CN108220902A - The Al on gamma-TiAl alloy surface2O3-Y2O3/ Al-Y compound protective coatings and preparation method thereof - Google Patents

The Al on gamma-TiAl alloy surface2O3-Y2O3/ Al-Y compound protective coatings and preparation method thereof Download PDF

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CN108220902A
CN108220902A CN201810127905.3A CN201810127905A CN108220902A CN 108220902 A CN108220902 A CN 108220902A CN 201810127905 A CN201810127905 A CN 201810127905A CN 108220902 A CN108220902 A CN 108220902A
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coating
composite coatings
gamma
preparation
tial alloy
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梁文萍
李姗
缪强
丁铮
王旭
林浩
易锦伟
安浩
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

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  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
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Abstract

The present invention relates to a kind of Al on γ TiAl alloys surface2O3‑Y2O3/ Al Y compound protective coatings and preparation method thereof.The composite coating from outward appearance to inner essence includes Al successively2O3‑Y2O3Ceramic layer, Al Y metal layers and Al Y diffusion layers.Preparation method：Al Y coating is prepared on γ TiAl alloys surface using magnetron sputtering method first, Al is then prepared in Al Y coating surfaces using Magnetron reactive sputtering2O3‑Y2O3Coating finally carries out diffusion in vacuum annealing, improves the binding force between coating and matrix.The present invention is in ceramic layer and matrix medium design metal layer, and rare earth element y is added in composite coating, alleviate the stress between coating, improve high temperature oxidation resistance, the high temperature oxidation resistance of γ TiAl alloys is finally improved, and then effectively improves and force difference is combined between conventional composite coating, the defects of high temperature oxidation resistance is insufficient.

Description

The Al on gamma-TiAl alloy surface2O3-Y2O3/ Al-Y compound protective coatings and its preparation Method
Technical field
The present invention relates to technical field of metal material surface modification, and in particular to a kind of gamma-TiAl alloy surface Al2O3-Y2O3/ Al-Y compound protective coatings and preparation method thereof.
Background technology
The performance of aero-engine has an high regard for when service life and has the contact of direct certainty to the use of space shuttle, because It is and of crucial importance to the selection of material.The service condition of materials for aeroengines is made a general survey of, nickel base superalloy occupies major portion, However, as its is expensive, temperature in use is limited etc., self shortcomings are gradually substituted.The hyperbaric aero-engine of a new generation The design of the structural members such as the blade, disk, casing, the rotor that use in the high temperature environment plays crucial effect.Between Ti-Al systems metal Compound has high specific strength, specific modulus, creep resistance and excellent high temperature as a kind of novel light high-temperature structural material The performances such as intensity, rigidity, make its be expected to substitute Ni-based or iron-base superalloy become contemporary aerospace industry, weapon industry with And one of structural material in fields such as civilian industry, there is important engineering application potential.
Gamma-TiAl alloy is typical non-stoichiometric type, has stable L below fusing point10Type face-centered tetragonal structure.In object In terms of managing characteristic, with other Ti alloys, Ti3Al is compared, and gamma-TiAl alloy fusing point is up to 1460 DEG C, and density is relatively low, and only 3.7 ~3.9g/cm3, the various aspects such as elasticity modulus, the creep resistant limit are respectively provided with advantage.Compared with nickel base superalloy, density is only It is its half, but other various aspects of performance are closely similar.Due to the presence of chemical element in alloy, α2Mutually account for about 2%~20%, Remaining is γ phases, so as to which alloy be made to have high mechanical strength.There is this advantage just because of gamma-TiAl alloy, compensate for Ti Based alloy and nickel base superalloy are applying upper limited deficiency, therefore be considered as the potential stocks of aerospace field, especially It is to bring Gospel for aero-engine field.
However, when ambient temperature is more than 700 DEG C, the great decline of antioxygenic property of gamma-TiAl alloy.Mainly due to Ectonexine forms respectively the TiO of short texture2Layer and TiO2+Al2O3Mixture, alloy surface is most difficult to be formed at last The oxide protective barrier of the Al of even densification.Oxidation film main component is the Ti oxides and Al of different valence state2O3.Al oxides Formation speed well below Ti oxides formation speed.This characteristic may finally lead to two kinds as a result, one is to be formed newly Ti oxide channels generate Al simultaneously2O3+TiO2Mixture；Second is that form Al in internal layer2O3+TiO2Mixture.With this Meanwhile the boundary of oxide layer and matrix alloy is Al layers and one layer dissolved a large amount of O poor Al layers of one layer of richness, i.e., in metallic matrix With the depletion layer that Al is formed at the combination interface of oxide.The zone of influence that such case will result in one layer of O, the zone of influence one As matter it is crisp, make mechanical properties decrease, eventually lead to coating failure.
Traditional technique is difficult to meet the requirement of modern technologies, and surface engineering technology becomes improves resistance to high temperature oxidation in recent years One of method, cause the concern of more and more people.Surface Engineering be lost it is low, easy to operate, using it is wide the advantages that it is wide General application so that Surface Engineering industrialization is rapidly developed in Aeronautics and Astronautics, new energy, new material.With plasma The development of surface metallurgical technology, to developing densification, anti-strip, heat safe protective coating propose the requirement of higher standard.
Invention content
For the defects in the prior art, the present invention is intended to provide a kind of Al on gamma-TiAl alloy surface2O3-Y2O3/ Al-Y compound protective coatings and preparation method thereof.The present invention is in ceramic layer and matrix medium design metal layer, and in compound painting Rare earth element y is added in layer, alleviates the stress between coating, improve high temperature oxidation resistance, finally improve γ-TiAl conjunctions The high temperature oxidation resistance of gold, and then effectively improve that force difference, high temperature oxidation resistance are combined between conventional composite coating is insufficient The defects of.
To achieve the above object, technical solution provided by the invention is：
In a first aspect, the present invention provides a kind of Al2O3-Y2O3/ Al-Y composite coatings, Al2O3-Y2O3The compound paintings of/Al-Y Layer is to be prepared in alloy surface, and Al2O3-Y2O3/ Al-Y composite coatings are from outward appearance to inner essence made of three parts, are followed successively by Al2O3-Y2O3Coating, Al-Y metal layers and Al-Y diffusion layers.
Preferably, Al2O3-Y2O3In coating, the atomic ratio of Al, Y and O are followed successively by (25~40)：(5~10)：(55~ 70)；In Al-Y metal layers, the atomic ratio of Al and Y are (60~75)：(25~35)；Al-Y diffusion layers and alloy surface fitting, and In Al-Y diffusion layers, the atomic ratio of Al, Y and Ti are followed successively by (35~55)：(10~25)：(15~35).
Preferably, Al2O3-Y2O3The thickness of coating is 5~10 μm, and the thickness of Al-Y metal layers is 15~20 μm, Al-Y The thickness of diffusion layer is 8~15 μm.
Preferably, alloy is titanium-aluminium alloy, and titanium-aluminium alloy is preferably gamma-TiAl alloy.
Second aspect, the present invention provide a kind of Al2O3-Y2O3The preparation method of/Al-Y composite coatings, includes the following steps： S101：Using gamma-TiAl alloy as matrix, Al-Y coating is prepared on gamma-TiAl alloy surface using magnetron sputtering method；S102： Al-Y coating surfaces prepare Al using Magnetron reactive sputtering2O3-Y2O3Coating；S103：The product that S102 is obtained is moved back Fire processing, Al is obtained on gamma-TiAl alloy surface2O3-Y2O3/ Al-Y composite coatings.
Preferably, in S101, the condition of magnetron sputtering method specifically includes：Al-Y targets are selected, the purity of Al-Y targets is big In or equal to 99.9%, Al and Y mass ratio be 7:3；The interpolar of Al-Y targets and matrix γ-TiAl alloy surfaces away from for 20~25mm, sputtering power are 180~230W, and operating air pressure is 3~4Pa, and soaking time is 3~3.5h, and protective gas is argon Gas.
Preferably, in S102, the condition of magnetron sputtering method specifically includes：Al-Y targets are selected, the purity of Al-Y targets is big In or equal to 99.9%, Al and Y mass ratio be 97:3；The interpolar of Al-Y targets and matrix γ-TiAl alloy surfaces away from for 15~20mm, sputtering power are 280~330W, and soaking time is 4~4.5h, and protective gas is oxygen and/or argon gas, and argon gas Flow-rate ratio with oxygen is preferably (5~10)：1.
Preferably, in S103, annealing specifically includes：The product that S102 is obtained is put into tube furnace, is vacuumized, it It is 800~900 DEG C to adjust temperature afterwards, and anneal 15~16h, closes argon gas, furnace cooling later.
Preferably, in annealing, selection argon gas is working gas.
The present invention has obtained the subsidy of project of national nature science fund project (fund project code name is 51474131).
Technical solution provided by the invention has following advantageous effect：
(1) present invention is in ceramic layer and matrix medium design metal layer, and rare earth element is added in composite coating Y alleviates the stress between coating, improves high temperature oxidation resistance, finally improves the high temperature oxidation resistance of gamma-TiAl alloy Can, and then effectively improve and force difference is combined between conventional composite coating, the defects of high temperature oxidation resistance is insufficient.
(2) Al prepared using Magnetron reactive sputtering of the present invention2O3-Y2O3Coating surface is fine and close, without apparent hole In metallurgical binding between crackle, with Al-Y coating, bond strength is high, and then obtains the high temperature protection ability of γ-TiAl alloys To raising.
(3) the Al-Y metal layer distribution gradients on the present invention time surface layer not only increase the cementability of matrix and ceramic layer, And when high-temperature oxydation has been replenished in time Al elements it is barren.
(4) Al of the present invention2O3-Y2O3The multilayered structure of/Al-Y reduces the internal stress between ceramic layer and metal layer, disappears In addition to the interface of layer structure significantly between layers, make mechanical property between them and linear expansion coefficient continuously excessive.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description It obtains significantly or is recognized by the practice of the present invention.
Description of the drawings
Fig. 1 is the Al being prepared in the embodiment of the present invention2O3-Y2O3/ Al-Y composite coating surface topography maps；
Fig. 2 is the Al being prepared in the embodiment of the present invention2O3-Y2O3/ Al-Y composite coating Cross Section Morphology figures；
Fig. 3 is the Al being prepared in the embodiment of the present invention2O3-Y2O3/ Al-Y composite coating surface scratch shape appearance figures；
Fig. 4 is the Al being prepared in the embodiment of the present invention2O3-Y2O3/ Al-Y composite coating surface scratch sound emission curves Figure；
Fig. 5 is the Al being prepared in the embodiment of the present invention2O3-Y2O3The thermal shock at different temperatures of/Al-Y composite coatings Oxidation weight gain kinetic curve；
Fig. 6 is the Al being prepared in the embodiment of the present invention2O3-Y2O3750 DEG C of cyclic oxidation 100h of/Al-Y composite coatings Cross Section Morphology figure afterwards；
Fig. 7 is the Al being prepared in the embodiment of the present invention2O3-Y2O3850 DEG C of cyclic oxidation 100h of/Al-Y composite coatings Cross Section Morphology figure afterwards；
Fig. 8 is the Al being prepared in the embodiment of the present invention2O3-Y2O3950 DEG C of cyclic oxidation 100h of/Al-Y composite coatings Cross Section Morphology figure afterwards.
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete Site preparation describes.The following examples are only intended to illustrate the technical solution of the present invention more clearly, therefore is intended only as example, without It can be limited the scope of the invention with this.
Experimental method in following embodiments is conventional method unless otherwise specified.Examination used in following embodiments Material is tested, is to be commercially available from regular shops unless otherwise specified.Quantitative test in following embodiment, is respectively provided with three Secondary to repeat to test, data are the average value or mean+SD of three repeated experiments.
The present invention provides a kind of Al2O3-Y2O3/ Al-Y composite coatings, Al2O3-Y2O3/ Al-Y composite coatings are in alloy table Face is prepared, Al2O3-Y2O3/ Al-Y composite coatings are from outward appearance to inner essence made of three parts, are followed successively by Al2O3-Y2O3Coating, Al-Y Metal layer and Al-Y diffusion layers, and Al2O3-Y2O3The thickness of coating is 5~10 μm, and the thickness of Al-Y metal layers is 15~20 μ The thickness of m, Al-Y diffusion layer is 8~15 μm.Wherein, Al2O3-Y2O3In coating, the atomic ratio of Al, Y and O be followed successively by (25~ 40)：(5~10)：(55~70)；In Al-Y metal layers, the atomic ratio of Al and Y are (60~75)：(25~35)；Al-Y is spread Layer and alloy surface fitting, and in Al-Y diffusion layers, the atomic ratio of Al, Y and Ti are followed successively by (35~55)：(10~25)： (15 ~35).With atomic percentage, Al2O3-Y2O3In Coating composition, Al accounts for 25~40at.%, and Y accounts for 5~10at.%, and O accounts for 55 ~70at.%；In Al-Y metal composition of layer, Al accounts for 60~75at.%, and Y accounts for 25~35 at.%；In Al-Y diffusion composition of layer, Al accounts for 35~55at.%, and Y accounts for 10~25at.%, and Ti accounts for 15~35at.%.In addition, the alloy of the present invention is titanium-aluminium alloy, and Titanium-aluminium alloy is preferably gamma-TiAl alloy.
In addition, the Al for the present invention2O3-Y2O3/ Al-Y composite coatings, the present invention specially provide preparation method, including Following steps：
S101：Using gamma-TiAl alloy as matrix, Al-Y platings are prepared on gamma-TiAl alloy surface using magnetron sputtering method Layer；Wherein, which specifically includes Al-Y metal layers and Al-Y diffusion layers, and Al-Y diffusion layers are closed with matrix γ-TiAl Gold is bonded to each other；S102：In Al-Y coating surfaces, Al is prepared using Magnetron reactive sputtering2O3-Y2O3Coating；S103：It will The product that S102 is obtained is made annealing treatment, and Al is obtained in γ-TiAl alloy surfaces2O3-Y2O3/ Al-Y composite coatings.
Specific experiment operating procedure is as follows：
(1) by matrix gamma-TiAl alloy, Al-Y targets are put into magnetron sputtering apparatus stove.Wherein, target material composition is：Al、 The mass ratio of Y is 7:3, purity 99.9%.
(2) 10 are evacuated to-4Pa is passed through argon gas, reaches starter level, testing and measuring technology parameter：
The interpolar of target and matrix surface away from：20~25mm
Sputtering power：180~230W
Operating air pressure：3~4Pa
Soaking time：3~3.5h
(3) power is reduced to zero, closes argon gas, is evacuated to 10-4Pa closes power supply.Room temperature is cooled to the furnace, so as to obtain Al-Y metal layers.
(4) target is removed, changes another piece of Al-Y target, mass ratio 97:3, purity 99.9%.It is evacuated to 10-4Pa is passed through argon gas starter.Testing and measuring technology parameter is：
The interpolar of target and matrix surface away from：15~20mm
Sputtering power：280~330W
The flow-rate ratio of argon gas and oxygen：(5~10)：1
Soaking time：4~4.5h
(5) power is reduced to zero, closes argon gas, oxygen, is evacuated to 10-4Pa closes power supply.Cool to room temperature with the furnace, from And obtain Al2O3-Y2O3Coating.
(6) the coating sample prepared is put into tube furnace, vacuumized, testing and measuring technology parameter is：Diffusion temperature：800 ~900 DEG C, diffusion time：15~16h, work atmosphere：Argon gas.Argon gas is closed, closes power supply, Al is completed in furnace cooling2O3- Y2O3The preparation of/Al-Y composite coatings.
It is described further with reference to specific embodiment.
Embodiment one
The present embodiment provides a kind of Al on gamma-TiAl alloy surface2O3-Y2O3The preparation side of/Al-Y compound protective coatings Method includes the following steps：
(1) gamma-TiAl alloy is cut into the cuboid of 10mm × 10mm × 1mm sizes, is polished step by step sample with sand paper, It is cleaned by ultrasonic 5~8min, is dried for standby.
(2) device Al-Y targets 1, wherein 1 ingredient of target are：The mass ratio of Al, Y are 7:3, purity 99.9%.Dress Ultrasonic cleaning, drying are carried out before putting to target.
(3) sample gamma-TiAl alloy is placed on objective table, the distance of control target to specimen surface is 20mm；Most Furnace interior is wiped with vacuum paper afterwards, falls equipment bell jar.
(4) it opens mechanical pump and is evacuated to 0.1Pa, be then turned on molecular pump and be evacuated to 10-4Pa；Argon gas is filled with, is adjusted Air pressure in stove, starter；Voltage is adjusted, guarantee power is 200W；It adjusts argon flow amount and ensures that operating air pressure is in 4Pa in furnace body；It protects Warm time 3h.Argon gas is closed, cuts off the power, cools to room temperature with the furnace, the system of Al-Y metal layers is completed on gamma-TiAl alloy surface It is standby.
(5) it opens bell jar and takes out target 1, device Al-Y targets 2, wherein 2 ingredient of target is：The mass ratio of Al, Y is 97:3, purity 99.9%.Debug the interpolar of target and matrix surface away from：15mm carries out ultrasonic cleaning before device to target, Drying.Bell jar is closed, vacuumizes, is passed through argon gas, starter.Oxygen is passed through, the flow-rate ratio for debugging argon gas and oxygen is 10:1, sputtering Power is 300W, soaking time 4h.Argon gas and oxygen are closed, cuts off the power, cools to room temperature with the furnace, in Al-Y metal layer tables Complete Al in face2O3-Y2O3The preparation of coating.
Wherein, Fig. 1 is the Al that the present embodiment is prepared2O3-Y2O3/ Al-Y composite coating surface topography maps；It can by figure Know：Coating surface is fine and close, without apparent hole and crackle, the basic glomeration growth mechanism of atom.Fig. 2 is prepared into for the present embodiment The Al arrived2O3-Y2O3/ Al-Y composite coating Cross Section Morphology figures；As seen from the figure：The Al2O3-Y2O3/ Al-Y composite coatings are from outward appearance to inner essence Respectively：Outermost layer Al2O3-Y2O3Coating, thickness are about 7 μm；Middle layer is Al-Y coatings (i.e. Al-Y metal layers), and thickness is about It is 20 μm；Innermost layer is diffusion layer, and thickness is about 8 μm, Al2O3-Y2O3Totally 35 μm of/Al-Y composite coatings；And mating surface pattern Understand that coating is fine and close, without apparent crackle, hole.
(1) power test is combined to the composite coating that the present embodiment is prepared, specific method is as follows：
Test equipment：The WS-2005 scratching instruments of Lanzhou Chemical Physics research institute production；
Concrete operation method is as follows：The Al prepared2O3-Y2O3/ Al-Y composite coatings sample is placed on objective table, if Put initial load 0.05N, final load 100N, loading velocity 30N/min, the lateral critical speeds of pressure head is 2mm/min, cut Length is 8mm.
Experimental result is as shown in Figure 3；As seen from the figure：With the increase of load, Al2O3-Y2O3/ Al-Y composite coatings are drawn Trace width is also continuously increased, and the irregular peeling in part occurs in part, and in end, coating breaks down peels off, entire coating failure.It draws It is not cracked and empty around trace, illustrate that coating has certain toughness, and is well combined with matrix.
As shown in Figure 4：When critical load reaches 58.7N, start acoustic signals occur, signal is steady, and intensity is not high, explanation Coating also has preferable plastic deformation at this time, stronger acoustic signals then occurs, coating starts to peel off.
(2) thermal shock resistance for the composite coating that the present embodiment is prepared is tested, and specific method is as follows：
Test equipment：High temperature Muffle furnace
Concrete operation method is as follows：
The Al that will be prepared2O3-Y2O3/ Al-Y composite coatings are put into high temperature Muffle furnace and are tested, and set warm in stove Degree, soaking time 10min then take out to be put into 20 DEG C of water and are cooled down, naturally dry after taking-up, this is a week Phase.Observe the degree of the disbonding of specimen surface, if whether the peeling area for apparent macroscopic cracking and coating occur reaches 5%, if carrying out next cycle cycle without if；If so, terminate experiment.
Experimental result is as shown in figure 5, the Al being prepared for the present embodiment2O3-Y2O3/ Al-Y composite coatings are in not equality of temperature The oxidation weight gain kinetic curve of the lower thermal shock of degree.As seen from the figure：Composite coating does not occur weightlessness at 750 DEG C after thermal shock； 850 DEG C and 950 DEG C early period oxidation weight gain linearly increase the later stage occur it is weightless.At 1050 DEG C thermal shock oxidation weight gain early period compared with Soon, then linear to reduce, later stage weightening and weightlessness are alternately present, and are illustrated that coating constantly peels off at this time, aoxidize, are peeled off again repeatedly It carries out, leads to coating failure.
(3) high temperature oxidation resistance for the composite coating that the present embodiment is prepared is tested, and specific method is such as Under：
Test equipment：High temperature Muffle furnace
Concrete operation method is as follows：By Al2O3-Y2O3/ Al-Y composite coatings are mounted in different crucibles and put Muffle into together Stove keeps the temperature 100h at 750 DEG C, 850 DEG C and 950 DEG C, measures the relationship of its oxidation weight gain and time.Every 10h furnace coolings Taking-up sample, which is weighed, places into heating and thermal insulation in Muffle furnace, this is a cycle.Until coating failure, terminates experiment.
Experimental result is as shown in Fig. 6, Fig. 7 and Fig. 8, Al that respectively the present embodiment is prepared2O3-Y2O3/ Al-Y is multiple Close the Cross Section Morphology figure after 750 DEG C, 850 DEG C and 950 DEG C cyclic oxidation 100h of coating.Coating is fine and close at 750,850 DEG C, with base Body is combined preferably without apparent cavity and crackle.In Al2O3-Y2O3There is pleated structure between coating and Al-Y metal layers, Mainly due to Y2O3Pinning effect, alleviate between coating due to coating warpage caused by coefficient of thermal expansion difference, peel off. Y2O3Pinning effect prevent well O elements inside diffusion and Ti elements to external diffusion, the Al elements in Al-Y layers Protectiveness Al has been replenished in time2O3Al elements needed for film.At 950 DEG C, between each layer combine relatively preferably, but diffusion layer with Occurs tiny crackle between matrix.This is because Ti elements, to external diffusion, O elements are inwardly spread, TiO is formed2.More than Embody the preferable high temperature protection power of coating.
Embodiment two
The present embodiment changes the interpolar of matrix and target away from for 18mm, the stream of argon gas and oxygen in reactive magnetron sputtering Amount is than being 5:1, sputtering power 280W, soaking time 3.5h, other steps and parameter are same
Embodiment one.
For the composite coating that the present embodiment is prepared, using scarification, gradually increase load, when being loaded onto 55.6N When, there are acoustic signals, show that rupture occurs in coating at this time.Acoustic signals are slower later, after plus load is more than 72N, Signal becomes intensive, illustrate at this time coating occur peel off, until external load reach matrix, it is known that coating combined with matrix compared with It is good.In addition, the high-temperature oxydation experiment at 750 DEG C, 850 DEG C and 950 DEG C shows：Coating does not occur apparent in 100h rear surfaces Peeling, combined with matrix preferably, increasing weight of oxidation is compared with the further reduction in embodiment one.In summary, the present embodiment system Standby obtained Al2O3-Y2O3/ Al-Y composite coating antioxygen properties are good.
The present invention is added to rare earth element y in ceramic layer and matrix medium design metal layer in composite coating, delays Stress, raising high temperature oxidation resistance between electrolytic coating finally improve the high temperature oxidation resistance of gamma-TiAl alloy, into And it effectively improves and force difference is combined between conventional composite coating, the defects of high temperature oxidation resistance is insufficient.
It should be noted that unless otherwise indicated, technical term or scientific terminology used in this application should be this hair The ordinary meaning that bright one of ordinary skill in the art are understood.Unless specifically stated otherwise, it otherwise illustrates in these embodiments Component and opposite step, numerical expression and the numerical value of step are not limit the scope of the invention.It is illustrated and described herein In all examples, unless otherwise prescribed, any occurrence should be construed as merely illustrative, not as limitation, because This, other examples of exemplary embodiment can have different values.
In the description of the present invention, it is to be understood that term " first ", " second " are only used for description purpose, and cannot It is interpreted as indicating or implies relative importance or imply the quantity of the technical characteristic indicated by indicating.Define as a result, " the One ", one or more this feature can be expressed or be implicitly included to the feature of " second ".In the description of the present invention, " multiple " are meant that two or more, unless otherwise specifically defined.
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent Pipe is described in detail the present invention with reference to foregoing embodiments, it will be understood by those of ordinary skill in the art that：Its according to Can so modify to the technical solution recorded in foregoing embodiments either to which part or all technical features into Row equivalent replacement；And these modifications or replacement, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution The range of scheme should all cover in protection scope of the present invention.

Claims (9)

1. a kind of Al2O3-Y2O3/ Al-Y composite coatings, it is characterised in that：
The Al2O3-Y2O3/ Al-Y composite coatings are prepared in alloy surface, and the Al2O3-Y2O3The compound paintings of/Al-Y Layer includes successively：Al2O3-Y2O3Coating, Al-Y metal layers and Al-Y diffusion layers.
2. Al according to claim 12O3-Y2O3/ Al-Y composite coatings, it is characterised in that：
The Al2O3-Y2O3In coating, the atomic ratio of Al, Y and O are followed successively by (25~40)：(5~10)：(55~70)；The Al- In Y metal layers, the atomic ratio of Al and Y are (60~75)：(25~35)；The Al-Y diffusion layers and alloy surface fitting, And in the Al-Y diffusion layers, the atomic ratio of Al, Y and Ti are followed successively by (35~55)：(10~25)：(15~35).
3. Al according to claim 12O3-Y2O3/ Al-Y composite coatings, it is characterised in that：
The Al2O3-Y2O3The thickness of coating is 5~10 μm, and the thickness of the Al-Y metal layers is 15~20 μm, and the Al-Y expands The thickness for dissipating layer is 8~15 μm.
4. according to claims 1 to 3 any one of them Al2O3-Y2O3/ Al-Y composite coatings, it is characterised in that：
The alloy is titanium-aluminium alloy, and the titanium-aluminium alloy is preferably gamma-TiAl alloy.
5. according to Claims 1 to 4 any one of them Al2O3-Y2O3The preparation method of/Al-Y composite coatings, which is characterized in that Include the following steps：
S101：Using gamma-TiAl alloy as matrix, Al-Y coating is prepared on the gamma-TiAl alloy surface using magnetron sputtering method；
S102：In the Al-Y coating surfaces, Al is prepared using Magnetron reactive sputtering2O3-Y2O3Coating；
S103：The obtained products of the S102 are made annealing treatment, Al is obtained on the gamma-TiAl alloy surface2O3-Y2O3/ Al-Y composite coatings.
6. Al according to claim 52O3-Y2O3The preparation method of/Al-Y composite coatings, it is characterised in that：
In the S101, the condition of magnetron sputtering method specifically includes：
Al-Y targets are selected, mass ratio of the purity more than or equal to 99.9%, Al and Y of Al-Y targets is 7:3；Al-Y targets With the interpolar on described matrix gamma-TiAl alloy surface away from for 20~25mm, sputtering power is 180~230W, operating air pressure for 3~ 4Pa, soaking time are 3~3.5h, and protective gas is argon gas.
7. Al according to claim 52O3-Y2O3The preparation method of/Al-Y composite coatings, it is characterised in that：
In the S102, the condition of magnetron sputtering method specifically includes：
Al-Y targets are selected, mass ratio of the purity more than or equal to 99.9%, Al and Y of Al-Y targets is 97:3；Al-Y targets The interpolar on material and described matrix gamma-TiAl alloy surface is away from for 15~20mm, and sputtering power is 280~330W, soaking time 4 ~4.5h, protective gas is oxygen and/or argon gas, and the flow-rate ratio of argon gas and oxygen is preferably (5~10)：1.
8. Al according to claim 52O3-Y2O3The preparation method of/Al-Y composite coatings, it is characterised in that：
In the S103, the annealing specifically includes：
The obtained products of the S102 are put into tube furnace, are vacuumized, it is 800~900 DEG C to adjust temperature later, annealing 15~ 16h closes argon gas, furnace cooling later.
9. Al according to claim 82O3-Y2O3The preparation method of/Al-Y composite coatings, it is characterised in that：
In the annealing, selection argon gas is working gas.
CN201810127905.3A 2018-02-08 2018-02-08 The Al on gamma-TiAl alloy surface2O3-Y2O3/ Al-Y compound protective coatings and preparation method thereof Pending CN108220902A (en)

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Application publication date: 20180629