CN105624617A - Method for preparing densified MCrAlRe type coating through arc ion plating - Google Patents
Method for preparing densified MCrAlRe type coating through arc ion plating Download PDFInfo
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Abstract
The invention relates to a method for preparing a densified MCrAlRe type coating through arc ion plating and belongs to the technical field of coatings. According to MCrAlRe, M represents Fe, Co, Ni, Ti or a combination of Fe, Co, Ni and Ti, Re is rare earth elements including Y, La, Hf, Ce, Dy or a combination of Y, La, Hf, Ce and Dy. The MCrAlRe type coating is a widely applied high-temperature protective coating. Working air pressure of traditional arc ion plating is usually 10-10<-1> Pa, therefore, the prepared MCrAlRe type coating is usually loose and has a gas inclusion phenomenon, and degassing and high-temperature densification treatment are needed. According to the method for preparing the densified MCrAlRe type coating through arc ion plating, the phenomenon of high vacuum arc discharge is adopted, the working air pressure of arc ion plating is lowered by 3-4 orders of magnitudes to reach 10<-3>-10<-4> Pa, and gas-free deposition is performed. The densified MCrAlRe coating without gas inclusion and with excellent binding force can be obtained through the method, the coating properties are greatly improved, the processes such as heat treatment subsequently used usually for preparing the coating through a conventional process can be avoided, the cost is low, and the method is suitable for industrial application.
Description
Technical field
The present invention relates to metal coating techniques, the method specifically providing the fine and close MCrAlRe type coating of a kind of arc ion plating preparation.
Background technology
As typical high-temperature protection coating, (M represents Fe, Co, Ni, Ti or its combination to MCrAlRe, Re is that rare earth element includes Y, La, Hf, Ce, Dy or its combination) type coating is widely used in the high temperature protection of the hot-end component such as aero-engine, gas turbine [referring to document: N.Birks because having the performance advantages such as certain plasticity and toughness, G.H.Meier, F.S.Pettit, Introductiontothehigh-temperatureoxidationofmetals, 2ndedition,CambridgeUniversityPress,Cambridge]��
Arc ion plating has the advantage that target ionization level is high, this technique coating binding force and the uniform coating ability prepared are better than other PVD and spraying coating process. And the manufacture of arc ion plating apparatus and maintenance cost lower than other such as the equipment such as plasma spraying and electro beam physics vapour deposition. Therefore, aforementioned MCrAlRe type high-temperature protection coating significant portion is prepared by arc ions depositing process. The operating air pressure of arc ions depositing process is generally 10-10-1Pa, in this air pressure range, electric arc can remain stable, passes into vacuum coating chamber typically by argon as working gas, and air pressure is maintained above-mentioned scope (referring to document: Tian Minbo, thin film technique and thin-film material, publishing house of Tsing-Hua University, the first edition in 2006). The problem of this technique be institute's plating coating generally in microstructure ratio more loose, and part working gas such as argon can be mingled with (referring to document: J.Andersson, A.Anders, Gaslesssputtering:Opportunitiesforultracleanmetallizatio n, coatingsinspace, andpropulsion, AppliedPhysicsLetters, 92,221503 (2008)), caused consequence is that coating performance declines. For preventing its hydraulic performance decline, generally coating is carried out post processing, such as high annealing so that coating densification. But due to coating entrained gas, directly annealing easily causes again the bulge of coating, thus, need before high annealing to increase low temperature degassing process. These additional techniques significantly increase overall efficiency and the reliability of technology of preparation coating. It addition, high-temperature process also makes coated grains alligatoring, the selective oxidation being unfavorable in coating aluminum isoreactivity element.
To this, it is achieved directly obtained densification by arc ion plating and the technique without the MCrAlRe type coating of gas inclusions is remarkably improved the preparation efficiency of coating and reliability of technology and coating performance. Concurrently facilitate promotion arc ions depositing process to be more widely applied. The present invention utilizes fine vacuum arcing events, higher than under vacuum degree condition more than two orders of magnitude of traditional handicraft, it is achieved that the technique of the fine vacuum arc ion plating MCrAlRe coating of obstructed any working gas such as argon. Under high vacuum condition, the mean free path of vapour particles dramatically increases, and has both decreased the collision of target particle and has improved the consistency of MCrAlRe coating deposited, has inhibited again in coating deposition process being mingled with gas.
The present invention and arc discharge type fine vacuum ion plating technique (ADIP, Shinko Seiki Company Ltd. of Japan) difference be the latter be on the basis of evaporation reaction, increase thermionic emission electrode realizes arc discharge and carrys out heating evaporation metal, and use ionization electrode ionization metal vapors to realize the ion plating under fine vacuum, substantially evaporation adds the process of ionization, because each elemental vapor pressure there are differences, coating composition and target there will be deviation, utilize the technique of this evaporation mode deposition coating to be unsuitable for the preparation as MReAlRe type multicomponent alloy coating; And the present invention utilizes is the mode of arc ion plating, electric arc is evaporation source and ionization source, evaporation and ionization are the indivisible processes of a unification, it is not necessary to other assist ionization device, and advantage is can to obtain and the multicomponent alloy target alloy coat that such as MCrAlRe composition is close.
The present invention utilizes fine vacuum arc discharge characteristics, it is possible to resolve current arc ion plating is prepared MCrAlRe type coating and be there is compactness difference, coating gas enclosure, problem that post processing reliability of technology that is loaded down with trivial details and that cause is low; And the low problem of such coating binding force of high vacuum electron beam physical vapour deposition (PVD) can be overcome, and there is significant cost advantage, it is suitable for industrial applications.
Summary of the invention
The invention aims to solve the arc ion plating MCrAlRe type coating of the working gas such as current commonly used argon and there is porosity height, compactness difference and a series of problem that there is gas inclusions and cause, and the method for the fine and close MCrAlRe type protective coating of arc ion plating preparation provided.
The method of the fine and close MCrAlRe type coating of arc ion plating preparation, it is characterised in that: MCrAlRe type target material surface parallel direction magnetic field intensity is 10-50G; Coating chamber vacuum is 3 �� 10-3-2��10-6Pa; Any gas such as obstructed Ar, directly ignite cathode arc; Matrix is biased and carries out plated film. When starting plated film, may select and bias is added to-600 to-1000V, dutycycle 10-40%, maintain several minutes, for icon bombardment cleaning workpiece.
In described MCrAlRe type target material composition: M represents Fe, Co, Ni, Ti or its combination, Re is that rare earth element includes Y, La, Hf, Ce, Dy or its combination, also can contain other nonmetal or metallic elements such as B, Si, C, Pt, Ag.
Coating chamber vacuum reaches 3 �� 10-3-2��10-6During Pa, contact method, laser or electron beam is adopted directly to ignite electric arc, wherein contact method simple in construction, less costly.
Arc current is 60-600A, and size of current can affect coating deposition rate; Electric current can be direct current or pulse direct current; When adopting pulse direct current, pulse current frequency is 1-1000Hz, and dutycycle is 10%-90%.
Matrix is applied direct current or pulsed negative bias; Bias amplitude is 10-1000V; Pulsed negative bias frequency is 5-50kHz, dutycycle 10%-90%.
The invention have the advantages that
The method of the fine and close MCrAlRe type coating of arc ion plating of the present invention preparation, can obtain the MCrAlRe type coating of densification, and coating is without gas inclusions.
When high-temperature oxydation or annealing, coating is absent from bulge phenomenon, can remove the subsequent heat treatment technique of As-deposited state coating from and directly use.
Coating composition is controlled, compact structure and adhesion are better than the MCrAlRe type coating of high vacuum electron beam physical vapour deposition (PVD).
Current arc ion plating can be solved prepare MCrAlRe type coating and there is compactness difference, coating gas enclosure, problem that post processing reliability of technology that is loaded down with trivial details and that cause is low; And there is significant cost advantage, it is suitable for industrial applications.
Accompanying drawing explanation
Below in conjunction with drawings and the embodiments, the present invention is further detailed explanation:
Fig. 1 is the NiCrAlY coating cross sections stereoscan photograph obtained by (a) conventional method and (b) the inventive method on nickel base superalloy K417G sample;
Fig. 2 is above two coating constant temperature oxidation kinetic curve schematic diagram in 1000 DEG C of air;
Fig. 3 is above two coating constant temperature oxidation cross-sectional scans electromicroscopic photograph after 100 hours in 1000 DEG C of air;
Fig. 4 is above two coating constant temperature oxidation surface scan electromicroscopic photograph after 100 hours in 1000 DEG C of air;
Fig. 5 is the fine and close NiCrAlY coating cross sections stereoscan photograph obtained under height biases by the inventive method on nickel base superalloy K417G sample;
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described.
Embodiment 1
The method of the fine and close NiCrAlY coating of arc ion plating preparation is illustrated by the present embodiment. First NiCrAlY (Ni-30Cr-10Al-0.5Y mass percent wt%) target is installed on negative electrode water cooled target set, then adjusts magnetic field and make target material surface parallel direction magnetic field intensity in 10-80G scope, it is preferred to 10-50G; Before nickel base superalloy K417G test piece is hung on target, closes door for vacuum chamber, bleed; Coating chamber vacuum reaches 0.5-2 �� 10-3During Pa, contact method is adopted directly to be ignited cathode arc by striking pin; Matrix is applied pulsed negative bias 20-50V and carries out plated film. Arc current is 60-600A, and size of current can affect coating deposition rate, and this example adopts 80A DC current. The pulsed negative bias frequency that matrix is applied is 10kHz, dutycycle 20%. This example plated film closes arc source after 4 hours.
As a comparison, equally with common process in logical argon vacuum for 1-2 �� 10-1When Pa, K417G alloy test piece is plated NiCrAlY coating. Arc current is similarly 80A DC current, pulsed negative bias and dutycycle ibid. The plated film time is similarly 4 hours.
The chemical composition of two type coatings is all close with target. Fig. 1 a illustrates the cross-sectional scans electron micrograph of the NiCrAlY coating that above-mentioned common process obtains, it is dispersed with substantial amounts of irregular holes in photo display coating, and there is space in coating with basal body interface place, it was shown that the compactness of this coating, adhesiveness are poor. Fig. 1 b illustrates the cross-sectional scans electron micrograph of the NiCrAlY coating of the technique acquisition that the invention described above provides, and photo shows, compares to common process, and quantity and the size of coating inside aperture significantly reduce; And it being absent from space in coating with basal body interface place, it was shown that the compactness of this coating, adhesiveness are better than the coating that common process obtains.
Embodiment 2
The high temperature oxidation resistance of coating prepared by the invention described above and common process is contrasted by the present embodiment. Fig. 2 illustrates two kinds of coatings constant temperature oxidation kinetic curve in 1000 DEG C of air. By weightening finish curve it can be seen that NiCrAlY coating weightening finish prepared by the present invention is consistently lower than coating prepared by common process, after aoxidizing 100 hours, the former unit are increases weight about 0.45mg/cm2, the latter then reaches about 0.85mg/cm2, it is seen then that the NiCrAlY coating high temperature oxidation resistance prepared by the inventive method is significantly better than coating prepared by common process.
Embodiment 3
The present embodiment compares the different antioxidant effect that NiCrAlY coating prepared by above two method shows in microstructure. Fig. 3 illustrates the cross-sectional scans electromicroscopic photograph after two kinds of coatings aoxidize 100 hours in 1000 DEG C of air (a is common process, and b is technique of the present invention). There occurs bulge after NiCrAlY coating oxidation prepared by common process, oxide-film is thicker, there occurs local internal oxidition, and coating and basal body interface occur in that a large amount of semicontinuous hole or be mingled with; And coating prepared by the inventive method occurs without bulge phenomenon, and oxide-film to be slightly thinner than the former, coating with basal body interface in conjunction with more complete.
Fig. 4 illustrates the surface scan electromicroscopic photograph after two kinds of coatings aoxidize 100 hours in 1000 DEG C of air (a is common process, and b is technique of the present invention). NiCrAlY coating oxidation rear surface (Fig. 4 a) prepared by common process occurs in that big bulge, and the high power photo display surface oxide-film on bulge surface has been covered with a large amount of pattern cracking, it is clear that the non-oxidizability of coating can be caused to reduce. And the surface after fine and close NiCrAlY coating oxidation prepared by the inventive method occurs without bulge, high power photo shows the dense flawless of the pellumina formed, and show further the method for the invention than common process superiority in preparing NiCrAlY.
Embodiment 4
The method of the fine and close NiCrAlY coating of arc ion plating preparation is further illustrated by the present embodiment, and high bias is lower can obtain finer and close coating. Technique is undertaken by the technique similar to described in embodiment 1. First NiCrAlY (Ni-30Cr-10Al-0.5Y mass percent) target is installed on negative electrode water cooled target set, then adjusts magnetic field and make target material surface parallel direction magnetic field intensity in 10-80G scope, it is preferred to 10-50G; Before nickel base superalloy K417G test piece is hung on target, closes door for vacuum chamber, bleed; Coating chamber vacuum reaches 0.5-2 �� 10-3During Pa, contact method is adopted directly to be ignited cathode arc by striking pin. As different from Example 1 matrix being applied higher pulsed negative bias 200-800V and carry out plated film, bias more high, coating compactness is more high, but too high bias can affect coating deposition rate. The present embodiment main presentation-200V arrives microstructure and the composition of coating when the pulsed negative bias of-300V. Arc current is 60-600A, size of current can affect coating deposition rate arc current when reaching 200A, coating deposition rate more than micro-up to 10 m/h, experiments show that, sedimentation rate and arc current are linear approximate relationship, the arc current of 600A can reach the sedimentation rate of more than 30 micro-ms/h, and this example adopts 80A DC current. The pulsed negative bias frequency that matrix is applied is 5-40kHz, and this example adopts 10kHz, dutycycle 10-90%, and the size of dutycycle affects the temperature of test piece, and this example mainly adopts 20%. This example plated film closes arc source after 4 hours.
The chemical composition of coating all with target close to but aluminum content is slightly lower. Fig. 5 illustrates the cross-sectional scans electron micrograph of the NiCrAlY coating that above-mentioned common process obtains. Comparing to low bias technique, the coating that photo display height bias obtains is finer and close. But some deviation of the chemical composition of coating and target, it is mainly manifested in coating aluminum content and reduces about 3-4% than target, this is of a relatively high relevant with the sputtering raste of aluminium element, the ion bom bardment being prone under being biased by height sputters away, aluminum content 5-6% lower than target particularly when dutycycle reaches 90%, in coating. Therefore, for obtaining the NiCrAlY coating of certain aluminum content, under height biases, the raising that the aluminum content in target should be suitable. High bias can obtain the coating matched in excellence or beauty with block materials, the pulsed negative bias of such as 700-900V can make coating very nearly the same with in block materials compactness, and owing to obtaining better adhesiveness with matrix generation phase counterdiffusion, but due to splash effect, the sedimentation rate of coating is affected. Therefore, concrete technological parameter should be accepted or rejected according to coating actual demand in consistency, adhesiveness, sedimentation rate etc.
Embodiment 5
Finer and close and pure MCrAlRe coating can be obtained under higher back end vacuum. By being toasted for a long time by plated film vacuum chamber and being bled by molecular pump, the vacuum of vacuum chamber enters 10-6Still can passing through common method such as striking pin contacting ignition arc during Pa, the vacuum degree in vacuum chamber after the starting the arc can enter into 10-3-10-4Pa magnitude, depends on target material composition and arc current size. The vacuum caused during the high MCrAlRe target plated film of chromium aluminum content changes greatly, and gas pressure in vacuum can be made to enter 10-3Pa; Arc current is more big, and vacuum degree in vacuum chamber is more low, and the target that chromium aluminum content is low can result in vacuum under the arc current effect of more than 400A and is lowered into 10-3Pa��
Embodiment 6
The method of the fine and close FeCrAlSiY coating of arc ion plating preparation is illustrated by the present embodiment. First FeCrAlSiY (Fe-30Cr-15Al-0.8Y mass percent) target is installed on negative electrode water cooled target set, then adjusts magnetic field to 60-80G; 304 rustless steel test pieces are hung on target front distance and are about 15cm place, close door for vacuum chamber and bleed. Coating chamber vacuum reaches 0.2-1 �� 10-3During Pa, adopting contact method directly to be ignited cathode arc by striking pin, arc current is the DC current of 150A. Matrix applies pulsed negative bias 20-50V and carries out plated film. Pulsed negative bias frequency 40kHz, dutycycle 20%. Sedimentation time is 2 hours.
The chemical composition of gained FeCrAlSiY coating is that Fe-32Cr-14Al-0.9Y is close with target, and sedimentation rate reaches 8-10 micro-m/h (test piece rotation). Coating has high consistency, exists with basal body interface tight, and resistance to high temperature oxidation and antistrip performance are better than FeCrAlSiY coating prepared by common process, and oxidizing process floating coat occurs without bulge phenomenon.
Embodiment 7
The MCrAlRe type coating of other compositions can prepare corresponding high compactness coating according to preparation technology similar to the above embodiments, and each composition target as shown in the table prepares the composition of coating under corresponding conditions in nickel base superalloy test piece.
Table 1. target and coating composition
Above in association with accompanying drawing, the specific embodiment of the present invention is described; but these explanations can not be considered as limiting the scope of the present invention; protection scope of the present invention is limited by appended claims, and any change on the claims in the present invention basis is all protection scope of the present invention.
Claims (6)
1. the method for the fine and close MCrAlRe type coating of arc ion plating preparation, it is characterised in that: MCrAlRe type target material surface parallel direction magnetic field intensity is 10-50G; Coating chamber vacuum is 3 �� 10-3-2��10-6Pa; Any gas such as obstructed Ar, directly ignite cathode arc; Matrix is biased and carries out plated film.
2. the method for the fine and close MCrAlRe type coating of arc ion plating preparation described in claim 1, it is characterised in that: in described MCrAlRe type target material composition: M represents Fe, Co, Ni, Ti or its combination; Re is that rare earth element includes Y, La, Hf, Ce, Dy or its combination.
3. the method for the fine and close MCrAlRe type coating of arc ion plating preparation described in claim 2, it is characterised in that: Re also includes B, Si, C, Pt and Ag one or a combination set of.
4. the method for the fine and close MCrAlRe type coating of arc ion plating preparation described in claim 1, it is characterised in that: coating chamber vacuum reaches 3 �� 10-3-2��10-6During Pa, contact method, laser or electron beam is adopted directly to ignite electric arc.
5. the method for the fine and close MCrAlRe type coating of arc ion plating preparation described in claim 1, it is characterised in that: arc current is 60-600A; Electric current is direct current or pulse direct current; When adopting pulse direct current, pulse current frequency is 1-1000Hz, and dutycycle is 10%-90%.
6. the method for the fine and close MCrAlRe type coating of arc ion plating preparation described in claim 1, it is characterised in that: matrix applies direct current or pulsed negative bias; Bias amplitude is 10-1000V; Pulsed negative bias frequency is 5-50kHz, dutycycle 10%-90%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106756819A (en) * | 2016-09-30 | 2017-05-31 | 广东省新材料研究所 | A kind of MCrAlY high-temperature protection coatings preparation method |
| CN108754386A (en) * | 2018-07-27 | 2018-11-06 | 北方工业大学 | Thermal shock resistant MCrAlY coating and preparation method thereof |
| CN108796453A (en) * | 2018-05-30 | 2018-11-13 | 广东工业大学 | A kind of AlCrSiN nano-composite coatings of high-temperature wearable and preparation method thereof |
| CN111636079A (en) * | 2019-03-01 | 2020-09-08 | 中国科学院金属研究所 | Preparation method of single-phase low-diffusion platinum-aluminum coating for single-crystal high-temperature alloy |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756819A (en) * | 2016-09-30 | 2017-05-31 | 广东省新材料研究所 | A kind of MCrAlY high-temperature protection coatings preparation method |
| CN108796453A (en) * | 2018-05-30 | 2018-11-13 | 广东工业大学 | A kind of AlCrSiN nano-composite coatings of high-temperature wearable and preparation method thereof |
| CN108754386A (en) * | 2018-07-27 | 2018-11-06 | 北方工业大学 | Thermal shock resistant MCrAlY coating and preparation method thereof |
| CN111636079A (en) * | 2019-03-01 | 2020-09-08 | 中国科学院金属研究所 | Preparation method of single-phase low-diffusion platinum-aluminum coating for single-crystal high-temperature alloy |
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