CN115806442A - SiC/SiC-SiBYb composite material and preparation method thereof - Google Patents
SiC/SiC-SiBYb composite material and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 38
- 239000001301 oxygen Substances 0.000 claims abstract description 36
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 29
- 239000011184 SiC–SiC matrix composite Substances 0.000 claims abstract description 26
- 239000002002 slurry Substances 0.000 claims abstract description 23
- 239000000919 ceramic Substances 0.000 claims abstract description 21
- 239000011159 matrix material Substances 0.000 claims abstract description 20
- 230000007797 corrosion Effects 0.000 claims abstract description 18
- 238000005260 corrosion Methods 0.000 claims abstract description 18
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 17
- 239000000956 alloy Substances 0.000 claims abstract description 17
- 229910008326 Si-Y Inorganic materials 0.000 claims abstract description 15
- 229910006773 Si—Y Inorganic materials 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 14
- 238000011065 in-situ storage Methods 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000001764 infiltration Methods 0.000 claims description 23
- 230000008595 infiltration Effects 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000000835 fiber Substances 0.000 claims description 11
- 239000011153 ceramic matrix composite Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 4
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 4
- 238000009941 weaving Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000011241 protective layer Substances 0.000 claims description 2
- 210000001161 mammalian embryo Anatomy 0.000 claims 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 abstract description 6
- 238000007598 dipping method Methods 0.000 abstract description 6
- 238000000626 liquid-phase infiltration Methods 0.000 abstract description 4
- 229910052727 yttrium Inorganic materials 0.000 abstract description 3
- 229910052769 Ytterbium Inorganic materials 0.000 abstract description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 53
- 229910010271 silicon carbide Inorganic materials 0.000 description 50
- 239000000543 intermediate Substances 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 7
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 7
- 238000000576 coating method Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- -1 rare earth silicate Chemical class 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 230000004584 weight gain Effects 0.000 description 3
- 235000019786 weight gain Nutrition 0.000 description 3
- 229910001029 Hf alloy Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
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- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910006283 Si—O—H Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
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- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 239000011521 glass Substances 0.000 description 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
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- 230000001629 suppression Effects 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
- FIIGRZYDBNZZFN-UHFFFAOYSA-N trioxido(trioxidosilyloxy)silane ytterbium(3+) Chemical compound [Si]([O-])([O-])([O-])O[Si]([O-])([O-])[O-].[Yb+3].[Yb+3] FIIGRZYDBNZZFN-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
The invention relates to a SiC/SiC-SiBYb composite material and a preparation method thereof, which comprises the steps of firstly utilizing a slurry dipping method to dip YbB 6 Ceramic powder is introduced into the porous SiC/SiC composite material, and Si-Y alloy is introduced by combining a reaction melt infiltration method, so that the SiC/SiC-SiBYb composite material is prepared. The technical scheme provided by the invention can realize that two water-oxygen resistant components of Yb and Y are simultaneously introduced into the porous SiC/SiC composite material, and provides a new idea for developing the preparation of the multi-element water-oxygen resistant matrix. The SiC/SiC-SiBYb composite material prepared by the method can generate a silicate phase in situ in the service process of a water-oxygen environment, and shows good water-oxygen corrosion resistance.
Description
Technical Field
The invention belongs to the field of composite materials, and relates to a SiC/SiC-SiBYb composite material and a preparation method thereof, which are mainly applied to the field of improving the water-oxygen corrosion resistance and self-healing performance of silicon carbide fiber toughened silicon carbide ceramic matrix composite materials (SiC/SiC).
Background
With the vigorous development of aerospace technology, higher requirements are put forward on the service performance of the composite material in a complex environment. Aiming at the development requirement of a novel high-Mach-number aircraft, the Ni-based high-temperature alloy approaches to the limit service temperature, and the SiC/SiC composite material has excellent performances of low density, high specific strength, high specific modulus, high temperature resistance, oxidation resistance, wear resistance, corrosion resistance and the like, overcomes the defect of poor toughness inherent in ceramics, and becomes a preferred high-temperature light-weight structural material of a high thrust-weight ratio engine.
Engine components prepared by SiC/SiC composite materials need to be in service for at least thousands of hours in a high-temperature water oxygen environment, however, the SiC/SiC composite materials are seriously damaged in service in the high-temperature water oxygen environment, and Si-O-H and H are respectively generated on SiC matrixes, siC fibers and BN interfaces under the action of high-temperature water vapor 3 BO 3 And volatile substances cause rapid failure of the composite material, and the long-life use requirement of the high-performance aircraft engine cannot be met. Therefore, the key problem of prolonging the service life of the SiC/SiC composite material is to improve the high-temperature water corrosion resistance of the material.
At present, rare earth silicate has excellent performances of low high-temperature volatility, low oxygen permeability and the like, and can be used for improving the high-temperature water-oxygen corrosion performance of composite materials. The existing methods for using the modified composite material containing the rare earth element mainly comprise EBC coating, interface modification, matrix modification and the like. However, the EBC coating has the problems of easy peeling in the service process, complex preparation process and the like; the interface modification method has the problems of uneven phase distribution, complex preparation process, difficulty in realizing large-scale production and the like. In contrast, the matrix modification method has the advantages of low preparation temperature, high mass fraction of introduced rare earth elements, uniform distribution, easy large-scale production and the like.
Document 3 Aoki T, ogasawara T, okubo Y, et al, fabrication and properties of Si-Hf alloy melt-embedded type ZMI fiber/SiC-based matrix Composites [ J ] Composites Part A Applied Science and Manufacturing,2014,66, 155-162."Aoki et al prepared a Tyranno I fiber/SiC-based composite material by RMI process using Si-8.5at Hf alloy at 1375 ℃ with bending strength 35% higher than that of a composite material prepared by MI process using Si melt, mainly because of the suppression effect of the strength damage to SiC fibers due to low temperature infiltration.
A Si-Y-C ternary ceramic matrix composite and a preparation method thereof are developed in the patent number CN202010083252.0, and Si-Y-C ternary ceramic matrix is generated by utilizing the in-situ reaction of Si-Y alloy and a C source in the composite through a reaction melt infiltration method. The method realizes the rapid preparation of the hydroxyl-resistant body, but alloy residue and C residue exist in the substrate, which is not beneficial to the service of the composite material in the water-oxygen composite environment.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a SiC/SiC-SiBYb composite material and a preparation method thereof, Y 2 Si 2 O 7 And Yb 2 Si 2 O 7 As oxygen transmission rate and high temperature volatilizationThe two rare earth silicates with lower rates can be used for improving the anti-water oxygen corrosion performance of the SiC/SiC composite material. In addition, the introduction of the B element can form a glass phase and play a role in healing cracks.
Technical scheme
A SiC/SiC-SiBYb composite material is characterized in that: in-situ generation of SiBYb quaternary compact matrix in the porous SiC/SiC composite material blank, wherein the matrix comprises YbB 4 Phase and YB 4 Phase, and residual Si phase and YSi 2 Phase (1); the YbB 4 Phase and YB 4 Phase consumes corrosive gas in the water-oxygen corrosion process and generates a water-oxygen resistant component (Y) in situ 2 Si 2 O 7 And Yb 2 Si 2 O 7 ) And the water-oxygen corrosion resistance and self-healing performance of the composite material are improved.
A preparation method of the SiC/SiC-SiBYb composite material is characterized by comprising the following steps:
step 1: a BN interface and a SiC protective layer are deposited in the porous SiC/SiC composite material blank;
step 2: impregnating the ceramic slurry into a porous SiC/SiC composite material blank, and drying to obtain a ceramic matrix composite material intermediate SiC/SiC-YbB 6 ；
The ceramic slurry comprises the component YbB 6 Water-based ceramic slurry of the powder;
and 3, step 3: to ceramic matrix composite intermediate SiC/SiC-YbB 6 Introducing Si-Y alloy by adopting a reaction infiltration method to prepare a SiC/SiC-SiBYb composite material; wherein the infiltration temperature is 1300-1500 ℃, and the infiltration time is 15-60 min.
Deionized water is used as a solvent in the water-based ceramic slurry; carboxymethyl cellulose CMC as dispersant, the mass fraction is 3.0-5.0 wt.%; ybB 6 The mass fraction of (b) is 20-60 wt.%.
The YbB 6 The particle diameter of the powder is 5 to 20 μm.
The structure of the porous SiC/SiC composite blank body comprises but is not limited to a 2D,2.5D or 3D fiber preform.
The 3D fiber preform weaving method includes but is not limited to 3D needling or three-dimensional four-way weaving.
The intermediate SiC/SiC-YbB 6 Middle YbB 6 The mass ratio of the active carbon is 20 to 50wt.%.
The components of the introduced Si-Y alloy are Si phase and YSi 2 And (4) phase(s).
Advantageous effects
The invention provides a SiC/SiC-SiBYb composite material and a preparation method thereof, which comprises the steps of firstly utilizing a slurry dipping method to dip YbB 6 Ceramic powder is introduced into the porous SiC/SiC composite material, and then Si-Y alloy is introduced by combining a reaction melt infiltration method, so that the SiC/SiC-SiBYb composite material is prepared. The technical scheme provided by the invention can realize that two water-oxygen resistant components of Yb and Y are simultaneously introduced into the porous SiC/SiC composite material, and provides a new idea for developing the preparation of the multi-element water-oxygen resistant matrix. The SiC/SiC-SiBYb composite material prepared by the method can generate a silicate phase in situ in the service process of a water-oxygen environment, and shows good water-oxygen corrosion resistance.
The invention lies in using Si-Y alloy and YbB 6 The SiBYb quaternary compact matrix is generated in situ in the porous SiC/SiC composite material blank body through the reaction between the two, and the matrix mainly comprises YbB 4 Phase and YB 4 Phase and part of the residual Si phase with YSi 2 Phase (1); ybB 4 Phase and YB 4 Phase energy consumes corrosive gas in the process of water-oxygen corrosion and generates a water-oxygen resistant component (Y) in situ 2 Si 2 O 7 And Yb 2 Si 2 O 7 ) The water-oxygen corrosion resistance and the self-healing performance of the composite material are effectively improved.
The invention adopts the slurry to dip in the porous SiC/SiC composite material and introduces YbB 6 Utilizing Si-Y alloys in combination with YbB in reaction melt infiltration 6 The SiBYb matrix is generated through in-situ reaction, and the obtained matrix contains a water-oxygen resistant component and a self-healing component. The method can solve the problems of high preparation temperature, long preparation period and complex process of the SiC/SiC-SiBYb composite material, and improve the water-oxygen corrosion resistance and self-healing performance of the composite material.
The invention has the beneficial effects that:
(1) The invention utilizes YbB 6 Reacting with Si-Y alloy melt in situ to generate a SiBYb matrix in the porous SiC/SiC composite material, wherein the matrix mainly comprises YbB 4 、YB 4 Si and YSi 2 Composition of, wherein, ybB 4 And YB 4 Phase is YbB 6 Phase with YSi in Si-Y alloy 2 The phase reaction is formed, and the method realizes the rapid preparation of the multi-element complex phase matrix.
(2) The invention utilizes the slurry dipping combined reaction infiltration method to realize the rapid preparation of the high-density composite material, and simultaneously, ybB in the matrix 4 And YB 4 The phase can form a silicate phase in a water-oxygen corrosion environment, and the water-oxygen corrosion resistance of the SiC/SiC composite material is effectively improved under the combined action of the silicate phase and the silicate phase.
(3) The invention utilizes the slurry dipping combined reaction infiltration method to reduce the infiltration temperature to be within the fiber bearing range, thereby reducing the thermal damage and energy consumption of the fiber, and meanwhile, the method has short preparation period and simple process, and is suitable for the large-scale production of the composite material.
Drawings
FIG. 1 is a schematic flow diagram of the process.
FIG. 2 shows the density and porosity of SiC/SiC-SiBYb composites prepared in examples 1 to 3.
FIG. 3 shows the bending strength of the SiC/SiC-SiBYb composite materials obtained in examples 1 to 3.
FIG. 4 is a cross-sectional back-scattering plot of the SiC/SiC-SiBYb composite material prepared in example 2.
FIG. 5 shows the microstructure of the SiC/SiC-SiBYb composite material prepared in example 2
FIG. 6 is a cross-sectional back-scattering plot of the SiC/SiC-SiBYb composite material prepared in example 2 after water-oxygen etching.
FIG. 7 is an X-ray diffraction pattern of the SiC/SiC-SiBYb composite material prepared in example 2 after water oxygen etching.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
EXAMPLE 1 sample with infiltration temperature 1300 ℃
Step 3, preparing the SiC/SiC-SiBYb composite material: the SiC/SiC-YbB prepared in the step 2 6 And (3) putting the intermediate and the Si-Y alloy into a vacuum infiltration furnace, wherein the infiltration temperature is 1300 ℃, and the infiltration time is 30min, so as to prepare the SiC/SiC-SiBYb composite material.
EXAMPLE 2 sample infiltration temperature 1400 deg.C
Step 3, preparing the SiC/SiC-SiBYb composite material: the SiC/SiC-YbB prepared in the step 2 6 And (3) putting the intermediate and the Si-Y alloy into a vacuum infiltration furnace, wherein the infiltration temperature is 1400 ℃, and the infiltration time is 30min, so as to prepare the SiC/SiC-SiBYb composite material.
EXAMPLE 3 samples with an infiltration temperature of 1500 deg.C
Step 3, preparing the SiC/SiC-SiBYb composite material: the SiC/SiC-YbB prepared in the step 2 6 And (3) putting the intermediate and the Si-Y alloy into a vacuum infiltration furnace, wherein the infiltration temperature is 1500 ℃, and the infiltration time is 15min, so as to prepare the SiC/SiC-SiBYb composite material.
The flow chart of the process is shown in figure 1.
The density and porosity of the SiC/SiC-SiBYb composites prepared in the above three examples are shown in FIG. 2. It can be seen that the composite prepared according to example 3 has a low density and a high porosity, which can be attributed to the high YbB 6 The slurry with mass fraction is sticky and is not beneficial to the infiltration process.
The bending strength of the SiC/SiC-SiBYb composite material prepared by the above three examples is shown in FIG. 3. Fig. 4 shows the macro morphology (fig. 4 (a)) and the microstructure (fig. 4 (b)) of the SiC/SiC-sibyb composite material prepared in example 2, and it can be seen that a complex phase formed by reaction, i.e., a sibyb quaternary matrix, exists inside the composite material.
FIG. 5 is a back scattering diagram of the microstructure of the SiC/SiC-SiBYb composite material prepared in example 2, wherein it can be seen that the SiBYb matrix is mainly composed of Si (# 1), YSi 2 (# 2), #3 and #4 all have YbB 4 And YB 4 Composition, the difference is only in the difference of Yb element content; wherein YbB 4 And YB 4 Phase is YbB 6 Phase with YSi in Si-Y alloy 2 And the phase reaction is formed.
FIG. 6 is a back scattering diagram of the microstructure of the SiC/SiC-SiBYb composite material prepared in example 2 after being corroded by 100h of water and oxygen at 1300 ℃, and the formation of ytterbium disilicate (YbDS) and SiO after corrosion can be seen from the diagram 2 And (4) phase(s).
FIG. 7 is an X-ray diffraction pattern of the SiC/SiC-SiBYb composite material prepared in example 2 after being corroded by 100h of water oxygen at 1300 ℃.
Claims (8)
1. A SiC/SiC-SiBYb composite material is characterized in that: in-situ generation of SiBYb quaternary compact matrix in the porous SiC/SiC composite material blank, wherein the matrix comprises YbB 4 Phase and YB 4 Phase, and residual Si phase and YSi 2 Phase (1); the YbB 4 Phase and YB 4 The phase consumes corrosive gas in the water-oxygen corrosion process and generates a water-oxygen resistant component (Y) in situ 2 Si 2 O 7 And Yb 2 Si 2 O 7 ) And the water-oxygen corrosion resistance and the self-healing performance of the composite material are improved.
2. A method for preparing the SiC/SiC-SiBYb composite material of claim 1, which is characterized by comprising the following steps:
step 1: a BN interface and a SiC protective layer are deposited in the porous SiC/SiC composite material blank;
step 2: impregnating the ceramic slurry into a porous SiC/SiC composite material blank, and drying to obtain a ceramic matrix composite material intermediate SiC/SiC-YbB 6 ；
The ceramic slurry comprises the component YbB 6 Water-based ceramic slurry of the powder;
and step 3: to ceramic matrix composite intermediate SiC/SiC-YbB 6 Introducing Si-Y alloy by adopting a reaction infiltration method to prepare a SiC/SiC-SiBYb composite material; wherein the infiltration temperature is 1300-1500 ℃, and the infiltration time is 15-60 min.
3. The method of claim 2, wherein: deionized water is used as a solvent in the water-based ceramic slurry; hydroxymethyl cellulose CMC as dispersant, the mass fraction is 3.0-5.0 wt.%; ybB 6 The mass fraction of (A) is 20 to 60wt.%.
4. A method according to claim 2 or 3, characterized in that: the YbB 6 The particle size of the powder is 5-20 μm.
5. The method of claim 2, wherein: the structure of the porous SiC/SiC composite embryo includes, but is not limited to, a 2D,2.5D or 3D fiber preform.
6. The method of claim 5, wherein: the 3D fiber preform weaving method includes but is not limited to 3D needling or three-dimensional four-way weaving.
7. The method of claim 2, wherein: the intermediate SiC/SiC-YbB 6 Middle YbB 6 The mass ratio of the active carbon is 20 to 50wt.%.
8. The method of claim 2, wherein: the components of the introduced Si-Y alloy are Si phase and YSi 2 And (4) phase.
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| CN116789465A (en) * | 2023-07-19 | 2023-09-22 | 西北工业大学 | Preparation method of quaternary Si-Y-B-Yb coating with self-healing and corrosion resistance |
| CN117923928A (en) * | 2024-03-20 | 2024-04-26 | 西北工业大学宁波研究院 | Complex-phase oxide ceramic modified ceramic matrix composite material and preparation method thereof |
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| CN116789465A (en) * | 2023-07-19 | 2023-09-22 | 西北工业大学 | Preparation method of quaternary Si-Y-B-Yb coating with self-healing and corrosion resistance |
| CN117923928A (en) * | 2024-03-20 | 2024-04-26 | 西北工业大学宁波研究院 | Complex-phase oxide ceramic modified ceramic matrix composite material and preparation method thereof |
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