CN107540400A - A kind of SiC with compound interfacef/ SiC ceramic based composites - Google Patents
A kind of SiC with compound interfacef/ SiC ceramic based composites Download PDFInfo
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Abstract
A kind of SiC with compound interfacef/ SiC ceramic based composites, it is characterised in that be made up of CVD SiC coatings, PIP SiC matrixes, compound interface and SiC fibers, described CVD SiC coatings are coat of silicon carbide prepared by chemical vapour deposition technique, and thickness is 100 ~ 500 μm；Described compound interface is BN interfaces, ZrO2Interface, LaPO4Interface and wherein any two kinds, three kinds of alternate cycle superpositions at SiC interfaces, cycle period number is 3 ~ 5 times, and described PIP SiC matrixes are the carborundum formed using Polycarbosilane pyrolysis in situ；The volume ratio that described SiC fibers account for composite is 40 ~ 60%, it is to prepare MULTILAYER COMPOSITE interface on silicon carbide fibre surface using Different Preparation that, which there are 5 ~ 20nm thickness pyrolytic carbon layer preparation methods on surface, then using PIP methods filling SiC matrix, surface SiC coatings are finally prepared using CVD.The present invention prepares SiCf/ SiC ceramic based composites obdurability is high, oxidation resistance is strong, and preparation technology is simple.
Description
Technical field
It is more particularly to a kind of with compound interface the present invention relates to a kind of ceramic matric composite and preparation method thereof
SiC f / SiC ceramic based composites and preparation method thereof.
Background technology
SiC ceramic has a systems such as good high temperature resistant, low-density, Gao Biqiang, Gao Bimo, anti-oxidant and anti-erosion because of it
Row excellent properties, potentiality of the metal as high-temperature structural material of new generation are taken over so as to have.Further, since its excellent is partly led
Metastable dielectric properties under bulk properties and high temperature, SiC also have good application prospect in terms of microwave absorbing material.So
And because the fracture toughness of SiC pure metals is low, brittle fracture is shown as, limits its application.Gradual quilt at present
SiC f / SiC ceramic matrix composite material is substituted.Continuous SiC fiber toughness reinforcing Si ceramic matric composites（SiC f /SiC）Because of excellent high temperature power
Learn performance, inoxidizability, thermodynamic stability, corrosion resistance and aero engine turbine blades, combustion liner set and
Nuclear reactor etc. has broad application prospects.
Numerous studies show that the boundary layer between fiber and matrix is for SiC f The mechanical property of/SiC ceramic matrix composite material has weight
The influence wanted.Boundary layer can prevent fiber from being etched, and effectively transmit the load between fiber and matrix so that fiber plays
Carrying acts on.Suitable boundary layer can enable the toughening mechanisms such as crack deflection, interfacial detachment and spike protein gene play, and then
Improve the mechanical property of composite.
Pyrolytic carbon（PyC）And hexagonal boron nitride（Hexagonal-BN）It is two kinds of most common improvement SiC f //SiC is compound
The layered interface layer of material mechanical performance.However, because PyC can be aoxidized more than 400 DEG C so that SiC f //SiC is compound
The mechanical property of material at high temperature is remarkably decreased, so as to limit SiC f The high temperature application of //SiC ceramic matrix composite material.H-BN has
With pyrolytic carbon（PyC）Similar layered crystal structure, in addition compared with pyrolytic carbon, it also has preferable antioxygenic property（800
℃）, the liquid B that is formed after oxidation2O3Crackle can be made up, be preferable interface phase candidate material, turn into Jiao of research this year
Point.
Another improves SiC f The method of/SiC ceramic matrix composite material high-temperature oxidation resistant is that introducing one is laminated in the composite
For suitable oxide as interface phase, these compounds have various stress induced processes（Such as interface shearing, twin, phase transformation）,
Fiber-matrix bonding, and the antioxygenic property having had can be weakened.The material of one of which possible application is ZrO2, coating
When reaching ideal structure, SiC f / SiC ceramic matrix composite material spike protein gene is obvious, shows and SiC f / BN/SiC composites are suitable
Or more preferable antioxygenic property and destruction life-span.Y2O3Stable t-ZrO2It can occur under the induction of matrix cracking growth stress
t-ZrO2To m-ZrO2Phase transformation, and become big with volume, so improve the fracture toughness of composite, and had
Antioxygenic property.
Document " BN coatings prepared by Low pressure chemical vapor deposition
Using boron trichloride-ammonia-hydrogen-argon mixture gases, Yu Cheng,
Surface and Coating Technology " are at 1000 DEG C and BCl3-NH3-H2Under-Ar system conditions, using low pressure
Learn vapour deposition process（LPCVD）BN coatings are deposited in graphite matrix, prepared coating is the t-BN of turbine layer structure,
It is changed into the good h-BN of crystal property more than 1300 DEG C.
Document " SiC f //SiC ceramic matrix composite material interface modification coating is studied, Liu Baolin, the National University of Defense technology " use chemical gas
Phase sedimentation prepares different-thickness BN interfaces in SiC fiber surfaces, have studied BN interface coating thickness to SiC f //SiC composite woods
Material mechanical property and influences, with BN coating layer thicknesses increase, SiC f The bending strength of //SiC ceramic matrix composite material, modulus of elasticity and disconnected
Split the trend that toughness is in first increases and then decreases.
Document " Microstructural features of the ZrO2 interfacial coatings on SiC
Fibers before and after exposition to air at high temperatures, N.I.
Baklanova, Journal of the European Ceramic Society ", which have studied, is deposited on SiC fiber surfaces
ZrO2Interface coating exposes the microstructure features before and after high temperature air to the open air, although ZrO2There is strong between SiC fibers
Si-O-Zr bondings, but fibre strength is not damaged substantially, the strong I/F interfaces of formation are advantageous to composite de-
The damage of external oxidation atmosphere is protected the fibers from during viscous.
Although BN interfaces, ZrO2Interface can improve the antioxygenic property of composite, but simple BN interfaces to a certain degree
Temperature in use or relatively low, simple ZrO2Interfacial phase change toughness reinforcing is limited, can not play a part of deflecting crackle.Therefore, in order to enter
One step improves the oxidation resistance of composite, and the multi-component multi-layer interface that micro-structural is mutually derived from layered crystal structure interface is set
Meter, multi-component multi-layer interface are mainly (X-Y)nMore bed boundary phases of type, wherein X are mainly crack deflection material, and Y is that one kind can
Oxidation resistant material, this interface can realize crack deflection and oxidation resistant function simultaneously.
The content of the invention
The technical problem to be solved in the present invention is overcome the deficiencies in the prior art, it is desirable to provide a kind of with compound interface
SiC f / SiC ceramic based composites, it is made up of CVD-SiC coatings, PIP-SiC matrixes, compound interface and SiC fibers, it is described
CVD-SiC coatings be chemical vapour deposition technique prepare coat of silicon carbide, thickness be 100 ~ 500 μm；Described compound interface
For BN interfaces, ZrO2Interface, LaPO4Interface and wherein any two kinds, three kinds of alternate cycle superpositions at SiC interfaces, cycle period
Number is 3 ~ 5 times, and individual layer BN interfacial thicknesses are 80 ~ 200nm, individual layer ZrO2Interfacial thickness is 50 ~ 200nm, individual layer LaPO4Interface
Thickness is 20 ~ 200nm, and individual layer SiC interfacial thicknesses are 50 ~ 100nm；Described PIP-SiC matrixes are in situ using Polycarbosilane
It is pyrolyzed the carborundum formed；The volume ratio that described SiC fibers account for composite is 40 ~ 60%, and there are 5 ~ 20nm thickness pyrolytic carbons on surface
Layer.
In addition, the present invention also provides a kind of SiC with compound interface f Its preparation of/SiC ceramic based composites
Method, it is characterised in that including following sequential steps：
（1）Silicon carbide fibre is woven into fiber preform, 1 ~ 2h is heat-treated in 700 ~ 900 DEG C of argon atmospheres；
（2）Using propylene as carbon source, argon gas is protective gas, 900 ~ 1000 DEG C, 3 ~ 5h of sedimentation time of depositing temperature, using chemical gas
Phase sedimentation prepares pyrocarbon coating in fiber surface；
（3）BN interfaces, boric acid and boron source and nitrogen source that urea is dip-coating method, sodium tetraborate are prepared using dip-coating method
For additive, boric acid and urea are pressed into mass fraction 1:2 ~ 3 proportioning dissolvings in ethanol, are made into boric acid-urea ethanol solution, so
The sodium tetraborate of mass fraction 3 ~ 9% is added afterwards, sodium tetraborate-boric acid-urea ethanol solution is obtained, using sodium tetraborate-boron
Acid-urea ethanol solution impregnating by pressure silicon carbide fibre precast body part, after 100 ~ 120 DEG C of drying, it is put into tube furnace in nitrogen
900 ~ 1100 DEG C are warming up to 1 ~ 3 DEG C/min under atmosphere, is incubated 3 ~ 5h；
（4）SiC interfaces are prepared using chemical vapor infiltration, reaction temperature is warming up under vacuum atmosphere, is passed through certain trichlorine
Methyl-monosilane, hydrogen are 1000 ~ 1200 DEG C as diluent gas, reaction temperature as carrier gas, argon gas, and silicochloroform flow is
30 ~ 50sccm, hydrogen flowing quantity are 200 ~ 300sccm, and argon flow amount is 200 ~ 300sccm, and infiltration sedimentation time is 3 ~ 6h；
（5）ZrO is prepared using sol-gel process2Interface, six water yttrium nitrates and eight water basic zirconium chlorides press 1:30 ~ 32 mol ratios are molten
In deionized water, ammoniacal liquor regulation PH to 12 is instilled, generates white oxide zirconium gel, deionized water cleaning zirconium oxide gel removes
Foreign ion, then instills dust technology regulation PH to 2, and white oxide zirconium gel switchs to white oxide zirconium colloidal sol, stirred at 80 DEG C
12 ~ 24h, white oxide zirconium colloidal sol are changed into transparent zirconium oxide colloidal sol, using zirconia sol impregnation carbonization silica fibre precast body,
It is put into after 80 ~ 100 DEG C of dryings in tube furnace, argon gas atmosphere constant-pressure and high-temperature sintering, 1000 ~ 1200 DEG C of sintering temperature, soaking time 1
~2h；
（6）LaPO is prepared using electrophoretic deposition4Interface, according to magnesium chloride hexahydrate：LaPO4Powder quality ratio is 1：（10~20）
After mixing, it is added in absolute ethyl alcohol and is made into suspension, LaPO4Concentration is 2 ~ 10g/L, is negative using silicon carbide fibre precast body
Pole, using graphite electrode as positive electrode, 10 ~ 25mA/cm of current density2, insert ultrasonic vibration rod, sedimentation time be 5 ~
10min, then 12 ~ 24h of drying at room temperature, then be warming up to 700 ~ 900 DEG C with 1 ~ 3 DEG C/min, is incubated 1 ~ 2h；
（7）Repeat step（3）、（4）、（5）、（6）Any two of which step 3 ~ 5 time；
（8）Then SiC matrix, using Polycarbosilane-xylene solution as precursor, impregnating by pressure are prepared using infiltration pyrolysis method
Afterwards, 150 ~ 200 DEG C of solidifications, then be warming up to 1100 ~ 1200 DEG C with 0.5 ~ 2 DEG C/min, are incubated 2 ~ 3h, and repeated impregnations cracking technology 9 ~
12 times, until material rate of body weight gain is less than 2%；
（7）SiC coatings are prepared using chemical vapour deposition technique, using trichloromethyl silane as carborundum source of the gas, hydrogen as carrier gas,
Argon gas is 1000 ~ 1200 DEG C as diluent gas, reaction temperature, and silicochloroform flow is 60 ~ 100sccm, and hydrogen flowing quantity is
600 ~ 1000sccm, argon flow amount are 600 ~ 1000sccm, and infiltration sedimentation time is 20 ~ 30h；
（8）Finally give the SiC with compound interface f / SiC ceramic based composites.
Beneficial effect of the present invention：1st, composite laminate periodicity interfacial structure temperature in use is higher, and toughening effect is more preferable；2nd, make
Standby technical process is simple；3rd, surface C VI-SiC coatings protection composite material base, the anti-oxidant energy of composite is further improved
Power.
Embodiment
With reference to specific embodiment, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention, after the present invention has been read, various equivalences of the those skilled in the art to the present invention
The modification of form falls within the application appended claims and limited.
Embodiment 1
With (BN/SiC)nThe SiC of compound interface f / SiC ceramic based composites
（1）Silicon carbide fibre is woven into fiber preform, 1h is heat-treated in 900 DEG C of argon atmospheres；
（2）Using propylene as carbon source, argon gas is protective gas, 900 DEG C of depositing temperature, sedimentation time 3h, using chemical vapor deposition
Method prepares pyrocarbon coating in fiber surface；
（3）BN interfaces, boric acid and boron source and nitrogen source that urea is dip-coating method, sodium tetraborate are prepared using dip-coating method
For additive, boric acid and urea are pressed into mass fraction 1:2 proportioning dissolvings in ethanol, are made into boric acid-urea ethanol solution, then
The sodium tetraborate of mass fraction 3% is added, sodium tetraborate-boric acid-urea ethanol solution is obtained, using sodium tetraborate-boric acid-urine
Plain ethanol solution impregnating by pressure silicon carbide fibre precast body part, after 120 DEG C of drying, it is put into tube furnace in a nitrogen atmosphere with 3
DEG C/min is warming up to 1100 DEG C, it is incubated 3 ~ 5h；
（4）SiC interfaces are prepared using chemical vapor infiltration, reaction temperature is warming up under vacuum atmosphere, is passed through certain trichlorine
Methyl-monosilane, hydrogen are 1100 DEG C as diluent gas, reaction temperature as carrier gas, argon gas, and silicochloroform flow is
30sccm, hydrogen flowing quantity 300sccm, argon flow amount 300sccm, infiltration sedimentation time are 5h；
（5）Repeat step（3）、（4）Two steps 5 time；
（6）Then SiC matrix, using Polycarbosilane-xylene solution as precursor, impregnating by pressure are prepared using infiltration pyrolysis method
Afterwards, 150 DEG C of solidifications, then 1200 DEG C are warming up to 2 DEG C/min, 2h, repeated impregnations cracking technology 11 times are incubated, until material increases weight
Rate is less than 2%；
（7）SiC coatings are prepared using chemical vapour deposition technique, using trichloromethyl silane as carborundum source of the gas, hydrogen as carrier gas,
For argon gas as diluent gas, reaction temperature is 1150 DEG C, and silicochloroform flow is 60sccm, hydrogen flowing quantity 600sccm, argon
Throughput is 600sccm, and infiltration sedimentation time is 20h；
（8）Finally giving has (BN/SiC)nThe SiC of compound interface f / SiC ceramic based composites.
Embodiment 2
With (ZrO2/SiC)nThe SiC of compound interface f / SiC ceramic based composites
（1）Silicon carbide fibre is woven into fiber preform, 1h is heat-treated in 900 DEG C of argon atmospheres；
（2）Using propylene as carbon source, argon gas is protective gas, 900 DEG C of depositing temperature, sedimentation time 3h, using chemical vapor deposition
Method prepares pyrocarbon coating in fiber surface；
（3）ZrO is prepared using sol-gel process2Interface, six water yttrium nitrates and eight water basic zirconium chlorides press 1:32 mol ratios are dissolved in
In ionized water, ammoniacal liquor regulation PH to 12 is instilled, generates white oxide zirconium gel, deionized water cleaning zirconium oxide gel removes impurity
Ion, dust technology regulation PH to 2 then being instilled, white oxide zirconium gel switchs to white oxide zirconium colloidal sol, 24h is stirred at 80 DEG C,
White oxide zirconium colloidal sol is changed into transparent zirconium oxide colloidal sol, and using zirconia sol impregnation carbonization silica fibre precast body, 100 DEG C dry
It is put into after dry in tube furnace, argon gas atmosphere constant-pressure and high-temperature sintering, 1200 DEG C of sintering temperature, soaking time 1h；
（4）SiC interfaces are prepared using chemical vapor infiltration, reaction temperature is warming up under vacuum atmosphere, is passed through certain trichlorine
Methyl-monosilane, hydrogen are 1100 DEG C as diluent gas, reaction temperature as carrier gas, argon gas, and silicochloroform flow is
30sccm, hydrogen flowing quantity 300sccm, argon flow amount 300sccm, infiltration sedimentation time are 5h；
（5）Repeat step（3）、（4）Two step 3 ~ 5 time；
（6）Then SiC matrix, using Polycarbosilane-xylene solution as precursor, impregnating by pressure are prepared using infiltration pyrolysis method
Afterwards, 150 DEG C of solidifications, then 1200 DEG C are warming up to 2 DEG C/min, 2h, repeated impregnations cracking technology 11 times are incubated, until material increases weight
Rate is less than 2%；
（7）SiC coatings are prepared using chemical vapour deposition technique, using trichloromethyl silane as carborundum source of the gas, hydrogen as carrier gas,
For argon gas as diluent gas, reaction temperature is 1150 DEG C, and silicochloroform flow is 60sccm, hydrogen flowing quantity 600sccm, argon
Throughput is 600sccm, and infiltration sedimentation time is 20h；
（8）Finally giving has (BN/SiC)nThe SiC of compound interface f / SiC ceramic based composites.
Two embodiments of the present invention are above are only, but the design concept of the present invention is not limited thereto, all profits
The change of unsubstantiality is carried out to the present invention with this design, the behavior for invading the scope of protection of the invention all should be belonged to.In every case it is
Any type of letter made without departing from the content of technical solution of the present invention, the technical spirit according to the present invention to above example
Single modification, equivalent variations and remodeling, still fall within the protection domain of technical solution of the present invention.
Claims (2)
- A kind of 1. SiC with compound interface f / SiC ceramic based composites, by CVD-SiC coatings, PIP-SiC matrixes, compound Interface and SiC fibers composition, described CVD-SiC coatings are coat of silicon carbide prepared by chemical vapour deposition technique, and thickness is 100~500μm；Described compound interface is BN interfaces, ZrO2Interface, LaPO4Wherein any two kinds of interface and SiC interfaces, Three kinds of alternate cycle superpositions, cycle period number is 3 ~ 5 times, and individual layer BN interfacial thicknesses are 80 ~ 200nm, individual layer ZrO2Interface is thick Spend for 50 ~ 200nm, individual layer LaPO4Interfacial thickness is 20 ~ 200nm, and individual layer SiC interfacial thicknesses are 50 ~ 100nm；Described PIP- SiC matrix is the carborundum formed using Polycarbosilane pyrolysis in situ；The volume ratio that described SiC fibers account for composite is 40 ~ 60%, there are 5 ~ 20nm thickness pyrolytic carbon layers on surface.
- A kind of 2. SiC with compound interface f Its preparation method of/SiC ceramic based composites, it is characterised in that including following The step of order：（1）Silicon carbide fibre is woven into fiber preform, 1 ~ 2h is heat-treated in 700 ~ 900 DEG C of argon atmospheres；（2）Using propylene as carbon source, argon gas is protective gas, 900 ~ 1000 DEG C, 1 ~ 5h of sedimentation time of depositing temperature, using chemical gas Phase sedimentation prepares pyrocarbon coating in fiber surface；（3）BN interfaces, boric acid and boron source and nitrogen source that urea is dip-coating method, sodium tetraborate are prepared using dip-coating method For additive, boric acid and urea are pressed into mass fraction 1:2 ~ 3 proportioning dissolvings in ethanol, are made into boric acid-urea ethanol solution, so The sodium tetraborate of mass fraction 3 ~ 9% is added afterwards, sodium tetraborate-boric acid-urea ethanol solution is obtained, using sodium tetraborate-boron Acid-urea ethanol solution impregnating by pressure silicon carbide fibre precast body part, after 100 ~ 120 DEG C of drying, it is put into tube furnace in nitrogen 900 ~ 1100 DEG C are warming up to 1 ~ 3 DEG C/min under atmosphere, is incubated 3 ~ 5h；（4）SiC interfaces are prepared using chemical vapor infiltration, reaction temperature is warming up under vacuum atmosphere, is passed through certain trichlorine Methyl-monosilane, hydrogen are 1000 ~ 1200 DEG C as diluent gas, reaction temperature as carrier gas, argon gas, and silicochloroform flow is 30 ~ 50sccm, hydrogen flowing quantity are 200 ~ 300sccm, and argon flow amount is 200 ~ 300sccm, and infiltration sedimentation time is 3 ~ 6h；（5）ZrO is prepared using sol-gel process2Interface, six water yttrium nitrates and eight water basic zirconium chlorides press 1:30 ~ 32 mol ratios are dissolved in In deionized water, ammoniacal liquor regulation PH to 12 is instilled, generates white oxide zirconium gel, deionized water cleaning zirconium oxide gel removes impurity elimination Matter ion, dust technology regulation PH to 2 then being instilled, white oxide zirconium gel switchs to white oxide zirconium colloidal sol, stirring 12 at 80 DEG C ~ 24h, white oxide zirconium colloidal sol are changed into transparent zirconium oxide colloidal sol, using zirconia sol impregnation carbonization silica fibre precast body, 80 ~ It is put into after 100 DEG C of dryings in tube furnace, argon gas atmosphere constant-pressure and high-temperature sintering, 1000 ~ 1200 DEG C of sintering temperature, soaking time 1 ~ 2h；（6）LaPO is prepared using electrophoretic deposition4Interface, according to magnesium chloride hexahydrate：LaPO4Powder quality ratio is 1：（10~20）It is mixed After conjunction, it is added in absolute ethyl alcohol and is made into suspension, LaPO4Concentration is 2 ~ 10g/L, using silicon carbide fibre precast body as negative pole, Using graphite electrode as positive electrode, 10 ~ 25mA/cm of current density2, ultrasonic vibration rod is inserted, sedimentation time is 5 ~ 10min, Then 12 ~ 24h of drying at room temperature, then 700 ~ 900 DEG C are warming up to 1 ~ 3 DEG C/min, it is incubated 1 ~ 2h；（7）Repeat step（3）、（4）、（5）、（6）Any two of which step 3 ~ 5 time；（8）Then SiC matrix, using Polycarbosilane-xylene solution as precursor, impregnating by pressure are prepared using infiltration pyrolysis method Afterwards, 150 ~ 200 DEG C of solidifications, then be warming up to 1100 ~ 1200 DEG C with 0.5 ~ 2 DEG C/min, are incubated 2 ~ 3h, and repeated impregnations cracking technology 9 ~ 12 times, until material rate of body weight gain is less than 2%；（7）SiC coatings are prepared using chemical vapour deposition technique, using trichloromethyl silane as carborundum source of the gas, hydrogen as carrier gas, Argon gas is 1000 ~ 1200 DEG C as diluent gas, reaction temperature, and silicochloroform flow is 60 ~ 100sccm, and hydrogen flowing quantity is 600 ~ 1000sccm, argon flow amount are 600 ~ 1000sccm, and infiltration sedimentation time is 20 ~ 30h；（8）Finally give the SiC with compound interface f / SiC ceramic based composites.
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2017
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