CN107937874B - A method of Pt-Al high-temperature protection coating is prepared on niobium alloy surface - Google Patents
A method of Pt-Al high-temperature protection coating is prepared on niobium alloy surface Download PDFInfo
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- CN107937874B CN107937874B CN201710961019.6A CN201710961019A CN107937874B CN 107937874 B CN107937874 B CN 107937874B CN 201710961019 A CN201710961019 A CN 201710961019A CN 107937874 B CN107937874 B CN 107937874B
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- niobium alloy
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/36—Embedding in a powder mixture, i.e. pack cementation only one element being diffused
- C23C10/48—Aluminising
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/46—Sputtering by ion beam produced by an external ion source
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Physical Vapour Deposition (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The invention discloses a kind of methods for preparing Pt-Al high-temperature protection coating on niobium alloy surface, comprising the following steps: (1) pre-processes to niobium alloy matrix surface, with being rinsed again with deionized water after acetone ultrasonic cleaning completely, dry up spare；(2) the niobium alloy matrix handled well through step (1) is put into the preparation of Pt layers of progress in ion sputtering instrument；(3) Pt-Al high-temperature protection coating is made on niobium alloy surface after carrying out embedding aluminizing containing Pt layers of niobium alloy matrix for what is be prepared through step (2).Al constituent content is 60~70wt% in the Pt-Al high-temperature protection coating, and Pt constituent content is 2~8wt%, and Nb constituent content is 20~30wt%.Pt-Al high-temperature protection coating prepared by the present invention is continuous fine and close smooth, is in metallurgical bonding with niobium alloy matrix, bond strength is high and preparation process is vacuum ion sputtering method has the advantages that easy to operate, energy saving different from traditional electro-plating method.
Description
Technical field
The present invention relates to high temperature coating protection technology fields, in particular to a kind of to prepare Pt-Al high temperature on niobium alloy surface
The method of protective coating.
Background technique
With the development of high thrust ratio aero-engine, the use environment of turbo blade is more harsh, this is to blade material
More stringent requirements are proposed for the performance of material.The fusing point of niobium is high, and medium density, high temperature specific strength is big, has excellent high-temperature mechanics
Performance and processing performance are considered one of important candidate material of high-temperature structural material.But the inoxidizability of niobium is poor, at 600 DEG C
" pest " oxidation is formed, its application is strongly limited.According to research reports, on niobium alloy surface, coating has protective to root
Coating, niobic alloy high temperature antioxidation can be effectively improved, and its mechanical behavior under high temperature can be taken into account, and coating Protection Code be easy
It realizes, significant effect, therefore is widely used.
Summary of the invention
Coat of aluminide is to rely primarily on aluminium under high temperature using most common coating at present and form fine and close oxygen in conjunction with oxygen
Change the diffusion that aluminium film stops oxygen, to improve the inoxidizability of material.But the single mechanical behavior under high temperature for being put into coat of aluminide
Difference, heat shock resistance external force is weak, and coating failure can be caused under loaded effect.Platinum modified aluminide coating has been found can be improved
Al2O3The binding force of film and matrix, and enhance the structure stability of coating, inhibit element to external diffusion.Oxidation can be improved in platinum
Film selectively produces, and new oxide layer can be comparatively fast generated after oxide layer deterioration, that is, is provided with self-healing function.Platinum element
Doping, can reduce the internal stress of oxidation film to a certain extent, improve the adhesiveness of oxidation film.In addition the presence of platinum also reduces
The enrichment of S element, so that metal layer and oxide interface lose the possibility for generating hole.It shows according to another report, platinum can be with
The rate that matrix element is spread to coating is reduced, and then reduces the generation of detrimental oxide.Multiple research achievements show, relatively
For other modified aluminide coatings, the high-temperature oxidation resistance of platinum modified aluminide coating will be much better than other coatings.Phase
Close the document of application such as: (1) Chinese invention patent, a kind of single-phase platinum modified aluminide coating and its preparation process, application number
20141061091.1；(2) Chinese invention patent, a kind of preparation method of nano platinum oxidation coating for high temperature alloy, application
Numbers 200810058933.0；(3) Chinese invention patent, a kind of protective coating and preparation method thereof for single crystal super alloy,
Application number 201310509194.3 etc..
The preparation method of platinum layer mainly has: (1) the compound platinum of metallurgical processing, is prepared using modes such as rolling, drawing, extruding
Compound platinum.The Material cladding interface bond strength of this method preparation is high, platinum layer is continuously non-porous, and thickness is controllable, but for preparation
10 μm of platinum layers below are difficult, and complex-shaped workpiece is more difficult to process.(2) electro-plating method prepares platinum layer, and utilization is additional
Metal ion in electroplate liquid is restored on cathode (workpiece) and is deposited as platinum by electric current, including Molten Salt Electroplating and aqueous solution electricity
Plate two ways.Fused salt platinum plating complex process operating environment is poor, costly；Aqueous solution plating is currently used acquisition platinum layer
More economical practical method generate more industrial wastewater the disadvantage is that required electroplate liquid formulation is complicated.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of less energy consumptions, easy to operate, obtained coating company
Continuous densification, is well combined with matrix, can effectively improve the side of the Pt-Al high-temperature protection coating of the high-temperature oxidation resistance of niobium alloy
Method.
The technical solution of the present invention is as follows: a kind of method for preparing Pt-Al high-temperature protection coating on niobium alloy surface, including with
Lower step:
(1) niobium alloy matrix surface is pre-processed, successively using 240#, 400#, 600#, 800#, 1000# and
The polishing of 1500# sand paper is bright and clean, with being rinsed again with deionized water after acetone ultrasonic cleaning completely, dries up spare；
(2) the niobium alloy matrix handled well through step (1) is put into the preparation of Pt layers of progress in ion sputtering instrument；Target is
Pt target, target to niobium alloy substrate of substrate stage 20~30mm of distance, evacuation rate be 20~25I/min, sputtering vacuum degree be 5~
15Pa, electric current are 45~48mA, and sputtering time is 2~5min, and the Pt with a thickness of 8~12nm is made in niobium alloy matrix surface
Layer；
(3) embedding aluminizing is carried out containing Pt layers of niobium alloy matrix by what is be prepared through step (2)；First containing Pt
The niobium alloy matrix of layer is sealed into the crucible full of aluminizing medium, and then the crucible is put into vacuum tube furnace, is vacuumized simultaneously
300~350 DEG C of 1~2h of heat preservation are warming up to, it is cooling with vacuum tube furnace after 4~6h of heat preservation it is further heated up to 900~1000 DEG C
To room temperature, Pt-Al high-temperature protection coating is made on niobium alloy surface.
Further, the Pt target purity in the step (1) is 99.9~99.999%.
Further, the aluminizing medium ingredient in the step (3) is 5~12% Al powder by weight percentage, 1~5%
NaF powder, surplus Al2O3Powder, three of the above powder were made through mixing and ball milling 1~5 hour.
Further, the Pt-Al high-temperature protection coating with a thickness of 60~75 μm, Al in Pt-Al high-temperature protection coating
Constituent content is 60~70wt%, and Pt constituent content is 2~8wt%, and Nb constituent content is 20~30wt%.
The beneficial effects of the present invention are:
1, the Pt layer preparation process that the present invention uses has for vacuum ion sputtering method different from traditional electro-plating method
The advantages of easy to operate, energy saving, highly shortened Pt layers of preparation time, and ion sputtering instrument has ultralow electric discharge electric
Pressure, electric current are not necessarily to through sample, and increasing extent of temperature is small, weaken sample damage.
2, Pt-Al high-temperature protection coating prepared by the present invention is continuous fine and close smooth, is in metallurgical bonding, knot with niobium alloy matrix
It is high to close intensity.
3, the Pt-Al high-temperature protection coating that the present invention obtains is compared with single coat of aluminide, at the same temperature
Oxidation resistance is greatly improved.
Detailed description of the invention
Fig. 1 is Pt-Al high-temperature protection coating Cross Section Morphology figure prepared by the embodiment of the present invention 1.
Fig. 2 is the high-temperature oxydation weight gain pair of Pt-Al high-temperature protection coating prepared by the embodiment of the present invention 1 and single calorized coating
Than figure.
Fig. 3 is the XRD spectrum of Pt-Al high-temperature protection coating oxidation front and back prepared by the embodiment of the present invention 1.
Fig. 4 is that Pt-Al high-temperature protection coating prepared by the embodiment of the present invention 1 aoxidizes rear surface shape appearance figure.
Fig. 5 is Cross Section Morphology figure after Pt-Al high-temperature protection coating oxidation prepared by the embodiment of the present invention 1.
Appended drawing reference: 1- Electroless Plating Ni protective layer, 2-Pt-Al high-temperature protection coating, 3-C103 niobium alloy matrix, 4- oxidation
Product.
Specific embodiment
Embodiment 1
A method of Pt-Al high-temperature protection coating is prepared on niobium alloy surface, comprising the following steps:
1, matrix selects C103 niobium alloy, and chemical component is as shown in the table
| Ingredient | Hf | Ti | Zr | W | Ta | Nb |
| Content wt(%) | 10.0 | 1.30 | 0.34 | 0.31 | 0.30 | Bal. |
Niobium alloy matrix surface is pre-processed, 240#, 400#, 600#, 800#, 1000# and 1500# sand are successively used
Paper polishing is bright and clean, with being rinsed again with deionized water after acetone ultrasonic cleaning completely, dries up spare；
2, the niobium alloy matrix handled well through step 1 is put into the preparation of Pt layers of progress in MSP-1S type ion sputtering instrument；
Target is Pt target, and purity is 99.9~99.999%；Target is to niobium alloy substrate of substrate stage distance 25mm, evacuation rate 20I/
Min, sputtering vacuum degree are 10Pa, electric current 47mA, sputtering time 2min, be made with a thickness of 8 in niobium alloy matrix surface~
The Pt layer of 12nm；
3, embedding aluminizing is carried out containing Pt layers of niobium alloy matrix by what is be prepared through step 2；First containing Pt layers
Niobium alloy matrix seal into the crucible full of aluminizing medium, the aluminizing medium ingredient is 10% Al powder by weight percentage, 3%
NaF powder, surplus Al2O3Powder, three of the above powder were made through mixing and ball milling 2 hours；Then the crucible is put into vacuum
In tube furnace, vacuumizes and be warming up to 300 DEG C of heat preservation 1h, it is cooling with vacuum tube furnace after heat preservation 4h it is further heated up to 940 DEG C
To room temperature, Pt-Al high-temperature protection coating is made on niobium alloy surface.
Embodiment 2
1, matrix selects C103 niobium alloy, and chemical component is as shown in the table
| Ingredient | Hf | Ti | Zr | W | Ta | Nb |
| Content wt(%) | 10.0 | 1.30 | 0.34 | 0.31 | 0.30 | Bal. |
Niobium alloy matrix surface is pre-processed, 240#, 400#, 600#, 800#, 1000# and 1500# sand are successively used
Paper polishing is bright and clean, with being rinsed again with deionized water after acetone ultrasonic cleaning completely, dries up spare；
2, the niobium alloy matrix handled well through step 1 is put into the preparation of Pt layers of progress in MSP-1S type ion sputtering instrument；
Target is Pt target, and purity is 99.9~99.999%；Target is to niobium alloy substrate of substrate stage distance 25mm, evacuation rate 20I/
Min, sputtering vacuum degree are 10Pa, electric current 47mA, sputtering time 2min, be made with a thickness of 8 in niobium alloy matrix surface~
The Pt layer of 12nm；
3, embedding aluminizing is carried out containing Pt layers of niobium alloy matrix by what is be prepared through step 2；First containing Pt layers
Niobium alloy matrix seal into the crucible full of aluminizing medium, the aluminizing medium ingredient is 10% Al powder by weight percentage, 5%
NaF powder, surplus Al2O3Powder, three of the above powder were made through mixing and ball milling 2 hours；Then the crucible is put into vacuum
In tube furnace, vacuumizes and be warming up to 300 DEG C of heat preservation 1h, it is cooling with vacuum tube furnace after heat preservation 4h it is further heated up to 940 DEG C
To room temperature, Pt-Al high-temperature protection coating is made on niobium alloy surface.
Embodiment 3
1, matrix selects C103 niobium alloy, and chemical component is as shown in the table
| Ingredient | Hf | Ti | Zr | W | Ta | Nb |
| Content wt(%) | 10.0 | 1.30 | 0.34 | 0.31 | 0.30 | Bal. |
Niobium alloy matrix surface is pre-processed, 240#, 400#, 600#, 800#, 1000# and 1500# sand are successively used
Paper polishing is bright and clean, with being rinsed again with deionized water after acetone ultrasonic cleaning completely, dries up spare；
2, the niobium alloy matrix handled well through step 1 is put into the preparation of Pt layers of progress in MSP-1S type ion sputtering instrument；
Target is Pt target, and purity is 99.9~99.999%；Target is to niobium alloy substrate of substrate stage distance 25mm, evacuation rate 20I/
Min, sputtering vacuum degree are 10Pa, electric current 47mA, sputtering time 2min, be made with a thickness of 8 in niobium alloy matrix surface~
The Pt layer of 12nm；
3, embedding aluminizing is carried out containing Pt layers of niobium alloy matrix by what is be prepared through step 2；First containing Pt layers
Niobium alloy matrix seal into the crucible full of aluminizing medium, the aluminizing medium ingredient is 10% Al powder by weight percentage, 5%
NaF powder, surplus Al2O3Powder, three of the above powder were made through mixing and ball milling 2 hours；Then the crucible is put into vacuum
In tube furnace, vacuumizes and be warming up to 300 DEG C of heat preservation 1h, it is cold with vacuum tube furnace after heat preservation 4h it is further heated up to 1000 DEG C
But to room temperature, Pt-Al high-temperature protection coating is made on niobium alloy surface.
Using the phase structure of X-ray diffraction detection coating, the Cross Section Morphology of coating is observed using scanning electron microscope (SEM),
When preparing cross-sectional sample, in advance in sample surfaces Electroless Plating Ni layer, to protect cross-sectional sample coating morphology.
As shown in Figure 1, Pt-Al high-temperature protection coating made from embodiment 1 is continuously fine and close, in conjunction with C103 niobium alloy matrix
Well, the defects of flawless, hole；It detects and finds through EDS, Al constituent content is 64.96wt% in coating, and Nb content is 22.34
Wt%, Pt content are 3.56 wt%.
As a comparative reference, in C103 niobium alloy matrix surface list aluminide coatings, the difference of preparation method and embodiment 1
It is: without the link of step 2.Pt-Al high-temperature protection coating made from embodiment 1 and niobium alloy matrix surface list are seeped Al to apply
Layer carries out high-temperature oxydation experiment in resistance furnace respectively, and experimental temperature is 1100 DEG C, and experimental period is 100 hours, respectively in reality
The quality of sample is weighed before testing, when 2h, 5h, 10h, 20h, 30h, 50h and 100h, and is recorded.
As shown in Fig. 2, it is relatively more flat to aoxidize Pt-Al coating and single both coating qualities of calorized coating growth before just 20h
Slow, single calorized coating starts quickly to be oxidized after 20h, and mass-change curve slope becomes larger, and Pt-Al coating is aoxidized before 30h
Relatively slow, the more single calorized coating of oxidation resistance after 30h is also significantly increased；In contrast, the Pt-Al that prepared by embodiment 1 is applied
Layer has preferable high temperature protection to act on C103 niobium alloy matrix.
As shown in figure 3, Pt-Al high-temperature protection coating is by Al made from embodiment 13Nb and PtAl2Two kinds of object phase compositions, Pt
Layer external diffusion forms PtAl in conjunction with Al2Phase, the Nb element in matrix alloy is to external diffusion, in conjunction with the Al element of surface deposition
Form Al3Nb phase.After oxidation, coating surface generates Al2O3With part Nb2O5Phase.As shown in connection with fig. 2, compared to single calorized coating, Pt
The presence of element makes Al element be easy to external diffusion to a certain extent, promotes Al2O3The formation of film layer, and improve Al2O3Film from
Healing ability improves coating oxidation resistance.As oxidation carries out, PtAl2It has mutually gradually used up, Al2O3Film gradually falls off,
Nb element generates Nb in conjunction with O in matrix2O5Phase.
As shown in Figure 4 and Figure 5, Pt-Al high-temperature protection coating made from embodiment 1 is after aoxidizing, the cotton-shaped oxygen of Surface Creation
Change product, detected through EDS, O constituent content is 35.64wt%, and Al constituent content is 41.02 wt%, and Nb constituent content is 8.10
Wt% can be obtained in conjunction with XRD Analysis of test results in Fig. 3, and oxidation product is Al2O3And Nb2O5.After oxidation in coating internal layer still
Fine and close and continuous, flawless and hole occur, and associativity is good.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
The variation or simple replacement expected without creative work, should all be included within the scope of the present invention.
Claims (3)
1. a kind of method for preparing Pt-Al high-temperature protection coating on niobium alloy surface, which comprises the following steps:
(1) niobium alloy matrix surface is pre-processed, successively uses 240#, 400#, 600#, 800#, 1000# and 1500# sand
Paper polishing is bright and clean, with being rinsed again with deionized water after acetone ultrasonic cleaning completely, dries up spare；
(2) the niobium alloy matrix handled well through step (1) is put into the preparation of Pt layers of progress in ion sputtering instrument；Target is Pt
Target, target to niobium alloy substrate of substrate stage 20~30mm of distance, evacuation rate be 20~25I/min, sputtering vacuum degree be 5~
15Pa, electric current are 45~48mA, and sputtering time is 2~5min, and the Pt with a thickness of 8~12nm is made in niobium alloy matrix surface
Layer；
(3) embedding aluminizing is carried out containing Pt layers of niobium alloy matrix by what is be prepared through step (2)；First containing Pt layers
Niobium alloy matrix is sealed into the crucible full of aluminizing medium, and then the crucible is put into vacuum tube furnace, vacuumizes and heats up
Room is cooled to vacuum tube furnace after 4~6h of heat preservation it is further heated up to 900~1000 DEG C to 300~350 DEG C of 1~2h of heat preservation
Pt-Al high-temperature protection coating is made on niobium alloy surface in temperature；Aluminizing medium ingredient in the step (3) is 5 by weight percentage
~12% Al powder, 1~5% NaF powder, surplus Al2O3Powder, three of the above powder were made through mixing and ball milling 1~5 hour.
2. the method according to claim 1 for preparing Pt-Al high-temperature protection coating on niobium alloy surface, it is characterised in that:
Pt target purity in the step (1) is 99.9~99.999%.
3. the method according to claim 1 for preparing Pt-Al high-temperature protection coating on niobium alloy surface, it is characterised in that:
The Pt-Al high-temperature protection coating with a thickness of 60~75 μm, in Pt-Al high-temperature protection coating Al constituent content be 60~
70wt%, Pt constituent content are 2~8wt%, and Nb constituent content is 20~30wt%.
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| CN114807709B (en) * | 2022-04-22 | 2023-11-10 | 昆明理工大学 | Rare noble metal niobium alloy gradient material and preparation method thereof |
| CN115011924B (en) * | 2022-04-24 | 2023-07-21 | 昆明理工大学 | High-temperature oxidation resistant alloy and preparation method and application thereof |
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