CN107266128A - A kind of silicate Environmental Barrier Coatings on Si-based Ceramics and preparation method thereof - Google Patents

A kind of silicate Environmental Barrier Coatings on Si-based Ceramics and preparation method thereof Download PDF

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CN107266128A
CN107266128A CN201710569981.5A CN201710569981A CN107266128A CN 107266128 A CN107266128 A CN 107266128A CN 201710569981 A CN201710569981 A CN 201710569981A CN 107266128 A CN107266128 A CN 107266128A
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based ceramics
barrier coatings
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silicate
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CN107266128B (en
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刘玲
马壮
郑伟
柳彦博
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Beijing Institute of Technology BIT
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
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    • C04B2235/5208—Fibers
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    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5244—Silicon carbide

Abstract

The present invention relates to a kind of silicate Environmental Barrier Coatings on Si-based Ceramics and preparation method thereof, belong to Environmental Barrier Coatings on Si-based Ceramics technical field.The composition of Environmental Barrier Coatings on Si-based Ceramics of the present invention is silicate material, and the material has good chemical stability and thermal shock resistance, and has and SiCfThe thermal coefficient of expansion that/SiC matrix is more matched；Comparatively dense, no through-wall crack and UNICOM's stomata inside the Environmental Barrier Coatings on Si-based Ceramics prepared using the material, are capable of the intrusion of starvation and vapor, it is to avoid SiC under high temperaturefThe oxidation of/SiC matrix and performance degradation.The present invention prepares silicate Environmental Barrier Coatings on Si-based Ceramics using air plasma spraying technique, by optimizing air plasma spraying technological parameter, can be with the molten state and surface topography of silicate powder in Regulate Environment barrier coating, and then the performance for barrier coating of optimizing the environment；Methods described technique is simple, strong adaptability, and production efficiency is high, suitable commercial introduction.

Description

A kind of silicate Environmental Barrier Coatings on Si-based Ceramics and preparation method thereof
Technical field
The present invention relates to a kind of silicate Environmental Barrier Coatings on Si-based Ceramics and preparation method thereof, belong to Environmental Barrier Coatings on Si-based Ceramics technical field.
Background technology
With the development of aircraft industry, the fuel gas temperature and gaseous-pressure of aeroengine combustor buring room will also be improved constantly, Aero-engine will face harsher Service Environment.Silicon substrate non-oxide ceramicses (such as SiC, Si3N4Deng) due to excellent Mechanical behavior under high temperature and the good characteristic such as chemical resistance and creep resistant, it is considered to be most hopeful to replace nickel-base high-temperature Alloy is able to the high-temperature structural material applied in engine thermal end pieces.Under high temperature air environment, SiC surface can be formed The SiO of protective2Film, but under engine combustion environment, due to the presence of a large amount of vapor, SiO2With vapor The volatile Si (OH) of reaction generation4, cause SiC surface to occur serious degenerate and fail.In order to obtain the longer use longevity Life, it is necessary to the protection of use environment barrier coating.
Environmental Barrier Coatings on Si-based Ceramics is a kind of high-temperature structural material surface protection coating used under engine operating environments, can Barrier together is set up between high-temperature structural material and engine adverse circumstances, prevents or reduces engine environmental to thermal structure The influence of material property.
Because the thermal coefficient of expansion of some silicate is low, SiC, Si are in close proximity to3N4；And rare earth silicate can be held By higher temperature, phase stability is good；The volatility as shown by data in the high burning situation of water vapour content, rare earth monosilicate Volatility than BSAS (1-xBaO-xSrO-Al2O3-2SiO2, 0≤x≤1) low, vapour resistant performance is excellent more than 1300 DEG C It is different, it is possible to replace BSAS to use at a higher temperature, the candidate material as novel environmental barrier coating surface layer；Except rare earth silicic acid Beyond salt, Group IVB element silicate is due to its outstanding stability and thermal coefficient of expansion is low, is also Environmental Barrier Coatings on Si-based Ceramics research institute One class material of concern.However, not being related to also silicates coating being directly applied to protection silicon substrate non-oxidized substance pottery at present The report of ceramic material.
The method of traditional prepares coating is mainly to brush, although this method prepares simple possible, cost is relatively low, deposits Poor in process controllability, bond strength is low, smaller using scope, it is impossible to suitable for Environmental Barrier Coatings on Si-based Ceramics in aeroengine combustor buring room High temperature and high speed combustion gas wash away and corrosive environment use.
The content of the invention
In view of this, an object of the present invention is to provide in a kind of silicate Environmental Barrier Coatings on Si-based Ceramics, the silicate coating Portion is comparatively dense, no through-wall crack and UNICOM's stomata, is capable of the intrusion of starvation and vapor, it is to avoid SiC under high temperaturef/SiC The oxidation of matrix and performance degradation；The second purpose is to provide a kind of preparation method of silicate Environmental Barrier Coatings on Si-based Ceramics, methods described By optimizing air plasma spraying technological parameter, the molten state and surface shape of the silicate Environmental Barrier Coatings on Si-based Ceramics can be regulated and controled Looks, and methods described technique is simple, strong adaptability, production efficiency are high and cost is relatively low.
Wherein, atmospheric plasma spraying technology is as thermal source, by materials such as ceramics, alloy, metals using plasma-arc Material is heated to melting or semi-molten state, and is prepared with spraying at a high speed by the workpiece surface of pretreatment with typical lamellar The method of the coating of tissue.
The purpose of the present invention is realized by following technical scheme：
A kind of silicate Environmental Barrier Coatings on Si-based Ceramics, the composition of the Environmental Barrier Coatings on Si-based Ceramics is AxSiOy, and with SiCf/ SiC is matrix；
Wherein, when A is rare earth element y, Er, Yb or Lu, x=2, y=5；When A is Group IVB element Zr, Ti or Hf, x =1, y=4.
Preferably 150 μm~250 μm of the thickness of the Environmental Barrier Coatings on Si-based Ceramics.
A kind of preparation method of silicate Environmental Barrier Coatings on Si-based Ceramics of the present invention, the preparation method step is as follows：
Step 1. is by AxSiOyPowder, water, binding agent and ball milling pearl are added in ball mill and mixed, and are mixed Uniform slurry；Slurry is transferred in spray drying granulation tower again and carries out agglomeration granulation, it is 20 μm~80 μm balls to obtain particle diameter Shape agglomeration granulation powder；
The spherical agglomerated powder of gained is placed in non-pressure sintering furnace and carries out calcination processing by step 2., obtains AxSiOySpraying Powder；
Step 3. is to SiCf/ SiC matrix is cleaned and roughening processing, reaches the roughness (Rz) on surface to be sprayed 25 μm~100 μm；
Step 4. uses air plasma spraying technique by AxSiOySpraying powder sprays to SiCfIn/SiC matrix, then will Spray AxSiOySiC afterwardsf/ SiC matrix is placed under argon atmosphere and is heat-treated, cooling, in SiCfIn/SiC matrix To the Environmental Barrier Coatings on Si-based Ceramics；
Wherein, air plasma spraying technological parameter is：Spray distance 70mm~80mm, electric current 800A~900A, main gas Flow 80L/min~100L/min, auxiliary throughput 25L/min~35L/min, carrier gas flux 8L/min~15L/min, powder sending quantity 2rpm~4rpm；Main gas and carrier gas are argon gas, and auxiliary gas is helium.
In step 1, the preferred polyvinyl alcohol of binding agent, the preferred zirconium oxide of material of the ball milling pearl；Binding agent with AxSiOyThe mass ratio of powder is 0.003~0.005:1, water and AxSiOyThe mass ratio of powder is 1~3:1, ball milling pearl with AxSiOyThe mass ratio of powder is 3~5:1；Ball milling mixing 2h~3h under 200r/min~300r/min.
The parameter setting of agglomeration granulation is carried out in spray drying granulation tower：280 DEG C~350 DEG C of inlet temperature, outlet temperature 100 DEG C~130 DEG C of degree, rotating speed of shower nozzle 35Hz~50Hz, wriggling revolution speed 30rpm~40rpm.
In step 2, calcination processing 2h~3h at 1100 DEG C~1400 DEG C.
In step 4,2h~4h is heat-treated at 1300 DEG C~1400 DEG C.
Beneficial effect：
(1) silicate material of the present invention has good chemical stability and a thermal shock resistance, and have with matrix compared with For the thermal coefficient of expansion of matching；On the surface of the Environmental Barrier Coatings on Si-based Ceramics prepared using the silicate material, AxSiOyPowder granule is complete Running down and drawout, show smooth shape characteristic；And Environmental Barrier Coatings on Si-based Ceramics inside comparatively dense, no through-wall crack and connection Passage, coating at basal body interface with being well combined and no significant defect, so oxygen passage will not be formed inside Environmental Barrier Coatings on Si-based Ceramics, It is capable of the intrusion of starvation and vapor, it is to avoid SiC under high temperaturefThe oxidation of/SiC matrix and performance degradation；The environment barrier Coating can be used for preparing the high-temperature heat engine fields such as aero-engine, promote the development of aircraft industry.
(2) during the present invention prepares Environmental Barrier Coatings on Si-based Ceramics, by optimizing air plasma spraying technological parameter, it can adjust Control A in Environmental Barrier Coatings on Si-based CeramicsxSiOyThe molten state and surface topography of powder, and then the performance for barrier coating of optimizing the environment；Institute of the present invention State method technique simple, strong adaptability, production efficiency is high, suitable commercial introduction.
Brief description of the drawings
Fig. 1 is silicate Environmental Barrier Coatings on Si-based Ceramics surface Scanning Electron microscope (SEM) figure prepared by embodiment 1.
Fig. 2 is X-ray diffraction (XRD) collection of illustrative plates of silicate Environmental Barrier Coatings on Si-based Ceramics prepared by embodiment 1.
Fig. 3 is silicate Environmental Barrier Coatings on Si-based Ceramics surface Scanning Electron microscope figure prepared by embodiment 2.
Fig. 4 is the X ray diffracting spectrum of silicate Environmental Barrier Coatings on Si-based Ceramics prepared by embodiment 2.
Embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Institute It is conventional method unless otherwise instructed to state method, and the raw material can be obtained from open commercial sources unless otherwise instructed.
In implementing below：
Agents useful for same and instrument：
Embodiment 1
(1) by 1000g ZrSiO4Powder, 2333mL deionized waters and 4g polyvinyl alcohol are placed in ball mill, are added Zirconia ball and ratio of grinding media to material are 4:1, the ball milling 3h under 200r/min, obtain well mixed slurry；By well mixed slurry It is transferred in spray drying granulation tower and carries out agglomeration granulation, it is 20 μm~60 μm spherical Zr SiO to obtain particle diameter4Agglomeration granulation powder Body；
Wherein, spray drying granulation parameter is：310 DEG C of inlet temperature, 110 DEG C of outlet temperature, rotating speed of shower nozzle 45Hz is wriggled Revolution speed 30rpm；
(2) by the ZrSiO of gained4Agglomeration granulation powder is placed in non-pressure sintering furnace, and 2h is calcined at 1400 DEG C, is obtained ZrSiO4Spraying powder；
(3) first using acetone to SiCf/ SiC matrix carries out purified treatment, removes the greasy dirt of matrix surface and other pollutions Thing with obtain cleaning matrix surface；Recycle jet absorption type sand-blasting machine to carry out blasting treatment to clean matrix surface, make to be painted The roughness (Rz) for applying matrix surface reaches 32 μm；
(4) air plasma spraying technique is used by ZrSiO4Spraying powder sprays to SiCfIn/SiC matrix；Again will spraying ZrSiO4SiC afterwardsf/ SiC matrix is placed under argon atmosphere, and is incubated 4h at 1400 DEG C, cooling, in SiCf/ SiC bases The ZrSiO that thickness is 200 μm is obtained on body4Environmental Barrier Coatings on Si-based Ceramics；
Wherein, air plasma spraying technological parameter is：Main gas (argon gas)：90L/min, auxiliary gas (helium)：30L/min, Carrier gas (argon gas)：10L/min, electric current：850A, feeding speed：3.0g/min, spray distance：75mm.
From ZrSiO4More put down on the surface SEM it can be seen from the figure thats of Environmental Barrier Coatings on Si-based Ceramics, prepared Environmental Barrier Coatings on Si-based Ceramics surface It is whole, most of ZrSiO4Powder granule is completely melt and drawout, shows smooth shape characteristic, and inside Environmental Barrier Coatings on Si-based Ceramics Comparatively dense molten condition is good, as shown in Figure 1.It is known that prepared Environmental Barrier Coatings on Si-based Ceramics from the XRD spectrum in Fig. 2 Principal phase be ZrSiO4, there is a small amount of ZrO2In the presence of.
By obtained ZrSiO4Environmental Barrier Coatings on Si-based Ceramics carries out grind away polishing, is then carried out in the case where light microscope amplifies 200 times Observation, 3 regions are randomly selected in the visual field observed and are analyzed, are quantitatively calculated made using quantitative Image Analysing system for Metallography The porosity of standby Environmental Barrier Coatings on Si-based Ceramics, test result refers to table 1；Prepared Environmental Barrier Coatings on Si-based Ceramics dense structure degree is very high, average Consistency is 99.60%.
Table 1
Embodiment 2
(1) by 600g Y2SiO5Powder, 1200mL deionized waters and 2.4g polyvinyl alcohol are placed in ball mill, are added Zirconia ball and ratio of grinding media to material are 4:1, the ball milling 2.5h under 250r/min, obtain well mixed slurry；By well mixed slurry Material, which is transferred in spray drying granulation tower, carries out agglomeration granulation, and it is 20 μm~70 μm spherical Y to obtain particle diameter2SiO5Agglomeration granulation powder Body；
Wherein, spray drying granulation parameter is：320 DEG C of inlet temperature, 100 DEG C of outlet temperature, rotating speed of shower nozzle 40Hz is wriggled Revolution speed 35rpm；
(2) by the Y of gained2SiO5Agglomeration granulation powder is placed in non-pressure sintering furnace, and 3h is calcined at 1100 DEG C, is obtained Y2SiO5Spraying powder；
(3) first using acetone to SiCf/ SiC matrix carries out purified treatment, removes the greasy dirt of matrix surface and other pollutions Thing with obtain cleaning matrix surface；Recycle jet absorption type sand-blasting machine to carry out blasting treatment to clean matrix surface, make to be painted The roughness (Rz) for applying matrix surface reaches 30 μm；
(4) air plasma spraying technique is used by Y2SiO5Spraying powder sprays to SiCfIn/SiC matrix；Again will spraying Y2SiO5SiC afterwardsf/ SiC matrix is placed under argon atmosphere, and is incubated 2h at 1400 DEG C, cooling, in SiCf/ SiC bases Thickness is obtained on body and obtains Y for 180 μm2SiO5Environmental Barrier Coatings on Si-based Ceramics；
Wherein, air plasma spraying technological parameter is：Main gas (argon gas)：85L/min, auxiliary gas (helium)：28L/min, Carrier gas (argon gas)：12L/min, electric current：800A, feeding speed：2.8g/min, spray distance：80mm；
Fig. 3 schemes for the SEM on prepared Environmental Barrier Coatings on Si-based Ceramics surface, as can be seen from the figure prepared Environmental Barrier Coatings on Si-based Ceramics table Face is more smooth, most of Y2SiO5Powder granule is completely melt and drawout, shows smooth shape characteristic, and in coating The comparatively dense molten condition in portion is good.It is known that prepared Environmental Barrier Coatings on Si-based Ceramics principal phase is from the XRD spectrum in Fig. 4 Y2SiO5, there is a small amount of Y2O3And Y4.67(SiO4)3O is present.
By obtained Y2SiO5Environmental Barrier Coatings on Si-based Ceramics carries out grind away polishing, then amplifies 200 times in light microscope and lower is seen Examine, 3 regions are randomly selected in the visual field observed and are analyzed, quantitatively calculate prepared using quantitative Image Analysing system for Metallography Environmental Barrier Coatings on Si-based Ceramics porosity, test result refers to table 2；Prepared coating structure consistency is very high, and average density is 99.43%.
Table 2
In summary, presently preferred embodiments of the present invention is these are only, is not intended to limit the scope of the present invention. Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., should be included in the present invention's Within protection domain.

Claims (10)

1. a kind of silicate Environmental Barrier Coatings on Si-based Ceramics, it is characterised in that：The composition of the Environmental Barrier Coatings on Si-based Ceramics is AxSiOy, and with SiCf/ SiC is matrix；
Wherein, when A is Y, Er, Yb or Lu, x=2, y=5；When A is Zr, Ti or Hf, x=1, y=4.
2. a kind of silicate Environmental Barrier Coatings on Si-based Ceramics according to claim 1, it is characterised in that：The thickness of the Environmental Barrier Coatings on Si-based Ceramics For 150 μm~250 μm.
3. a kind of preparation method of silicate Environmental Barrier Coatings on Si-based Ceramics as claimed in claim 1 or 2, it is characterised in that：It is described to prepare Method and step is as follows：
Step 1. is by AxSiOyPowder, water, binding agent and ball milling pearl are added in ball mill and mixed, and are well mixed Slurry；Slurry is transferred in spray drying granulation tower again and carries out agglomeration granulation, it is 20 μm~80 μm spherical groups to obtain particle diameter Poly- granulation powder；
The spherical agglomerated powder of gained is placed in non-pressure sintering furnace and carries out calcination processing by step 2., obtains AxSiOySpraying powder；
Step 3. is to SiCf/ SiC matrix is cleaned and roughening processing, the roughness on surface to be sprayed is reached 25 μm~100 μm；
Step 4. uses air plasma spraying technique by AxSiOySpraying powder sprays to SiCfIn/SiC matrix, then will spraying AxSiOySiC afterwardsf/ SiC matrix is placed under argon atmosphere and is heat-treated, cooling, in SiCfInstitute is obtained in/SiC matrix State Environmental Barrier Coatings on Si-based Ceramics；
Wherein, air plasma spraying technological parameter is：Spray distance 70mm~80mm, electric current 800A~900A, primary air amount 80L/min~100L/min, auxiliary throughput 25L/min~35L/min, carrier gas flux 8L/min~15L/min, powder sending quantity 2rpm ~4rpm；Main gas and carrier gas are argon gas, and auxiliary gas is helium.
4. a kind of preparation method of silicate Environmental Barrier Coatings on Si-based Ceramics according to claim 3, it is characterised in that：In step 1, glue Tie the quality and A of agentxSiOyThe mass ratio of powder is 0.003~0.005:1, the quality and A of waterxSiOyThe mass ratio of powder is 1 ~3:1, the quality and A of ball milling pearlxSiOyThe mass ratio of powder is 3~5:1.
5. a kind of preparation method of silicate Environmental Barrier Coatings on Si-based Ceramics according to claim 3, it is characterised in that：In step 1, Ball milling mixing 2h~3h under 200r/min~300r/min.
6. a kind of preparation method of silicate Environmental Barrier Coatings on Si-based Ceramics according to claim 3, it is characterised in that：In step 1, The parameter setting of agglomeration granulation is carried out in spray drying granulation tower：280 DEG C~350 DEG C of inlet temperature, 100 DEG C of outlet temperature~ 130 DEG C, rotating speed of shower nozzle 35Hz~50Hz, wriggling revolution speed 30rpm~40rpm.
7. a kind of preparation method of silicate Environmental Barrier Coatings on Si-based Ceramics according to claim 3, it is characterised in that：In step 2, Calcination processing 2h~3h at 1100 DEG C~1400 DEG C.
8. a kind of preparation method of silicate Environmental Barrier Coatings on Si-based Ceramics according to claim 3, it is characterised in that：In step 4, 2h~4h is heat-treated at 1300 DEG C~1400 DEG C.
9. a kind of preparation method of silicate Environmental Barrier Coatings on Si-based Ceramics according to claim 4, it is characterised in that：In step 1, institute Binding agent is stated for polyvinyl alcohol.
10. a kind of preparation method of silicate Environmental Barrier Coatings on Si-based Ceramics according to claim 4, it is characterised in that：The ball milling The material of pearl is zirconium oxide.
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CN108373342A (en) * 2018-03-19 2018-08-07 广东省新材料研究所 A kind of composite construction Environmental Barrier Coatings on Si-based Ceramics and the preparation method and application thereof, aero-engine
CN109837496A (en) * 2017-11-27 2019-06-04 深圳航发复合材料有限公司 A kind of preparation method of ytterbium silicate plasma spraying powder
CN111978087A (en) * 2019-05-22 2020-11-24 北京理工大学 Composite material and preparation method and application thereof
CN112779534A (en) * 2020-07-20 2021-05-11 绍兴科霆新材料有限公司 Anticorrosive coating for aluminum alloy casting mold and preparation process thereof
CN113860920A (en) * 2021-09-13 2021-12-31 中国科学院金属研究所 Environmental barrier coating with excellent CMAS corrosion resistance and preparation method thereof
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CN114920559A (en) * 2022-06-07 2022-08-19 西北工业大学 High-entropy oxide powder material for thermal barrier coating and preparation method and application thereof

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CN107880590A (en) * 2017-10-27 2018-04-06 北京理工大学 A kind of composite granule of coated with silica zirconium diboride carborundum
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CN112779534A (en) * 2020-07-20 2021-05-11 绍兴科霆新材料有限公司 Anticorrosive coating for aluminum alloy casting mold and preparation process thereof
CN113860920A (en) * 2021-09-13 2021-12-31 中国科学院金属研究所 Environmental barrier coating with excellent CMAS corrosion resistance and preparation method thereof
CN113860920B (en) * 2021-09-13 2023-02-17 中国科学院金属研究所 Environmental barrier coating with excellent CMAS corrosion resistance and preparation method thereof
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
CN114920559A (en) * 2022-06-07 2022-08-19 西北工业大学 High-entropy oxide powder material for thermal barrier coating and preparation method and application thereof

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