CN116463589A - Pt-Si co-modified aluminide coating and preparation method thereof - Google Patents
Pt-Si co-modified aluminide coating and preparation method thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 101
- 239000011248 coating agent Substances 0.000 title claims abstract description 98
- 229910000951 Aluminide Inorganic materials 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 85
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 40
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 31
- 229910000601 superalloy Inorganic materials 0.000 claims abstract description 29
- 238000009792 diffusion process Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 14
- 238000007747 plating Methods 0.000 claims abstract description 11
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 4
- 229910000676 Si alloy Inorganic materials 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims 2
- 238000005238 degreasing Methods 0.000 claims 2
- 239000004519 grease Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 86
- 238000007254 oxidation reaction Methods 0.000 abstract description 86
- 238000005260 corrosion Methods 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 7
- 239000011253 protective coating Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 230000004584 weight gain Effects 0.000 description 33
- 235000019786 weight gain Nutrition 0.000 description 33
- 238000005269 aluminizing Methods 0.000 description 17
- 239000010410 layer Substances 0.000 description 17
- 239000011651 chromium Substances 0.000 description 12
- 239000000758 substrate Substances 0.000 description 12
- 230000001681 protective effect Effects 0.000 description 11
- 238000005303 weighing Methods 0.000 description 10
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 9
- 125000004122 cyclic group Chemical group 0.000 description 9
- 238000003618 dip coating Methods 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 9
- 229910052804 chromium Inorganic materials 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 230000007423 decrease Effects 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000005553 drilling Methods 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 230000004580 weight loss Effects 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron 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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
- C23C2/12—Aluminium or alloys based thereon
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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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/26—After-treatment
- C23C2/28—Thermal after-treatment, e.g. treatment in oil bath
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/021—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal alloy layer
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Thermal Sciences (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
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Abstract
The application belongs to the technical field of high-temperature protective coatings, and particularly relates to a Pt-Si co-modified aluminide coating and a preparation method thereof, wherein the preparation method comprises the following steps: (1) A platinum layer is applied to the surface of the nickel-based superalloy by a magnetron sputtering method, and then the nickel-based superalloy is subjected to vacuum diffusion treatment to obtain the nickel-based superalloy deposited with platinum; (2) Applying an aluminum-silicon coating on the surface of the nickel-based superalloy platinum layer deposited with platinum in the step (1) by adopting a hot dip plating method; (3) And (3) carrying out vacuum diffusion treatment on the base body subjected to hot dip plating in the step (2) to obtain the Pt-Si co-modified aluminide coating. According to the invention, the content of platinum and silicon is regulated, so that the platinum can improve the structural stability of the coating, the silicon can improve the hot corrosion resistance of the coating, and the problem of insufficient high-temperature oxidation resistance of a single aluminide coating is solved.
Description
The application is a divisional application of 2021, 07 and 08, 202110774822.5 and named Pt-Si co-modified aluminide coating and preparation process thereof.
Technical Field
The application relates to the technical field of high-temperature protective coatings, in particular to a Pt-Si co-modified aluminide coating and a preparation method thereof.
Background
The K438 nickel-based casting superalloy has excellent high-temperature protection performance and is widely applied to ships and ground heavy gas turbines. However, under high temperature conditions, the K438 alloy has poor oxidation resistance, and in order to ensure long-term stable operation of the gas turbine, an aluminide coating with protective properties may be applied to the surface.
The hot dip aluminizing is a high-efficiency aluminide coating implementation method, has the advantages of high production efficiency, low cost, simple operation, long effective protection period and the like, and has been widely applied to diffusion coating preparation. However, single aluminide coatings often suffer from insufficient high temperature oxidation resistance.
Disclosure of Invention
The technical problem mainly solved by the application is to provide the Pt-Si co-modified aluminide coating and the preparation method thereof, so as to solve the problem of insufficient high-temperature oxidation resistance of a single aluminide coating.
In order to solve the technical problems, one technical scheme adopted by the application is as follows: a preparation method of a Pt-Si co-modified aluminide coating comprises the following steps:
(1) A platinum layer is applied to the surface of the nickel-based superalloy by a magnetron sputtering method, and then the nickel-based superalloy is subjected to vacuum diffusion treatment to obtain the nickel-based superalloy deposited with platinum;
(2) Applying an aluminum-silicon coating on the surface of the nickel-based superalloy platinum layer deposited with platinum in the step (1) by adopting a hot dip plating method;
(3) Carrying out vacuum diffusion treatment on the base body subjected to hot dip plating in the step (2) to obtain a Pt-Si co-modified aluminide coating;
the Pt-Si co-modified aluminide coating comprises the following components in percentage by mass: 10-35% of Ni, 5-10% of Cr, 2-10% of Si, 1-12% of Pt and the balance of Al.
The beneficial effects of this application are: the nickel with relatively high content can improve the high-temperature creep resistance of the aluminide coating by setting the mass percent of nickel in the Pt-Si co-modified aluminide coating to be 10-35%, the mass percent of chromium to be 5-10%, the mass percent of silicon to be 2-10% and the mass percent of platinum to be 1-12%, wherein the coating contains 5-10% of chromium, so that the coating forms Cr with protective effect in oxidation 2 O 3 Film, and appropriate amounts of platinum and silicon are added. The platinum can improve the tissue stability of the aluminide coating, and the silicon can improve the hot corrosion resistance of the aluminide coating, so that the service life of the aluminide coating in a high-temperature environment can be prolonged, and thus, the problem of insufficient high-temperature oxidation resistance of a single aluminide coating can be effectively improved by configuring the components of the coating according to the proportion, and the use requirement of the nickel-based superalloy in a severe service environment can be better met.
Drawings
FIG. 1 is a cross-sectional profile of the PVD platinized material of the present application;
FIG. 2 is a cross-section and component area scan of a Pt-Si co-modified aluminide coating of the present application;
FIG. 3 is a graph of 250 cycles oxidation at 1000℃for a Pt-Si co-modified aluminide coating of the present application;
FIG. 4 is a cross-section and component area scan of a single aluminide coating of the present application;
FIG. 5 is a graph of oxidation curves for a single aluminide coating of the present application at 1000℃for 250 cycles.
Detailed Description
The following description of the technical solutions in the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
The Pt-Si co-modified aluminide coating described in the Pt-Si co-modified aluminide coating examples herein comprises the following components in mass percent: 10-35% of Ni, 5-10% of Cr, 2-10% of Si, 1-12% of Pt and the balance of Al.
The relatively high content of chromium and aluminum enables the coating to form Cr during oxidation 2 O 3 And Al 2 O 3 The film can prevent oxygen from corroding the matrix and form good protection for the matrix, thereby improving the high-temperature oxidation resistance of the matrix, the nickel with the content can improve the high-temperature creep resistance of the coating, the silicon with the content based on the aluminum, nickel and chromium with the content in the proportion can improve the hot corrosion resistance of the coating, and the platinum with the content can improve the Al 2 O 3 And the tissue stability of the aluminide coating, thereby improving the high temperature oxidation resistance of the coating. According to the scheme, the problem of insufficient high-temperature oxidation resistance of a single aluminide coating can be effectively solved by cooperatively configuring the mass percentages of nickel, chromium, platinum, silicon and other elements.
Optionally, the mass percent of nickel is 15% -30%, the mass percent of chromium is 6% -10%, the mass percent of silicon is 3% -6%, and the mass percent of platinum is 1% -8%.
The oxidation resistance of the coating can be further improved by preparing 6-10% of chromium by mass percent, the service life of the coating is prolonged, and the corrosion resistance of the coating can be further improved by preparing 15-30% of nickel by mass percent on the basis.
Optionally, the mass percent of nickel is 20% -25%, the mass percent of chromium is 6% -9%, the mass percent of Si is 4% -6%, and the mass percent of platinum is 1% -2%.
Wherein, by configuring the nickel element with the mass percentages, the hot corrosion resistance of the coating can be improved, the chromium element and the aluminum element can provide a protective film for the nickel-based superalloy, the oxidation of the substrate is delayed, the hot corrosion resistance of the coating can be improved by adding silicon, and the Al can be improved by adding platinum 2 O 3 By configuring the content of the element, the coating can provide good protection for the nickel-based superalloy.
The preparation process of the Pt-Si co-modified aluminide coating can comprise the following steps:
(1) And (3) applying a platinum layer on the surface of the nickel-based superalloy by adopting a magnetron sputtering method, and then carrying out vacuum diffusion treatment on the nickel-based superalloy to obtain the nickel-based superalloy deposited with platinum.
Wherein the thickness of the applied platinum layer is 1-10 mu m, the temperature of the vacuum diffusion treatment is 1000-1200 ℃ and the time is 2-5 hours. SEM testing was performed on the nickel-base superalloy with the platinum coating applied, and the cross-sectional structure morphology is shown in fig. 1.
First, the nickel-base superalloy is cut into small pieces of 10mm×8mm×2mm in specification by a wire cutting machine, or into small pieces of other specification, which are not limited herein, and then the small pieces are used as a base. The type of nickel-base superalloy may be various, for example, the nickel-base superalloy may be K438, without limitation. Then a small round hole of phi 3.0mm is drilled in the surface of the substrate by a drilling machine. Removing the oxide on the surface of the matrix by using a pre-grinding machine, grinding the matrix to be flat and bright, and then putting the matrix into absolute ethyl alcohol for standby.
The prepared substrate is divided into two groups, one of which is to deposit a layer of platinum element on the surface by PVD, and the thickness of the platinum layer may be 1-10 μm, for example, the thickness of the platinum layer is 2 μm. The thickness of the platinum layer may be in other ranges between 1 and 10 μm, for example, the thickness of the platinum layer may be 2 to 9 μm, 3 to 8 μm, 4 to 7 μm, or 5 to 6 μm. Then, the substrate on which the platinum element is deposited is subjected to vacuum diffusion at a temperature of 1000 to 1200 ℃ for 2 to 5 hours, for example, 1050 ℃ for 2 hours. The temperature of the vacuum diffusion may be in other ranges of 1000 to 1200 ℃, for example, the temperature of the vacuum diffusion may be 1000 to 1100 ℃, 1050 to 1150 ℃, or 1100 to 1200 ℃. The time of vacuum diffusion may be in other ranges of 2 to 5 hours, for example, the time of vacuum diffusion may be 2 to 4 hours, 3 to 5 hours, 3.5 to 5 hours, or 4 to 5 hours. After vacuum diffusion, a hot dip aluminum plating test was performed.
The other group of substrates are directly subjected to a hot dip aluminum plating test without depositing platinum element.
Wherein, when the base body deposited with the platinum element and the base body not deposited with the platinum element are subjected to a hot dip aluminizing test, the hot dip coating temperature is 700-750 ℃, the time is 30-360 s, for example, the hot dip aluminizing temperature is 710 ℃, and the hot dip aluminizing time is 30s, 60s, 90s, 120s and 180s. And carrying out vacuum diffusion treatment on the two groups of samples subjected to hot dip aluminizing, wherein the temperature of the vacuum diffusion is 950-1200 ℃ for 1-10 hours, for example, the temperature of the vacuum diffusion is 1000 ℃ and the time is 1 hour. The vacuum diffusion temperature is in other ranges of 950 to 1200 ℃, for example, the vacuum diffusion temperature may be 950 to 1100 ℃, 1000 to 1150 ℃, or 1050 to 1100 ℃. The time for the vacuum diffusion is in other ranges of 1 to 10 hours, for example, 2 to 9 hours, 3 to 8 hours, 4 to 7 hours, or 5 to 6 hours.
The molten pool adopted in the hot dip plating method is aluminum-silicon alloy, and the components of the molten pool are 2-10% of silicon and 90-98% of aluminum by mass, for example, the components of the molten pool are 5% of silicon and 95% of aluminum by mass.
Oxidation experiments were then performed on both sets of samples. The experiment adopts a cyclic oxidation method. And the coating with the same process condition is provided with three parallel samples for cyclic oxidation experiments so as to ensure the accuracy of the follow-up weighing data. And (3) placing the sample into static air of a high-temperature furnace for oxidation for 50min, wherein air cooling is carried out for 10min to obtain one cycle, the total time is 250 cycles, and the temperature of the cyclic oxidation experiment is 1000 ℃. The following specific experimental steps are as follows:
(1) Firing a ceramic crucible: removing volatile matters from the crucible at 1000 ℃ and burning to constant weight;
(2) Sample size measurement: measuring the length, width, height and hole diameter of each sample by using a vernier caliper;
(3) Weighing: the sample was placed in a corresponding ceramic crucible, the weight before oxidation was recorded, and the crucible was placed in a tubular resistance furnace (model SK 2-4-12) for high temperature oxidation. The first 10 cycles, 1, 4, 7, 10 cycles are called emphasis; weighing once every 20 cycles in 20-100 cycles; in 100-250 cycles, weigh once every 50 cycles. Weight gain values were taken as an average of 3 parallel samples. All data are recorded in the designed table. The weighing mode of cyclic oxidation is adopted, only the mass of the sample is weighed, and the weight of the crucible and the fallen oxide scale is not calculated. The experiment was performed with an electronic balance to a precision of 0.0001g.
(4) And (3) data processing: according to the experimental data processing of the weight increasing method, the oxidation rate is calculated from the weight increasing variation and the surface area of each sample at different time.
Example 1:
in this example, a K438 nickel-based superalloy was used as the substrate, and the nominal composition is shown in Table 1.
Table 1 nominal composition of k438 nickel-base superalloy
The substrate K438 was cut into small pieces of 10mm by 8mm by 2mm in size by a wire cutting machine, and small round holes of 3.0mm in diameter were drilled in the surface by a drilling machine. And removing oxides on the surfaces of the small sample by using a pre-grinding machine, grinding the small sample to be flat and bright, and then putting the small sample into absolute ethyl alcohol for standby.
The prepared sample was deposited with a layer of platinum element of about 2 μm on the surface by PVD. The cross-sectional morphology of the substrate after the platinum element is deposited on the surface is shown in figure 1. The platinum-deposited substrate was then subjected to vacuum diffusion at 1050 c for 2 hours.
After vacuum diffusion, a hot dip aluminum plating test was performed. Wherein the temperature of hot dip aluminizing is 710 ℃ and the time is 90s. The cross-sectional morphology of the Pt-Si co-modified aluminide coating, wherein the hot dip aluminizing time was 90s, is shown in fig. 2. And four other control test samples with hot dip coating times of 30s, 60s, 120s and 180s, respectively, were set. Then, the samples after hot dip aluminizing were subjected to vacuum diffusion treatment at 1000℃for 1 hour.
And then carrying out a cyclic oxidation experiment on the sample. The method comprises the following specific steps:
(1) Firing a ceramic crucible: removing volatile matters from the crucible at 1000 ℃ and burning to constant weight;
(2) Sample size measurement: measuring the length, width, height and hole diameter of each sample by using a vernier caliper;
(3) Weighing: the sample was placed in a corresponding ceramic crucible, the weight before oxidation was recorded, and the crucible was placed in a tubular resistance furnace (model SK 2-4-12) for high temperature oxidation. The first 10 cycles, 1, 4, 7, 10 cycles are called emphasis; weighing once every 20 cycles in 20-100 cycles; in 100-250 cycles, weigh once every 50 cycles. The weighing mode of cyclic oxidation is adopted, only the mass of the sample is weighed, and the weight of the crucible and the fallen oxide scale is not calculated. The experiment was performed with an electronic balance to a precision of 0.0001g.
(4) And (3) data processing: according to the experimental data processing of the weight increasing method, the oxidation rate is calculated from the weight increasing variation and the surface area of each sample at different time.
The oxidation weight gain curves for the Pt-Si co-modified aluminide coatings with hot dip times of 30s, 60s, 90s, 120s, and 180s at 1000 c for 250 cycles of oxidation are shown in fig. 3.
As can be seen from FIG. 3, the oxidation weight gain increases rapidly during the first 10 cycles at the initial stage of oxidation, indicating that the oxide is rapidly formed on the surface of the coating, and thus the oxidation kinetics curve rises rapidly, the oxidation kinetics curve rises slowly during 10-40 cycles, and the oxidation weight gain reaches maximum values of 1.87, 1.05, 1.06, 1.31, 1.51mg/cm at 40 cycles, respectively 2 . Pt-Si co-modified aluminideThe hot dip aluminum coating of the object coating has the hot dip aluminum coating time of 30s and 60s, the oxidation weight gain is gradually reduced in 40-250 cycles, and the oxidation weight gain value is respectively 1.35 and 0.58mg/cm in 250 cycles 2 This is due to the oxide layer beginning to flake off, resulting in sample weight loss. The Pt-Si co-modified aluminide coating has the advantages that the hot dip aluminizing time is 90s, the oxidation weight gain is gradually reduced in 40-60 cycles, the oxidation weight loss of a sample is caused by the initial peeling of an oxide layer, the oxidation dynamics curve is slowly increased in 60-150 cycles, the Pt-Si co-modified aluminide coating has the self-healing property, the protective oxide film is regenerated after the initial peeling of the oxide layer, and the oxidation dynamics curve is gradually flattened in 150-250 cycles, so that the coating still has good protective performance. The Pt-Si co-modified aluminide coating has hot dip aluminizing time of 120s and 180s, and the oxidation weight gain is gradually reduced in 40-80 cycles, because the oxide layer begins to peel off, resulting in weight loss of the sample; the oxidation kinetics curve slowly rises in 80-100 cycles, which shows that the Pt-Si co-modified aluminide coating has self-healing property when the hot dip aluminizing time is 120s and 180s, and the protective oxide film is regenerated after the oxide layer begins to peel off; wherein the oxidation weight gain of the 120s coating is reduced when the coating circulates for 100-150 times, which indicates that the coating begins to peel off again and the protection performance is poor; the oxidation kinetics curve tends to be gentle when the cycle is 150-200 times, which indicates that the coating still has good protection performance at the moment, and the oxidation weight gain gradually decreases when the cycle is 200-250 times, which indicates that the oxide film begins to peel off again, and the protection performance becomes poor; the oxidation weight gain gradually decreases when the coating layer of 180s is cycled for 100-250 times, which indicates that the coating layer begins to peel off and the protection performance is poor. From the above analysis, it is found that the high temperature oxidation resistance is best when the hot dip aluminizing time of the Pt-Si co-modified aluminide coating is 90s.
Example 2:
in this example, a K438 nickel-based superalloy was used as the substrate, and the nominal composition is shown in Table 1.
The substrate K438 was cut into small pieces of 10mm by 8mm by 2mm in size by a wire cutting machine, and small round holes of 3.0mm in diameter were drilled in the surface by a drilling machine. And removing oxides on the surfaces of the small sample by using a pre-grinding machine, grinding the small sample to be flat and bright, and then putting the small sample into absolute ethyl alcohol for standby.
The prepared sample was subjected to a hot dip aluminizing test. Wherein the temperature of hot dip aluminizing is 710 ℃ and the time is 30s. The cross-sectional morphology of the substrate after hot dip aluminizing is shown in fig. 4. And four other control test samples with hot dip coating times of 60s, 90s, 120s and 180s, respectively, were set. Then, the samples after hot dip aluminizing were subjected to vacuum diffusion treatment at 1000℃for 1 hour.
And then carrying out a cyclic oxidation experiment on the sample. The method comprises the following specific steps:
(1) Firing a ceramic crucible: removing volatile matters from the crucible at 1000 ℃ and burning to constant weight;
(2) Sample size measurement: measuring the length, width, height and hole diameter of each sample by using a vernier caliper;
(3) Weighing: the sample was placed in a corresponding ceramic crucible, the weight before oxidation was recorded, and the crucible was placed in a tubular resistance furnace (model SK 2-4-12) for high temperature oxidation. The first 10 cycles, 1, 4, 7, 10 cycles are called emphasis; weighing once every 20 cycles in 20-100 cycles; in 100-250 cycles, weigh once every 50 cycles. The weighing mode of cyclic oxidation is adopted, only the mass of the sample is weighed, and the weight of the crucible and the fallen oxide scale is not calculated. The experiment was performed with an electronic balance to a precision of 0.0001g.
(4) And (3) data processing: according to the experimental data processing of the weight increasing method, the oxidation rate is calculated from the weight increasing variation and the surface area of each sample at different time.
The oxidation weight gain curves for the single aluminide coatings at 1000 c for 250 cycles of oxidation for hot dip times of 30s, 60s, 90s, 120s and 180s are shown in fig. 5. As can be seen from FIG. 5, the single aluminide coating, the coating samples with hot dip times of 30s, 60s, 90s, 120s and 180s, showed a rapid increase in the oxidation weight gain during the first 10 cycles of the cyclic oxidation, indicating a rapid oxide formation on the coating surface, and thus a rapid rise in the oxidation profile, a slightly slower rise in the oxidation weight gain profile during the 10-40 cycles, and an oxygen increase during the 40 cyclesThe chemical weight gain reaches the maximum value of 1.75, 1.76, 1.72, 2.23 and 2.06mg/cm respectively 2 . Obviously, the maximum value of the oxidation weight gain of the samples of the single aluminide coating in other hot dip coating times is larger than that of the Pt-Si co-modified aluminide coating except the samples with the hot dip coating time of 30s, which indicates that the Pt-Si co-modified aluminide coating can more effectively slow down the reaction of internal elements and oxygen after a compact oxide film is rapidly generated at high temperature, and has better high-temperature oxidation resistance. A30 s hot dip single aluminide coating sample showed a rapid decrease in oxidation weight gain during the 40-250 cycles and a reduction in oxidation weight gain to 0.38mg/cm at 250 cycles 2 This is due to the exfoliation of the oxide layer, resulting in a dramatic decrease in the oxidation weight gain. The sample of the single aluminide coating hot dip coating for 60 seconds had a gradual decrease in the oxidation weight gain during the 40-80 cycles, due to spalling of the oxide layer, a decrease in the oxidation weight gain, a gradual increase in the oxidation weight gain during the 80-150 cycles, indicating continued formation of an oxide film on the coating surface, and a gradual decrease in the oxidation weight gain during the 150-250 cycles, indicating that the oxide film again began to spall, and the protective properties were poor. The oxidation weight gain of a sample of single aluminide coating hot dip coating for 90 seconds is basically unchanged in 40-250 cycles, and the oxidation weight gain value is 1.60mg/cm in 250 cycles 2 The surface of the coating is rapidly formed with a continuous and compact protective film, and the protective film can greatly reduce the internal diffusion rate of oxygen, plays a role in reducing the oxidation rate of the coating, and ensures that the coating has good high-temperature oxidation resistance. Compared with a coating of Pt-Si co-modified aluminide coating hot dip coating for 90 seconds, (the oxidation weight gain value of the single aluminide coating is obviously increased.) the oxidation weight gain curve of a sample of the single aluminide coating hot dip coating 120 seconds is kept stable in 40-60 cycles, which shows that a continuous and compact oxide film is generated on the surface of the sample, the sample has good protection property, the oxidation weight gain is sharply reduced in 60-250 cycles, which shows that the oxide film generated on the surface of the coating begins to peel off, and the oxidation weight gain is reduced to 0mg/cm in 200 cycles 2 Indicating that the coating had failed at this time and lost protective properties. The oxidation weight gain of the sample subjected to hot dip 180s is slowly reduced in 40-100 cycles, and the oxidation weight gain value is 1.98mg/cm in 100 cycles 2 The coating has good high-temperature oxidation resistance in 40-100 cycles, oxidation weight gain is rapidly reduced in 100-250 cycles, and oxidation weight gain value is reduced to 1.05mg/cm in 250 cycles 2 Indicating that the oxide film formed on the surface rapidly peels off and the protective performance is deteriorated.
From the analysis of examples 1 and 2, it is seen that the Pt-Si co-modified aluminide coating has more excellent high temperature oxidation resistance than the single aluminide coating. In the hot dip aluminizing coating with different time, the high-temperature oxidation resistance of the coating with the hot dip time of 60-90 s is better, and the oxidation resistance of the coating with the hot dip 120s is also better after the Pt-Si is co-modified, which indicates that the hot dip time range of the Pt-Si co-modified to obtain higher oxidation resistance can be enlarged.
According to the method, the content of platinum and silicon is regulated, the structure stability of the coating can be improved by platinum, and the hot corrosion resistance of the coating can be improved by silicon, so that the problem of insufficient high-temperature oxidation resistance of a single aluminide coating is solved, and the use requirement of nickel-based superalloy in increasingly severe service environment is better met.
With the above-described preferred embodiments according to the present invention as an illustration, the above-described descriptions can be used by persons skilled in the relevant art to make various changes and modifications without departing from the scope of the technical idea of the present invention. The technical scope of the present invention is not limited to the description, but must be determined according to the scope of claims.
Claims (8)
1. A preparation method of a Pt-Si co-modified aluminide coating comprises the following steps:
(1) A platinum layer is applied to the surface of the nickel-based superalloy by a magnetron sputtering method, and then the nickel-based superalloy is subjected to vacuum diffusion treatment to obtain the nickel-based superalloy deposited with platinum;
(2) Applying an aluminum-silicon coating on the surface of the nickel-based superalloy platinum layer deposited with platinum in the step (1) by adopting a hot dip plating method;
(3) Carrying out vacuum diffusion treatment on the base body subjected to hot dip plating in the step (2) to obtain a Pt-Si co-modified aluminide coating;
the Pt-Si co-modified aluminide coating comprises the following components in percentage by mass: 10-35% of Ni, 5-10% of Cr, 2-10% of Si, 1-12% of Pt and the balance of Al.
2. The preparation method according to claim 1, wherein the Pt-Si co-modified aluminide coating comprises the following components in percentage by mass: 15-30% of Ni, 6-10% of Cr, 3-6% of Si, 1-8% of Pt and the balance of Al.
3. The preparation method according to claim 2, wherein the Pt-Si co-modified aluminide coating comprises the following components in percentage by mass: 20-25% of Ni, 6-9% of Cr, 4-6% of Si, 1-2% of Pt and the balance of Al.
4. The method according to claim 1, wherein the step (1) is preceded by degreasing and activating the nickel-base superalloy, and removing grease and oxides on the surface of the nickel-base superalloy by degreasing and activating.
5. The method according to claim 1, wherein the platinum layer in the step (1) has a thickness of 1 to 10 μm.
6. The method according to claim 1, wherein the vacuum diffusion treatment in the step (1) is performed at a temperature of 1000 to 1200 ℃ for a time of 2 to 5 hours.
7. The method according to claim 1, wherein the molten pool used in the hot dip plating method is an aluminum-silicon alloy, and the composition thereof is silicon with a mass fraction of 5% and aluminum with a mass fraction of 95%.
8. The method according to claim 1, wherein the vacuum diffusion treatment in the step (3) is performed at a temperature of 950 to 1200 ℃ for a time of 1 to 10 hours.
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