CN101310971B - Ni-base superalloy complex gradient coating and preparation technique thereof - Google Patents
Ni-base superalloy complex gradient coating and preparation technique thereof Download PDFInfo
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- CN101310971B CN101310971B CN2007100114318A CN200710011431A CN101310971B CN 101310971 B CN101310971 B CN 101310971B CN 2007100114318 A CN2007100114318 A CN 2007100114318A CN 200710011431 A CN200710011431 A CN 200710011431A CN 101310971 B CN101310971 B CN 101310971B
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Abstract
The invention mainly relates to the coating technique, in particular to a gradient MCrAlY coating used for protecting high-temperature alloy and a preparation method thereof. The invention prepares an MCrAlY composite gradient coating by adopting the method combining the arc ion plating (AIP) and the diffusion aluminizing. The thickness of an aluminum-rich layer on the surface of the MCrAlY composite coating can be controlled by setting the aluminizing temperature and the period of heat preservation and the Al elements are distributed in a gradient way along the depth direction; in addition, the chemical vapor deposition method used for the aluminizing has the advantages of good uniformity on the aluminum-rich layer and being not affected by the size and shape of a sample. Since the method of direct diffusion is adopted without introducing a weak interface, the MCrAlY high-temperature protective coating can increase the content of Al memory phase to the utmost extent under the condition that the mechanical property of the coating is guaranteed, so as to improve the high-temperature oxidization resistance and the heat corrosion resistance of the coating, and can effectively prolong the service life of the coating. The MCrAlY composite gradient coating and the preparation method of the invention can be applied to the protection of Ni-based and Co-based high-temperature alloys.
Description
Technical field
The present invention relates to the high-temperature protection coating technology, specifically a kind of MCrAlY adds complex gradient high-temperature protection coating and preparation method.
Background technology
As a kind of MCrAlY (M=Ni with good resistance oxidation, hot corrosion resistance; Co or Ni+Co) coating; Be widely used in the protection of heat-resistant parts such as aero-engine, gas turbine blades; It both can use separately, also can be used as adhesive linkage (bond coat) and surface ceramic layer (like Y
2O
3Partially stabilized ZrO
2) constitute thermal barrier coating (TBCs, i.e. thermal barrier coatings) system together, improve resistance to high temperature oxidation, the hot corrosion resistance of parts, prolong the service life of parts.The document of related application is like 1. Chinese invention patent, and a kind of detonation flame spraying prepares the method for thermal barrier coating, application number 01133423.1; 2. Chinese invention patent, a kind of oxidation-inhibited thermal barrier coating and preparation method, application number 02133193.6; 3. Chinese invention patent, a kind of preparation method of heat shock resistance thermal barrier coating, application number 03133344.3; 4. Chinese invention patent, a kind of NiCoCrAlYSiB corrosion and heat resistant coating and preparation method thereof, application number 03111363.X; Or the like.
For high temperature alloy and high-temperature protection coating parts, oxidation is one of major reason that causes component failure, and the raising of its antioxygenic property mainly depends on the slowly Al of growth of surface
2O
3Film.At high temperature, the pellumina of even compact, particularly α-Al
2O
3Film has excellent heat endurance, and the element diffusion coefficient of portion within it is very little, so hopes to add the Al element of high level in high temperature alloy or the high-temperature protection coating usually, utilizes the selective oxidation of Al to generate single even Al
2O
3Film does not protect inner base oxidated or reduce oxidation rate, prolongs parts service life.In the Ni base high temperature protection MCrAlY coating between common Al metal element compound Ni is arranged
2Al
3, β-NiAl and γ '-Ni
3Al etc., wherein Ni
2Al
3Compare crisp, γ '-Ni
3Al content is too low and can not keep for a long time and generate single Al among the Al
2O
3Film, and β-NiAl is to have higher Al content and relative good mechanical performance as Al storage phase (Al-reservoir) common in the coating simultaneously.
The element counterdiffusion of high-temperature oxydation and coating and matrix is the major reason that causes coating system to lose efficacy for a long time, is characterized in the storage of Al element by lot of consumption, and the inner Al concentration of final coating is not enough to selective oxidation and generates single Al
2O
3Film and no longer have protective value.In order to improve service life under the coating high-temp; Can improve the reserves of outer surface Al element through the method that design MCrAlY adds NiAl two-layer compound coating; But this method has increased the multilayer interface in the coating system, can cause the increase of weak link in the coating system.Therefore, how do not changing or guaranteeing that the content that improves Al element in the coating under the prerequisite of coating mechanical property becomes the key issue that prolongs the high-temperature protection coating active time.
Summary of the invention
In order to delay the degeneration of high-temperature protection coating, prolong the active time of coating, the object of the present invention is to provide a kind of MCrAlY of Al element distribution gradient to add complex gradient coating and preparation method.Because Gradient Effect makes coating under the prerequisite that guarantees mechanical property, improve β-NiAl to greatest extent and stores phase content, thereby can delay the coating degradation process, improves the protection effect and the military service cycle of coating.
To achieve these goals, technical scheme of the present invention is:
A kind of MCrAlY adds complex gradient coating, compound Al element gradient coating on the MCrAlY coating, and the Al concentration of element is along the depth direction distribution gradient, and top layer Al concentration of element is 20-30wt%, and nexine Al concentration of element is 5-10wt%.
The MCrAlY that the present invention adopts the method for solid-state embedding or low-pressure vapor phase Diffusional aluminizing to prepare the distribution of Al concentration gradient on the conventional MCrAlY coating that deposits with arc ion plating (AIP) method adds composite coating.
Said conventional MCrAlY coating alloy system composition is Co:0～40, Cr:15～40, Al:6～16, Y:0.1～1, Si:0～2, B:0.01～0.03, Hf:0～1.5, Ni: surplus by mass percentage.
The concrete preparation method of said gradient Ni-base superalloy coating is: 1) the conventional MCrAlY coating of arc ion plating (AIP, i.e. Arc IonPlating) preparation; 2) on conventional MCrAlY coating basis, adopt: a.) powder embedding+vacuum diffusion annealing method, b.) low-pressure chemical vapor deposition (CVD) method, the MCrAlY that preparation Al concentration in gradient distributes adds complex gradient coating.
Running parameter is following: during arc ion plating, operating room's vacuum is evacuated to 2 * 10 in advance
-3～1 * 10
-2Pa, and sample carried out preparatory sputter clean, pulsed bias is-800～1000V, target-substrate distance 230～250mm, dutycycle 20～40%, time 2～5min; During deposition, arc voltage 20～25V, arc current 50～70A, pulsed bias-150～-300V, dutycycle 20～40%, 300～400 ℃ of depositing temperatures are controlled coating layer thickness according to sedimentation time, and coating layer thickness is 40～60 μ m;
When on the MCrAlY coating, adopting the aluminising of pressed powder investment, penetration enhancer is that 95-99wt%FeAl powder (Al content is 48～52wt% mass ratio, powder size 100～300 orders) adds 1～5wt%NH
4Cl (FeAl powder content and NH
4The Cl sum is 100%); 850～1050 ℃ of pack cementation aluminizing temperature, the rate of heat addition are controlled in the 8 ℃/min, and normal pressure is insulation 3～5h down, and air cooling is to room temperature subsequently.The composite coating that obtains is carried out vacuum heat, and vacuum diffusion annealing temperature is 900～1000 ℃, time 4～6h, and heating rate≤8 ℃/min cool to room temperature with the furnace, obtain the MCrAlY that the Al concentration in gradient distributes and add complex gradient coating;
When on conventional MCrAlY coating, adopting the aluminising of low-pressure chemical vapor deposition (CVD) method, penetration enhancer adds the NH of 1～5wt% oven dry for dry 95-99wt%FeAl powder (Al content is 48～52wt% mass ratio, powder size 100～300 orders)
4Cl (FeAl powder content and NH
4The Cl sum is 100%); The interior vacuum of furnace chamber is evacuated to 0.1～0.01 atmospheric pressure during the CVD aluminising; Temperature is 800～1050 ℃, and heating rate is no more than 8 ℃/min, insulation 3～6h; Be quickly cooled to room temperature, obtain Al concentration and add complex gradient coating along the MCrAlY of depth direction distribution gradient.
The gradient coating of the present invention's preparation can satisfy mechanical property and the double requirements that improves the Al constituent content; Its inner Al element distribution gradient promptly can improve the mark of the storage of Al in coating phase to greatest extent under the condition that does not reduce or seldom reduce the coating mechanical property.In the gradient coating, surface Al concentration is high, helps forming the Al of protectiveness
2O
3Film and long-time supplemental film be the required Al element of growth slowly; The inner Al content of coating is relatively low, and is limited with the Al element that the matrix alloy counterdiffusion is consumed, and therefore this structure can generate Al mutually to greatest extent with the Al storage of inside
2O
3Film becomes effective Al source.In addition, because Al element distribution gradient, coating surface combines with the metal that inner combining belongs to the continuous transition state; There is not weak interface; And surperficial rich Al layer thickness is limited, and its fragility reduces because of small-size effect greatly, can not bring results of serious failure such as coating stripping.
The present invention has the following advantages:
1. coating longer service life.Owing to improved the content of coating storage inside phase β-NiAl, make the interior Al source of coating can give replenishing of surface film oxide longer time, thereby delayed the degeneration of coating, promptly prolonged the active time of coating.
2. Al concentration has the characteristics of Gradient distribution among the present invention, does not increase the combination of weak interface, and its mechanical property is excellent.This MCrAlY adds the thickness of the rich aluminium lamination in composite coating surface and can control through setting aluminising temperature and temperature retention time, and the Al element is along the depth direction distribution gradient.
3. the present invention adopts the MCrAlY of preparation to add that rich Al layer has the adjustable characteristics of thickness in the complex gradient coating, promptly through regulating the thickness that aluminising temperature and temperature retention time are controlled β-NiAl layer of rich Al.
4. the present invention's MCrAlY adds the protection that complex gradient coating can be applicable to Ni base, Co based high-temperature alloy.
5. the present invention adopts the chemical vapour deposition technique aluminising to have rich aluminium lamination good uniformity and does not receive the advantage of specimen size shape affects.Owing to adopt the directly method of diffusion; Do not introduce weak interface; This MCrAlY increases temperature protective coating can improve Al storage phase to greatest extent under the condition that guarantees the coating mechanical property content; Then improve coating resistance to high temperature oxidation, hot corrosion resistance, and can prolong coating service life effectively.
Description of drawings
Fig. 1 (a)-(b) is (a) and annealing back (b) before 1000 ℃ of annealing, pack aluminizing MCrAlY+ composite coating cross section pattern (backscattered electron image).
Fig. 2 is M ℃ of rAlY+ composite coating XRD diffracting spectrum after deposited MCrAlY coating and the 950 ℃ of aluminisings before the aluminising of low pressure chemical vapor deposition gas phase.
Fig. 3 is the section S EM pattern (backscattered electron image) that MCrAlY adds complex gradient coating behind 950 ℃ of low pressure chemical vapor deposition gas phase aluminising 4h.
Fig. 4 is the section S EM pattern (backscattered electron image) that MCrAlY adds complex gradient coating behind 900 ℃ of low pressure chemical vapor deposition gas phase aluminising 4h.
Fig. 5 is the section S EM pattern (backscattered electron image) that MCrAlY adds complex gradient coating behind 1000 ℃ of low pressure chemical vapor deposition gas phase aluminising 6h.
The specific embodiment
Through instance the present invention is done further explain below.
Embodiment 1
Base material adopts directional solidification nickel-base high-temperature alloy DSM11, and its composition is (mass percent) as follows: Co:9.5, Cr:14, W:3.8, Mo:1.5, Al:3, Ti:4.8, Ta:2.8, C:0.1, Ni: surplus.On base material, adopt the conventional MCrAlY coating of arc ion plating (AIP) deposition, MCrAlY target composition is (mass percent meter) as follows, Co:32; Cr:20; Al:8; Y:0.5; Si:1; B:0.03, Ni: surplus.Concrete operations technology is following: before the deposition sample is carried out preliminary treatment; Being about to the base material sample polishes to Ra=0.4 μ m; Adopt 200 order hollow glass ball wet abrasive blastings to handle, successively adopt metal detergent, deionized water, acetone ultrasonic cleaning 15min immediately, with dry for standby after the alcohol rinsing.Adopt homemade MIP-8-800 type multi-arc ion plating equipment to deposit conventional MCrAlY coating, forvacuum to 7 * 10
-3Pa feeds Ar gas when bombardment and deposition, and vacuum is 2.2 * 10
-1Pa.Sample is carried out preparatory sputter bombardment clean, target-substrate distance is 240mm, and pulsed bias is-800V dutycycle 33%, scavenging period 5min; Arc voltage is 20V during deposition, and arc current 62A, pulsed bias be-250V, dutycycle 33%, and 350 ℃ of depositing temperatures, sedimentation time 500min, the conventional MCrAlY coating layer thickness of acquisition is about 60 μ m.
Adopt powder investment Diffusional aluminizing, penetration enhancer adopts the FeAl powder (contain Al and be about 51wt%, powder size is about 250 orders) of 98wt% to add 2wt%NH
4Cl, sample are the conventional MCrAlY coating of deposited or annealed state.Sample is coated in the penetration enhancer, 900 ℃ of insulation 4h in the Muffle furnace under the normal pressure, the rate of heat addition is no more than 8 ℃/min during intensification, and last air cooling is to room temperature.With the aluminising sample that obtains under vacuum condition, 1000 ℃ of annealing 4h, SEM cross section pattern photo is like Fig. 1 (a) with (b) before and after the annealing.
Can know that by Fig. 1 (a)-(b) behind the pack cementation aluminizing, the MCrAlY coating surface has formed rich Al district; Annealed back coating surface partly changes β-NiAl layer of rich Al into; β-NiAl layer thickness of rich Al is about 20 μ m, and Al content is about 30.4wt%, mainly exists with pure β-NiAl form; Inner for MCrAlY adds β-NiAl phase that disperse distributes, inner average Al content is about 14.7wt%, and this MCrAlY adds the characteristics that composite coating has gradient-structure.
Embodiment 2
Base material adopts directional solidification Ni based high-temperature alloy DZ125, and its composition is (mass percent) as follows, Co:10, Cr:9, W:7, Al:5, Ti:2.5, Ta:3.5, C: trace, Ni: surplus.The composition of conventional MCrAlY coating and depositing operation are with embodiment 1, and the conventional MCrAlY coating layer thickness of acquisition is about 50 μ m.Carrying out the low pressure chemical vapor deposition gas phase should be with NH before oozing Al
4The method of 120 ℃ of normal pressure insulation 12h is adopted in Cl oven dry, present embodiment.NH with 96wt%FeAl powder (Al content is 48wt%, and powder size is about 250 orders) and 4wt% oven dry
4Cl puts into the CVD furnace chamber after fully mixing, and after vacuum was evacuated to 0.1 atmospheric pressure (atm), 950 ℃ of insulation 5h obtained dry FeAl powder with stove cooling back.The MCrAlY sample of deposited or annealed state is hung in the low pressure chemical vapor deposition stove, put into the dry NH of dry FeAl powder of 800g and 25g
4Cl, vacuum is evacuated to 0.08atm, behind 950 ℃ of insulation 4h, opens the quick air cooling of furnace enclosure to room temperature.It is as shown in Figure 2 that the MCrAlY that obtains adds composite coating surface XRD diffracting spectrum, and it is as shown in Figure 3 that MCrAlY adds composite coating cross section pattern photo.
Can know by Fig. 2, after the low pressure chemical vapor deposition aluminising, amorphous " steamed bun " peak γ/γ '-Ni in the former deposited MCrAlY coating
3Al disappears, and the MCrAlY of acquisition adds the pure β-NiAl phase composition of composite coating top layer by complete crystallization.Fig. 3 shows that β-NiAl layer thickness of rich Al in the gradient Ni-base superalloy coating that this method obtains is about 17 μ m, and the β of rich Al-NiAl layer Al content is 31.2wt%, and Al mainly exists with β-NiAl mutually; Internal layer adds β-NiAl phase that disperse distributes by MCrAlY, and its average A l content is about 16.3wt%, and Al is with β-NiAl and γ '-Ni
3Al exists mutually, adds in the complex gradient coating at this MCrAlY, and Al content has the characteristic of Gradient distribution along depth direction.
Embodiment 3
Base material adopts Co based high-temperature alloy K40, and its nominal composition is (mass percent): 10.5%Ni, 25.5%Cr, and 7.5%W, 0.45%C, Co surplus, specimen size are 15 * 10 * 1.5mm
3Adopt homemade MIP-8-800 type multi-arc ion plating equipment codeposition MCrAlY+Al (SiY) composite coating.MCrAlY alloy target material composition is (mass percent meter) as follows, Co:32; Cr:20; Al:10; Y:0.5; Si:1; B:0.03, Ni: surplus.Before the deposition sample is carried out preliminary treatment, be about to the base material sample and polish, adopt 200 order hollow glass ball wet abrasive blastings to handle, successively adopt metal detergent, deionized water, acetone ultrasonic cleaning 15min immediately, with dry for standby after the alcohol rinsing to Ra=0.4 μ m.Adopt MIP-8-800 type arc ion plating apparatus to deposit conventional MCrAlY coating, forvacuum to 7 * 10
-3Pa feeds Ar gas when bombardment and deposition, and vacuum is 2 * 10
-1Pa.Sample is carried out preparatory sputter bombardment clean, target-substrate distance is 240mm, and pulsed bias is-800V dutycycle 33%, scavenging period 5min; Arc voltage is 20V during deposition, and arc current 60～65A, pulsed bias be-250V, dutycycle 33%, and depositing temperature is 350 ℃, and sedimentation time is 500min, and the conventional MCrAlY coating layer thickness of acquisition is about 60 μ m.
The conventional MCrAlY deposited coating that obtains is carried out vacuum heat, and heating rate is controlled at 8 ℃/min, is incubated after 4 hours to cool off with stove, obtains annealed state MCrAlY coating.Annealed state MCrAlY coating is put into the low pressure gas phase deposition stove, and vacuum is evacuated to 0.01atm, adds the FeAl powder and the NH of oven dry according to embodiment 2 prescriptions
4Cl is warming up to 900 ℃ with the speed of 8 ℃/min, is quickly cooled to room temperature behind the insulation 4h, and it is as shown in Figure 4 that the MCrAlY of acquisition adds the cross section pattern of gradient coating; Heating rate with 8 ℃/min is heated to 1000 ℃ equally, and insulation 6h is quickly cooled to room temperature, and it is as shown in Figure 5 that the MCrAlY of acquisition adds the cross section pattern of complex gradient coating.
Can be known that by Fig. 4 rich Al layer thickness is thinner in this complex gradient coating, be about 10 μ m, coated inside adds that by MCrAlY β-NiAl that disperse distributes constitutes mutually; Can know that by Fig. 5 β-NiAl layer thickness of the rich Al in this complex gradient coating top layer is thicker, has surpassed 20 μ m, and has had Interim.The MCrAlY that obtains under two kinds of gas phase aluminising temperature adds composite coating, and the β of its rich Al-NiAl top layer Al content is respectively 30.4wt% (900 ℃) and 29.6wt% (1000 ℃), and Al element wherein mainly exists with β-NiAl mutually; Internal layer adds β-NiAl phase that disperse distributes by MCrAlY, and its average A l content is about 18wt%, and Al is with β-NiAl phase and γ '-Ni
3Al exists mutually; Hence one can see that, and the chemical vapour deposition (CVD) aluminising can come the thickness of the rich Al layer of control surface according to aluminising temperature and temperature retention time, and this MCrAlY adds complex gradient coating and has the adjustable characteristics of thickness.
Claims (2)
1. a MCrAlY adds complex gradient coating; It is characterized in that: compound Al element gradient coating on the MCrAlY coating; The Al concentration of element is along the depth direction distribution gradient, and this complex gradient coating top layer Al concentration of element is 20-30wt%, and nexine Al concentration of element is 5-10wt%; MCrAlY coating alloy system composition is Co:0～40, Cr:15～40, Al:6～16, Y:0.1～1, Si:0～2, B:0.01～0.03, Hf:0～1.5, Ni: surplus by mass percentage.
2. the described MCrAlY of claim 1 adds the preparation technology of complex gradient coating, it is characterized in that:
Method through arc ion plating and Diffusional aluminizing prepares MCrAlY and adds complex gradient coating, and said Diffusional aluminizing adopts pressed powder investment or Low Pressure Chemical Vapor Deposition;
Adopt arc ion plating (aip) to deposit conventional MCrAlY coating, deposition parameter is: the base vacuum of vacuum chamber is evacuated to 2 * 10
-3～1 * 10
-2Pa; Feed Ar gas, make pressure in vacuum tank rise to 5 * 10
-2～3 * 10
-1Pa; Target-substrate distance is 230～250mm, bombardment bias voltage-800～-1000V, dutycycle 20～40%, 2～5 minutes sputter clean time; During deposition MCrAlY coating, arc current 50～70A, arc voltage 20～25V, pulsed bias-150～-300V, dutycycle 20～40%, 300～400 ℃ of depositing temperatures, coating layer thickness 40～60 μ m of preparation;
On conventional MCrAlY coating, adopt the aluminising of pressed powder investment, penetration enhancer is that 95-99wt% FeAl powder adds 1～5wt%NH
4Cl, FeAl powder content and NH
4The Cl sum is 100%, and the Al content of FeAl powder is 48～52wt% mass ratio, powder size 100～300 orders; Heating rate≤8 ℃/min, 850～1050 ℃ of insulation 3～5h under the normal pressure, air cooling is to room temperature subsequently;
The composite coating that obtains is carried out vacuum heat, and subsequently with sample 900～1000 ℃ of diffusion annealing 4～6h under vacuum condition, heating rate≤8 ℃/min cool to room temperature with the furnace, obtain the MCrAlY that the Al concentration in gradient distributes and add complex gradient coating;
On conventional MCrAlY coating, adopt the aluminising of low pressure chemical vapor deposition method, penetration enhancer adds the NH of 1～5wt% oven dry for dry 95-99wt%FeAl powder
4Cl, FeAl powder content and NH
4The Cl sum is 100%, and the Al content of FeAl powder is 48～52wt% mass ratio, powder size 100～300 orders; The interior vacuum of furnace chamber is evacuated to 0.1～0.01 atmospheric pressure during the CVD aluminising; Temperature is 800～1050 ℃, and heating rate is no more than 8 ℃/min, insulation 3～6h; Be quickly cooled to room temperature, obtain Al concentration and add complex gradient coating along the MCrAlY of depth direction distribution gradient.
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| JP5445670B2 (en) * | 2010-03-25 | 2014-03-19 | 株式会社Ｉｈｉ | Method for forming oxidation resistant coating layer |
| CN102774089A (en) * | 2012-08-10 | 2012-11-14 | 昆山乔锐金属制品有限公司 | Novel gradient thermal barrier coating |
| CN103590002A (en) * | 2012-08-17 | 2014-02-19 | 中国科学院金属研究所 | Preparation method for Al-Cr coating on nickel-based superalloy |
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| CN108950489B (en) * | 2018-08-21 | 2020-10-16 | 中国科学院金属研究所 | Pt and Y modified gradient Al coating and preparation process thereof |
| CN110295383B (en) * | 2019-07-19 | 2021-04-13 | 中国科学院金属研究所 | Cr modified aluminide coating and preparation method thereof |
| CN111575645A (en) * | 2020-06-30 | 2020-08-25 | 中国航发动力股份有限公司 | Oxidation-resistant coating containing aluminum storage layer and preparation method thereof |
| CN112575296A (en) * | 2020-11-12 | 2021-03-30 | 中国航发沈阳黎明航空发动机有限责任公司 | Turbine blade high-temperature protective coating and preparation method thereof |
| CN114086101A (en) * | 2021-11-19 | 2022-02-25 | 华能国际电力股份有限公司 | High-temperature oxidation and hot corrosion resistant thermal barrier coating and preparation method thereof |
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| CN1045425A (en) * | 1989-03-06 | 1990-09-19 | 联合工艺公司 | The aluminide coating of the enrichment yttrium that the confession ultrahigh temperature alloy is used |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045425A (en) * | 1989-03-06 | 1990-09-19 | 联合工艺公司 | The aluminide coating of the enrichment yttrium that the confession ultrahigh temperature alloy is used |
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| 王启民等.电弧离子镀Ni-Co-Cr-Al-Y-Si-B涂层的热腐蚀性能.《金属学报》.2004,第40卷(第4期),第399－403页，第399页右栏第1段，第400页表1. * |
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| CN101310971A (en) | 2008-11-26 |
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