CN106083117A - There is fiber reinforced ceramic matric composite of ternary layered MAX phase boundary surface layer and preparation method thereof - Google Patents
There is fiber reinforced ceramic matric composite of ternary layered MAX phase boundary surface layer and preparation method thereof Download PDFInfo
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Abstract
The present invention proposes a kind of fiber reinforced ceramic matric composite with ternary layered MAX phase boundary surface layer.By the ternary layered MAX phase material of introducing as boundary layer, can effectively promote the radiation-resistant property of ceramic matric composite, heat conductivility and antioxygenic property;It addition, the multiple tensile energy absorption mechanism that MAX phase material has can effectively absorb energy to failure, hinder crackle in the extension within ceramic matric composite, improve toughness and the damage tolerance of ceramic matric composite;Therefore, effectively expanded the application of this composite, such as, had a good application prospect in fields such as Aero-Space thermal structure material, nuclear energy structural materials.
Description
Technical field
The invention belongs to fiber reinforced technology field of ceramic matrix composite material, be specifically related to one and there is ternary layered MAX
Fiber reinforced ceramic matric composite of phase boundary surface layer and preparation method thereof.
Background technology
Fiber reinforced ceramic matric composite has high intensity, high temperature resistant, low-density, the good characteristic such as corrosion-resistant, in boat
The empty field such as spacecraft heat structural material, nuclear energy structural material has important application.In fiber reinforced ceramic matric composite, pottery
Boundary layer between porcelain basal body and fiber is its important component part, to the mechanical property of composite, antioxygenic property, heat conduction
Performance, radiation-resistant property etc. all have material impact.
Traditional composite material interface layer mainly includes pyrolytic carbon (Pyrolytic Carbon, PyC), hexagonal boron nitride
And (PyC/SiC) (Hexagonal-BN)n, (BN/SiC)nMany interfacial layer.PyC i.e. starts oxidation more than 400 DEG C, and BN exists
Start oxidation for more than 850 DEG C, cause composite performance degradation at high temperature, it is difficult to competent such as Aero-Space etc. are tight
Severe Service Environment.The composite application in fields such as nuclear energy need to face radiation environment, and PyC issues in neutron irradiation effect
The transformation of raw contraction-swelling-partial amorphism, the B element in BN boundary layer under neutron irradiation then can quickly transmuting and lost efficacy.
Additionally, self thermal conductivity of traditional interface layer is relatively low, the serious overall thermal conductivity reducing composite.Therefore, traditional interface
Layer has been increasingly difficult to meet ceramic matric composite application demand in every respect.
With Ti3SiC2, Ti3AlC2For represent ternary layered MAX phase ceramics have concurrently metal and pottery characteristic, MAX phase from
Metal material inherits excellent electric conductivity and heat conductivity, good thermal shock resistance and damage tolerance, relatively low hardness and relatively
Good machining property;The highest elastic modelling quantity and elevated temperature strength, and outstanding non-oxidizability is inherited from ceramic material
With corrosion resistance etc..Micro analysis shows that the layer structure of MAX phase ceramics uniqueness and density of electronic states distribution cause multiple
Tensile energy absorption mechanism, such as crack deflection, laminated tearing, intercrystalline sliding, intra-die dislocation deformation, flake crystalline gauffer etc..
Additionally, MAX phase ceramics also shows good radiation-resistant property, in fields such as nuclear energy, there is important application potential.
Summary of the invention
The present invention provides a kind of ceramic matric composite, with ceramic material as matrix, is toughness reinforcing phase with fiber, described matrix
Ternary layered MAX phase material is comprised with the boundary layer between toughness reinforcing phase.
That is, present invention introduces ternary layered MAX phase material as ceramic matric composite interlayer materials, pottery can be promoted
The radiation-resistant property of porcelain based composites, heat conductivility and antioxygenic property;It addition, MAX phase material had crack deflection,
The multiple tensile energy absorption mechanism such as laminated tearing, intercrystalline sliding, intra-die dislocation deformation, flake crystalline gauffer can be effectively
Absorb energy to failure, hinder crackle in the extension within ceramic matric composite, improve toughness and the damage of ceramic matric composite
Tolerance limit.
Described ceramic material does not limits, including carborundum, titanium carbide, zirconium carbide, silicon nitride, aluminium oxide, mullite, zirconium oxide
A kind of material in Deng or two or more mixture.
Described fiber does not limits, and can choose carbon fiber, silicon carbide fibre, alumina fibre, quartz fibre, not as required
Come in mineral wool etc. one or several.
Described MAX phase configuration does not limits, the configuration such as including 211,312,413,514,615,716.
Described MAX phase material does not limits, including Ti3SiC2、Ti3AlC2、Ti2AlC、V3AlC2、V2AlC、Cr2AlC、Ti3SnC2
One or more kinds of mixture in Deng.
The monolayer boundary layer that described boundary layer can be constituted with congener ternary layered MAX phase, it is also possible to be by the most of the same race
The multiple structure boundary layer of the ternary layered MAX phase composition of class.
It addition, described boundary layer can be the multiple structure boundary layer of doping phase layer and MAX phase layer alternately composition, described in mix
Dephasign layer includes PyC, BN, SiC etc., thus constitutes (PyC/MAX)n, (BN/MAX)n, (SiC/MAX)nAt multiple structure interface
Layer.
Described ceramic matric composite, the bending that can control ceramic matric composite by controlling interfacial layer thickness is strong
The performances such as degree, fracture toughness, thermal conductivity.As preferably, described interfacial layer thickness is 50nm-2 μm, more preferably 100nm-
1μm。
As preferably, described fiber volume fraction in the composite is 5%-80%, more preferably 30%-60%.
Present invention also offers and a kind of prepare the above-mentioned ceramic matric composite with continuous ternary layered MAX phase boundary surface layer
Method, comprise the steps:
(1) prepared by fiber preform
Utilize fiber winding machine by the prefabricated-member mould of fiber uniform winding to fiber winding machine, obtain fibre preforms
Body.Or, fibrage is become fiber cloth, prepares boundary layer on fiber cloth surface, then fiber cloth is sewed up as fibre preforms
Body.
(2) prepared by boundary layer
Boundary layer is prepared in fibre preforms surface.
The preparation method of described boundary layer does not limits, and can pass through chemical gaseous phase deposition, physical vapour deposition (PVD), polymer pyrolysis
Prepared by the method such as method, molten-salt growth method.
(3) prepared by ceramic matrix
Matrix is prepared at interface layer surfaces.
The preparation method of described matrix does not limits, can pass through chemical vapor infiltration, precursor pyrolysis and hot pressing, melt infiltration method,
Prepared by the methods such as sol-gal process, nm immersion instantaneous eutectic phase method.
In described step (1), the weaving manner of fiber can choose 2D braiding, 2.5D braiding or 3D braiding as required
Deng.
In described step (1), in fiber preform, shared by fiber, volume fraction is controlled, preferably 5%-80%, further
It is preferably 30%-60%.
In described step (2), PyC or SiC can be deposited in fiber surface chemical gaseous phase in advance, pass through PyC the most again
Or SiC generates required MAX phase coating with element-specific reaction in-situ.
Described step (2) may be repeated several times, and coordinates traditional interface layer preparation method, obtains different (MAX/MAX)n,
(PyC/MAX)n, (SiC/MAX)n, (BN/MAX)nDeng multiple structure boundary layer.
Present invention also offers another kind and prepare the above-mentioned ceramic base composite wood with continuous ternary layered MAX phase boundary surface layer
The method of material, comprises the steps:
Fibrage is become fiber cloth, prepares boundary layer on fiber cloth surface, then fiber cloth is sewed up as fibre preforms
Body, finally prepares ceramic matrix in fibre preforms surface.
In described fiber preform, shared by fiber, volume fraction is controlled, preferably 5%-80%, more preferably
30%-60%.
Can be in advance at fiber cloth surface chemistry vapour deposition PyC or SiC, the most again by PyC or SiC and specific unit
Element reaction in-situ generates required MAX phase coating.
When boundary layer is prepared on fiber cloth surface, traditional interface layer preparation method can be coordinated, obtain different (MAX/
MAX)n, (PyC/MAX)n, (SiC/MAX)n, (BN/MAX)nDeng multiple structure boundary layer.
In sum, the present invention introduces ternary layered MAX phase ceramics as boundary in fiber reinforced ceramic matric composite
Surface layer, is effectively increased the antioxygenic property of this composite, radiation-resistant property and heat conductivility;Meanwhile, MAX phase is had
The multiple tensile energy absorption mechanism such as crack deflection, laminated tearing, intercrystalline sliding, intra-die dislocation deformation, flake crystalline gauffer
Effectively hinder crackle in the extension within ceramic matric composite, the toughness of lifting composite;Therefore, it is effectively improved this
Composite is in the application prospect in the fields such as Aero-Space thermal structure material, nuclear energy structural material.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, it should be pointed out that embodiment described below purport
It is being easy to the understanding of the present invention, and it is not being played any restriction effect.
Embodiment 1:
In the present embodiment, ceramic matric composite, with silicon carbide ceramics as matrix, is toughness reinforcing phase with carbon fiber, described matrix
It is ternary layered MAX phase material Ti with the boundary layer between toughness reinforcing phase3SiC2。
The preparation process of this ceramic matric composite is as follows:
(1) the T300 carbon fiber of 1K being woven into 3D prefabricated carbon fiber body, carbon fibrous body fraction is 45%.
(2) use chemical vapour deposition technique in prefabricated carbon fiber surface depositing Ti3SiC2Boundary layer, sedimentary condition is: with
Silicon chloride. is silicon source, and with titanium tetrachloride for titanium source, with carbon tetrachloride as carbon source, with hydrogen as carrier gas, depositing temperature is 1300
℃。
(3) using chemical vapor infiltration to deposit SiC ceramic matrix at interface layer surfaces, sedimentary condition is: trichloromethyl
Silane is source material, and argon is diluent gas, and hydrogen is carrier gas, and depositing temperature is 1000 DEG C-1100 DEG C.
(4) use chemical vapour deposition technique at C/SiC composite material surface deposition SiC protective layer produced above.
Embodiment 2:
In the present embodiment, ceramic matric composite, with silicon carbide ceramics as matrix, is toughness reinforcing phase with carbon fiber, described matrix
It is Ti with the boundary layer between toughness reinforcing phase3SiC2The many bed boundarys of/PyC.
The preparation process of this ceramic matric composite is as follows:
(1) the T300 carbon fiber of 1K being woven into 3D fiber preform, fiber volume fraction is 45%.
(2) using chemical vapour deposition technique to deposit PyC boundary layer in prefabricated carbon fiber surface, sedimentary condition is: with third
Alkene is source material, and argon is diluent gas, and depositing temperature is 900-1000 DEG C.Then, chemical vapor deposition is used
Ti3SiC2Boundary layer, sedimentary condition is: with Silicon chloride. for silicon source, with titanium tetrachloride for titanium source, with carbon tetrachloride as carbon source, with
Hydrogen is carrier gas, and depositing temperature is 1300 DEG C, obtains Ti3SiC2The many bed boundarys of/PyC.
(3) use chemical vapor infiltration at Ti3SiC2/ PyC multilamellar interface layer surfaces deposition SiC matrix, sedimentary condition
For: trichloromethyl silane is source material, and argon is diluent gas, and hydrogen is carrier gas, and depositing temperature is 1000 DEG C-1100 DEG C.
(4) use chemical vapour deposition technique at C/SiC composite material surface deposition SiC protective layer produced above.
Embodiment 3:
In the present embodiment, ceramic matric composite, with silicon carbide ceramics as matrix, is toughness reinforcing phase with silicon carbide fibre, described
Boundary layer between matrix with toughness reinforcing phase is ternary layered MAX phase material Ti3SiC2。
The preparation process of this ceramic matric composite is as follows:
(1) the Tyranno SA-3 silicon carbide fibre of 1K is woven into 3D silicon carbide fibre precast body, silicon carbide fibre body
Fraction is 45%.
(2) use chemical vapour deposition technique in silicon carbide fibre precast body surface depositing Ti3SiC2Boundary layer, sedimentary condition
For: with Silicon chloride. for silicon source, with titanium tetrachloride for titanium source, with carbon tetrachloride as carbon source, with hydrogen as carrier gas, depositing temperature is
1300℃。
(3) using chemical vapor infiltration to deposit SiC matrix at interface layer surfaces, sedimentary condition is: trichloromethyl silane
For source material, argon is diluent gas, and hydrogen is carrier gas, and depositing temperature is 1000 DEG C-1100 DEG C.
(4) use chemical vapour deposition technique at SiC/SiC composite material surface deposition SiC protective layer produced above.
Embodiment 4:
In the present embodiment, ceramic matric composite, with silicon carbide ceramics as matrix, is toughness reinforcing phase with silicon carbide fibre, described
Boundary layer between matrix with toughness reinforcing phase is ternary layered MAX phase material Ti2AlC。
The preparation process of this ceramic matric composite is as follows:
(1) the Tyranno SA-3 silicon carbide fibre of 1K is woven into two dimension plain weave silicon carbide fibre cloth.
(2) physical vaporous deposition is used to prepare Ti at silicon carbide fibre cloth positive and negative2AlC boundary layer, technological parameter is:
Use reaction cathodic arc deposition, with TiAl alloy target for titanium source and aluminum source, with CH4For carbon source, depositing temperature is 1300 DEG C, heavy
Long-pending time 1h.
(3) silicon carbide fibre cloth step (2) obtained is sewed up as 2D fiber preform.
(4) using chemical vapor infiltration deposition SiC matrix, sedimentary condition is: trichloromethyl silane is source material, argon
For diluent gas, hydrogen is carrier gas, and depositing temperature is 1000 DEG C-1100 DEG C.
(5) chemical vapour deposition technique is used to deposit SiC protective layer at above SiC/SiC composite material surface.
Technical scheme has been described in detail by embodiment described above, it should be understood that the above is only
For the specific embodiment of the present invention, be not limited to the present invention, all made in the spirit of the present invention any amendment,
Supplement or similar fashion replacement etc., should be included within the scope of the present invention.
Claims (10)
1. there is the fiber reinforced ceramic matric composite of ternary layered MAX phase boundary surface layer, it is characterised in that: with ceramic material be
Matrix, is toughness reinforcing phase with fiber, and the boundary layer between described matrix with toughness reinforcing phase comprises ternary layered MAX phase material.
The fiber reinforced ceramic matric composite with ternary layered MAX phase boundary surface layer the most according to claim 1, it is special
Levy and be: described fiber include the one in carbon fiber, silicon carbide fibre, alumina fibre, quartz fibre, mullite fiber or
Person is several.
The fiber reinforced ceramic matric composite with ternary layered MAX phase boundary surface layer the most according to claim 1, it is special
Levy and be: described ceramic material includes in carborundum, titanium carbide, zirconium carbide, silicon nitride, aluminium oxide, mullite, zirconium oxide
Kind or two or more mixture.
The fiber reinforced ceramic matric composite with ternary layered MAX phase boundary surface layer the most according to claim 1, it is special
Levy and be: described MAX phase includes 211,312,413,514,615,716 configurations;
As preferably, described MAX phase material includes Ti3SiC2、Ti3AlC2、Ti2AlC、V3AlC2、V2AlC、Cr2AlC、Ti3SnC2
In one or more kinds of mixture;
As preferably, described boundary layer is the monolayer boundary layer that congener ternary layered MAX phase is constituted, or by the most of the same race
The ternary layered MAX of class alternate composition multiple structure boundary layer;
As preferably, described boundary layer is the multiple structure boundary layer that doping phase layer is alternately constituted with MAX phase layer, described doping phase
Layer includes one or several in PyC, BN, SiC.
The fiber reinforced ceramic matric composite with ternary layered MAX phase boundary surface layer the most according to claim 1, it is special
Levy and be: control the bending strength of ceramic matric composite, fracture toughness, thermal conductivity by controlling interfacial layer thickness.
The fiber reinforced ceramic matric composite with ternary layered MAX phase boundary surface layer the most according to claim 1, it is special
Levy and be: described interfacial layer thickness is 50nm-2 μm, preferably 100nm-1 μm.
7. according to the fiber reinforced pottery with ternary layered MAX phase boundary surface layer described in any claim in claim 1 to 6
The preparation method of porcelain based composites, it is characterised in that: comprise the steps:
(1) utilize fiber winding machine by the prefabricated-member mould of fiber uniform winding to fiber winding machine, obtain fiber preform;
(2) boundary layer is prepared in fibre preforms surface;
(3) matrix is prepared at interface layer surfaces.
The system of the fiber reinforced ceramic matric composite with ternary layered MAX phase boundary surface layer the most according to claim 7
Preparation Method, it is characterised in that: prepare institute by chemical gaseous phase deposition, physical vapour deposition (PVD), precursor pyrolysis and hot pressing, or molten-salt growth method
State boundary layer;
By chemical vapor infiltration, precursor pyrolysis and hot pressing, melt infiltration method, sol-gal process, or the instantaneous eutectic of nm immersion
Phase method prepares described matrix;
In described step (1), the weaving manner of fiber chooses 2D braiding, 2.5D braiding or 3D braiding;
In described step (1), in fiber preform, shared by fiber, volume fraction is controlled, preferably 5%-80%, further preferably
For 30%-60%.
9. according to the fiber reinforced pottery with ternary layered MAX phase boundary surface layer described in any claim in claim 1 to 6
The preparation method of porcelain based composites, it is characterised in that: comprise the steps:
Fibrage being become fiber cloth, prepares boundary layer on fiber cloth surface, then fiber cloth being sewed up is fiber preform,
After prepare ceramic matrix in fibre preforms surface.
The system of the fiber reinforced ceramic matric composite with ternary layered MAX phase boundary surface layer the most according to claim 9
Preparation Method, it is characterised in that: in described fiber preform, shared by fiber, volume fraction is controlled, preferably 5%-80%, further
It is preferably 30%-60%.
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