long-pending technological parameter to gas phase and is not limited, it is preferred that can be using argon gas as carrier gas
Body.It is that argon gas is not involved in gas phase and oozes product as rare gas, stable chemical nature as the benefit of diluent gas using argon gas
Reaction, it is cheap, can effectively be played as diluent gas and slow down reaction rate, increase the effect of gas molecule free path,
Be conducive to obtaining uniform, fine and close SiC interfaces phase.
The embodiment of the present invention is oozed long-pending technological parameter to gas phase and is not limited, it is preferred that it can be 1000 DEG C to ooze accumulated temperature degree.
Table 1 oozes the relation of accumulated temperature degree and bending strength
| Ooze accumulated temperature degree (DEG C) | Bending strength (MPa) |
| 900 | 329 |
| 950 | 573 |
| 1000 | 860 |
| 1050 | 683 |
| 1100 | 554 |
As shown in table 1, the bending strength of composite changes with accumulated temperature degree is oozed.
Method in the embodiment of the present invention is not limited the type of be applicable fiber preform, it is preferred that initial fine
Dimension precast body is Hi-Nicalon fibers or Hi-Nicalon type S fibers.As the Hi- of 2nd generation silicon carbide fibre
Nicalon fibers, the mass fraction reduction of its oxygen, the mass fraction of free carbon is of a relatively high, and the size of carborundum grain is compared with the 1st
Dai great, the heat resistance of fiber improves, and keeps the temperature of the maximum tensile strength to bring up to 1300 from 1200 DEG C of 1st generation
℃；Hi-Nicalon type S fibers are made up of sub-micron β-SiC crystal grain, a small amount of carbon and trace oxygen, embody Young mould high
Amount, good heat endurance at creep resistant high and antioxygenic property and 1600 DEG C.
On the basis of above-mentioned any embodiment, the embodiment of the present invention can also include：To the three-level fiber preform
It is densified, is prepared superhigh temperature thermostructural composite.
The embodiment of the present invention is not limited the mode that three-level fiber preform is densified, it is preferred that it can be specially：
Vacuum impregnation and Pintsch process are carried out to three-level fiber preform, superhigh temperature heat structure intermediate product is prepared；To superhigh temperature thermojunction
Structure intermediate product is weighed, when superhigh temperature heat structure intermediate product is more than or equal to relative to the weightening of three-level fiber preform
During predetermined ratio, repetition carries out vacuum impregnation and Pintsch process to superhigh temperature heat structure intermediate product；When in superhigh temperature heat structure
Between product relative to three-level fiber preform weightening be less than predetermined ratio when, from the superhigh temperature heat structure intermediate product conduct
Superhigh temperature thermostructural composite.Superhigh temperature heat structure composite wood is prepared by the way of multiple vacuum impregnation and Pintsch process
Material, its technical maturity, efficiency high.
The embodiment of the present invention to superhigh temperature heat structure intermediate product prepared after vacuum impregnation and Pintsch process relative to
The weightening of three-level fiber preform is not limited, it is preferred that superhigh temperature heat structure intermediate product is relative to three-level fiber preform
Weightening predetermined ratio be 1%.
In the embodiment of the present invention, in the step of carrying out vacuum impregnation to three-level fiber preform, to selected dipping
Agent is not limited, it is preferred that can be using the xylene solution of Polycarbosilane as impregnating agent.
The embodiment of the present invention is not limited the Solute mass fraction of the xylene solution of Polycarbosilane, and the two of Polycarbosilane
Toluene solution mass fraction is higher, and pyrolysis gained ceramic yield is higher, while, it is contemplated that dipping effect, the diformazan of Polycarbosilane
The mass fraction of benzole soln should be more low better, to ensure that viscosity is low as far as possible, it is preferred, therefore, that the dimethylbenzene of Polycarbosilane
The Solute mass fraction of solution is 50%.As shown in table 2, when the Solute mass fraction of the xylene solution of Polycarbosilane is 50%
When~70%, composite viscosity is 83~1027mPas.
The Solute mass fraction of the xylene solution of the Polycarbosilane of table 2 and the relation of viscosity
| The Solute mass fraction (%) of the xylene solution of Polycarbosilane | Viscosity (mPas) |
| 70 | 1027 |
| 60 | 525 |
| 50 | 83 |
The embodiment of the present invention is oozed long-pending technological parameter to gas phase and is not limited, it is preferred that gas phase is oozed in long-pending technique, can be used
Trichloromethyl silane is silicon source, and argon gas is diluent gas, and hydrogen is carrier gas.Its specific process parameter can be as follows：With three chloromethanes
Base silane is silicon source, and argon gas is diluent gas, and air velocity is 50~80cm3/ min, thinner ratio is 9~11, and hydrogen is carrier gas,
Air velocity is 150~200cm3/ min, pressure is 5~10kPa in stove, oozes accumulated temperature degree for 900 DEG C~1100 DEG C, oozes the long-pending time
It is 2h.
The gas phase of table 3 oozes the relation of long-pending technological parameter and composite bending strength
As shown in table 3, the change of long-pending technological parameter is oozed with gas phase, the bending strength of composite also changes therewith.
Specific embodiment two
The embodiment of the invention provides a kind of preparation method of superhigh temperature thermostructural composite boundary layer, and basis herein
On to the composite with the boundary layer, its performance is tested, flow is as follows：
Step 1, SiC layer is prepared on 3D Hi-Nicalon fiber preforms：To 3D Hi-Nicalon fiber preforms
Cleaned, being put into gaseous phase deposition stove carries out gas phase and ooze product.Oozing long-pending technique is：With trichloromethyl silane (MTS) as silicon source, put
In 60 DEG C of bubbling tanks, with hydrogen (H2) it is carrier gas, air velocity is 200cm3/ min, argon gas (Ar) is diluent gas, gas velocity
It is 70cm to spend3/ min, mixed gas pressure intensity is 5kPa, oozes accumulated temperature degree for 1000 DEG C, oozes the long-pending time for 2h；
Step 2, porous 3Al2O3 is prepared on step 1 gained fiber3·2SiO22Layer：
1) using aluminium secondary butylate (ASB) as silicon source, tetraethyl orthosilicate (TEO) is used as silicon source, ethyl acetoacetate (EAcAc)
As chelating agent, according to mass ratio (ASB：TEO：EAcAc it is) 50:1:26, it is dissolved in ethanol, stir, obtain quality
Fraction is 20% solution.
2) according to mass ratio (H2O：ASB it is) 1:2 to adding distilled water in mixed liquor, and stir and be allowed to uniform hydrolysis.
3) step 1 gained fiber is placed in vacuum impregnation tank and is impregnated, and 5h is incubated at 70 DEG C, be allowed to gelation.
4) N is led to2Protection, is heated to 100 DEG C of insulation 1h in cvd furnace, free organic simple substance in volatilization gel, then
500 DEG C of insulation 1h are warming up to 5 DEG C/min, organic cracking is converted into inorganic matter, be then warming up to 1200 DEG C with 1 DEG C/min
Insulation 1h, makes Al2O3And SiO2Reaction produces mullite, then is cooled to room temperature with 1 DEG C/min, obtains porous 3Al2O3·2SiO2
Layer；
Step 3, SiC layer is prepared on step 2 gained fiber：With trichloromethyl silane (MTS) as silicon source, 60 DEG C of drums are placed in
In bubble tank, with hydrogen (H2) it is carrier gas, air velocity is 200cm3/ min, argon gas (Ar) is diluent gas, and air velocity is
70cm3/ min, mixed gas pressure intensity is 5kPa, oozes accumulated temperature degree for 1000 DEG C, oozes the long-pending time for 2h；
Step 4, SiC is prepared using PIP methods on step 3 gained precast bodyf/ SiC ceramic matrix composite material：
1) by the xylene solution of Polycarbosilane that mass fraction is 50%, Vaccum Permeating is put into step 3 gained precast body
In stain machine, vacuum impregnation.
2) 1) gained precast body is put into gaseous phase deposition stove and heats cracking, cracking technology is：Under argon gas protection, with 5
DEG C/after min is warming up to 1200 DEG C and is incubated 1h, room temperature is cooled to 5 DEG C/min；
3) repeat 1), 2) process, untill material weightening is less than 1%.
Step 5, carries out carrying out still air high-temperature oxidation resistant in tube furnace to examine to the composite obtained by step 4
Core：Examination condition is：Tubular type in-furnace temperature is 1100 DEG C, and air velocity 4.4cm/s, total duration is 300h.Respectively 0,5h,
10h, 25h, 50h, 100h, 150h, 200h, 250h, 300h measure sample weight, the result of appraisal as shown in Fig. 2 curve 1 is this
The hot arc composite oxidation quality change that inventive embodiments are provided, curve 2 is the hot junction composite oxidation with carbon interface
Mass change.Contrast finds, substantially, the phase rapid weight loss before oxidation of curve 2 resists for curve 1 and the early stage mass change difference of curve 2
Oxidability is poor, and the extension over time of curve 1 slightly has weightening by comparison, and later stage mass change is identical with the trend of curve 2,
This is caused by matrix SiC is aoxidized.
Step 6, to step 4 gained SiCf/ SiC ceramic matrix composite material carries out bending strength test：Specimen size is 45*4*3mm,
Span is 30mm, and loading velocity is 0.5mm/min, the bending strength tested before and after its 1100 DEG C oxidation 10h.And with PyC interfaces
SiCf/ SiC ceramic matrix composite material is contrasted.As shown in table 4, the hot arc composite that numbering 1 is referred to for the embodiment of the present invention, compiles
Numbers 2 is the hot arc composite with carbon interface.Contrast finds that bending strength of the numbering 1 when for oxidation is slightly below numbering 2, but
It is the bending strength loss 54% of numbering 2 after being aoxidized through 10h, and the bending strength of numbering 1 shows the present invention without significant change
The hot junction composite that embodiment is referred to has excellent normal temperature and mechanical behavior under high temperature, with good oxidation resistance.
Table 4 aoxidizes the bending strength of front and rear composite
The invention provides a kind of preparation method of superhigh temperature thermostructural composite boundary layer, the method is warmed in superelevation
The composite material interface layer of three-decker is provided between the fiber and matrix of structural composite material, is outwards respectively from fiber and is carbonized
Silicon layer, porous mullite layer, silicon carbide layer.Silicon carbide layer can prevent elements diffusion, protect matrix not lost with fibre property；
Porous mullite layer has excellent high-temperature oxidation resistance, and high-temperature stability is good, and loose structure plays induction micro-crack deflection
Effect, the performance of the toughening mechanisms such as effective guarantee fiber-bridged, spike protein gene；MULTILAYER COMPOSITE boundary layer is conducive to micro-crack
Deflection.Therefore the superhigh temperature thermostructural composite that prepared by the method has excellent high-temperature oxidation resistance and excellent high temperature
Mechanical property.
Although present invention has been a certain degree of description, it will be apparent that, do not departing from the spirit and scope of the present invention
Under the conditions of, the appropriate change of each condition can be carried out.It is appreciated that the invention is not restricted to the embodiment, and it is attributed to right
It is required that scope, its equivalent for including each factor.
Claims (10)
1. a kind of preparation method of superhigh temperature thermostructural composite boundary layer, it is characterised in that including：
Silicon carbide layer is prepared on the surface of initial fiber precast body, one-level fiber preform is prepared；
Porous mullite layer is prepared on the surface of the one-level fiber preform, secondary fiber precast body is prepared；
Silicon carbide layer is prepared on the surface of the secondary fiber precast body.
2. the preparation method of superhigh temperature thermostructural composite boundary layer according to claim 1, it is characterised in that in institute
The surface for stating one-level fiber preform prepares porous mullite layer, the step of prepare secondary fiber precast body, specially：
Using aluminium secondary butylate as silicon source, mass ratio is by tetraethyl orthosilicate as chelating agent as silicon source, ethyl acetoacetate
The aluminium secondary butylate of the first predetermined ratio, tetraethyl orthosilicate, ethyl acetoacetate are dissolved in ethanol, are stirred, and prepare first
Mixed liquor；
The water that mass ratio with aluminium secondary butylate is the second predetermined ratio is added in first mixed liquor, is stirred, made
Standby second mixed liquor；
The one-level fiber preform is carried out into vacuum impregnation in second mixed liquor, insulation makes its gelation, prepared solidifying
The fiber preform of gel；
Using the technique of Pintsch process, mullite layer is prepared on the surface of the fiber preform of the gelation, prepare two grades of fibres
Dimension precast body.
3. the preparation method of superhigh temperature thermostructural composite boundary layer according to claim 2, it is characterised in that described
First predetermined ratio is 50:1:26.
4. the preparation method of superhigh temperature thermostructural composite boundary layer according to claim 2, it is characterised in that described
Second predetermined ratio is 1:2.
5. the preparation method of superhigh temperature thermostructural composite boundary layer according to claim 1 and 2, it is characterised in that
In the step of surface in initial fiber precast body prepares silicon carbide layer, preparation one-level fiber preform, oozed using gas phase
Product technique prepares silicon carbide layer.
6. the preparation method of superhigh temperature thermostructural composite boundary layer according to claim 5, it is characterised in that described
Gas phase is oozed in long-pending technique, with trichloromethyl silane as silicon source.
7. the preparation method of superhigh temperature thermostructural composite boundary layer according to claim 5, it is characterised in that described
Gas phase is oozed in long-pending technique, with argon gas as diluent gas.
8. the preparation method of superhigh temperature thermostructural composite boundary layer according to claim 5, it is characterised in that described
Gas phase is oozed in long-pending technique, oozes accumulated temperature degree for 1000 DEG C.
9. the preparation method of superhigh temperature thermostructural composite boundary layer according to claim 1 and 2, it is characterised in that
In the step of surface in the secondary fiber precast body prepares silicon carbide layer, long-pending technique is oozed using gas phase and prepares carborundum
Layer.
10. the preparation method of superhigh temperature thermostructural composite boundary layer according to claim 1 and 2, it is characterised in that
The initial fiber precast body is Hi-Nicalon fibers or Hi-Nicalon type S fibers.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6759151B1 (en) * | 2002-05-22 | 2004-07-06 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Multilayer article characterized by low coefficient of thermal expansion outer layer |
| CN102126868A (en) * | 2011-04-07 | 2011-07-20 | 中国人民解放军国防科学技术大学 | Three-dimensional carbon fiber fabric reinforced mullite ceramic and preparation method thereof |
| CN104264455A (en) * | 2014-09-24 | 2015-01-07 | 中国人民解放军国防科学技术大学 | Low-cost preparation method of fiber surface silicon carbide coating |
| CN104788130A (en) * | 2015-04-21 | 2015-07-22 | 中国人民解放军国防科学技术大学 | C/(SiC/BN)n compound interface phase coating, coating fiber and preparation method of coating fiber |
| CN104817336A (en) * | 2015-04-21 | 2015-08-05 | 中国人民解放军国防科学技术大学 | (BN/SiC)n composite interface-phase coating, coating fiber and preparation method |
-
2016
- 2016-06-03 CN CN201610390103.2A patent/CN106747671B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6759151B1 (en) * | 2002-05-22 | 2004-07-06 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Multilayer article characterized by low coefficient of thermal expansion outer layer |
| CN102126868A (en) * | 2011-04-07 | 2011-07-20 | 中国人民解放军国防科学技术大学 | Three-dimensional carbon fiber fabric reinforced mullite ceramic and preparation method thereof |
| CN104264455A (en) * | 2014-09-24 | 2015-01-07 | 中国人民解放军国防科学技术大学 | Low-cost preparation method of fiber surface silicon carbide coating |
| CN104788130A (en) * | 2015-04-21 | 2015-07-22 | 中国人民解放军国防科学技术大学 | C/(SiC/BN)n compound interface phase coating, coating fiber and preparation method of coating fiber |
| CN104817336A (en) * | 2015-04-21 | 2015-08-05 | 中国人民解放军国防科学技术大学 | (BN/SiC)n composite interface-phase coating, coating fiber and preparation method |
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