CN113481470A - Pt-Si co-modified aluminide coating and preparation process thereof - Google Patents
Pt-Si co-modified aluminide coating and preparation process thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 104
- 239000011248 coating agent Substances 0.000 title claims abstract description 99
- 229910000951 Aluminide Inorganic materials 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 71
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 33
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 17
- 239000010703 silicon Substances 0.000 claims abstract description 16
- 229910000601 superalloy Inorganic materials 0.000 claims abstract description 16
- 238000009792 diffusion process Methods 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 23
- 239000011651 chromium Substances 0.000 claims description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 12
- 238000007747 plating Methods 0.000 claims description 12
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 11
- 229910052804 chromium Inorganic materials 0.000 claims description 10
- 238000003618 dip coating Methods 0.000 claims description 9
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 239000000956 alloy Substances 0.000 claims description 7
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910000676 Si alloy Inorganic materials 0.000 claims description 2
- 238000005240 physical vapour deposition Methods 0.000 claims 2
- 230000003213 activating effect Effects 0.000 claims 1
- 239000004519 grease Substances 0.000 claims 1
- 238000001755 magnetron sputter deposition Methods 0.000 claims 1
- 239000003921 oil Substances 0.000 claims 1
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- 238000007254 oxidation reaction Methods 0.000 abstract description 91
- 230000003647 oxidation Effects 0.000 abstract description 89
- 238000005260 corrosion Methods 0.000 abstract description 8
- 230000007797 corrosion Effects 0.000 abstract description 8
- 239000011253 protective coating Substances 0.000 abstract description 2
- 230000004584 weight gain Effects 0.000 description 39
- 235000019786 weight gain Nutrition 0.000 description 39
- 239000000758 substrate Substances 0.000 description 20
- 238000005303 weighing Methods 0.000 description 19
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- 238000002474 experimental method Methods 0.000 description 10
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- 239000000919 ceramic Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 125000004122 cyclic group Chemical group 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000003818 cinder Substances 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000008021 deposition Effects 0.000 description 2
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- 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
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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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
-
- 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
-
- 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
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 process thereof, wherein 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 and 1-12% of Pt, and the balance of Al. According to the preparation method, the platinum can improve the tissue stability of the coating by adjusting the contents of the platinum and the silicon, and the silicon can improve the hot corrosion resistance of the coating, so that the problem that the high-temperature oxidation resistance of a single aluminide coating is insufficient is solved, and the use requirement of the nickel-based superalloy in an increasingly severe service environment is better met.
Description
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 process 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 property can be applied on the surface of the K438 alloy.
Hot dip aluminizing is an efficient method for implementing aluminide coating, has the advantages of high production efficiency, low cost, simple operation, long effective protection period and the like, and is widely applied to diffusion coating preparation. However, single aluminide coatings tend to 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 that the single aluminide coating is insufficient in high-temperature oxidation resistance.
In order to solve the technical problem, the application adopts a technical scheme that: 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 and 1-12% of Pt, and the balance of Al.
In order to solve the above technical problem, another technical solution adopted by the present application is: provides a preparation process of a Pt-Si co-modified aluminide coating.
The beneficial effect of this application is: according to the method, the Pt-Si co-modified aluminide coating contains 10-35% by mass of nickel, 5-10% by mass of chromium, 2-10% by mass of silicon and 1-12% by mass of platinum, and the nickel with relatively high content can improve the high-temperature creep resistance of the aluminide coating, wherein the coating contains 5-10% by mass of chromium, so that the coating can form Cr with a protection effect in oxidation2O3Film, and appropriate amounts of platinum and silicon are added. Platinum can improve the structure stability of the aluminide coating, and 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 solved by preparing the components of the coating according to the proportionAnd better meets the heavy use requirement of the nickel-based high-temperature alloy in increasingly severe service environment.
Drawings
FIG. 1 is a cross-sectional view of the subject PVD after platinization;
FIG. 2 is a cross-sectional and compositional profile scan of a Pt-Si co-modified aluminide coating in accordance with the present application;
FIG. 3 is a graph of Pt-Si co-modified aluminide coatings of the present application at 1000 deg.C for 250 cycles of oxidation;
FIG. 4 is a cross-sectional and compositional profile scan of a single aluminide coating according to the present application;
FIG. 5 is a graph of the oxidation of a single aluminide coating of the present application at 1000 ℃ for 250 cycles.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The Pt-Si co-modified aluminide coating described in the examples of 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 and 1-12% of Pt, and the balance of Al.
The relatively high amounts of chromium and aluminum described above enable the coating to form Cr in oxidation2O3And Al2O3The film can prevent oxygen from corroding the substrate, and form good protection on the substrate, so that the high-temperature oxidation resistance of the substrate is improved, the high-temperature creep resistance of the coating can be improved by the nickel with the content, the hot corrosion resistance of the coating can be improved by adding the silicon with the content on the basis of the aluminum, the nickel and the chromium with the content in the proportion, and the hot corrosion resistance of the coating can be improved by adding the platinum with the content2O3The anti-stripping capability and the structure stability of the aluminide coating, thereby improving the high-temperature oxidation resistance of the coating. The scheme of the application is through cooperative configurationThe mass percentages of the elements such as nickel, chromium, platinum, silicon and the like can effectively solve the problem that the single aluminide coating has insufficient high-temperature oxidation resistance.
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 configuring the chromium with the mass percent of 6-10%, the service life of the coating is prolonged, and the corrosion resistance of the coating can be further improved by configuring the nickel with the mass percent of 15-30% 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, the heat corrosion resistance of the coating can be improved by configuring the nickel element with each mass percentage, the chromium element and the aluminum element can provide a protective film for the nickel-based superalloy and delay the oxidation of a matrix, the heat corrosion resistance of the coating can be improved by adding silicon, and the Al can be improved by adding platinum2O3The anti-stripping capability of the coating can provide good protection for the nickel-based superalloy by configuring the content of the elements.
The preparation process of the Pt-Si co-modified aluminide coating comprises the following steps:
(1) and applying a platinum layer on the surface of the nickel-based superalloy by adopting the PVD method, and then performing vacuum diffusion treatment on the platinum layer.
Wherein the thickness of the applied platinum layer is 1-10 μm, the temperature of the vacuum diffusion treatment is 1000-1200 ℃, and the time is 2-5 hours. The cross-sectional structure morphology of the platinum-coated nickel-base superalloy is shown in fig. 1 by SEM testing.
First, the nickel-base superalloy is cut into chips having a size of 10mm × 8mm × 2mm by a wire cutter, or into chips having other sizes, which are not limited herein, and then the chips are used as a substrate. The type of nickel-base superalloy may be various, for example, the nickel-base superalloy may be K438, which is not limited herein. Then, a drilling machine is used for drilling a small round hole with the diameter of phi 3.0mm on the surface of the substrate. Removing oxides on the surface of the substrate by using a pre-grinding machine, polishing the substrate to be flat and bright, and then putting the substrate into absolute ethyl alcohol for later use.
The prepared substrate is divided into two groups, wherein one group is used for depositing a layer of platinum element on the surface by a PVD method, and the thickness of the platinum layer can 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 1-10 μm, for example, the thickness of the platinum layer may be 2-9 μm, 3-8 μm, 4-7 μm, or 5-6 μm. Then, the substrate deposited with the platinum element is subjected to vacuum diffusion, wherein the temperature of the vacuum diffusion can be 1000-1200 ℃, and the time can be 2-5 hours, for example, the temperature of the vacuum diffusion is 1050 ℃, and the time is 2 hours. The temperature of the vacuum diffusion can be in other ranges of 1000-1200 ℃, for example, the temperature of the vacuum diffusion can be 1000-1100 ℃, 1050-1150 ℃ or 1100-1200 ℃. The time for vacuum diffusion may be in other ranges of 2-5 hours, for example, the time for vacuum diffusion may be 2-4 hours, 3-5 hours, 3.5-5 hours, or 4-5 hours. And carrying out hot dip aluminizing test after vacuum diffusion.
The other group of substrates directly carry out the hot dip aluminizing test without platinum element deposition.
When a hot dip aluminum plating test is performed on a substrate deposited with platinum element and a substrate not deposited with platinum element, the hot dip plating temperature is 700-. And performing vacuum diffusion treatment on the two groups of samples subjected to hot dip aluminum plating, wherein the temperature of the vacuum diffusion is 950-1200 ℃, and the time is 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-. The vacuum diffusion time is in other ranges of 1-10h, for example, the vacuum diffusion time is 2-9h, 3-8h, 4-7h or 5-6 h.
The molten pool used in the hot dip coating method is an aluminum-silicon alloy, and the components of the molten pool are 2-10% of silicon and 90-98% of aluminum by mass fraction, for example, the components of the molten pool are 5% of silicon and 95% of aluminum by mass fraction.
The two sets of samples were then subjected to an oxidation experiment. The experiment employed a cyclic oxidation method. And three parallel samples are arranged on the coating under the same process condition for carrying out a cyclic oxidation experiment so as to ensure the accuracy of subsequent weighing data. And (3) oxidizing the sample in static air of a high-temperature furnace for 50min, air cooling for 10min to form a cycle, wherein the total time is 250 cycles, and the temperature of the cyclic oxidation experiment is 1000 ℃. The following are the specific experimental procedures:
(1) firing of the ceramic crucible: removing volatile substances from the crucible at 1000 ℃ and burning the crucible to constant weight;
(2) and (3) measuring the size of the sample: 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 and the pre-oxidation weight 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 and 10 cycles are called key points; weighing every 20 cycles in 20-100 cycles; in 100-250 cycles, weighing is performed every 50 cycles. The weight gain value was taken as the average measurement of 3 parallel samples. All data are recorded in a designed table. And only weighing the mass of the sample by adopting a weighing mode of circular oxidation, wherein the weight of the crucible and the scale cinder which falls off is not counted. The weighing experiment was carried out using an electronic balance with an accuracy of 0.0001 g.
(4) Data processing: and (4) according to the experimental data processing of a weight gain method, calculating the oxidation rate according to the weight gain variable quantity and the surface area of each sample at different time.
Example 1:
the substrate in this example was a K438 Ni-base superalloy with the nominal composition shown in Table 1.
TABLE 1 nominal composition of K438 Ni-base superalloys
The substrate K438 was cut into small pieces of 10 mm. times.8 mm. times.2 mm in size by a wire cutter, and a small round hole of 3.0mm in diameter was drilled on the surface thereof by a drill. And removing oxides on the surface of the small sample by using a pre-grinding machine, polishing the small sample to be flat and bright, and then putting the small sample into absolute ethyl alcohol for later use.
The prepared sample is deposited with a layer of platinum element with the diameter of about 2 mu m on the surface by a PVD method. The cross-sectional morphology of the substrate after platinum element deposition on the surface is shown in FIG. 1. Then, the substrate on which platinum is deposited is subjected to vacuum diffusion at 1050 ℃ for 2 hours.
And carrying out hot dip aluminizing test after vacuum diffusion. Wherein the temperature of hot dip aluminum plating is 710 ℃ and the time is 90 s. The Pt-Si co-modified aluminide coating has the cross-sectional morphology of the coating with the hot dip aluminizing time of 90s shown in FIG. 2. And the hot dip plating times were set to four other control test samples of 30s, 60s, 120s, and 180s, respectively. Then, the sample after hot dip aluminizing was subjected to vacuum diffusion treatment at 1000 ℃ for 1 hour.
The samples were then subjected to cyclic oxidation experiments. The method comprises the following specific steps:
(1) firing of the ceramic crucible: removing volatile substances from the crucible at 1000 ℃ and burning the crucible to constant weight;
(2) and (3) measuring the size of the sample: 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 and the pre-oxidation weight 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 and 10 cycles are called key points; weighing every 20 cycles in 20-100 cycles; in 100-250 cycles, weighing is performed every 50 cycles. And only weighing the mass of the sample by adopting a weighing mode of circular oxidation, wherein the weight of the crucible and the scale cinder which falls off is not counted. The weighing experiment was carried out using an electronic balance with an accuracy of 0.0001 g.
(4) Data processing: and (4) according to the experimental data processing of a weight gain method, calculating the oxidation rate according to the weight gain variable quantity and the surface area of each sample at different time.
The oxidation weight gain curves of Pt-Si co-modified aluminide coatings with hot dip coating times of 30s, 60s, 90s, 120s and 180s at 1000 ℃ and 250 cycles of oxidation are shown in FIG. 3.
As can be seen from FIG. 3, the oxidation weight gain rapidly increased in the first 10 cycles of the initial oxidation period, indicating that the oxide is rapidly formed on the surface of the coating, so the oxidation kinetic curve rapidly increased, and the oxidation kinetic curve increased slowly in 10-40 cycles, and the oxidation weight gain reached the maximum values at 40 cycles, which are 1.87, 1.05, 1.06, 1.31, and 1.51mg/cm2. The Pt-Si co-modified aluminide coating is coated on the coating with the hot dip aluminizing time of 30s and 60s, the oxidation weight gain is gradually reduced in 40-250 cycles, and the oxidation weight gain values are 1.35 and 0.58mg/cm respectively in 250 cycles2This is due to the fact that the oxide layer starts to flake off, resulting in a loss of weight of the sample. The coating with the Pt-Si co-modified aluminide coating hot-dip aluminizing time of 90s is characterized in that oxidation weight gain is gradually reduced in 40-60 cycles because an oxidation layer begins to peel off to cause sample weight loss, an oxidation kinetic curve slowly rises in 60-150 cycles, the coating with the Pt-Si co-modified aluminide coating hot-dip aluminizing time of 90s has self-healing property, a protective oxidation film is regenerated after the oxidation layer begins to peel off, the oxidation kinetic curve tends to be gentle in 150-250 cycles, and the coating still has good protective performance. The Pt-Si co-modified aluminide coating is a coating with the hot dip aluminizing time of 120s and 180s, and the oxidation weight gain is gradually reduced in 40-80 cycles, because an oxidation layer begins to peel off, so that the sample is weightless; when the cycle is 80-100 times, the oxidation kinetic curve slowly rises, which shows that the coating with the Pt-Si co-modified aluminide coating hot-dip aluminizing time of 120s and 180s has self-healing property, and a protective oxide film is regenerated after the oxide layer begins to peel off; wherein, the oxidation weight gain of the coating of 120s is reduced when the coating is cycled for 100-150 times, which indicates that the coating begins to peel off again and the protective performance is deteriorated; when the cycle is 200 times and 150 times, the oxidation kinetic curve tends to be flat, which shows that the coating still has good protective performance, and when the cycle is 250 times and 200 times, the oxidation weight gain is gradually reduced, which shows that the oxide film begins to peel off again, and the protective performance is deteriorated; the oxidation weight gain of the 180s coating gradually decreased during the 100-250 cycles, which indicates that the coating begins to peel off and the protective performance is deteriorated. From the above analysis, when the hot dip aluminum plating time of the Pt-Si co-modified aluminide coating is 90s,the high temperature oxidation resistance is the best.
Example 2:
the substrate in this example was a K438 Ni-base superalloy with the nominal composition shown in Table 1.
The substrate K438 was cut into small pieces of 10 mm. times.8 mm. times.2 mm in size by a wire cutter, and a small round hole of 3.0mm in diameter was drilled on the surface thereof by a drill. And removing oxides on the surface of the small sample by using a pre-grinding machine, polishing the small sample to be flat and bright, and then putting the small sample into absolute ethyl alcohol for later use.
The prepared sample was subjected to a hot dip aluminizing test. Wherein the temperature of hot dip aluminum plating is 710 ℃ and the time is 30 s. The cross-sectional profile of the substrate after hot dip aluminizing is shown in fig. 4. And the hot dip plating times were set at 60s, 90s, 120s, and 180s, respectively. Then, the sample after hot dip aluminizing was subjected to vacuum diffusion treatment at 1000 ℃ for 1 hour.
The samples were then subjected to cyclic oxidation experiments. The method comprises the following specific steps:
(1) firing of the ceramic crucible: removing volatile substances from the crucible at 1000 ℃ and burning the crucible to constant weight;
(2) and (3) measuring the size of the sample: 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 and the pre-oxidation weight 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 and 10 cycles are called key points; weighing every 20 cycles in 20-100 cycles; in 100-250 cycles, weighing is performed every 50 cycles. And only weighing the mass of the sample by adopting a weighing mode of circular oxidation, wherein the weight of the crucible and the scale cinder which falls off is not counted. The weighing experiment was carried out using an electronic balance with an accuracy of 0.0001 g.
(4) Data processing: and (4) according to the experimental data processing of a weight gain method, calculating the oxidation rate according to the weight gain variable quantity and the surface area of each sample at different time.
The oxidation weight gain curves of the single aluminide coatings with hot dip coating times of 30s, 60s, 90s, 120s and 180s at 1000 ℃ and 250 cycles of oxidation are shown in FIG. 5.As can be seen from FIG. 5, the oxidation weight gain of the single aluminide coating and the coating samples with hot dip coating time of 30s, 60s, 90s, 120s and 180s all increased rapidly in 10 cycles of the initial cycle oxidation period, which indicates that the oxide is rapidly generated on the coating surface, so the oxidation curve rises rapidly, the rising speed of the oxidation weight gain curve is slightly slowed down in 10-40 cycles, and the oxidation weight gain reaches the maximum values of 1.75, 1.76, 1.72, 2.23 and 2.06mg/cm at 40 cycles2. Obviously, in addition to the sample with the hot dipping time of 30s, the maximum oxidation weight gain value of the sample with the single aluminide coating in other hot dipping times is larger than that of the Pt-Si co-modified aluminide coating, which shows 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. The sample of single aluminide coating hot dip plated for 30s has a rapid reduction in oxidation weight gain during 40-250 cycles and a reduction in oxidation weight gain to 0.38mg/cm at 250 cycles2This is due to the oxide layer flaking off, resulting in a sharp decrease in the oxide weight gain. In the sample of the single aluminide coating hot dip coating for 60s, the oxidation weight gain is gradually reduced during 40-80 cycles, which is caused by the peeling of the oxidation layer, so that the oxidation weight gain is reduced, the oxidation weight gain is gradually increased during 80-150 cycles, which indicates that the oxidation film continues to be generated on the surface of the coating, and the oxidation weight gain is gradually reduced during 150-250 cycles, which indicates that the oxidation film begins to peel again, so that the protection performance is deteriorated. The oxidation weight gain of the sample hot dip coated with the single aluminide coating for 90s is basically unchanged within 40-250 cycles, and the oxidation weight gain value is 1.60mg/cm at 250 cycles2The continuous and compact protective film is rapidly generated on the surface of the coating, and the protective film can greatly reduce the oxygen internal diffusion rate, plays a role in reducing the oxidation rate of the coating and enables the coating to have good high-temperature oxidation resistance. Compared with the coating with the Pt-Si co-modified aluminide coating hot dip coating for 90s, (the oxidation weight gain value of the single aluminide coating is obviously increased, in the sample with the single aluminide coating hot dip coating for 120s, the oxidation weight gain curve is kept stable within 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 performance, and in 60-250 cyclesIn the ring, the oxidation weight gain is reduced sharply, which indicates 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 at 200 cycles2Indicating that the coating has failed and lost protective properties. The sample hot-dip plated for 180s has the oxidation weight gain slowly reduced within 40-100 cycles, and the oxidation weight gain value is 1.98mg/cm at 100 cycles2The coating has good high-temperature oxidation resistance in 40-100 cycles, the oxidation weight gain is rapidly reduced in 100-250 cycles, and the oxidation weight gain value is reduced to 1.05mg/cm in 250 cycles2The oxide film formed on the surface was rapidly peeled off, and the protective performance was deteriorated.
From the analysis of examples 1 and 2, it can be seen that the Pt-Si co-modified aluminide coating has superior high temperature oxidation resistance to a single aluminide coating. In the hot dip aluminum plating coatings at different times, the coating with the hot dip plating time of 60-90s has better high-temperature oxidation resistance, and after Pt-Si co-modification, the oxidation resistance of the hot dip 120s coating is also better, which shows that the hot dip plating time range of obtaining higher oxidation resistance by Pt-Si co-modification can be enlarged.
According to the preparation method, the platinum can improve the tissue stability of the coating by adjusting the contents of the platinum and the silicon, and the silicon can improve the hot corrosion resistance of the coating, so that the problem that the high-temperature oxidation resistance of a single aluminide coating is insufficient is solved, and the use requirement of the nickel-based superalloy in an increasingly severe service environment is better met.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (9)
1. A Pt-Si co-modified aluminide coating, characterized by: the paint comprises the following components in percentage by mass: 10-35% of Ni, 5-10% of Cr, 2-10% of Si and 1-12% of Pt, and the balance of Al.
2. The Pt-Si co-modified aluminide coating of claim 1, wherein: the mass percent of the nickel is further 15-30%, the mass percent of the chromium is further 6-10%, the mass percent of the silicon is further 3-6%, and the mass percent of the platinum is further 1-8%.
3. The Pt-Si co-modified aluminide coating of claim 2, wherein: the mass percent of the nickel is further 20-25%, the mass percent of the chromium is further 6-9%, the mass percent of the silicon is further 4-6%, and the mass percent of the platinum is further 1-2%.
4. A preparation process of a Pt-Si co-modified aluminide coating is characterized by comprising the following steps: firstly, applying a platinum layer on a nickel-based high-temperature alloy by adopting a magnetron sputtering (PVD) method, then applying an aluminum-silicon coating on the surface of the nickel-based high-temperature alloy by adopting a hot dip coating method, and finally obtaining the Pt-Si co-modified aluminide coating; the method specifically comprises the following steps:
(1) applying a platinum layer on the surface of the nickel-based superalloy by adopting the PVD method, and then performing vacuum diffusion treatment on the platinum layer;
(2) applying an aluminum-silicon coating on the alloy surface in the step (1) by adopting the hot dip plating method;
(3) and (3) carrying out vacuum diffusion treatment on the alloy in the step (2).
5. The process according to claim 4, characterized in that: the method is characterized in that the method also comprises the steps of (1) removing oil and activating the nickel-based superalloy, and removing grease and oxides on the surface of the nickel-based superalloy through pretreatment.
6. The process according to claim 4, characterized in that: the thickness of the platinum layer in the step (1) is 1-10 μm.
7. The process according to claim 4, characterized in that: the temperature of the vacuum diffusion treatment in the step (1) is 1000-1200 ℃, and the time is 2-5 hours.
8. The process according to claim 4, characterized in that: the molten pool adopted in the hot dip coating method is aluminum-silicon alloy, and the components of the molten pool are 5 mass percent of silicon and 95 mass percent of aluminum.
9. The process according to claim 4, characterized in that: the temperature of the vacuum diffusion treatment in the step (3) is 950-.
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| 刘培生: "《钴基合金铝化物涂层的高温氧化行为》", 31 January 2008, 冶金工业出版社 * |
| 宁愿涛等: "《铂》", 31 March 2010, 冶金工业出版社 * |
| 材料科学技术百科全书编辑委员会编, 中国大百科全书出版社 * |
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