CN111961908A - Preparation method for in-situ generation of binary boride reinforced noble metal high-temperature alloy - Google Patents
Preparation method for in-situ generation of binary boride reinforced noble metal high-temperature alloy Download PDFInfo
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- CN111961908A CN111961908A CN202010879145.9A CN202010879145A CN111961908A CN 111961908 A CN111961908 A CN 111961908A CN 202010879145 A CN202010879145 A CN 202010879145A CN 111961908 A CN111961908 A CN 111961908A
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- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 43
- 239000000956 alloy Substances 0.000 title claims abstract description 32
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 26
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 22
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000137 annealing Methods 0.000 claims abstract description 9
- 238000005266 casting Methods 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000003723 Smelting Methods 0.000 claims abstract description 5
- 239000011812 mixed powder Substances 0.000 claims abstract description 5
- 238000010791 quenching Methods 0.000 claims abstract description 4
- 230000000171 quenching effect Effects 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 12
- 229910000601 superalloy Inorganic materials 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 229910052741 iridium Inorganic materials 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052703 rhodium Inorganic materials 0.000 claims description 3
- 239000010948 rhodium Substances 0.000 claims description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052707 ruthenium Inorganic materials 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052702 rhenium Inorganic materials 0.000 claims description 2
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 2
- 239000010970 precious metal Substances 0.000 claims 6
- 238000002844 melting Methods 0.000 abstract description 6
- 230000008018 melting Effects 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 239000011159 matrix material Substances 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
- C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/04—Alloys based on a platinum group metal
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
Abstract
The invention relates to the technical field of high-temperature alloys, and particularly discloses a preparation method of a binary boride reinforced noble metal high-temperature alloy, which comprises the steps of carrying out ball milling on noble metal powder and boron powder, wherein the molar ratio of the noble metal powder to the boron powder is more than 2:1, and the noble metal powder is single noble metal powder or the mixture of multiple noble metal powders; smelting the mixed powder subjected to ball milling by using a vacuum arc melting furnace, and casting into a sample; and annealing the sample at 1200-1650 ℃, and quenching to room temperature to obtain the in-situ generated binary boride reinforced noble metal high-temperature alloy. The high-temperature alloy can still keep good high-temperature creep and oxidation resistance at the high temperature of more than 1200 ℃.
Description
Technical Field
The invention relates to the technical field of high-temperature alloys, in particular to a preparation method of a binary boride reinforced noble metal high-temperature alloy generated in situ.
Background
With the development of fields such as modern scientific research, aerospace industry, military industry and the like, the flying speed of aircrafts, aircrafts and the like is higher and higher, and the high-temperature alloy material also has higher requirements on the performance of the high-temperature alloy material, the traditional high-temperature alloy is most widely applied as a nickel-based high-temperature alloy, although the melting point of the nickel-based high-temperature alloy is higher, the nickel-based high-temperature alloy material actually has a softening phenomenon and gradually has the problem of high-temperature creep when being in service for a long time in an environment with the melting point of about 80%, namely under the condition of long-term high-temperature stress, the crystal boundary in the material migrates, so that the high-temperature alloy material has the problems of softening and failure, and the high-temperature.
The noble metals are ruthenium, rhodium, palladium, silver, osmium, iridium, platinum and gold, most of the metals have extremely high melting points and strong chemical stability, and have the potential of becoming a new-generation high-temperature alloy.
Disclosure of Invention
The invention provides a preparation method of a binary boride reinforced noble metal high-temperature alloy in situ, which is used for obtaining a high-temperature alloy with good creep resistance and oxidation resistance at a higher temperature.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a binary boride reinforced noble metal high-temperature alloy in situ comprises the following steps:
step 1: ball-milling noble metal powder and boron powder, wherein the molar ratio of the noble metal powder to the boron powder is more than 2:1, and the noble metal powder is single noble metal powder or mixture of a plurality of noble metal powders;
step 2: smelting the mixed powder subjected to ball milling in the step 1 by using a vacuum arc smelting furnace, and casting into a sample;
and step 3: and (3) annealing the sample obtained in the step (2) at 1200-1650 ℃, and quenching to room temperature to obtain the in-situ generated binary boride reinforced noble metal high-temperature alloy.
The technical principle and the effect of the technical scheme are as follows:
1. in the application, because the molar ratio of the noble metal powder to the boron powder is greater than 2:1, boron and the noble metal form binary boride, and boron does not extract charges from metal atoms in a matrix but forms covalent bonds, the binary boride can increase the cohesive force at the grain boundary and achieve the effect of strengthening the grain boundary or phase boundary. The binary boride is used as a strengthening phase in the noble metal, has excellent physical and chemical properties, can be well combined with the matrix noble metal high-temperature alloy, and can well improve the high-temperature performance of the alloy by adding the boron element.
2. The binary boride reinforced noble metal obtained in the scheme can also be used as a coating, so that the cost can be reduced, and meanwhile, the high-temperature performance of a base material can be ensured.
Further, in the step 1, during ball grinding, the ball-material ratio is 10:1 to 15:1, the grinding aid is absolute ethyl alcohol, and the ball grinding time is not less than 2 hours.
Has the advantages that: this arrangement can further improve the uniformity of grinding of the powder.
Further, a water-cooling copper mold is adopted for casting in the step 2, and the cooling rate of casting is 5-10K s-1In the meantime.
Has the advantages that: under the speed setting, the structure of a cast sample can be ensured to be uniform, and the binary boride is uniformly distributed at the grain boundary of the noble metal matrix.
Further, the annealing time in the step 3 is 12-24 hours.
Has the advantages that: sufficient annealing time is provided to ensure that the stress between the binary boride and the noble metal matrix is fully relaxed.
Further, the noble metal powder is one or a mixture of rhenium, ruthenium, rhodium, palladium, iridium or platinum.
Has the advantages that: the noble metals can meet the high-temperature performance of the alloy.
Further, the purity of the noble metal powder and the boron powder is higher than 99.99%.
Has the advantages that: thus reducing the introduction of impurity elements and improving the high-temperature performance of the alloy material.
Further, the binary boride reinforced noble metal high-temperature alloy generated in situ can be used as a coating material.
Drawings
FIG. 1 is a high temperature nanoindentation graph for inventive example 1, example 11, and comparative example 3.
Detailed Description
The following is further detailed by way of specific embodiments:
example 1:
a preparation method of a binary boride reinforced noble metal high-temperature alloy in situ comprises the following steps:
step 1: weighing iridium powder and boron powder with the purity of more than 99.99 percent (mass fraction) according to the molar ratio of 2.5:1, mixing the materials, putting the powder into a ball milling tank, and mixing the materials by adopting a planetary ball mill, wherein the ball-material ratio is 10:1, and the ball milling time is 3 hours.
Step 2: taking out the mixed powder obtained in the step 1, putting the mixed powder into a copper crucible of a vacuum arc melting furnace, melting under the protection of argon, continuously treating the melt through electromagnetic stirring to completely homogenize the melt, refining a precipitated phase (BIr) and a matrix structure, casting by adopting a water-cooling copper mold to obtain a sample, wherein the cooling rate is 5K s-1。
And step 3: and (3) annealing the sample obtained by casting in the step (2) for 24h at 1650 ℃ in an argon atmosphere, and then quenching to room temperature to obtain the BIr reinforced noble metal iridium high-temperature alloy material generated in situ.
Examples 2 to 10:
the difference from the example 1 is that the mixture ratio and the process parameters of the examples 2 to 10 are different, and the details are shown in the table 1.
Table 1 shows the formulation and process parameters of examples 2 to 10 (in the table, "-" means none)
Comparative example 1:
the difference from example 1 is that the annealing temperature in step 3 is 1100 ℃.
Comparative example 2:
the difference from example 1 is that the annealing temperature in step 3 is 2000 ℃.
Comparative example 3:
is a common nickel-based high-temperature alloy with the mark GH 4099.
Example 11:
the in-situ formed BIr strengthened noble metal iridium superalloy prepared in example 1 was deposited on the surface of the nickel-base superalloy in comparative example 3 to a thickness of about 10 μm.
The high-temperature alloys of examples 1 to 11 and comparative examples 1 to 3 were prepared into samples for high-temperature nanoindentation detection at 1250 ℃. The high-temperature nano indentation creep experiment can press a sample in through a nano pressure head at an extremely high temperature, the nano pressure head continuously increases the pressing force in the process to continuously press the sample in and record the pressing depth, and the sample can rapidly exit after the sample cannot bear the pressure of the pressure head and fails. The high-temperature nanoindentor can visually observe the high-temperature creep condition of the tested sample, and is a very reliable high-temperature creep measuring instrument at the present stage.
Taking examples 1 and 11 and comparative example 3 as examples, the high temperature nanoindentation curves are shown in fig. 1, and it can be observed that: at 1250 ℃, after the nano pressure head is pressed into the sample of the comparative example 3, the pressure head is quickly withdrawn after being pressed in, and the sample of the comparative example 3 is completely invalid; while the samples of example 1 and example 11 have three stages: the first stage is longer, the sample keeps good creep property under the pressure of the pressure head, the creep deformation at the second stage is rapidly developed, the pressure head is rapidly pressed into the sample, the third stage enters into a creep deformation period, the pressure head is continuously pressurized until the material is damaged and fails, the sample of example 11 is influenced by factors such as the thickness of the coating, the performance of the matrix, the thermal expansion of the two materials and the like, the mechanical property is slightly reduced compared with that of the sample of example 1, and the original high-temperature performance can still be kept.
Therefore, it can be found that the sample of comparative example 3 can not bear the pressure head pressure and thus can not be failed in a very short time at 1250 ℃, which indicates that at the ultrahigh temperature, the nickel-based superalloy can not maintain good mechanical properties and can not bear higher load, while the samples of example 1 and example 11 can maintain good mechanical properties at 1250 ℃ and can not be failed for a long time, and have excellent high temperature resistance.
The foregoing is merely an example of the present invention and common general knowledge of the known specific materials and characteristics thereof has not been described herein in any greater extent. It should be noted that, for those skilled in the art, without departing from the scope of the invention, several variations and modifications can be made, which should also be regarded as the protection scope of the invention, and these will not affect the effect of the implementation of the invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (7)
1. A preparation method of a binary boride reinforced noble metal high-temperature alloy in situ is characterized by comprising the following steps: the method comprises the following steps:
step 1: ball-milling noble metal powder and boron powder, wherein the molar ratio of the noble metal powder to the boron powder is more than 2:1, and the noble metal powder is single noble metal powder or mixture of a plurality of noble metal powders;
step 2: smelting the mixed powder subjected to ball milling in the step 1 by using a vacuum arc smelting furnace, and casting into a sample;
and step 3: and (3) annealing the sample obtained in the step (2) at 1200-1650 ℃, and quenching to room temperature to obtain the in-situ generated binary boride reinforced noble metal high-temperature alloy.
2. The method for preparing the in-situ generated binary boride reinforced precious metal superalloy as claimed in claim 1, wherein the method comprises the following steps: in the step 1, during ball grinding, the ball-material ratio is 10:1 to 15:1, the grinding aid is absolute ethyl alcohol, and the ball grinding time is not less than 2 hours.
3. The method for preparing the in-situ generated binary boride reinforced precious metal superalloy as claimed in claim 1, wherein the method comprises the following steps: and 2, adopting a water-cooling copper mold for casting, wherein the cooling rate of casting is 5-10K s-1In the meantime.
4. The method for preparing the in-situ generated binary boride reinforced precious metal superalloy as claimed in claim 1, wherein the method comprises the following steps: the annealing time in the step 3 is 12-24 hours.
5. The method for preparing the in-situ generated binary boride reinforced precious metal superalloy as claimed in claim 1, wherein the method comprises the following steps: the noble metal powder is one or a mixture of rhenium, ruthenium, rhodium, palladium, iridium or platinum.
6. The method for preparing the in-situ generated binary boride reinforced precious metal superalloy as claimed in claim 1, wherein the method comprises the following steps: the purities of the noble metal powder and the boron powder are higher than 99.99%.
7. The method for preparing the in-situ generated binary boride reinforced precious metal superalloy as claimed in claim 1, wherein the method comprises the following steps: the binary boride reinforced noble metal high-temperature alloy generated in situ can be used as a coating material.
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Citations (6)
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|---|---|---|---|---|
| US20020114725A1 (en) * | 2000-05-19 | 2002-08-22 | Miles Melvin H. | Palladium-boron alloys and methods for making and using such alloys |
| CA2561865A1 (en) * | 2004-05-10 | 2005-12-01 | Deringer-Ney, Inc. | Palladium alloy |
| CN101633985A (en) * | 2009-05-21 | 2010-01-27 | 瑞科稀土冶金及功能材料国家工程研究中心有限公司 | Preparation method of RE-Fe-B part hydrogen storage alloy |
| CN105950952A (en) * | 2016-07-06 | 2016-09-21 | 昆明理工大学 | Production method for in-situ generation of titanium zirconium boride reinforced high-modulus and high-hardness steel |
| CN108118190A (en) * | 2016-11-29 | 2018-06-05 | 沈阳黎明航空发动机(集团)有限责任公司 | A kind of environment resistant deposit corrosion thermal barrier coating and preparation method thereof |
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-
2020
- 2020-08-27 CN CN202010879145.9A patent/CN111961908B/en active Active
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| US20020114725A1 (en) * | 2000-05-19 | 2002-08-22 | Miles Melvin H. | Palladium-boron alloys and methods for making and using such alloys |
| CA2561865A1 (en) * | 2004-05-10 | 2005-12-01 | Deringer-Ney, Inc. | Palladium alloy |
| CN101633985A (en) * | 2009-05-21 | 2010-01-27 | 瑞科稀土冶金及功能材料国家工程研究中心有限公司 | Preparation method of RE-Fe-B part hydrogen storage alloy |
| CN105950952A (en) * | 2016-07-06 | 2016-09-21 | 昆明理工大学 | Production method for in-situ generation of titanium zirconium boride reinforced high-modulus and high-hardness steel |
| CN108118190A (en) * | 2016-11-29 | 2018-06-05 | 沈阳黎明航空发动机(集团)有限责任公司 | A kind of environment resistant deposit corrosion thermal barrier coating and preparation method thereof |
| CN110144482A (en) * | 2019-06-24 | 2019-08-20 | 昆明理工大学 | A kind of rare earth enhancing palldium alloy and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| DAO CHI TUE、TE-KANG TSAO等: "Microstructure and Oxidation Behavior of Pt and PtIr Diffusion Coatings on Ni-Based Single Crystal Superalloy", 《MATERIALS TRANSACTIONS》 * |
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