CN103483009A - Preparation method of multilayer environmental barrier coating (EBC) structure with anti-cracking expansion ability - Google Patents
Preparation method of multilayer environmental barrier coating (EBC) structure with anti-cracking expansion ability Download PDFInfo
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Abstract
The invention relates to a preparation method of a multilayer environmental barrier coating (EBC) structure with anti-cracking expansion ability. The designed EBC coating comprises two basic structural layers, wherein the inner layer is a dense water and oxygen corrosion resistant coating, and the outer layer is an elastic modulus graded layer. The dense water and oxygen corrosion resistant coating on the inner layer is mainly used for resisting the chemical corrosion of such matters in the environment on a matrix material as water vapor and fused salt impurity, and the elastic modulus graded layer on the outer layer is mainly used for resisting the expansion of cracks in the EBC coating caused by impact of foreign particles (mainly referring to expansion along the longitudinal direction of the coating, namely, the cracks penetrate through the coating).
Description
Technical field
The present invention relates to a kind of preparation method who possesses the multilayer environment barrier coating structure of resistance to crack extension ability, relate to a kind of multilayer environment barrier coating (Environmental barrier coating that possesses the resistance to crack extension ability, EBC) the Design & preparation method of structure, belong to structure design and the preparation field of coating.
Background technology
Silicon based ceramic and ceramic matric composite have the characteristics such as high specific strength, high ratio modulus, anti-oxidant and low density, have now become the candidate material of aircraft engine hot-end component coideal.But, under the engine combustion room environmental, on the silica-base material surface, formed silicon oxide protective membrane can be corroded by the water in combustion gas and fused salt, thereby the antioxidant property of silica-base material parts is sharply descended.By on the silica-base material surface, preparing the EBC coating, can overcome the silica-base material problem that antioxidant property lost efficacy under the engine combustion room environmental, ensure that the silica-base material parts are at the environment durability had under water vapour and corrosive impurity existence condition, to meet the long-life requirement of aircraft engine parts.
Under the real environment for use of aircraft engine, the chemical corrosion of the water vapour of the influence factor that affects EBC coating weather resistance in environment, fused salt etc., also comprise the physical impact effect to the EBC coating of foreign particles (the small grains of sand, the volcanic ash particle of hard etc.) in environment.Foreign particles in environment enters into engine interior by the engine suction opening, under the drive of high velocity air with high velocity shock to the surface of EBC coating, consequent surging force can make the EBC coating produce a large amount of crackles to cause final cracking and spalling failure.Therefore, the resistance to crack extension ability of raising EBC coating just seems particularly important.
Summary of the invention
The technical problem solved
For fear of the deficiencies in the prior art part, the present invention proposes a kind of preparation method who possesses the multilayer environment barrier coating structure of resistance to crack extension ability,
Technical scheme
A kind of preparation method who possesses the multilayer environment barrier coating structure of resistance to crack extension ability is characterized in that step is as follows:
Step 1: body material is machined to desired size, and cleans up;
Step 2: at the matrix specimen surface, prepare internal layer water resistant oxygen corrosion coating;
Step 3: the preparation of outer Young's modulus gradient layer
(1) select Young's modulus to be greater than 150GPa, fusing point is greater than the EBC material of 1800 ℃ and prepares porous coating, and porosity is 10%～30%;
(2) select Young's modulus to be less than 100GPa, fusing point is less than EBC powder body material and dispersion agent, binding agent and the solvent of 1600 ℃ and is mixed with slurry through ball milling.Concrete proportioning is: EBC powder body material+2wt% that 40wt%～80wt% Young's modulus is lower～10wt% dispersion agent+2wt%～10wt% binding agent+30wt%～80wt% solvent;
(3), at the more much higher hole of the Young's modulus prepared coatingsurface, the method for using brushing or dipping to lift prepares the EBC coating that Young's modulus is lower;
At 1350 ℃～1600 ℃; prepared coating green compact are heat-treated 3 hours under argon shield; the EBC coating that under high temperature, Young's modulus is lower can produce a large amount of liquid phases and infiltrate in the EBC coating that the Young's modulus of porous is higher, forms the gradient layer that Young's modulus increases from top to down gradually.
The preparation method of described internal layer water resistant oxygen corrosion coating comprises plasma spraying method, slurry method, chemical Vapor deposition process Chemical Vapor Deposition, CVD, electron beam Aided Physical vapour deposition Electron Beam-Physical Vapor deposition, EB-PVD, sol-gel method or polymkeric substance transform cracking process.
The preparation method of described porous coating comprises slurry method, electron beam Aided Physical vapour deposition Electron Beam-Physical Vapor deposition, and EB-PVD, sol-gel method or polymkeric substance transform cracking process.
Beneficial effect
A kind of preparation method who possesses the multilayer environment barrier coating structure of resistance to crack extension ability that the present invention proposes, designed EBC coating basic structure is two-layer, internal layer is fine and close water resistant oxygen corrosion coating, skin be Young's modulus graded layer (Elastic-modulus-graded layer, as shown in Figure 1).Wherein the fine and close water resistant oxygen corrosion coating of internal layer is mainly used in resisting the chemical corrosion to body material such as water vapour in environment and fused salt impurity, and outer field elastic modulus change layer is mainly used in the expansion (mainly refer to along coating longitudinally expand, i.e. penetration of cracks coating) of crackle in the EBC coating that opposing produces because foreign particles impacts.
The accompanying drawing explanation
Fig. 1 resistance to crack extension EBC coated designs model.
Fig. 2 resistance to crack extension EBC coating preparation process model.
Each layer of surface topography of Fig. 3 multilayer EBC coating and Cross Section Morphology.(a) inner layer B SAS+Sc
2si
2o
7the coatingsurface pattern; (b) porous Sc
2si
2o
7the coatingsurface pattern; (c) outer Young's modulus gradient layer surface topography; (d) multilayer EBC coating Cross Section Morphology.
Surface and Cross Section Morphology after Fig. 4 impression precrack is processed.(a) surface topography; (b) Cross Section Morphology.
Fig. 5 multilayer EBC coating is through 1250 ℃, 50%H
2o-50%O
2corrode surface and Cross Section Morphology after 200 hours.(a) surface topography; (b) Cross Section Morphology.
embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Designed EBC coating basic structure is two-layer, and internal layer is fine and close water resistant oxygen corrosion coating, skin be Young's modulus graded layer (Elastic-modulus-graded layer, as shown in Figure 1).Wherein the fine and close water resistant oxygen corrosion coating of internal layer is mainly used in resisting the chemical corrosion to body material such as water vapour in environment and fused salt impurity, and outer field elastic modulus change layer is mainly used in the expansion (mainly refer to along coating longitudinally expand, i.e. penetration of cracks coating) of crackle in the EBC coating that opposing produces because foreign particles impacts.
The preparation of Young's modulus graded layer mainly comprises two steps: the first, and the preparation of porous high-elastic modulus layer; The second, the method that adopts slurry method to lift by brushing or dipping is combined in high temperature and bends down elastic modulus E BC material and form liquid phase it is penetrated in porous high-elastic modulus layer gradually, thereby obtains the Young's modulus gradient layer.Because high at outer field low modulus of elasticity materials content, low at the low modulus of elasticity materials content of internal layer, so its Young's modulus of Young's modulus gradient layer obtained increases from outside to inside gradually.The height of so-called elasticity modulus of materials is comparatively speaking.
Theoretical basis of the present invention is: the expansion of (1) crackle in material is relevant to material fracture toughness, and the expansion of the larger crackle of the fracture toughness property of material in material is more difficult.And the fracture toughness property of material is proportional with the Young's modulus of material.What Young's modulus characterized is an index of material production recoverable deformation complexity, and its value is larger, makes material that the stress of certain recoverable deformation occur also larger, and material stiffness is larger, that is, under certain stress, the generation recoverable deformation is less.Therefore, can think crackle more difficult expansion in thering is the material of larger Young's modulus, expand run into resistance in the material that crackle is larger at Young's modulus larger; (2) resistance run into while expanding in the material increased gradually to Young's modulus when the crackle material lower from Young's modulus also increases gradually, and now crackle can stop the Directional Extension of expanding or edge increases perpendicular to Young's modulus.
Embodiment 1: select slurry method to prepare the internal layer coating.The internal layer coating is selected BSAS+Sc
2si
2o
7mixolimnion.Using polysilazane as dispersion agent and binding agent, and solvent is selected alcohol, and high elastic coefficient EBC material is selected Sc
2si
2o
7(E=～200GPa), low modulus of elasticity materials is selected BSAS(E=～60-70GPa) preparation has the Young's modulus gradient layer of opposing crack propagation ability.Its preparation flow and basic structure are as shown in Figure 2.Concrete preparation process is as follows:
1. the preparation of body material: select C/SiC as body material, C/SiC is made to the bar-shaped sample that is of a size of 40 * 5 * 3.5mm, adopt ultrasonic cleaning clean.
2.BSAS+Sc
2si
2o
7the preparation of mixolimnion:
The polysilazane that 1) will account for gross weight 5wt% is as dispersion agent, accounts for gross weight 15wt% polysilazane and joins as binding agent in the alcohol that accounts for gross weight 80% and prepare polysilazane solution.
2) will account for respectively the BSAS powder and the Sc that accounts for gross weight 70wt% of gross weight 50wt%
2si
2o
7powder joins in polysilazane solution, then adds the Li that accounts for gross weight 3wt%
2cO
3as sintering aid, use shake swing ball grinding machine to mix and within 1 hour, prepare slurry.
3) method that adopts dipping to lift prepares BSAS+Sc at the C/SiC matrix surface
2si
2o
7the coating green compact, and the spirit solvent in 70 ℃ of insulations make coating in 3 hours volatilizees away.
4) lead to argon gas as shielding gas in vacuum tube furnace; after first with the temperature rise rate of 5 ℃/min, being warming up to 400 ℃ of insulations and within 1 hour, making polysilazane in coating solidify again the temperature rise rate with 1 ℃/min be warming up to 1350 ℃ of insulations 2 hours, last 1 ℃/min is cooled to room temperature and obtains fine and close BSAS+Sc
2si
2o
7coating.Its surface topography as shown in Figure 3 a.
3. the preparation of Young's modulus gradient layer:
1) preparation method of polysilazane solution is with in 2 1) preparation process identical.
2) will account for the higher Sc of gross weight 50wt% Young's modulus
2si
2o
7powder joins in polysilazane solution, uses shake swing ball grinding machine ball milling within 1 hour, to prepare slurry.
3) BSAS+Sc that the method that adopts dipping to lift is preparing
2si
2o
7coatingsurface prepares Sc
2si
2o
7the coating green compact.
4) lead to argon gas as shielding gas in vacuum tube furnace; after first with the temperature rise rate of 5 ℃/min, being warming up to 400 ℃ of insulations and within 1 hour, making polysilazane in coating solidify again the temperature rise rate with 1 ℃/min be warming up to 1350 ℃ of insulations 2 hours, last 1 ℃/min is cooled to room temperature.Due to Sc
2si
2o
7powder can not make up volumetric shrinkage that polysilazane produces because of Pintsch process and at 1350 ℃ of lower Sc
2si
2o
7being difficult to sintering causes at Sc
2si
2o
7coatingsurface forms a large amount of holes and exists.As shown in Fig. 3 b.
5) will account for 70% the lower BSAS powder of Young's modulus and join in polysilazane, then add the H that accounts for gross weight 2wt%
3bO
3as sintering aid, use shake swing ball grinding machine ball milling within 1 hour, to prepare slurry.
6) the porous Sc that the method that adopts dipping to lift is preparing
2si
2o
7coatingsurface prepares BSAS coating green compact.
7) lead to argon gas as shielding gas in vacuum tube furnace; after first with the temperature rise rate of 5 ℃/min, being warming up to 400 ℃ of insulations and within 1 hour, making polysilazane in coating solidify again the temperature rise rate with 1 ℃/min be warming up to 1400 ℃ of insulations 3 hours, last 1 ℃/min is cooled to room temperature.Under high temperature, BSAS forms a large amount of liquid phases and penetrates into porous Sc
2si
2o
7form the gradient layer that Young's modulus increases from outside to inside gradually in coating.As shown in Figure 3 c, prepared multilayer EBC coating Cross Section Morphology as shown in Figure 3 d for its surface topography.
4. adopt the Rockwell Hardness meter to carry out the impression processing at the multilayer EBC coatingsurface prepared, load is 0.5 kilogram, 10 seconds dwell times.The pattern that Fig. 4 is impression surface and cross section.Can see that from surface topography four drift angles of impression only have a small amount of crackle to produce, and have the fold produced due to extruding on four limits of impression.And can see that on the cross section of impression the drift angle place has tiny crack to exist, but basically all along being parallel to surface direction.This is that crackle trends towards being parallel to the surface direction expansion because the crackle resistance that inwardly expansion runs into is larger.This illustrates that prepared Young's modulus gradient layer possesses the ability that the opposing crackle is longitudinally expanded.
5. prepared multilayer EBC coating is carried out in water oxygen corrosion device to the Performance Assessment of coating.Whole water oxygen corrosion experiment condition is as follows: in stove, temperature is 1250 ℃, and atmosphere is 50%H
2o-50%O
2, gas flow rate is 8.5 * 10
-4m/s (this flow velocity is the estimated value under room temperature), pressure is 1atm, the whole water oxygen corrosion time is 200 hours.Fig. 5 is the surface after 200 hours and Cross Section Morphology through the water oxygen corrosion.Can see from surface topography, process because of impression the crackle produced and substantially heal.Can see that from Cross Section Morphology the tiny crack at the impression drift angle also disappears substantially, this is, because BSAS has liquid phase to generate in high-temperature corrosion environment, the crackle in coating has been played to Healing.
6. in the 0th, 5,10,20,50 of water oxygen experiment, the weight of 100,150,200 hours test samples, the 0th, the remaining bending strength of 10,50,100,200 hours test samples.
7. from obtained oxidation weight loss curve and remaining bending strength curve, can see, prepared multilayer EBC coating is processed through the impression precrack, again under 1250 ℃ of water oxygen environment through 200 hours the corrosion after rate of weight loss be only 1.2% left and right, its strength retention is 84% left and right.The multilayer EBC coating with Young's modulus graded that designed preparation is described has ability that the opposing crackle longitudinally expands and good water resistant oxygen corrosion ability.
Embodiment 2: select slurry method to prepare the coating internal layer.The internal layer coating is selected BSAS+Y
2siO
5mixolimnion.Using polysilazane as dispersion agent and binding agent, and solvent is selected alcohol, and high elastic coefficient EBC material is selected Y
2siO
5low modulus of elasticity materials selects the BSAS preparation to have the Young's modulus gradient layer of opposing crack propagation ability.Its preparation flow is identical with embodiment 1.
Embodiment 3: select sol-gel method to prepare the coating internal layer.The internal layer coating is selected BAS+Sc
2si
2o
7mixolimnion.Using polysilazane as dispersion agent and binding agent, and solvent is selected alcohol, and high elastic coefficient EBC material is selected Sc
2si
2o
7low modulus of elasticity materials selects the BAS preparation to have the Young's modulus gradient layer of opposing crack propagation ability.Its preparation flow is identical with embodiment 1.
Claims (3)
1. a preparation method who possesses the multilayer environment barrier coating structure of resistance to crack extension ability, is characterized in that step
As follows:
Step 1: body material is machined to desired size, and cleans up;
Step 2: at the matrix specimen surface, prepare internal layer water resistant oxygen corrosion coating;
Step 3: the preparation of outer Young's modulus gradient layer
(1) select Young's modulus to be greater than 150GPa, fusing point is greater than the EBC material of 1800 ℃ and prepares porous coating, and porosity is 10%～30%;
(2) select Young's modulus to be less than 100GPa, fusing point is less than EBC powder body material and dispersion agent, binding agent and the solvent of 1600 ℃ and is mixed with slurry through ball milling.Concrete proportioning is: EBC powder body material+2wt% that 40wt%～80wt% Young's modulus is lower～10wt% dispersion agent+2wt%～10wt% binding agent+30wt%～80wt% solvent;
(3), at the more much higher hole of the Young's modulus prepared coatingsurface, the method for using brushing or dipping to lift prepares the EBC coating that Young's modulus is lower;
At 1350 ℃～1600 ℃; prepared coating green compact are heat-treated 3 hours under argon shield; the EBC coating that under high temperature, Young's modulus is lower can produce a large amount of liquid phases and infiltrate in the EBC coating that the Young's modulus of porous is higher, forms the gradient layer that Young's modulus increases from top to down gradually.
2. the preparation method who possesses according to claim 1 the multilayer environment barrier coating structure of resistance to crack extension ability, it is characterized in that: the preparation method of described internal layer water resistant oxygen corrosion coating comprises plasma spraying method, slurry method, chemical Vapor deposition process Chemical Vapor Deposition, CVD, electron beam Aided Physical vapour deposition Electron Beam-Physical Vapor deposition, EB-PVD, sol-gel method or polymkeric substance transform cracking process.
3. the preparation method who possesses according to claim 1 the multilayer environment barrier coating structure of resistance to crack extension ability, it is characterized in that: the preparation method of described porous coating comprises slurry method, electron beam Aided Physical vapour deposition Electron Beam-Physical Vapor deposition, and EB-PVD, sol-gel method or polymkeric substance transform cracking process.
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Cited By (9)
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| CN105405474A (en) * | 2015-11-02 | 2016-03-16 | 西北工业大学 | Structure and preparation method of nuclear fuel cladding tube with crack expansion resisting capability |
| CN106083208A (en) * | 2016-06-23 | 2016-11-09 | 上海交通大学 | A kind of method preparing SiCN hafnium acid yttrium composite coating |
| CN106083209A (en) * | 2016-06-23 | 2016-11-09 | 上海交通大学 | A kind of preparation method of micro-structured configuration interlayer interface Mullite/ yttrium silicate composite coating |
| CN106966761A (en) * | 2016-06-02 | 2017-07-21 | 北京航空航天大学 | MULTILAYER COMPOSITE environment barrier coating with crackle self-healing function and preparation method thereof |
| CN108727066A (en) * | 2017-04-21 | 2018-11-02 | 通用电气公司 | Segmented environment barrier coat system and forming method thereof |
| CN108794068A (en) * | 2018-06-28 | 2018-11-13 | 航天材料及工艺研究所 | A kind of preparation method of porous material surface layer gradient transitional lay |
| CN109609886A (en) * | 2019-01-17 | 2019-04-12 | 北京矿冶科技集团有限公司 | A kind of process improving resisting corrosion of molten zinc coating life |
| CN111448339A (en) * | 2017-12-22 | 2020-07-24 | 欧瑞康表面处理解决方案股份公司普费菲孔 | Corrosion and corrosion resistant coating for turbine blades of gas turbines |
| CN114276169A (en) * | 2021-12-30 | 2022-04-05 | 广东省科学院新材料研究所 | Self-healing high-density environmental barrier coating and preparation method and application thereof |
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| CN106966761B (en) * | 2016-06-02 | 2020-03-31 | 北京航空航天大学 | Multilayer composite environmental barrier coating with crack self-healing function and preparation method thereof |
| CN106966761A (en) * | 2016-06-02 | 2017-07-21 | 北京航空航天大学 | MULTILAYER COMPOSITE environment barrier coating with crackle self-healing function and preparation method thereof |
| CN106083209A (en) * | 2016-06-23 | 2016-11-09 | 上海交通大学 | A kind of preparation method of micro-structured configuration interlayer interface Mullite/ yttrium silicate composite coating |
| CN106083209B (en) * | 2016-06-23 | 2018-09-11 | 上海交通大学 | A kind of preparation method of micro-structured configuration interlayer interface Mullite/ yttrium silicate composite coatings |
| CN106083208B (en) * | 2016-06-23 | 2018-09-11 | 上海交通大学 | A method of preparing SiCN- hafnium acid yttrium composite coatings |
| CN106083208A (en) * | 2016-06-23 | 2016-11-09 | 上海交通大学 | A kind of method preparing SiCN hafnium acid yttrium composite coating |
| CN108727066A (en) * | 2017-04-21 | 2018-11-02 | 通用电气公司 | Segmented environment barrier coat system and forming method thereof |
| US11851769B2 (en) | 2017-04-21 | 2023-12-26 | General Electric Company | Segmented environmental barrier coating systems and methods of forming the same |
| CN111448339A (en) * | 2017-12-22 | 2020-07-24 | 欧瑞康表面处理解决方案股份公司普费菲孔 | Corrosion and corrosion resistant coating for turbine blades of gas turbines |
| US11479862B2 (en) | 2017-12-22 | 2022-10-25 | Oerlikon Surface Solutions Ag, Pfäffikon | Corrosion- and erosion-resistant coating for turbine blades of gas turbines |
| CN108794068A (en) * | 2018-06-28 | 2018-11-13 | 航天材料及工艺研究所 | A kind of preparation method of porous material surface layer gradient transitional lay |
| CN109609886A (en) * | 2019-01-17 | 2019-04-12 | 北京矿冶科技集团有限公司 | A kind of process improving resisting corrosion of molten zinc coating life |
| CN114276169A (en) * | 2021-12-30 | 2022-04-05 | 广东省科学院新材料研究所 | Self-healing high-density environmental barrier coating and preparation method and application thereof |
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