CN105603424B - β (Ni, Pt) Al coatings that a kind of Si is modified and preparation method thereof - Google Patents
β (Ni, Pt) Al coatings that a kind of Si is modified and preparation method thereof Download PDFInfo
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- CN105603424B CN105603424B CN201410687157.6A CN201410687157A CN105603424B CN 105603424 B CN105603424 B CN 105603424B CN 201410687157 A CN201410687157 A CN 201410687157A CN 105603424 B CN105603424 B CN 105603424B
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Abstract
The invention discloses a kind of Si β (Ni, Pt) Al coatings being modified and preparation method thereof, belong to high-temperature protection coating technical field.It is combined by using plating with arc ions depositing process, β (Ni, Pt) Al coatings of Si modifications is prepared on nickel base superalloy matrix.The present invention technological process be：First high temperature alloy matrix is pre-processed；One layer of micron-sized pure Pt coating is prepared by electroplating technology；After completing plating, anneal at high temperature, make Pt layers that counterdiffusion occur with matrix；Again one layer of AlSiY coating is deposited on surface；Related heat treatment finally is carried out to coating, makes β (Ni, Pt) the Al coatings being modified in matrix surface generation Si.The present invention, which solve thes problems, such as to prepare using traditional alumetizing process, contains field trash in platinum aluminized coating, β (Ni, Pt) Al coatings can be obtained by being simply heat-treated.
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 of Si changes
β-(Ni, Pt) Al coatings of property and preparation method thereof.
Background technology
With the development of aeronautical and space technology, requirement of the people to its engine also more and more higher.To improve engine
Service efficiency, entrance point temperature need to be improved, this requires that engine material has excellent high-temperature behavior, such as anti-oxidant and high temperature resistance
Corrosive power.But common high temperature alloy can not meet these performances, therefore need to coat high-temperature protection coating on its surface, utilize
The anti-oxidant and corrosion and heat resistant ability of coating, protects matrix not aoxidize at high temperature.Conventional high-temperature protection coating can divide
For MCrAlY coatings and aluminide diffusion coating.
Due to being widely used with good hot corrosion resistance and high-temp plastic by people, it is applied MCrAlY coatings
Al content is typically in 8~14wt.% in layer.But when temperature in use is higher than 1100 DEG C and the above, will coating surface generate compared with
Thick aluminum oxide film, the Al elements for causing to shield in coating are largely consumed, so that coating occurs to degenerate and lost
Effect.
By pack cementation aluminizing or chemical gaseous phase aluminising method, one layer of aluminide typically is generated in matrix surface for coat of aluminide
Coating, generally β-NiAl phases.Because its Al constituent content is higher, about 30wt.%, therefore there is good resistance to high temperature oxidation energy
Power.But common coat of aluminide fragility is larger, and corrosion and heat resistant and antifatigue croop property are poor, are moved back in corrosive atmosphere floating coat
Change very fast.Therefore people design modified aluminide coating on the basis of traditional coat of aluminide, as platinum modified aluminide applies
Layer, it has more preferable antioxygenic property and hot corrosion resistance.Traditional platinum aluminized coating, passes through plating in high-temperature alloy surface first
Or the methods of magnetron sputtering, obtains one layer of platinum layer, after certain temperature is annealed, then uses pack cementation aluminizing or chemical vapor infiltration
The mode of aluminium obtains platinum aluminized coating.
But because pack cementation aluminizing method is directly to contact high temperature alloy with powder, cause to introduce folder during aluminising
It is miscellaneous, reduce the service life of coating.Therefore how to avoid powder impurity pollution coating is one of focus of platinum aluminized coating research.This
Outside, the platinum aluminized coating that prepared by pack cementation aluminizing method, its surface can typically generate substantial amounts of PtAl2Phase, this is mutually in applied at elevated temperature temperature
Undergone phase transition in the range of degree, cause coating surface fold to rise and fall, reduce its cycle life.Chemical gaseous phase aluminizing technology is nearest one
A kind of aluminizing technology of development in 20 years, avoids powder and alloy contact, can prepare the platinum aluminized coating of excellent performance, but the system
Preparation Method is higher to aluminising equipment requirement, and the sample composition controllability prepared using gas phase aluminising is relatively low.Therefore, study new
Platinum aluminized coating preparation technology is current study hotspot.
The content of the invention
It is an object of the invention to provide β-(Ni, Pt) Al coatings and preparation method thereof that a kind of Si is modified, using plating and
Arc ion plating (aip), prepare Si and be modified β-(Ni, Pt) Al coatings, efficiently solve and platinum aluminium is prepared using traditional alumetizing process
The problem of containing field trash in coating.
To achieve the above object, the technical solution adopted in the present invention is as follows：
A kind of preparation method of β-(Ni, Pt) Al coatings that Si is modified, this method comprise the following steps：
(1) pre-treatment, electrochemical degreasing processing and activation process are carried out successively to matrix (nickel base superalloy), to improve
The adhesion of Pt layers and matrix is plated, is to matrix preplating Ni layers, the preplating Ni layer processes before Pt is electroplated：By the base after activation
Body is put into preplating nickel plating bath and electroplated, and matrix is as negative electrode, and anode is nickel plate, current density 4A/dm2, electroplating time
1min；The plating solution forms：200~250g/L of nickel chloride, 180~250ml/L of hydrochloric acid, remaining is deionized water；
(2) Pt layers are electroplated：The matrix of preplating Ni layers is put into plating Pt liquid and electroplated, technological parameter is：70 DEG C of electroplating temperature,
Current density 2A/dm2, 10~30min of electroplating time；Matrix is negative electrode, and platinum titanium net is anode；Plating solution formula is：Two nitrous
The ammino platinum of base two (calculates) 6g/L, 20~65g/L of sulfamic acid with platinum equivalent, and remaining is deionized water；Electroplate liquid pH is 1.5；
1~4 μm of Pt thickness degree；
(3) matrix after step (2) plating Pt layers is carried out carrying out dehydrogenation and prediffusion is handled, detailed process is：First exist
260 DEG C of insulation 1h carry out dehydrogenation, then the 1~2h that annealed at 1050~1100 DEG C, make element in matrix occur mutually to expand with Pt
Dissipate；Sample after annealed processing is cleaned by ultrasonic, and to remove the impurity on surface, then carries out step (4).
(4) arc ion plating (AIP) technique is used, depositing Al SiY coatings, sedimentation time are on sample after the annealing process
At 10~20 μm, the composition of AlSiY targets used is 3~5h, AlSiY coating layer thickness：Al is that 94.1wt.%, Y are
1.2wt.%, Si 4.7wt.%；Deposition process parameters are：Arc voltage 19-21V, arc 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) sample through step (4) depositing Al SiY coatings being made annealing treatment, annealing temperature is 1000~1100 DEG C,
2~5h is incubated, that is, obtains β-(Ni, Pt) Al coatings that the Si is modified.
In step (1), the pre-treatment refers to polish to matrix, sandblasting (is carried out at wet abrasive blasting with 200 mesh glass balls
Reason) or be ultrasonically treated.
In step (1), the electrochemical degreasing concrete operations are：Matrix through pre-treatment is put into 5wt.%NaOH solution
Middle plating oil removing, matrix are negative electrode, and pure nickel plate is anode, current density 8A/dm2, electroplating time 30s；After electrochemical degreasing
Cleaned with deionized water, then carry out activation process；The activation process be by matrix be put into chloroazotic acid (37wt.% concentrated hydrochloric acids with
65wt.% concentrated nitric acids are according to 3:1 volume proportion mix) in activation 10s, with obtain it is fresh and with certain roughness matrix table
Face.The chloroazotic acid used during activation process, need to be now with the current, and effective time is less than 4h.
In step (3) and step (5) annealing process, annealed using under vacuum condition and argon atmosphere, be
Prevent disbonding, the rate of heat addition is 4~6 DEG C/min, furnace cooling.
Plating in the step (4) and step (5), using double anode, negative electrode is positioned at the center of two anode surfaces, sun
Pole-face product/cathode area=2:1.
In β-(Ni, Pt) Al coatings that Si prepared by the above method is modified, Pt contents are 3~6at.%, Al content 30
~45at.%, Si content are 0.5~2at.%.Main coordinate of the coating is divided into β-(Ni, Pt) Al, also containing γ `-Ni3Al
Phase and/or PtAl2Phase.
The invention has the advantages that：
1st, the present invention electroplates one layer of Pt layer first on high temperature alloy, then carries out high annealing, makes Pt and matrix element
Generation counterdiffusion, then using arc ion plating (AIP) method depositing Al SiY coatings, Si modifications can be obtained through certain heat treatment
β-(Ni, Pt) Al coatings.It is using plating and arc ion plating (aip) depositing coating, then in conjunction with corresponding diffusion annealing work
Skill, prepare β-(Ni, Pt) Al coatings of Si modifications.
2nd, it is nickel base superalloy, generally monocrystalline that the present invention is matrix used, has preferable mechanical behavior under high temperature, and make
For matrix when its profile it is simple, the labyrinth such as no deep hole or bending.
3rd, the present invention can reach accurate by adjusting plating Pt thickness degree, AlSiY thickness degree, composition and parameter and annealing
Coating chemical composition, the purpose of thickness are controlled, while compensate for introducing the deficiency being mingled with pack cementation aluminizing method.
Brief description of the drawings
Fig. 1 is the Cross Section Morphology after plating Pt layer annealing.
Fig. 2 is the Cross Section Morphology of Si modification β-(Ni, Pt) Al coatings after annealing.
Fig. 3 analyzes for coating XRD spectrum after annealing.
Fig. 4 is the section essential element distribution situation of coating after annealing.
Embodiment
With reference to embodiment be described in detail the present invention, the tissue and composition characterization method of coating, including ESEM (SEM) and
Energy spectrum analysis (EDS).
Embodiment 1
The present embodiment is that β-(Ni, Pt) Al coatings that Si is modified are prepared on nickel base superalloy matrix, Ni-based height used
Temperature alloy (DD5) composition is (wt.%):Co 7.5%, Cr 7.0%, Al 6.2%, Re 3.0%, Mo 1.5%, W
5.0%, Ta 6.5%, Hf 0.15%, C 0.05%, B 0.004%, Y 0.01%, surplus Ni.Preparation process is as follows：
First, to high temperature alloy matrix carry out pre-treatment, pre-treatment include matrix is polished, sandblasting, supersound process
Deng；
Before Pt layers are electroplated, electrochemical degreasing, activation, preplating Ni processing are carried out to matrix, to remove the oil of matrix surface
Dirty, oxide skin, improve the adhesion between matrix and plating Pt layers.Electrochemical degreasing specific process parameter is：At room temperature by matrix
It is put into the 5wt.%NaOH aqueous solution and is used as negative electrode, in 8A/dm2Taken out under current density after oil removing 30s, anode is pure Ni plates.
Activating process parameter is：37wt.% concentrated hydrochloric acids and 65wt.% concentrated nitric acids are according to volume ratio (3~4):1 mixing, matrix is put into
Taken out after wherein activating 10s.Preplating Ni specific process parameters are：Nickel chloride 200g/L, hydrochloric acid 200ml/L, remaining is deionization
Water, after being well mixed, matrix is put into plating solution as negative electrode, in 4A/dm2Preplating Ni mono- minute, anode are under current density
Pure nickel plate；
After being cleaned with deionized water, using high temperature alloy matrix as cathode suspension in the plating solution, specific process parameter is as follows：
70 DEG C of electroplating temperature, current density 2A/dm2, pH=1.5, platinum titanium net is anode.Plating solution formula is：The ammino of dinitroso two
Platinum (calculates) 6g/L, 20~65g/L of sulfamic acid with platinum equivalent, and remaining is deionized water.20min is electroplated, thickness is 2 μm；
After the completion of plating, sample is enclosed in vacuum silicone tube and made annealing treatment, vacuum 10-2Pa, it is filled with 0.2Pa argon gas guarantor
Coating is protected, temperature is 1080 DEG C, soaking time 90min, and the rate of heat addition is 5 DEG C/min, furnace cooling.Before annealing, first 260
1h dehydrogenations are incubated at DEG C；
After the completion of annealing, sample is subjected to ultrasonic cleaning processing (acetone → deionized water), after cold wind drying, is linked into electric arc
In ion plating stove, depositing Al SiY coatings, 3h is deposited, thickness is 10~15 μm, and AlSiY target material compositions used are shown in Table 1, deposition ginseng
Number is shown in Table 2；
The characteristics of due to arc ion plating itself, sedimentary particle size range is larger, by a small amount of bulky grain and uniform point
The little particle composition of cloth (size is at hundreds of nanometers)；
The composition (wt.%) of the AlSiY targets of table 1
The technological parameter of the arc ion plating of table 2 (AIP) depositing Al SiY coatings
Deposited coating is encapsulated in vacuum silicone tube, vacuum 10-2Pa, is filled with 0.2Pa argon gas protective coatings, and temperature is
1050 DEG C, soaking time 4h, the rate of heat addition is 5 DEG C/min, furnace cooling.
Annealed state Pt layer cross section patterns are as shown in Figure 1.After annealing, with matrix element counterdiffusion occurs for Pt, passes through EDS power spectrums
Analysis, top layer Pt contents are 50wt.% or so, and Ni contents are 35wt.%, simultaneously containing elements such as a small amount of Co, Cr.
In this example, sample is annealed after depositing Al SiY, after annealing, composition redistributes coating, and surface has
One layer of porous intermetallic Ni-Al compound, blasting treatment is carried out to it to remove porous layer.Ni is finally obtained on coating
Protective layer.For Cross Section Morphology after annealing as shown in Fig. 2 outermost layer is electroplated Ni layer, coating outer layer is mainly β-(Ni, Pt) Al phases,
Contain a small amount of PtAl simultaneously2Phase, γ '-Ni3Al phases, about 20 μm of coating layer thickness, internal layer are diffusion zone, about 15 μm of thickness.
In this example, the phase composition in coating is detected with XRD.According to Fig. 3 XRD spectrum analyze, coating mainly by β-
(Ni, Pt) Al is formed, simultaneously containing a small amount of PtAl2Phase.
In this example, for each essential element distribution in further characterization coating, EDS is carried out to coating and gets analysis ready, is obtained
The distribution of coating interface essential element, along as shown in Figure 4：
(1) coating ecto-entad, Al, Pt, Si constituent content gradually reduce；
(2) in coating outer layer, Al content is between 30~38at.%, and Pt contents are in 4.0~6.0at.%, Si contents about 1
~2at.%.
Claims (10)
- A kind of 1. preparation method of β-(Ni, Pt) Al coatings that Si is modified, it is characterised in that：This method comprises the following steps：(1) matrix is carried out successively pre-treatment, electrochemical degreasing processing and activation process after preplating Ni layers, the preplating Ni layer mistakes Cheng Wei：Matrix after activation is put into preplating nickel plating bath and electroplated, matrix is anode as negative electrode, pure nickel plate, and electric current is close Spend for 4A/dm2, electroplating time 1min；The plating solution forms：200~250g/L of nickel chloride, 180~250ml/L of hydrochloric acid, its Remaining is deionized water；(2) Pt layers are electroplated：The matrix of preplating Ni layers is put into plating Pt liquid and electroplated, technological parameter is：70 DEG C of electroplating temperature, electric current Density 2A/dm2, 10~30min of electroplating time；Matrix is negative electrode, and platinum titanium net is anode；Plating solution formula is：Dinitroso two Ammino platinum 6g/L, 20~65g/L of sulfamic acid, remaining is deionized water；Electroplate liquid pH is 1.5；1~4 μm of Pt thickness degree；(3) matrix after step (2) plating Pt layers is carried out carrying out dehydrogenation and prediffusion is handled, detailed process is：First at 260 DEG C It is incubated 1h and carries out dehydrogenation, then the 1~2h that annealed at 1050~1100 DEG C, make element in matrix that counterdiffusion occur with Pt；(4) arc ions depositing process being used, after the annealing process depositing Al SiY coatings on sample, sedimentation time is 3~5h, At 10~20 μm, the composition of AlSiY targets used is AlSiY coating layer thicknesses：Al is 94.1wt.%, Y 1.2wt.%, Si are 4.7wt.%；Deposition process parameters are：Arc voltage 19-21V, arc current 53-65A, DC pulse back bias voltage 220-230V, duty Than 0.3, partial pressure of ar gas (3.0~3.3) × 10-1Pa；(5) sample through step (4) depositing Al SiY coatings is made annealing treatment, annealing temperature is 1000~1100 DEG C, insulation 2~5h, that is, obtain β-(Ni, Pt) Al coatings that the Si is modified.
- 2. the preparation method of β-(Ni, Pt) Al coatings that Si according to claim 1 is modified, it is characterised in that：The base Body is nickel base superalloy.
- 3. the preparation method of β-(Ni, Pt) Al coatings that Si according to claim 1 is modified, it is characterised in that：Step (1) In, the pre-treatment refers to polish to matrix, sandblasting or supersound process.
- 4. the preparation method of β-(Ni, Pt) Al coatings that Si according to claim 1 is modified, it is characterised in that：Step (1) In, the electrochemical degreasing concrete operations are：Matrix through pre-treatment is put into 5wt.%NaOH solution and electroplates oil removing, matrix For negative electrode, pure nickel plate is anode, current density 8A/dm2, electroplating time 30s；Cleaned after electrochemical degreasing with deionized water, Then activation process is carried out；The activation process is that matrix is put into chloroazotic acid to activate 10s, to obtain fresh and have certain thick The matrix surface of rugosity.
- 5. the preparation method of β-(Ni, Pt) Al coatings that Si according to claim 1 is modified, it is characterised in that：By step (3) sample after annealed processing is cleaned by ultrasonic, and to remove the impurity on surface, then carries out step (4).
- 6. the preparation method of β-(Ni, Pt) Al coatings that Si according to claim 1 is modified, it is characterised in that：Step (3) In step (5) annealing process, annealed using under vacuum condition and argon atmosphere, to prevent disbonding, added Hot speed is 4~6 DEG C/min, furnace cooling.
- 7. the preparation method of β-(Ni, Pt) Al coatings that Si according to claim 1 is modified, it is characterised in that：The step Suddenly the plating in (4) and step (5), using double anode, negative electrode is positioned at the center of two anode surfaces, annode area/cathode plane Product=2:1.
- 8. the preparation method of β-(Ni, Pt) Al coatings that Si according to claim 4 is modified, it is characterised in that：The work Change the chloroazotic acid used during processing, need to be now with the current, effective time is less than 4h.
- A kind of 9. β-(Ni, Pt) Al coatings that Si prepared using claim 1 methods described is modified, it is characterised in that：The painting In layer, Pt contents are 3~6at.%, and Al content is 30~45at.%, and Si contents are 0.5~2at.%.
- 10. β-(Ni, Pt) Al coatings that Si according to claim 9 is modified, it is characterised in that：The main of the coating coordinates It is divided into β-(Ni, Pt) Al, also containing γ `-Ni3Al phases and/or PtAl2Phase.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109136849B (en) * | 2018-08-21 | 2021-01-26 | 中国科学院金属研究所 | Pt-modified gradient Al coating and preparation method thereof |
| 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 |
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| CN101748375A (en) * | 2008-12-12 | 2010-06-23 | 中国科学院金属研究所 | Preparation process of AlSiY diffusion coating |
| CN102615876A (en) * | 2012-03-23 | 2012-08-01 | 上海大学 | Beta-NiAl thermal barrier coating with modified Pt+Si and method for preparing beta-NiAl thermal barrier coating |
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| DE602005014877D1 (en) * | 2004-08-18 | 2009-07-23 | Univ Iowa State Res Found Inc | MADE OF -Ni+ '-Ni3Al ALLOYS MODIFIED WITH ONE OF THE PT GROUP AND HAVING HIGH TEMPERATURE CORROSION RESISTANCE |
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| CN101748375A (en) * | 2008-12-12 | 2010-06-23 | 中国科学院金属研究所 | Preparation process of AlSiY diffusion coating |
| CN102615876A (en) * | 2012-03-23 | 2012-08-01 | 上海大学 | Beta-NiAl thermal barrier coating with modified Pt+Si and method for preparing beta-NiAl thermal barrier coating |
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