CN106966738A - Self-healing ceramic matric composite combustion chamber flame drum and preparation method and application - Google Patents
Self-healing ceramic matric composite combustion chamber flame drum and preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of self-healing ceramic matric composite combustion chamber flame drum and preparation method and application, preparation method comprises the following steps:Combustion chamber flame drum precast body is prepared into SiC interfaces with chemical vapour deposition technique;It is densified again using precursor infiltration and pyrolysis method;It is 1.6~1.8g/cm to repeat precursor infiltration and pyrolysis method to the density of obtained silicon carbide substrate3;SiC matrix layer and BCx base layers are prepared using chemical vapor infiltration area method on the surface of silicon carbide substrate, density is obtained for 2.0~2.5g/cm3Carbon borosilicate self-healing matrix, then at 1000 DEG C carry out 1~3h modifications, obtain composite combustion chamber flame drum.The composite combustion chamber flame drum that the present invention is provided, can improve bending strength, heat-resisting ability, oxidation resistance, self-healing performance and the efficiency gas of combustion chamber flame drum, reduce the quality of combustion chamber flame drum and the discharge of discarded object.
Description
Technical field
The present invention relates to aviation technical field of structural materials, and in particular to a kind of self-healing ceramic matric composite burning
Room burner inner liner and preparation method and application.
Background technology
Combustion chamber is one of core component of aero-engine, and its major function is to turn the chemical energy of fuel by burning
It is changed into heat energy, to improve the ability that combustion gas expands in turbine and jet pipe.In the structure composition of combustion chamber, burner inner liner is tissue
The place of burning, is the critical component for ensureing that air share split, burning are abundant, blending is uniform and being winding is effectively cooled wall.Combustion
Reliability, economy and the life-span for burning room depend greatly on the reliability and significant degree of burner inner liner, therefore develop
The combustion chamber flame drum of high performance and long service life plays vital effect for improving engine performance.
Combustion chamber flame drum belongs to high-temperature component in engine components, the environment temperature being chronically at 1300 DEG C with
On, the temperature in use and military service performance of existing superalloy turbine part are usually taken high-temperature component close to the limit
The safeguard procedures such as air cooling and thermal barrier coating.But, the application of cold air can not only reduce engine combustion efficiency;Part can also be made
Complicatedization, increase design and difficulty of processing.High Performance Aeroengine pursues constantly lifting turbine inlet temperature, and thrust-weight ratio is
During 12-15, inlet temperature is up to more than 1800 DEG C, the temperature in use and military service performance of existing superalloy turbine part before turbine
Close to the limit, even if taking cooling technology and Thermal Barrier Coating Technologies, it is also difficult to which the design for meeting aero-engine of future generation will
Ask.It is an advanced technology to prepare combustion chamber flame drum using refractory ceramics based composites, and ceramic matric composite has
The features such as high temperature resistant, density are low, corrosion-resistant and anti-oxidant, disclosure satisfy that hot-end component is used under higher temperature environment, not only
It is beneficial to significantly loss of weight, can also saves cold air even without cooling, so as to improves overall pressure tatio (Overall Pressure
Ratios, OPR), realize and 300~500 DEG C of operating temperature, structure loss of weight 50% are further lifted on the basis of high temperature alloy heatproof
~70%, the crucial heat resistant structure that certainly will turn into high thrust-weight ratio aero-engine prepares material.
Existing carbon/silicon carbide ceramic matrix composite has excellent performance, is that instead of high temperature alloy as aero-engine
The candidate materials of hot junction component material, but under high-temperature oxidation environment, SiCfThe micro-crack produced in composite and hole
Hole easily turns into Oxidant (O2And H2O) and exhaust gas corrosion passage, cause interface phase and fiber oxidation in SiC constituent elements by
Damage;In addition, the stress in Service Environment can promote matrices of composite material to ftracture, the damage and corrosion of accelerated material, influence
Its long-life requirement of being on active service under high temperature combustion environment, so that seriously restriction SiC ceramic based composites are in engine combustion
The application of room burner inner liner.
The content of the invention
For defect of the prior art, present invention aims at provide a kind of self-healing ceramic matric composite combustion chamber
Burner inner liner and preparation method and application, with improve the bending strength of combustion chamber flame drum, heat-resisting ability, oxidation resistance and
Efficiency gas, reduces the quality of combustion chamber flame drum and the discharge of NOx, COx the like waste, and assign combustion chamber flame drum certainly
Healing properties, when there is crackle and hole in material, can in-situ authigenic into glass phase, reach the effect of active packing, prevent
Oxidant inwardly spreads, the oxide etch damage of reduction interface and fiber, improves the life-span of combustion chamber flame drum.
To achieve the above object, the technical scheme that provides of the present invention is:
In a first aspect, the invention provides a kind of preparation method of composite combustion chamber flame drum, comprising the following steps:
S1:Combustion chamber flame drum precast body is prepared into SiC interfaces with chemical vapour deposition technique;Wherein, the reaction of chemical vapour deposition technique
Gas is trichloromethyl silane;S2:Using the mixed solution of Polycarbosilane and dimethylbenzene as precursor solution, the production that step S1 is obtained
Thing is densified using precursor infiltration and pyrolysis method;Repeat using precursor infiltration and pyrolysis method to obtained silicon carbide substrate
Density is 1.6~1.8g/cm3;S3:SiC matrix layer and BCx are prepared using chemical vapor infiltration area method on the surface of silicon carbide substrate
Base layer, obtains density for 2.0~2.5g/cm3Carbon borosilicate self-healing matrix;Wherein, using trichloromethyl silane as deposition gas
SiC matrix layer is prepared, BCx base layers are prepared using boron chloride and methane as deposition gas;S4:Carbon borosilicate self-healing matrix is existed
1~3h modifications are carried out at 1000 DEG C, composite combustion chamber flame drum is obtained.It should be noted that changing in step S4
Property processing, be in order in the hole of carbon borosilicate self-healing intrinsic silicon and a large amount of fine and close Pyrex phases are filled on surface;Through
Composite combustion chamber flame drum after multi-component multi-layer self-healing matrix modification, under water oxygen combustion gas stress coupling environment, carbon boron
The substantial amounts of glass phase of silicon self-healing intrinsic silicon self-healing constituent element formation, on the one hand can prevent the carborundum phase oxidation of inside rotten
Erosion is impaired, on the other hand makes carbon borosilicate self-healing matrix densification, composite combustion chamber flame drum is obtained so as to improve
Bending strength and modulus.
In the further embodiment of the present invention, in step S1, chemical vapour deposition technique is specially:With trichloromethyl silicon
Alkane is reaction gas, and hydrogen is carrier gas, and argon gas is carrier gas, and depositing temperature is 1100~1230 DEG C, and pressure is 1~5kPa, deposition
Time is 5~15h;Wherein, the volume ratio of hydrogen and trichloromethyl silane is 1:8~1:12.It should be noted that preparing
SiC interfaces be single-phase, interfacial thickness is preferably 3~10 μm.In combustion chamber flame drum (silicon carbide fibre) precast body surface
One layer of carborundum is deposited, can make to form weak interface combination between fiber and matrix so that fiber can pass through unsticking and extraction
Effective consumed energy, so as to get composite show obvious ductile rupture feature in destruction, be conducive to composite wood
Expect the raising of mechanical property.
In the further embodiment of the present invention, in step S2, precursor infiltration and pyrolysis method includes:In vacuum condition
Under, the obtained products of step S1 are impregnated in 4~6h in the mixed solution of Polycarbosilane and dimethylbenzene, then done for 100~140 DEG C
It is dry;Dried product is cracked into 3~6h in nitrogen or argon gas in 800~1200 DEG C;Repeat precursor infiltration and pyrolysis method
Step, the density to obtained silicon carbide substrate is 1.6~1.8g/cm3;Wherein, the mixed solution of Polycarbosilane and dimethylbenzene
The mass fraction of middle Polycarbosilane is 20%~50%.It should be noted that dipping process can be carried out in impregnating autoclave, true
Under empty condition, according to capillarity and diffusion, Polycarbosilane can penetrate into the inside of combustion chamber flame drum precast body, and
Fill hole therein;Pintsch process is that by polymer Polycarbosilane is converted into ceramic base, obtains silicon carbide-based
Body.
In the further embodiment of the present invention, in step S3, the preparation method of SiC matrix layer is specially:With trichlorine
Methyl-monosilane (CH3SiCl3) it is deposition gas, hydrogen is carrier gas, and argon gas is carrier gas, and depositing temperature is 800~1100 DEG C, deposition
Time is 10~30h, and pressure is 1kPa;Wherein, the flow of hydrogen is 100~400ml/min, the flow of argon gas for 100~
300ml/min;The preparation method of BCx base layers is specially:Using boron chloride and methane as deposition gas, hydrogen and argon gas are load
Gas, depositing temperature is 900~1000 DEG C, and sedimentation time is 10~30h, and pressure is 1kPa;Wherein, the stream of boron chloride and methane
Amount is than being 2:1~6:1, the flow velocity of hydrogen and argon gas is 50~80mL/min.
In the further embodiment of the present invention, in step S3, on the surface of silicon carbide substrate, alternately prepare successively
SiC matrix layer and BCx base layers, obtain density for 2.0~2.5g/cm3Carbon borosilicate self-healing matrix;Wherein, carbon borosilicate from
The outermost layer of healing matrices is SiC matrix layer.It should be noted that:On the surface of silicon carbide substrate, SiC matrix is first prepared
Layer, then BCx base layers are prepared, circulate according to this, obtain density for 2.0~2.5g/cm3Carbon borosilicate self-healing matrix, and protect
The outermost layer for demonstrate,proving carbon borosilicate self-healing matrix is SiC matrix layer, that is to say, that in obtained carbon borosilicate self-healing matrix,
SiC matrix layer is at least two layers, and BCx base layers are at least one layer;The order setting of base layer allows for PIP methods and prepared
SiC matrix there is thermal matching, when the thermal coefficient of expansion of matrix is similar, it is possible to reduce material is in hot environment because of thermal expansion
The crackle that coefficient difference is produced, therefore first deposit on the surface of silicon carbide substrate one layer of SiC matrix, redeposited one layer of BCx matrix,
Circulate according to this, successively alternating deposit SiC matrix and BCx matrixes;And last layer is set to SiC matrix, allows for SiC matrix
There is more high temperature tolerance and inoxidizability than BCx matrix.
In the further embodiment of the present invention, on the surface of composite combustion chamber flame drum, rare earth silicic acid is prepared
Salt environment barrier coating;The raw material of rare earth silicate Environmental Barrier Coatings on Si-based Ceramics includes the first component and the second component, and the first component is not come
Stone, ytterbium silicate (Yb2SiO5), polyvinyl butyral (PVB) and phosphate, the second component is ethanol;Wherein:First component and
The mass ratio of two components is 1:1~1:3, mass fraction of the polyvinyl butyral in the first component is 4%~8%, phosphate
Mass fraction in the first component is 0.4%~1.0%, and the mass ratio of mullite and ytterbium silicate is 88:12.Need explanation
It is:Rare earth silicate Environmental Barrier Coatings on Si-based Ceramics is prepared on the surface of composite combustion chamber flame drum, that is, in composite burning
Set up and shield together between the adverse circumstances that room flame barrel component surface and engine superhigh temperature, Korrosionsmedium, high velocity air wash away
Barrier coating, can reduce influence of the engine environmental to composite combustion chamber flame drum component performance, it is to avoid the stabilization of material
Property deteriorates, and prevents that the mechanical property of material is decreased obviously, can further improve the ring of composite combustion chamber flame drum
Border tolerance and resistance to combustion gas corrosion performance.
In the further embodiment of the present invention, the preparation method of rare earth silicate Environmental Barrier Coatings on Si-based Ceramics includes:By first
Component and second component 12~16h of ball milling mixing, by obtained mixture brushing on the surface of composite combustion chamber flame drum,
Then 2~5h is sintered at 1400 DEG C~1500 DEG C.
In the further embodiment of the present invention, combustion chamber flame drum precast body is to use silicon carbide fibre with three-dimensional four
Footwork braiding is formed, wherein, braid angle is 20~45 °, the volume fraction 30%~50% of silicon carbide fibre.Need explanation
It is:Combustion chamber flame drum is the core component of engine chamber, including flame tube head and cylinder, and cylinder includes inwall and outer
Wall;During braiding, flame tube head and inside and outside wall are woven respectively, and the precast body of three parts is then sutured into skill using fiber
Art connects together shaping, and obtained product is carried out into high-temperature heat treatment, to remove the glue and impurity on surface, is burnt
Room burner inner liner precast body;Using three-dimensional four step braiding combustion chamber flame drum precast body, combustion chamber flame drum can be improved prefabricated
The intensity of body, it is ensured that excellent mechanical property, coupling part use fiber suturing skill, can avoid ceramic matric composite with
High temperature alloy fastener is destroyed because caused by difference of linear expansion is big, it is ensured that bonding strength, while cancelling cooling system.
Second aspect, the invention provides the composite combustion chamber flame drum prepared according to above-mentioned method.
The third aspect, the invention provides the above-mentioned composite combustion chamber flame drum prepared to prepare engine outstanding
It is to prepare the application in aero-engine.
The technical scheme that the present invention is provided, has the following advantages:
(1) present invention prepares precast body using three dimensional knitting method, not only makes precast body in many axial planes in space and between face
It is complete continuous, fundamentally avoid two-dimension laminate precast body intensity and modulus be poor in a thickness direction, interlaminar shear strength is low and
The relatively low shortcoming of damage tolerance, and 3 D weaving precast body comprehensive mechanical property is good, and thermal shock resistance properties is excellent.
(2) silicon carbide interface that the present invention is used has more preferable inoxidizability compared with carbon interface, is pyrolyzed carbon boundary layer
Easily aoxidized more than 400 DEG C, composite can be because intensity occurs in the rapid oxidation at carbon interface under high-temperature oxidation environment
Dramatic decrease, and silicon carbide interface with applied at elevated temperature environment oxidation resistance it is strong, it is not oxidizable, play interface transmission and carry
The effect of lotus, makes material have more preferable mechanical property in hot environment.
(3) present invention prepares self-healing using PIP+CVI United Technologies (precursor infiltration and pyrolysis method+chemical vapor infiltration area method)
Modified matrix is closed, the silicon carbide substrate of certain density is prepared using PIP techniques (precursor infiltration and pyrolysis method) first, presoma holds
The hole of fiber interfascicular is easily immersed, the densification degree of fiber interfascicular is high after ceramic, then use CVI technique (chemical gas
Mutually ooze area method) BCx and SiC matrix are alternately prepared, solve composite caused by single PIP methods (precursor infiltration and pyrolysis method)
Final densities it is low and brought by volume contraction component internal stress and micro-crack the problems such as, using the process integration in the present invention
Prepared ceramic matric composite and component have higher final densities and relatively low porosity, reduce material and component exists
The defects such as the internal stress and micro-crack that are produced in preparation process, are also solved individually using CVI techniques (chemical vapor infiltration area method)
It is difficult to the problem of composite consistency is not high enough caused by fiberfill fibers interfascicular space when preparing self-healing matrix.
(4) Environmental Barrier Coatings on Si-based Ceramics that the present invention is prepared using brushing method to prepared ceramic matric composite, combustion chamber fire
Flame cylinder long-term use temperature 1300~1500 DEG C even more than, the long-term use substantially beyond SiC/SiC composites
Temperature, makes the surface stability of SiC/SiC composite combustion chamber flame drums occur drastically to deteriorate, causes the mechanics of composite
Performance is decreased obviously, and causes its life-span to substantially reduce, and Environmental Barrier Coatings on Si-based Ceramics is disliked in composite material surface and aero-engine high temperature
One of barrier coatings is set up between bad use environment, prevents or reduces influence of the engine environmental to composite wood material list, prepare at present
Plasma spraying method being used the technique of Environmental Barrier Coatings on Si-based Ceramics, the present invention can be greatly reduced using slurry brushing method and is prepared into more
Sheet and manufacturing cycle.
(5) technical scheme that provides of the present invention, can improve the bending strength of combustion chamber flame drum, heat-resisting ability and anti-
Oxidability, reduces the quality of combustion chamber flame drum, and weight loss effect reaches 50% or so, high mechanical properties;And structure design
Simply, cooling system is saved, increases efficiency gas, the discharge of NOx and COx the like waste is reduced;Furthermore, combustion chamber of the invention
Burner inner liner has self-healing performance by modified BCx+SiC matrixes, when crackle and hole occurs in material, in crackle and hole
Place can in-situ authigenic into glass phase, reach the effect of active packing, prevent Oxidant from inwardly spreading, reduction interface and fibre
The oxide etch damage of dimension, meets the long-life use requirement of combustion chamber flame drum.The invention provides a kind of high-temperature behavior is steady
Fixed, the carbon/silicon carbide ceramic matrix composite combustion chamber flame drum with self-healing matrix of excellent in mechanical performance, is solved existing
Flame tube structure design is complicated, and weight is big, and difficulty of processing is big, and heatproof is low and needs air cooling, and fuel gas buring is insufficient, material easily quilt
The technical problems such as exhaust gas corrosion.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Embodiment
Technical scheme is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that retouched
The embodiment stated is only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, sheet
The every other embodiment that field those of ordinary skill is obtained under the premise of creative work is not made, belongs to the present invention
The scope of protection.
Experimental method in following embodiments, is conventional method unless otherwise specified.
Test material used, is to be commercially available from conventional reagent shop unless otherwise specified in following embodiments.
Quantitative test in following examples, is respectively provided with three repetition experiments, and data are the average value of three repetition experiments
Or mean+SD.
The present invention provides a kind of preparation method of composite combustion chamber flame drum, comprises the following steps:
S1:Combustion chamber flame drum precast body is prepared into SiC interfaces with chemical vapour deposition technique;Wherein, chemical vapor deposition
The reaction gas of method is trichloromethyl silane;Combustion chamber flame drum precast body is to use silicon carbide fibre with three-dimensional four step braiding
Into, wherein, braid angle is 20~45 °, the volume fraction 30%~50% of silicon carbide fibre;Chemical vapour deposition technique is specially:
Using trichloromethyl silane as reaction gas, hydrogen is carrier gas, and argon gas is carrier gas, and depositing temperature is 1100~1230 DEG C, and pressure is 1
~5kPa, sedimentation time is 5~15h;Wherein, the volume ratio of hydrogen and trichloromethyl silane is 1:8~1:12.
S2:Using the mixed solution of Polycarbosilane and dimethylbenzene as precursor solution, the product that step S1 is obtained is using first
Body infiltration pyrolysis method is driven to be densified;Repeat to use precursor infiltration and pyrolysis method to obtained silicon carbide substrate density for
1.6~1.8g/cm3;Precursor infiltration and pyrolysis method includes:Under vacuum, the obtained products of step S1 are impregnated in poly- carbon
4~6h in the mixed solution of silane and dimethylbenzene, then 100~140 DEG C of dryings;By dried product in nitrogen or argon gas
3~6h is cracked in 800~1200 DEG C;The step of repeating precursor infiltration and pyrolysis method, the density to obtained silicon carbide substrate is
1.6~1.8g/cm3;Wherein, in the mixed solution of Polycarbosilane and dimethylbenzene the mass fraction of Polycarbosilane for 20%~
50%.
S3:SiC matrix layer and BCx base layers are prepared using chemical vapor infiltration area method on the surface of silicon carbide substrate, obtained
Density is 2.0~2.5g/cm3Carbon borosilicate self-healing matrix;Wherein, SiC matrix is prepared by deposition gas of trichloromethyl silane
Layer, BCx base layers are prepared using boron chloride and methane as deposition gas;SiC matrix layer preparation method be specially:With trichloromethyl
Silane is deposition gas, and hydrogen is carrier gas, and argon gas is carrier gas, and depositing temperature is 800~1100 DEG C, and sedimentation time is 10~30h,
Pressure is 1kPa;Wherein, the flow of hydrogen is 100~400ml/min, and the flow of argon gas is 100~300ml/min;BCx matrixes
Layer preparation method be specially:Using boron chloride and methane as deposition gas, hydrogen and argon gas are carrier gas, depositing temperature is 900~
1000 DEG C, sedimentation time is 10~30h, and pressure is 1kPa;Wherein, the flow-rate ratio of boron chloride and methane is 2:1~6:1, hydrogen
The flow velocity of gas and argon gas is 50~80mL/min;On the surface of silicon carbide substrate, SiC matrix layer and BCx are alternately prepared successively
Base layer, obtains density for 2.0~2.5g/cm3Carbon borosilicate self-healing matrix;Wherein, the outermost of carbon borosilicate self-healing matrix
Side layer is SiC matrix layer.
S4:Carbon borosilicate self-healing matrix is subjected to 1~3h modifications at 1000 DEG C, composite combustion chamber fire is obtained
Flame cylinder.
S5:On the surface of composite combustion chamber flame drum, rare earth silicate Environmental Barrier Coatings on Si-based Ceramics is prepared;Rare earth silicate ring
The raw material of border barrier coating includes the first component and the second component, and the first component is mullite, ytterbium silicate, polyvinyl butyral and phosphorus
Acid esters, the second component is ethanol;Wherein:The mass ratio of first component and the second component is 1:1~1:3, polyvinyl butyral exists
Mass fraction in first component is 4%~8%, and mass fraction of the phosphate in the first component is 0.4%~1.0%, not
The mass ratio for coming stone and ytterbium silicate is 88:12;The preparation method of rare earth silicate Environmental Barrier Coatings on Si-based Ceramics includes:By the first component and
Two component 12~16h of ball milling mixing, by obtained mixture brushing on the surface of composite combustion chamber flame drum, Ran Hou
1400 DEG C~1500 DEG C 2~5h of the lower sintering of argon gas protection.
The preparation method of the composite combustion chamber flame drum provided with reference to specific embodiment the present invention is made into one
Walk explanation.
Embodiment one
By silicon carbide fibre three-dimensional four step braiding combustion chamber flame drum precast body, wherein braid angle is 40 °, carborundum
The volume fraction of fiber is 35%;Obtained combustion chamber flame drum precast body chemical vapour deposition technique is prepared into SiC interfaces, its
In using trichloromethyl silane as reaction gas, hydrogen is carrier gas, and argon gas is carrier gas, and the volume ratio of hydrogen and trichloromethyl silane is
1:10, depositing temperature is 1130 DEG C, and pressure is 4.5kPa, and sedimentation time is 8h, and the SiC interfacial thicknesses prepared are 6 μm.
Product obtained above is impregnated into 6h with the mixed solution of Polycarbosilane and dimethylbenzene under vacuum, then
120 DEG C of dryings;Dried product is cracked into 4h in nitrogen in 1000 DEG C;Precursor infiltration and pyrolysis 10 cycles of method are repeated,
The density of obtained silicon carbide substrate is 1.73g/cm3;Wherein, Polycarbosilane in the mixed solution of Polycarbosilane and dimethylbenzene
Mass fraction is 30%.Obtained silicon carbide substrate is alternately prepared into SiC matrix layer and BCx matrixes using chemical vapor infiltration area method
Layer, first prepares SiC matrix layer:Using trichloromethyl silane as deposition gas, hydrogen is carrier gas, and argon gas is carrier gas, and depositing temperature is
980 DEG C, sedimentation time is 15h, and pressure is 1kPa;Wherein, the flow of hydrogen is 150ml/min, and the flow of argon gas is 180ml/
min;BCx base layers are prepared again:Using boron chloride and methane as deposition gas, hydrogen and argon gas are carrier gas, and depositing temperature is 980
DEG C, sedimentation time is 15h, and pressure is 1kPa;Wherein, the flow-rate ratio of boron chloride and methane is 4:1, the flow velocity of hydrogen and argon gas
It is 60mL/min;Above-mentioned method is recycled successively and prepares SiC matrix layer and BCx base layers, obtains density for 2.3g/
cm3Carbon borosilicate self-healing matrix, also, carbon borosilicate self-healing matrix outermost layer for SiC matrix layer.By obtained carbon boron
Silicon self-healing matrix carries out 1.5h modifications at 1000 DEG C, obtains composite combustion chamber flame drum.
Rare earth silicate Environmental Barrier Coatings on Si-based Ceramics is prepared in obtained composite combustion chamber flame drum:Rare earth silicate environment hinders
The raw material of coating includes the first component and the second component, and the first component is mullite, ytterbium silicate, polyvinyl butyral and phosphoric acid
Ester, the second component is ethanol;Wherein:The mass ratio of first component and the second component is 1:3, polyvinyl butyral is in the first component
In mass fraction be 4%, mass fraction of the phosphate in the first component is 0.6%, the mass ratio of mullite and ytterbium silicate
For 88:12;By the first component and the second component ball milling mixing 15h, by obtained mixture brushing in composite combustion chamber fire
The surface of flame cylinder, then sinters 3h under 1450 DEG C of argon gas protections, obtains finished product.
Embodiment two
By silicon carbide fibre three-dimensional four step braiding combustion chamber flame drum precast body, wherein braid angle is 30 °, carborundum
The volume fraction of fiber is 35%;Obtained combustion chamber flame drum precast body chemical vapour deposition technique is prepared into SiC interfaces, its
In using trichloromethyl silane as reaction gas, hydrogen is carrier gas, and argon gas is carrier gas, and the volume ratio of hydrogen and trichloromethyl silane is
1:9, depositing temperature is 1150 DEG C, and pressure is 3kPa, and sedimentation time is 6h, and the SiC interfacial thicknesses prepared are 4 μm.
Product obtained above is impregnated into 5h with the mixed solution of Polycarbosilane and dimethylbenzene under vacuum, then
120 DEG C of dryings;Dried product is cracked into 6h in nitrogen in 950 DEG C;Precursor infiltration and pyrolysis 8 cycles of method are repeated, are obtained
The density of the silicon carbide substrate arrived is 1.62g/cm3;Wherein, in the mixed solution of Polycarbosilane and dimethylbenzene Polycarbosilane matter
It is 35% to measure fraction.Obtained silicon carbide substrate is alternately prepared into SiC matrix layer and BCx matrixes using chemical vapor infiltration area method
Layer, first prepares SiC matrix layer:Using trichloromethyl silane as deposition gas, hydrogen is carrier gas, and argon gas is carrier gas, and depositing temperature is
900 DEG C, sedimentation time is 13h, and pressure is 1kPa;Wherein, the flow of hydrogen is 200ml/min, and the flow of argon gas is 300ml/
min;BCx base layers are prepared again:Using boron chloride and methane as deposition gas, hydrogen and argon gas are carrier gas, and depositing temperature is 950
DEG C, sedimentation time is 13h, and pressure is 1kPa;Wherein, the flow-rate ratio of boron chloride and methane is 3:1, the flow velocity of hydrogen and argon gas
It is 65mL/min;Above-mentioned method is recycled successively and prepares SiC matrix layer and BCx base layers, obtains density for 2.1g/
cm3Carbon borosilicate self-healing matrix, also, carbon borosilicate self-healing matrix outermost layer for SiC matrix layer.By obtained carbon boron
Silicon self-healing matrix carries out 2h modifications at 1000 DEG C, obtains composite combustion chamber flame drum.
Rare earth silicate Environmental Barrier Coatings on Si-based Ceramics is prepared in obtained composite combustion chamber flame drum:Rare earth silicate environment hinders
The raw material of coating includes the first component and the second component, and the first component is mullite, ytterbium silicate, polyvinyl butyral and phosphoric acid
Ester, the second component is ethanol;Wherein:The mass ratio of first component and the second component is 1:2, polyvinyl butyral is in the first component
In mass fraction be 5%, mass fraction of the phosphate in the first component is 0.6%, the mass ratio of mullite and ytterbium silicate
For 88:12;By the first component and the second component ball milling mixing 12h, by obtained mixture brushing in composite combustion chamber fire
The surface of flame cylinder, then argon gas sinters 3h at 1400 DEG C, obtains finished product.
Embodiment three
By silicon carbide fibre three-dimensional four step braiding combustion chamber flame drum precast body, wherein braid angle is 20 °, carborundum
The volume fraction of fiber is 30%;Obtained combustion chamber flame drum precast body chemical vapour deposition technique is prepared into SiC interfaces, its
In using trichloromethyl silane as reaction gas, hydrogen is carrier gas, and argon gas is carrier gas, and the volume ratio of hydrogen and trichloromethyl silane is
1:8, depositing temperature is 1100 DEG C, and pressure is 1kPa, and sedimentation time is 10h, and the SiC interfacial thicknesses prepared are 8 μm.
Product obtained above is impregnated into 4h with the mixed solution of Polycarbosilane and dimethylbenzene under vacuum, then
100 DEG C of dryings;Dried product is cracked into 4h in nitrogen in 900 DEG C;The cycle of precursor infiltration and pyrolysis method 8 is repeated, is obtained
Silicon carbide substrate density be 1.64g/cm3;Wherein, in the mixed solution of Polycarbosilane and dimethylbenzene Polycarbosilane quality
Fraction is 50%.Obtained silicon carbide substrate is alternately prepared into SiC matrix layer and BCx base layers using chemical vapor infiltration area method,
First prepare SiC matrix layer:Using trichloromethyl silane as deposition gas, hydrogen is carrier gas, and argon gas is carrier gas, and depositing temperature is 800
DEG C, sedimentation time is 10h, and pressure is 1kPa;Wherein, the flow of hydrogen is 100ml/min, and the flow of argon gas is 100ml/min;
BCx base layers are prepared again:Using boron chloride and methane as deposition gas, hydrogen and argon gas are carrier gas, and depositing temperature is 980 DEG C, is sunk
The product time is 10h, and pressure is 1kPa;Wherein, the flow-rate ratio of boron chloride and methane is 2:1, the flow velocity of hydrogen and argon gas is
50mL/min;Above-mentioned method is recycled successively and prepares SiC matrix layer and BCx base layers, obtains density for 2.05g/cm3's
Carbon borosilicate self-healing matrix, also, the outermost layer of carbon borosilicate self-healing matrix is SiC matrix layer.By obtained carbon borosilicate certainly
Healing matrices carry out 1h modifications at 1000 DEG C, obtain composite combustion chamber flame drum.
Rare earth silicate Environmental Barrier Coatings on Si-based Ceramics is prepared in obtained composite combustion chamber flame drum:Rare earth silicate environment hinders
The raw material of coating includes the first component and the second component, and the first component is mullite, ytterbium silicate, polyvinyl butyral and phosphoric acid
Ester, the second component is ethanol;Wherein:The mass ratio of first component and the second component is 1:1, polyvinyl butyral is in the first component
In mass fraction be 4%, mass fraction of the phosphate in the first component is 0.4%, the mass ratio of mullite and ytterbium silicate
For 88:12;By the first component and the second component ball milling mixing 12h, by obtained mixture brushing in composite combustion chamber fire
The surface of flame cylinder, then the Ar-sintering 2h at 1400 DEG C, obtains finished product.
Example IV
By silicon carbide fibre three-dimensional four step braiding combustion chamber flame drum precast body, wherein braid angle is 45 °, carborundum
The volume fraction of fiber is 50%;Obtained combustion chamber flame drum precast body chemical vapour deposition technique is prepared into SiC interfaces, its
In using trichloromethyl silane as reaction gas, hydrogen is carrier gas, and argon gas is carrier gas, and the volume ratio of hydrogen and trichloromethyl silane is
1:12, depositing temperature is 1230 DEG C, and pressure is 5kPa, and sedimentation time is 8h, and the SiC interfacial thicknesses prepared are 9 μm.
Product obtained above is impregnated into 6h with the mixed solution of Polycarbosilane and dimethylbenzene under vacuum, then
140 DEG C of dryings;Dried product is cracked into 6h in nitrogen in 1200 DEG C;Precursor infiltration and pyrolysis 12 cycles of method are repeated,
The density of obtained silicon carbide substrate is 1.8g/cm3;Wherein, Polycarbosilane in the mixed solution of Polycarbosilane and dimethylbenzene
Mass fraction is 50%.Obtained silicon carbide substrate is alternately prepared into SiC matrix layer and BCx matrixes using chemical vapor infiltration area method
Layer, first prepares SiC matrix layer:Using trichloromethyl silane as deposition gas, hydrogen is carrier gas, and argon gas is carrier gas, and depositing temperature is
1100 DEG C, sedimentation time is 30h, and pressure is 1kPa;Wherein, the flow of hydrogen is 400ml/min, and the flow of argon gas is 200ml/
min;BCx base layers are prepared again:Using boron chloride and methane as deposition gas, hydrogen and argon gas are carrier gas, and depositing temperature is 1000
DEG C, sedimentation time is 30h, and pressure is 1kPa;Wherein, the flow-rate ratio of boron chloride and methane is 6:1, the flow velocity of hydrogen and argon gas
It is 80mL/min;Above-mentioned method is recycled successively and prepares SiC matrix layer and BCx base layers, obtains density for 2.5g/
cm3Carbon borosilicate self-healing matrix, also, carbon borosilicate self-healing matrix outermost layer for SiC matrix layer.By obtained carbon boron
Silicon self-healing matrix carries out 3h modifications at 1000 DEG C, obtains composite combustion chamber flame drum.
Rare earth silicate Environmental Barrier Coatings on Si-based Ceramics is prepared in obtained composite combustion chamber flame drum:Rare earth silicate environment hinders
The raw material of coating includes the first component and the second component, and the first component is mullite, ytterbium silicate, polyvinyl butyral and phosphoric acid
Ester, the second component is ethanol;Wherein:The mass ratio of first component and the second component is 1:3, polyvinyl butyral is in the first component
In mass fraction be 8%, mass fraction of the phosphate in the first component is 1.0%, the mass ratio of mullite and ytterbium silicate
For 88:12;By the first component and the second component ball milling mixing 16h, by obtained mixture brushing in composite combustion chamber fire
The surface of flame cylinder, then the Ar-sintering 5h at 1500 DEG C, obtains finished product.
The composite combustion chamber flame drum that the embodiment of the present invention one to example IV is prepared carries out performance measurement,
And using TiAl high temperature alloys combustion chamber flame drum of the prior art as comparative example, concrete outcome is as shown in table 1 below:
The performance of the composite combustion chamber flame drum of table 1
It should be noted that situation about enumerating except above-described embodiment one to example IV, from other preparation methods
Parameter is also feasible.
The self-healing ceramic matric composite aero-engine for the offer that the preparation method provided by the present invention is obtained is fired
Room burner inner liner is burnt, is had the following advantages:(1) present invention prepares precast body using three dimensional knitting method, not only precast body is existed
It is complete continuous between in many axial planes in space and face, fundamentally avoid two-dimension laminate precast body intensity and modulus in a thickness direction
Difference, the shortcoming that interlaminar shear strength is low and damage tolerance is relatively low, and 3 D weaving precast body comprehensive mechanical property is good, thermal shock
Excellent performance.(2) silicon carbide interface that the present invention is used has more preferable inoxidizability compared with carbon interface, is pyrolyzed carbon boundary layer
Easily aoxidized more than 400 DEG C, composite can be because intensity occurs in the rapid oxidation at carbon interface under high-temperature oxidation environment
Dramatic decrease, and silicon carbide interface with applied at elevated temperature environment oxidation resistance it is strong, it is not oxidizable, play interface transmission and carry
The effect of lotus, makes material have more preferable mechanical property in hot environment.(3) present invention is (first using PIP+CVI United Technologies
Drive body infiltration pyrolysis method+chemical vapor infiltration area method) self-healing modification matrix is prepared, using PIP techniques, (precursor dipping splits first
Solution) silicon carbide substrate of certain density is prepared, presoma easily immerses the hole of fiber interfascicular, the fiber interfascicular after ceramic
Densification degree it is high, BCx and SiC matrix are alternately then prepared using CVI techniques (chemical vapor infiltration area method), solved single
Composite final densities are low caused by PIP methods (precursor infiltration and pyrolysis method) and the component internal stress brought by volume contraction
And the problems such as micro-crack, had using the ceramic matric composite and component prepared by the process integration in the present invention higher most
Whole density and relatively low porosity, reduce the defects such as internal stress and micro-crack that material and component produce in preparation process,
Solve and be difficult to fiberfill fibers interfascicular space when individually preparing self-healing matrix using CVI techniques (chemical vapor infiltration area method) and lead
The problem of composite consistency of cause is not high enough.(4) present invention uses brushing method to prepared ceramic matric composite system
Standby Environmental Barrier Coatings on Si-based Ceramics, the long-term use temperature of combustion chamber flame drum 1300~1500 DEG C even more than, substantially beyond
The long-term use temperature of SiC/SiC composites, makes the surface stability of SiC/SiC composite combustion chamber flame drums occur suddenly
Play deteriorates, and causes the mechanical property of composite to be decreased obviously, causes its life-span to substantially reduce, and Environmental Barrier Coatings on Si-based Ceramics is in composite wood
Barrier coatings together are set up between material surface and aero-engine high temperature hostile use environment, prevents or reduces engine environmental to multiple
The influence of condensation material list, plasma spraying method is used the technique that Environmental Barrier Coatings on Si-based Ceramics is prepared at present more, and the present invention is applied using slurry
Brush method can greatly reduce preparation cost and manufacturing cycle.
Using the technical scheme that provides of the present invention, can improve the bending strength of combustion chamber flame drum, heat-resisting ability and
Oxidation resistance, reduces the quality of combustion chamber flame drum, and weight loss effect reaches 50% or so, high mechanical properties;And structure is set
Meter is simple, saves cooling system, increases efficiency gas, reduces the discharge of NOx and COx the like waste;Furthermore, burning of the invention
Room burner inner liner has self-healing performance by modified BCx+SiC matrixes, when crackle and hole occurs in material, in crackle and hole
At hole can in-situ authigenic into glass phase, reach the effect of active packing, prevent Oxidant from inwardly spreading, reduction interface and
The oxide etch damage of fiber, meets the long-life use requirement of combustion chamber flame drum.The invention provides a kind of high-temperature behavior
Stable, the carbon/silicon carbide ceramic matrix composite combustion chamber flame drum with self-healing matrix of excellent in mechanical performance, is solved existing
There is flame tube structure design complicated, greatly, difficulty of processing is big, and heatproof is low and needs air cooling, and fuel gas buring is insufficient, and material is easy for weight
By technical problems such as exhaust gas corrosions.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means to combine specific features, structure, material or the spy that the embodiment or example are described
Point is contained at least one embodiment of the present invention or example.In this manual, to the schematic representation of above-mentioned term not
Identical embodiment or example must be directed to.Moreover, specific features, structure, material or the feature of description can be with office
Combined in an appropriate manner in one or more embodiments or example.In addition, in the case of not conflicting, the skill of this area
Art personnel can be tied the not be the same as Example or the feature of example and non-be the same as Example or example described in this specification
Close and combine.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changed, replacing and modification, and the essence of appropriate technical solution is departed from various embodiments of the present invention skill
The scope of art scheme, it all should cover among the claim of the present invention and the scope of specification.
Claims (10)
1. a kind of preparation method of composite combustion chamber flame drum, it is characterised in that comprise the following steps:
S1:Combustion chamber flame drum precast body is prepared into SiC interfaces with chemical vapour deposition technique;Wherein, the chemical vapor deposition
The reaction gas of method is trichloromethyl silane;
S2:Using the mixed solution of Polycarbosilane and dimethylbenzene as precursor solution, the product that the step S1 is obtained is using first
Body infiltration pyrolysis method is driven to be densified;Repeat the density to obtained silicon carbide substrate using the precursor infiltration and pyrolysis method
For 1.6~1.8g/cm3;
S3:SiC matrix layer and BCx base layers are prepared using chemical vapor infiltration area method on the surface of the silicon carbide substrate, obtained
Density is 2.0~2.5g/cm3Carbon borosilicate self-healing matrix;Wherein, the SiC is prepared by deposition gas of trichloromethyl silane
Base layer, the BCx base layers are prepared using boron chloride and methane as deposition gas;
S4:The carbon borosilicate self-healing matrix is subjected to 1~3h modifications at 1000 DEG C, composite combustion chamber fire is obtained
Flame cylinder.
2. the preparation method of composite combustion chamber flame drum according to claim 1, it is characterised in that:The step S1
In, the chemical vapour deposition technique is specially:Using trichloromethyl silane as reaction gas, hydrogen is carrier gas, and argon gas is carrier gas, is sunk
Accumulated temperature degree is 1100~1230 DEG C, and pressure is 1~5kPa, and sedimentation time is 5~15h;Wherein, the hydrogen and three chloromethane
The volume ratio of base silane is 1:8~1:12.
3. the preparation method of composite combustion chamber flame drum according to claim 1, it is characterised in that:The step S2
In, the precursor infiltration and pyrolysis method includes:Under vacuum, the obtained products of the step S1 are impregnated in Polycarbosilane
With 4~6h in the mixed solution of dimethylbenzene, then 100~140 DEG C of dryings;By the dried product in nitrogen or argon gas
3~6h is cracked in 800~1200 DEG C;The step of repeating the precursor infiltration and pyrolysis method, it is close to obtained silicon carbide substrate
Spend for 1.6~1.8g/cm3;Wherein, the mass fraction of Polycarbosilane is in the mixed solution of the Polycarbosilane and dimethylbenzene
20%~50%.
4. the preparation method of composite combustion chamber flame drum according to claim 1, it is characterised in that:The step S3
In, the preparation method of the SiC matrix layer is specially:Using trichloromethyl silane as deposition gas, hydrogen is carrier gas, and argon gas is dilution
Gas, depositing temperature is 800~1100 DEG C, and sedimentation time is 10~30h, and pressure is 1kPa;Wherein, the flow of the hydrogen is
100~400ml/min, the flow of the argon gas is 100~300ml/min;The preparation method of the BCx base layers is specially:
Using boron chloride and methane as deposition gas, hydrogen and argon gas are carrier gas, and depositing temperature is 900~1000 DEG C, and sedimentation time is 10
~30h, pressure is 1kPa;Wherein, the flow-rate ratio of the boron chloride and the methane is 2:1~6:1, the hydrogen and described
The flow velocity of argon gas is 50~80mL/min.
5. the preparation method of composite combustion chamber flame drum according to claim 1, it is characterised in that:The step S3
In, on the surface of the silicon carbide substrate, the SiC matrix layer and the BCx base layers are alternately prepared successively, obtaining density is
2.0~2.5g/cm3Carbon borosilicate self-healing matrix;Wherein, the outermost layer of the carbon borosilicate self-healing matrix is the SiC
Base layer.
6. the preparation method of composite combustion chamber flame drum according to claim 1, it is characterised in that:Described compound
The surface of material combustion room burner inner liner, prepares rare earth silicate Environmental Barrier Coatings on Si-based Ceramics;The original of the rare earth silicate Environmental Barrier Coatings on Si-based Ceramics
Material includes the first component and the second component, and first component is mullite, ytterbium silicate, polyvinyl butyral and phosphate, institute
The second component is stated for ethanol;Wherein:The mass ratio of first component and second component is 1:1~1:3, the polyethylene
Mass fraction of the butyral in first component is 4%~8%, the phosphate quality in first component point
Number is 0.4%~1.0%, and the mass ratio of the mullite and the ytterbium silicate is 88:12.
7. the preparation method of composite combustion chamber flame drum according to claim 6, it is characterised in that:The rare earth silicon
The preparation method of hydrochlorate Environmental Barrier Coatings on Si-based Ceramics includes:By first component and the second component 12~16h of ball milling mixing, will
The mixture brushing arrived on the surface of the composite combustion chamber flame drum, then at 1400 DEG C~1500 DEG C sintering 2~
5h。
8. the preparation method of composite combustion chamber flame drum according to claim 1, it is characterised in that:The combustion chamber
Burner inner liner precast body is to use silicon carbide fibre to be formed with three-dimensional four step braiding, wherein, braid angle is 20~45 °, the carbon
The volume fraction 30%~50% of SiClx fiber.
9. the composite combustion chamber flame drum that the method described in any one of claim 1~8 is prepared.
10. composite combustion chamber flame drum described in claim 9 is being prepared during engine especially prepares aero-engine
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CN108316977A (en) * | 2018-01-22 | 2018-07-24 | 北京航空航天大学 | Multi-component multi-layer self-healing ceramic matric composite engine turbine outer shroud |
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CN111704468A (en) * | 2020-06-19 | 2020-09-25 | 宜兴市新立织造有限公司 | Three-dimensional woven aviation flame tube and preparation method thereof |
CN112479717A (en) * | 2020-11-19 | 2021-03-12 | 航天特种材料及工艺技术研究所 | Self-healing matrix modified SiC/SiC composite material and preparation method thereof |
CN112341235A (en) * | 2020-11-24 | 2021-02-09 | 西北工业大学 | Multiphase coupling rapid densification method for ultrahigh-temperature self-healing ceramic matrix composite |
CN114057491A (en) * | 2021-11-19 | 2022-02-18 | 西北工业大学 | Preparation method of ceramic matrix composite material pulse detonation engine combustion chamber |
CN114057491B (en) * | 2021-11-19 | 2022-07-12 | 西北工业大学 | Preparation method of ceramic matrix composite material pulse detonation engine combustion chamber |
CN115160005A (en) * | 2022-06-22 | 2022-10-11 | 西安鑫垚陶瓷复合材料有限公司 | Preparation method of two-dimensional silicon carbide/silicon carbide composite material nut |
CN115385694A (en) * | 2022-10-26 | 2022-11-25 | 中南大学 | Phosphate/carbide composite material with interpenetrating network structure and preparation method thereof |
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