CN105603424A - Si-modified beta-(Ni,Pt)Al coating and preparation method thereof - Google Patents
Si-modified beta-(Ni,Pt)Al coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an Si-modified beta-(Ni,Pt)Al coating and a preparation method thereof, and belongs to the field of high temperature protection coating technology. Electroplating and arc ion plating process are combined for usage, and the Si-modified beta-(Ni,Pt)Al coating is prepared on a nickel-base superalloy substrate. The process flow comprises the following steps: pretreatment is carried out for the superalloy substrate; a layer of micron pure Pt coating is prepared by electroplating; after electroplating, high temperature annealing is carried out, so that mutual diffusion is carried out for the Pt layer and the substrate; a layer of AlSiY coating is deposited on the surface; finally related heat treatment is carried out for the coating, and the Si-modified beta-(Ni,Pt)Al coating is produced on the surface of the substrate. The method effectively solves the problem that the platinum-aluminium coating prepared by the traditional aluminizing process contains inclusions, and the beta-(Ni,Pt)Al coating is obtained by the simple heat treatment.
Description
Technical field
The present invention relates to the preparing technical field of high-temperature protection coating on high temperature alloy matrix, specifically a kind ofβ-(Ni, Pt) Al coating of Si modification and preparation method thereof.
Background technology
Along with the development of aeronautical and space technology, people are also more and more higher to the requirement of its engine. Start for improvingThe service efficiency of machine, needs to improve entrance point temperature, and this requires engine material to have excellent high-temperature behavior, asAnti-oxidant and resistance to high temperature corrosion ability. But common high temperature alloy can not meet these performances, therefore need show at itFace coated with high temperature protective coating, utilizes the anti-oxidant of coating and corrosion and heat resistant ability, and protection matrix is not at high temperatureBe oxidized. Conventional high-temperature protection coating can be divided into MCrAlY coating and aluminide diffusion coating.
MCrAlY coating is subject to people and extensively makes owing to having good hot corrosion resistance and high-temp plasticWith, in its coating, Al content is generally at 8～14wt.%. But when serviceability temperature is higher than 1100 DEG C and when above,To generate thicker aluminum oxide film at coating surface, cause the Al element shielding in coating by a large amount ofConsume, thereby make coating occur to degenerate and lost efficacy.
Coat of aluminide, generally by pack cementation aluminizing or chemical gaseous phase aluminising method, generates one deck aluminium at matrix surfaceCompound coating, is generally β-NiAl phase. Because its Al constituent content is higher, about 30wt.%, therefore hasGood oxidation-resistance property. But common coat of aluminide fragility is larger, corrosion and heat resistant and antifatigue creep propertiesCan be poor, degenerate at corrosive atmosphere floating coat very fast. Therefore people establish on the basis of traditional coat of aluminideCount out modified aluminide coating, as platinum modified aluminide coating, it has better antioxygenic property and heat erosionPerformance. Tradition platinum aluminized coating, first obtains one deck at high-temperature alloy surface by methods such as plating or magnetron sputteringsPlatinum layer, after uniform temperature annealing, adopts the mode of pack cementation aluminizing or chemical gaseous phase aluminising to obtain platinum aluminium subsequentlyCoating.
But, because pack cementation aluminizing method is that high temperature alloy is directly contacted with powder, cause drawing in aluminising processEnter to be mingled with, reduce the service life of coating. Therefore how avoiding powder contaminating impurity coating is the research of platinum aluminized coatingOne of focus. In addition, platinum aluminized coating prepared by pack cementation aluminizing method, its surface generally can generate a large amount ofPtAl2Phase, this undergoes phase transition in applied at elevated temperature temperature range, causes coating surface fold to rise and fall, and reducesIts cycle life. Chemical gaseous phase aluminizing technology is a kind of aluminizing technology of nearest ten or twenty year development, avoids powderContact with alloy, can prepare the platinum aluminized coating of excellent performance, but this preparation method be higher to aluminising equipment requirement,And the sample composition controllability that adopts gas phase aluminising to prepare is lower. Therefore, study novel platinum aluminized coating preparation technologyIt is current study hotspot.
Summary of the invention
The object of this invention is to provide β-(Ni, Pt) Al coating of a kind of Si modification and preparation method thereof, utilize electricityPlating and arc ion plating (aip), prepare Si modification β-(Ni, Pt) Al coating, efficiently solves and adopt tradition to oozeAluminium technique is prepared the problem that contains field trash in platinum aluminized coating.
For achieving the above object, the technical solution adopted in the present invention is as follows:
A preparation method for β-(Ni, Pt) Al coating of Si modification, the method comprises the steps:
(1) matrix (nickel base superalloy) is carried out to pre-treatment, electrochemical degreasing processing and activation place successivelyReason, is the adhesion that improves plating Pt layer and matrix, before plating Pt to matrix preplating Ni layer, described preplatingNi layer process is: the matrix after activation is put into nickel preplating plating solution and electroplated, and matrix is as negative electrode, sunVery nickel plate, current density is 4A/dm2, electroplating time 1min; Described plating solution consists of: nickel chloride200～250g/L, hydrochloric acid 180～250ml/L, all the other are deionized water;
(2) electroplate Pt layer: the matrix of preplating Ni layer is put into plating Pt liquid and electroplate, technological parameter is: electricityPlating temperature 70 C, current density 2A/dm2, electroplating time 10～30min; Matrix is negative electrode, and platinum titanium net is sunThe utmost point; Plating solution formula is: dinitroso two ammino platinum (with platinum equivalent calculation) 6g/L, and sulfamic acid 20～65g/L,All the other are deionized water; Electroplate liquid pH is 1.5; Pt layer thickness 1～4 μ m;
(3) matrix of step (2) being electroplated after Pt layer carries out dehydrogenation and prediffusion processing, concrete mistakeCheng Wei: first carry out dehydrogenation at 260 DEG C of insulation 1h, then the 1～2h that anneals at 1050～1100 DEG C, make baseIn body there is counterdiffusion in element and Pt; Sample after annealing in process carries out ultrasonic cleaning, with remove surfaceImpurity, then carries out step (4).
(4) adopt arc ion plating (AIP) technique, depositing Al SiY coating on sample after annealing in process, heavyThe long-pending time is 3～5h, and AlSiY coating layer thickness is at 10～20 μ m, and the composition of AlSiY target used is: Al is94.1wt.%, Y are that 1.2wt.%, Si are 4.7wt.%; Deposition process parameters is: arc voltage 19-21V, arcElectric current 53-65A, DC pulse back bias voltage 220-230V, dutycycle 0.3, partial pressure of ar gas (3.0～3.3) × 10-1Pa；
(5) will carry out annealing in process through the sample of step (4) depositing Al SiY coating, annealing temperature is1000～1100 DEG C, be incubated 2～5h, obtain β-(Ni, Pt) Al coating of described Si modification.
In step (1), described pre-treatment refer to matrix polish, sandblast (enters with 200 order glass ballsRow wet abrasive blasting processing) or ultrasonic processing.
In step (1), described electrochemical degreasing concrete operations are: the matrix through pre-treatment is put intoIn 5wt.%NaOH solution, electroplate oil removing, matrix is negative electrode, and pure nickel plate is anode, and current density is 8A/dm2，Electroplating time 30s; After electrochemical degreasing, by washed with de-ionized water, then carry out activation processing; Described activation placeReason is matrix to be put into chloroazotic acid (37wt.% concentrated hydrochloric acid mixes according to 3:1 volume proportion with 65wt.% red fuming nitric acid (RFNA)) liveChange 10s, to obtain fresh and to there is the matrix surface of certain roughness. The chloroazotic acid adopting when activation processing, needsNow with the current, be less than 4h effective time.
In step (3) and step (5) annealing process, adopt and carry out under vacuum condition and argon shield atmosphereAnnealing, for preventing disbonding, the rate of heat addition is 4～6 DEG C/min, cooling with stove.
Plating in described step (4) and step (5), all adopt double anode, and negative electrode is arranged in two anode surfacesThe heart, annode area/cathode area=2:1.
In β-(Ni, Pt) Al coating of Si modification prepared by said method, Pt content is 3～6at.%, Al contentBe 30～45at.%, Si content is 0.5～2at.%. The main phase composition of this coating is β-(Ni, Pt) Al, also containsγ`-Ni3Al phase and/or PtAl2Phase.
Tool of the present invention has the following advantages:
1, first the present invention electroplates one deck Pt layer on high temperature alloy, then carries out high annealing, make Pt withMatrix element generation counterdiffusion, then adopt arc ion plating (AIP) method depositing Al SiY coating, through certain heatProcessing can obtain β-(Ni, Pt) Al coating of Si modification. It utilizes electroplates and arc ion plating (aip) deposited coatings,Then in conjunction with corresponding diffusion annealing process, prepare β-(Ni, Pt) Al coating of Si modification.
2, the present invention is matrix used is nickel base superalloy, is generally monocrystalline, has good high-temperature mechanicsCan, and its profile is simple during as matrix, without the labyrinth such as deep hole or bending.
3, the present invention plates Pt layer thickness, AlSiY layer thickness, composition and parameter and annealing by adjusting, canReach the object of accurate control coating chemical composition, thickness, made up in pack cementation aluminizing method simultaneously and introduced and be mingled withDeficiency.
Brief description of the drawings
Fig. 1 is the Cross Section Morphology of electroplating after the annealing of Pt layer.
Fig. 2 is the Cross Section Morphology of rear Si modification β-(Ni, Pt) Al coating of annealing.
Fig. 3 is the rear coating XRD atlas analysis of annealing.
Fig. 4 is the cross section essential element distribution situation of coating after annealing.
Detailed description of the invention
Below in conjunction with embodiment in detail the present invention is described in detail, the microstructure and composition characterization method of coating, comprises ESEMAnd energy spectrum analysis (EDS) (SEM).
Embodiment 1
The present embodiment is β-(Ni, Pt) Al coating of preparing Si modification on nickel base superalloy matrix, nickel usedBased high-temperature alloy (DD5) composition is (wt.%): Co7.5%, Cr7.0%, and Al6.2%, Re3.0%, Mo1.5%,W5.0%, Ta6.5%, Hf0.15%, C0.05%, B0.004%, Y0.01%, surplus is Ni. PreparationProcess is as follows:
First, high temperature alloy matrix is carried out to pre-treatment, pre-treatment comprise to matrix polish, sandblast, superSonication etc.;
Electroplating before Pt layer, matrix is carried out to electrochemical degreasing, activation, preplating Ni processing, to remove matrixGreasy dirt, the oxide skin on surface, improve the adhesion between matrix and plating Pt layer. Electrochemical degreasing concrete technologyParameter is: under room temperature, matrix is put into the 5wt.%NaOH aqueous solution as negative electrode, at 8A/dm2Electric current is closeAfter the lower oil removing 30s of degree, take out, anode is pure Ni plate. Activating process parameter is: 37wt.% concentrated hydrochloric acid and 65wt.%Red fuming nitric acid (RFNA) is according to volume ratio (3～4): 1 mixes, and matrix is put into after wherein activating 10s and taken out. Preplating NiConcrete technology parameter is: nickel chloride 200g/L, and hydrochloric acid 200ml/L, all the other are deionized water, after mixing,Matrix is put into plating solution as negative electrode, at 4A/dm2Preplating Ni mono-minute under current density, anode is pure nickelPlate;
With after washed with de-ionized water, using high temperature alloy matrix as cathode suspension in plating solution, concrete technology parameterAs follows: 70 DEG C of electroplating temperatures, current density 2A/dm2, pH=1.5, platinum titanium net is anode. Plating solution formulaFor: dinitroso two ammino platinum (with platinum equivalent calculation) 6g/L, sulfamic acid 20～65g/L, all the other are deionizationWater. Electroplate 20min, thickness is 2 μ m;
After plating completes, sample is enclosed to annealing in process in vacuum silicone tube, vacuum is 10-2Pa, is filled with 0.2PaArgon shield coating, temperature is 1080 DEG C, temperature retention time 90min, the rate of heat addition is 5 DEG C/min, cold with stoveBut. Before annealing, first at 260 DEG C, be incubated 1h dehydrogenation;
After having annealed, sample is carried out to ultrasonic cleaning processing (acetone → deionized water), after cold wind dries up, hangEnter in arc ion plating stove, depositing Al SiY coating, deposition 3h, thickness is 10～15 μ m, AlSiY usedTarget composition is in table 1, and deposition parameter is in table 2;
Due to arc ion plating self, sedimentary deposit particle size range is larger, by a small amount of bulky grain and equalThe granule composition (size is in hundreds of nanometer) of even distribution;
The composition (wt.%) of table 1AlSiY target
The technological parameter of table 2 arc ion plating (AIP) depositing Al SiY coating
Deposited coating is encapsulated in vacuum silicone tube, and vacuum is 10-2Pa, is filled with 0.2Pa argon shield coating,Temperature is 1050 DEG C, temperature retention time 4h, and the rate of heat addition is 5 DEG C/min, cooling with stove.
Annealed state Pt layer cross section pattern as shown in Figure 1. After annealing, Pt and matrix element generation counterdiffusion, logicalCross EDS energy spectrum analysis, top layer Pt content is 50wt.% left and right, and Ni content is 35wt.%, contains few simultaneouslyThe elements such as amount Co, Cr.
In this example, after depositing Al SiY, sample is annealed, coating is after annealing, and composition occurs to distribute again,There is the intermetallic Ni-Al compound of one deck porous on surface, and it is carried out to blasting treatment to remove porous layer. Finally existOn coating, obtain Ni protective layer. After annealing, as shown in Figure 2, outermost layer is electroplated Ni layer to Cross Section Morphology, is coated withLayer skin is mainly β-(Ni, Pt) Al phase, contains a small amount of PtAl simultaneously2Phase, γ '-Ni3Al phase, coating layer thickness approximately20 μ m, internal layer is diffusion zone, thickness approximately 15 μ m.
In this example, with the phase composition in XRD detection coating. According to the XRD atlas analysis of Fig. 3, be coated withLayer is mainly made up of β-(Ni, Pt) Al, contains a small amount of PtAl simultaneously2Phase.
In this example, be further in characterizing coating each essential element distribute, coating is carried out to EDS and gets ready pointAnalyse, obtain the distribution of coating interface essential element, along as shown in Figure 4:
(1) coating ecto-entad, Al, Pt, Si constituent content reduce gradually;
(2) at coating skin, Al content is between 30～38at.%, and Pt content is at 4.0～6.0at.%, Si contentApproximately 1～2at.%.
Claims (10)
1. a preparation method for the β of Si modification-(Ni, Pt) Al coating, is characterized in that: the method comprise asLower step:
(1) matrix is carried out to pre-treatment, electrochemical degreasing are processed successively and activation processing after preplating Ni layer, instituteStating preplating Ni layer process is: the matrix after activation is put into nickel preplating plating solution and electroplate, matrix is as the moonThe utmost point, pure nickel plate is anode, current density is 4A/dm2, electroplating time 1min; Described plating solution consists of: chlorineChange nickel 200～250g/L, hydrochloric acid 180～250ml/L, all the other are deionized water;
(2) electroplate Pt layer: the matrix of preplating Ni layer is put into plating Pt liquid and electroplate, technological parameter is: electricityPlating temperature 70 C, current density 2A/dm2, electroplating time 10～30min; Matrix is negative electrode, and platinum titanium net is sunThe utmost point; Plating solution formula is: dinitroso two ammino platinum (with platinum equivalent calculation) 6g/L, and sulfamic acid 20～65g/L,All the other are deionized water; Electroplate liquid pH is 1.5; Pt layer thickness 1～4 μ m;
(3) matrix of step (2) being electroplated after Pt layer carries out dehydrogenation and prediffusion processing, concrete mistakeCheng Wei: first carry out dehydrogenation at 260 DEG C of insulation 1h, then the 1～2h that anneals at 1050～1100 DEG C, make baseIn body there is counterdiffusion in element and Pt;
(4) adopt arc ion plating (AIP) technique, depositing Al SiY coating on sample after annealing in process, heavyThe long-pending time is 3～5h, and AlSiY coating layer thickness is at 10～20 μ m, and the composition of AlSiY target used is: Al is94.1wt.%, Y are that 1.2wt.%, Si are 4.7wt.%; Deposition process parameters is: arc voltage 19-21V, arcElectric current 53-65A, DC pulse back bias voltage 220-230V, dutycycle 0.3, partial pressure of ar gas (3.0～3.3) × 10-1Pa；
(5) will carry out annealing in process through the sample of step (4) depositing Al SiY coating, annealing temperature is1000～1100 DEG C, be incubated 2～5h, obtain β-(Ni, Pt) Al coating of described Si modification.
2. the preparation method of the β of Si modification according to claim 1-(Ni, Pt) Al coating, its feature existsIn: described matrix is nickel base superalloy.
3. the preparation method of the β of Si modification according to claim 1-(Ni, Pt) Al coating, its feature existsIn: in step (1), described pre-treatment refer to matrix polish, sandblast or ultrasonic processing.
4. the preparation method of the β of Si modification according to claim 1-(Ni, Pt) Al coating, its feature existsIn: in step (1), described electrochemical degreasing concrete operations are: the matrix through pre-treatment is put into 5wt.%NaOHIn solution, electroplate oil removing, matrix is negative electrode, and pure nickel plate is anode, and current density is 8A/dm2, electroplating time30s; After electrochemical degreasing, by washed with de-ionized water, then carry out activation processing; Described activation processing is by baseBody is put into chloroazotic acid and is activated 10s, to obtain fresh and to have a matrix surface of certain roughness.
5. the preparation method of the β of Si modification according to claim 1-(Ni, Pt) Al coating, its feature existsIn: the sample by step (3) after annealing in process carries out ultrasonic cleaning, to remove surperficial impurity, thenCarry out step (4).
6. the preparation method of the β of Si modification according to claim 1-(Ni, Pt) Al coating, its feature existsIn: in step (3) and step (5) annealing process, adopt and carry out under vacuum condition and argon shield atmosphereAnnealing, for preventing disbonding, the rate of heat addition is 4～6 DEG C/min, cooling with stove.
7. the preparation method of the β of Si modification according to claim 1-(Ni, Pt) Al coating, its feature existsIn plating in described step (4) and step (5), all adopt double anode, negative electrode is arranged in two anode surfacesThe heart, annode area/cathode area=2:1.
8. the preparation method of the β of Si modification according to claim 4-(Ni, Pt) Al coating, its feature existsIn: the chloroazotic acid adopting when described activation processing, need be now with the current, be less than 4h effective time.
9. β-(Ni, Pt) Al coating of the Si modification that according to claim 1 prepared by method, is characterized in that:In this coating, Pt content is 3～6at.%, and Al content is 30～45at.%, and Si content is 0.5～2at.%.
10. the β of Si modification according to claim 9-(Ni, Pt) Al coating, is characterized in that: this paintingThe main phase composition of layer is β-(Ni, Pt) Al, also contains γ `-Ni3Al phase and/or PtAl2Phase.
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| CN108998794A (en) * | 2018-08-21 | 2018-12-14 | 中国科学院金属研究所 | A kind of Re-Si is total to modified aluminide coating and preparation method thereof |
| CN109136849A (en) * | 2018-08-21 | 2019-01-04 | 中国科学院金属研究所 | A kind of gradient Al coating and preparation method thereof that Pt is modified |
| CN110306216A (en) * | 2019-07-19 | 2019-10-08 | 中国科学院金属研究所 | A kind of modified β-(Ni, the Pt)-Al coating of active element Re and its preparation process |
| CN110735162A (en) * | 2019-10-18 | 2020-01-31 | 齐鲁工业大学 | Hf modified PtAl coating as well as preparation method and application thereof |
| CN112064072A (en) * | 2020-08-28 | 2020-12-11 | 中国科学院金属研究所 | Method for preparing single-phase Pt-Al coating on surface of nickel-based single-crystal superalloy |
| CN113481470A (en) * | 2021-07-08 | 2021-10-08 | 湘潭大学 | Pt-Si co-modified aluminide coating and preparation process thereof |
| CN114672859A (en) * | 2022-03-11 | 2022-06-28 | 沈阳梅特科航空科技有限公司 | Platinum modified aluminide coating capable of being used as thermal barrier coating bonding layer and preparation process thereof |
| CN117758193A (en) * | 2024-02-22 | 2024-03-26 | 北矿新材科技有限公司 | Preparation method of nickel-aluminum hydrogen-resistant coating and nickel-aluminum hydrogen-resistant coating |
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| CN109136849A (en) * | 2018-08-21 | 2019-01-04 | 中国科学院金属研究所 | A kind of gradient Al coating and preparation method thereof that Pt is modified |
| CN108998794A (en) * | 2018-08-21 | 2018-12-14 | 中国科学院金属研究所 | A kind of Re-Si is total to modified aluminide coating and preparation method thereof |
| CN108998794B (en) * | 2018-08-21 | 2020-11-03 | 中国科学院金属研究所 | Re-Si co-modified aluminide coating and preparation method thereof |
| CN110306216A (en) * | 2019-07-19 | 2019-10-08 | 中国科学院金属研究所 | A kind of modified β-(Ni, the Pt)-Al coating of active element Re and its preparation process |
| CN110306216B (en) * | 2019-07-19 | 2021-06-29 | 中国科学院金属研究所 | Active element Re modified beta- (Ni, Pt) -Al coating and preparation process thereof |
| CN110735162A (en) * | 2019-10-18 | 2020-01-31 | 齐鲁工业大学 | Hf modified PtAl coating as well as preparation method and application thereof |
| CN112064072A (en) * | 2020-08-28 | 2020-12-11 | 中国科学院金属研究所 | Method for preparing single-phase Pt-Al coating on surface of nickel-based single-crystal superalloy |
| CN113481470A (en) * | 2021-07-08 | 2021-10-08 | 湘潭大学 | Pt-Si co-modified aluminide coating and preparation process thereof |
| CN114672859A (en) * | 2022-03-11 | 2022-06-28 | 沈阳梅特科航空科技有限公司 | Platinum modified aluminide coating capable of being used as thermal barrier coating bonding layer and preparation process thereof |
| CN114672859B (en) * | 2022-03-11 | 2024-05-17 | 沈阳梅特科航空科技有限公司 | Platinum modified aluminide coating capable of being used as thermal barrier coating bonding layer and preparation process thereof |
| CN117758193A (en) * | 2024-02-22 | 2024-03-26 | 北矿新材科技有限公司 | Preparation method of nickel-aluminum hydrogen-resistant coating and nickel-aluminum hydrogen-resistant coating |
| CN117758193B (en) * | 2024-02-22 | 2024-04-30 | 北矿新材科技有限公司 | Preparation method of nickel-aluminum hydrogen-resistant coating and nickel-aluminum hydrogen-resistant coating |
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