CN112458416A - Method for preparing quinary high-entropy alloy spinel coating by magnetron sputtering method - Google Patents
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- 238000000576 coating method Methods 0.000 title claims abstract description 61
- 239000011248 coating agent Substances 0.000 title claims abstract description 60
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 45
- 239000000956 alloy Substances 0.000 title claims abstract description 45
- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 30
- 239000011029 spinel Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000001755 magnetron sputter deposition Methods 0.000 title claims description 7
- 238000004544 sputter deposition Methods 0.000 claims abstract description 49
- 239000011159 matrix material Substances 0.000 claims abstract description 22
- 238000000151 deposition Methods 0.000 claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 230000008021 deposition Effects 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 7
- 230000003647 oxidation Effects 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 22
- 229910001220 stainless steel Inorganic materials 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 238000005488 sandblasting Methods 0.000 claims description 7
- 239000013077 target material Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- 239000004576 sand Substances 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000000446 fuel Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 7
- 230000007774 longterm Effects 0.000 abstract 1
- 238000009792 diffusion process Methods 0.000 description 10
- 239000010935 stainless steel Substances 0.000 description 7
- 238000004506 ultrasonic cleaning Methods 0.000 description 5
- 244000137852 Petrea volubilis Species 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000007605 air drying Methods 0.000 description 3
- 238000005422 blasting Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000009713 electroplating Methods 0.000 description 2
- 238000004372 laser cladding Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910020630 Co Ni Inorganic materials 0.000 description 1
- 229910002440 Co–Ni Inorganic materials 0.000 description 1
- 229910003264 NiFe2O4 Inorganic materials 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
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- 239000000203 mixture Substances 0.000 description 1
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000007613 slurry method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009772 tissue formation 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
- C23C14/22—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
- 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
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/5853—Oxidation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a method for manufacturing a Fe-Co-Ni-Mn-Cu five-element high-entropy alloy spinel coating of an SOFC connector. The component of the alloy is Fe-Co-Ni-Mn-Cu quinary high-entropy alloy coating. The preparation method comprises the steps of 1) matrix pretreatment; 2) sputtering and depositing to obtain an alloy coating; 3) and thermally converting to obtain the spinel coating. The method has the characteristics of stable sputtering rate, high deposition rate, simple operation process and the like; the prepared high-entropy alloy coating has a compact structure and good bonding force with a substrate; the spinel formed by thermal conversion has larger disorder degree, can effectively prevent Cr in the matrix from diffusing outwards, and has excellent conductivity under the action of long-term high-temperature oxidation; in the field of high-entropy alloy, a brand new door is opened for selection of SOFC connector coating materials.
Description
Technical Field
The invention relates to the field of preparation of five-element high-entropy alloy coatings, in particular to a method for preparing a spinel coating of an SOFC connector Fe-Co-Ni-Mn-Cu alloy by a magnetron sputtering method and application thereof.
Background
A Solid Oxide Fuel Cell (SOFC) is a novel energy conversion device which directly converts chemical energy in fuel into electric energy, and can solve the increasingly serious problems of energy shortage and environmental pollution in the current society. The connector is one of the key parts of the SOFC and plays important roles in connecting single cells, isolating the atmosphere of a cathode and an anode and assisting in supporting a cell stack structure. At present, the metal connectors used in the intermediate temperature (600-: cr-based alloys, Ni-based alloys, and Cr-containing ferritic stainless steels. Since the ferritic stainless steel has the advantages of high-temperature oxidation resistance, good electrical and thermal conductivity, matching of thermal expansion coefficient with other components and the like, and is low in price, the ferritic stainless steel becomes the most promising connector material at present. However, the ferritic stainless steel has serious oxidative corrosion in the working environment of the SOFC, especially in the high-temperature oxidizing environment of the cathode, and the volatilization of the Cr element poisons the SOFC cathode, which seriously affects the electrical conductivity of the cathode, thereby causing the performance degradation of the cell.
In practical applications, the main solution to the problem of Cr diffusion in ferritic stainless steel joints is to apply a protective coating on its surface that is free of Cr. NiFe2Fe-Co-Ni, Mn-Cu and other alloys are oxidized at high temperature of 650-800 ℃ to form corresponding NiFe2O4、(Fe,Co,Ni)3O4、(Mn,Cu)3O4The spinel can prevent the diffusion of Cr to a certain extent. The spinel formed by the thermal conversion of the Fe-Co-Ni-Mn-Cu high-entropy alloy has the performance of the spinel, has larger disorder degree, can more effectively prevent the outward diffusion of Cr, and has great significance for improving the performance of a connector and prolonging the service life of the connector.
The main method for preparing the spinel coating on the surface of the stainless steel comprises the following steps: electroplating, sol-gel, slurry, laser cladding, sputter coating, and the like. The composition of the finally obtained spinel is difficult to control by the electroplating method; the metal alkoxides used in the sol-gel process are expensive and not readily available; the spinel coating formed by the slurry method is loose and porous, the components can not be accurately controlled, and the problem of uneven coating of a matrix with a complex shape exists; the laser cladding technology has the problems of large difference between the outer edge and the inner edge of a light spot, uneven tissue formation, uneven stress distribution, insufficient exhaust and slag discharge and the like caused by too short melting time of a cladding layer due to fast heating and cooling. The sputtering coating technology can realize large-area and rapid deposition of the film, the prepared film has few pores, good adhesion with a substrate, and controllable film components and thickness.
Disclosure of Invention
In order to overcome the defects of the technology, the invention aims to provide a spinel coating of Fe-Co-Ni-Mn-Cu quinary high-entropy alloy and a preparation method thereof.
The technical scheme of the invention is as follows:
1. a quinary high-entropy alloy coating is characterized in that: the quinary high-entropy alloy comprises the components of Fe-Co-Ni-Mn-Cu.
2. The thickness of the Fe-Co-Ni-Mn-Cu quinary high-entropy alloy coating is 4-12 mu m.
3. A preparation method of a spinel coating of a quinary high-entropy alloy comprises the following steps;
1) pretreatment: sequentially using 240#, 400# and 600# SiC water grinding sand paper to grind the surface of the Cr-containing ferritic stainless steel substrate, and carrying out edge grinding and chamfering treatment; after polishing, ultrasonically cleaning in acetone for 10-15 min; after the end, airing the sample, and performing sand blasting by using silica sand grains, wherein the pressure intensity range of compressed air is 0.2-0.5 MPa; after sandblasting the matrix, ultrasonically cleaning the matrix in acetone for 10-15 min again, and taking out and airing the matrix;
2) pre-sputtering: closing the metal baffle, and pre-sputtering for about 10-20 min to remove oxides and other impurities on the surface of the target material so as to ensure the sputtering stability and the coating quality;
3) preparing a high-entropy alloy by sputtering deposition: opening a metal baffle, taking the high-entropy alloy target as a cathode and the substrate as an anode, and performing sputtering deposition for 1-3 h to prepare a high-entropy alloy coating on the sample;
4) thermal conversion to obtain spinel coating: the sputter deposited sample was then oxidized in a 800 ℃ chamber resistance furnace to obtain a spinel coating.
In the step 1, the ultrasonic cleaning with acetone is carried out for 10-15 min, and the ultrasonic power is 80-100 w. Cr in the matrix: 16 to 25 mass%.
The target base distance in the step 2 is 8 cm. Firstly, opening a mechanical pump, pre-pumping to about 5Pa, then starting a diffusion pump to finely pump to vacuum of 5 multiplied by 10-3Pa or so. The mole ratio of each element of the Fe-Co-Ni-Mn-Cu quinary high-entropy alloy target material is as follows: fe, Co, Ni, Mn, Cu, 1:1:1:1: 1.
In the step 3, the sputtering current is 3.0A, the sputtering pressure is 0.1-0.15 Pa, the sputtering temperature is 200 ℃, the rotating speed of the rotary frame is 40-60 r/min, and sampling is carried out when the temperature of the vacuum chamber is reduced to below 70 ℃.
The invention has the beneficial effects that:
the method has simple and easy operation process, and is green and environment-friendly; the sputtering rate is stable, the Fe-Co-Ni-Mn-Cu quinary high-entropy alloy coating of the SOFC connector with uniform thickness can be prepared, and the thickness of the coating can be controlled by controlling the sputtering time; the prepared coating has compact structure and is tightly combined with the matrix; the spinel coating formed by thermal conversion effectively blocks the external diffusion of Cr in the matrix and inhibits the mutual diffusion of elements of the matrix and the coating; the oxidation resistance and the conductivity of the matrix under the high-temperature oxidation condition are obviously improved, and the method can be applied to a solid oxide fuel cell connector coating material.
The examples of the invention are as follows:
example 1 this example uses SUS430 stainless steel as a base (Cr:18 mass%)
The embodiment successfully prepares the Fe-Co-Ni-Mn-Cu quinary high-entropy alloy coating material with the molar ratio of elements (Fe: Co: Ni: Mn: Cu ═ 1:1:1:1) by adopting the direct-current magnetron sputtering method mentioned in the invention.
The preparation method of the spinel coating of the quinary high-entropy alloy comprises the following steps:
1) pretreatment: sequentially using 240#, 400# and 600# SiC water grinding sand paper to grind the surface of the Cr-containing ferritic stainless steel substrate, and carrying out edge grinding and chamfering treatment; ultrasonic cleaning in acetone for 10min at an ultrasonic power of 80w, taking out, air drying, and blasting with silica sand with a pressure range of 0.3 MPa; after the matrix is subjected to sand blasting, ultrasonically cleaning the matrix in acetone for 10min at the ultrasonic power of 80 w;
2) pre-sputtering: the target base distance is 8 cm. Firstly, opening a mechanical pump, pre-pumping to about 5Pa, then starting a diffusion pump to finely pump to a vacuum of 5 multiplied by 10-3Pa, carrying out pre-sputtering for 15min to remove oxides and other impurities on the surface of the target material so as to ensure the sputtering stability and the coating quality;
3) preparing a high-entropy alloy by sputtering deposition: setting the rotating speed of a rotating frame to be 40r/min, opening a metal baffle, taking a high-entropy alloy target as a cathode and a substrate as an anode, sputtering current to be 3.0A, sputtering pressure to be 0.12Pa, sputtering temperature to be 200 ℃, and sputtering and depositing for 2h to prepare the quinary high-entropy alloy coating on the sample. Sampling when the temperature of the vacuum chamber is reduced to below 70 ℃;
4) thermal conversion to obtain spinel coating: the sputter deposited sample was then oxidized in a 800 ℃ chamber resistance furnace to obtain a spinel coating.
Drawings
FIG. 1 shows the cross-sectional morphology of a stainless steel substrate deposited Fe-Co-Ni-Mn-Cu coating sample prepared according to example 1 after being oxidized in air at 800 ℃ for 5 min.
FIG. 2 shows the cross-sectional morphology of a stainless steel substrate deposited Fe-Co-Ni-Mn-Cu coating sample prepared according to example 1 after being oxidized in air at 800 ℃ for 30 min.
FIG. 3 shows the cross-sectional morphology of a stainless steel substrate deposited Fe-Co-Ni-Mn-Cu coating sample prepared according to example 1 after being oxidized in air at 800 ℃ for 60 min.
The examples of the invention are as follows:
example 2 this example uses SUS430 stainless steel as a base (Cr:20 mass%)
The embodiment successfully prepares the Fe-Co-Ni-Mn-Cu quinary high-entropy alloy coating material with the molar ratio of elements (Fe: Co: Ni: Mn: Cu ═ 1:1:1:1) by adopting the direct-current magnetron sputtering method mentioned in the invention.
The preparation method of the spinel coating of the quinary high-entropy alloy comprises the following steps:
1) pretreatment: sequentially using 240#, 400# and 600# SiC water grinding sand paper to grind the surface of the Cr-containing ferritic stainless steel substrate, and carrying out edge grinding and chamfering treatment; ultrasonic cleaning in acetone for 12min with ultrasonic power of 90w, taking out, air drying, and blasting with silica sand with compressed air pressure of 0.3 MPa; after the matrix is subjected to sand blasting, carrying out ultrasonic cleaning in acetone for 12min, wherein the ultrasonic power is 90 w;
2) pre-sputtering: the target base distance is 8 cm. Firstly, opening a mechanical pump, pre-pumping to about 5Pa,then the diffusion pump is started to pump to vacuum of 5X 10-3Pa, carrying out pre-sputtering for 15min to remove oxides and other impurities on the surface of the target material so as to ensure the sputtering stability and the coating quality;
3) preparing a high-entropy alloy by sputtering deposition: setting the rotating speed of a rotating frame to be 50r/min, opening a metal baffle, taking a high-entropy alloy target as a cathode and a substrate as an anode, sputtering current to be 3.0A, sputtering pressure to be 0.13Pa, sputtering temperature to be 200 ℃, and sputtering and depositing for 1h to prepare the quinary high-entropy alloy coating on the sample. Sampling when the temperature of the vacuum chamber is reduced to below 70 ℃;
4) thermal conversion to obtain spinel coating: the sputter deposited sample was then oxidized in a 700 ℃ chamber resistance furnace to obtain a spinel coating.
The examples of the invention are as follows:
example 3 this example uses SUS430 stainless steel as a base (Cr:22 mass%)
The embodiment successfully prepares the Fe-Co-Ni-Mn-Cu quinary high-entropy alloy coating material with the molar ratio of elements (Fe: Co: Ni: Mn: Cu ═ 1:1:1:1) by adopting the direct-current magnetron sputtering method mentioned in the invention.
The preparation method of the spinel coating of the quinary high-entropy alloy comprises the following steps:
1) pretreatment: sequentially using 240#, 400# and 600# SiC water grinding sand paper to grind the surface of the Cr-containing ferritic stainless steel substrate, and carrying out edge grinding and chamfering treatment; ultrasonic cleaning in acetone for 15min with ultrasonic power of 100w, taking out, air drying, and blasting with silica sand with compressed air pressure of 0.3 MPa; after the matrix is subjected to sand blasting, ultrasonically cleaning the matrix in acetone for 15min at the ultrasonic power of 100 w;
2) pre-sputtering: the target base distance is 8 cm. Firstly, opening a mechanical pump, pre-pumping to about 5Pa, then starting a diffusion pump to finely pump to a vacuum of 5 multiplied by 10-3Pa, pre-sputtering for 20min to remove oxides and other impurities on the surface of the target material so as to ensure the sputtering stability and the coating quality;
3) preparing a high-entropy alloy by sputtering deposition: setting the rotating speed of a rotating frame to be 60r/min, opening a metal baffle, taking a high-entropy alloy target as a cathode and a substrate as an anode, sputtering current to be 3.0A, sputtering pressure to be 0.15Pa, sputtering temperature to be 200 ℃, sputtering and depositing for 3h, preparing a quinary high-entropy alloy coating on a sample, and sampling when the temperature of a vacuum chamber is reduced to be below 70 ℃;
4) thermal conversion to obtain spinel coating: the sputter deposited samples were then oxidized in a 750 ℃ box resistance furnace to obtain a spinel coating.
The spinel coating prepared by the invention has compact structure, good bonding force with a matrix, can effectively inhibit the external diffusion of matrix Cr, has excellent oxidation resistance and electrical conductivity, meets the requirements of the SOFC connector coating, is used for explaining the invention, is not limited by the invention, and can be modified and changed within the spirit and the protection scope of the claims.
Claims (6)
1. A method for producing a spinel coating of a pentabasic high entropy alloy according to claim I, characterized in that the method comprises the following steps:
1) pretreatment: sequentially grinding the surface of a Cr-containing ferritic stainless steel substrate by using No. 240, No. 400 and No. 600 SiC water grinding sandpaper, and carrying out edge grinding and chamfering treatment; after polishing, ultrasonically cleaning in acetone for 10-15 min; after the end, airing the sample, and performing sand blasting by using silica sand grains, wherein the pressure intensity range of compressed air is 0.2-0.5 MPa; after sandblasting the matrix, ultrasonically cleaning the matrix in acetone for 10-15 min again, and taking out and airing the matrix;
2) pre-sputtering: closing the metal baffle, and pre-sputtering for about 10-20 min to remove oxides and other impurities on the surface of the target material so as to ensure the sputtering stability and the coating quality;
3) preparing an alloy coating by sputtering deposition: opening a metal baffle, taking the Fe-Co-Ni-Mn-Cu high-entropy alloy target as a cathode and the matrix as an anode, and carrying out sputtering deposition for 1-3 h to obtain a Fe-Co-Ni-Mn-Cu high-entropy alloy coating;
4) preparing a spinel coating by thermal conversion: then, placing the sample subjected to sputtering deposition in a box type resistance furnace at 650-800 ℃ for oxidation to obtain the product(Fe,Co,Ni,Mn,Cu)3O4A spinel coating.
2. The method of claim 1, wherein: (said step 1) wherein the ratio of Cr: 16 to 25 mass%.
3. The method of claim 1, wherein: (the mole ratio of each element of the Fe-Co-Ni-Mn-Cu quinary high-entropy alloy target material in the step 2) is as follows: fe, Co, Ni, Mn, Cu =1:1:1:1: 1.
4. The method of claim 3, wherein: (the sputtering parameters in the step 2) are as follows: the sputtering current is 3.0A, the sputtering pressure is 0.1-0.15 Pa, and the sputtering temperature is 200 ℃.
5. The method according to claim 1, wherein the thickness of the Fe-Co-Ni-Mn-Cu alloy coating obtained by sputtering in step 3) is about 4 to 12 μm.
6. The Fe-Co-Ni-Mn-Cu quinary high-entropy alloy coating prepared by magnetron sputtering according to claim 1, characterized in that: the Fe-Co-Ni-Mn-Cu high-entropy alloy coating can be applied to a solid oxide fuel cell connector coating material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114606492A (en) * | 2022-03-10 | 2022-06-10 | 江苏科技大学 | High-temperature-resistant medium-entropy alloy coating composite metal connector and preparation method thereof |
| CN114606457A (en) * | 2022-03-15 | 2022-06-10 | 江苏科技大学 | High-entropy alloy oxide coating and preparation method thereof |
| CN116288219A (en) * | 2023-05-19 | 2023-06-23 | 西南交通大学 | FeCoNiCu high-entropy alloy doped amorphous carbon film, and preparation method and application thereof |
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2020
- 2020-11-18 CN CN202011297054.0A patent/CN112458416A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114606492A (en) * | 2022-03-10 | 2022-06-10 | 江苏科技大学 | High-temperature-resistant medium-entropy alloy coating composite metal connector and preparation method thereof |
| CN114606492B (en) * | 2022-03-10 | 2023-06-09 | 江苏科技大学 | High-temperature-resistant medium-entropy alloy coating composite metal connector and preparation method thereof |
| CN114606457A (en) * | 2022-03-15 | 2022-06-10 | 江苏科技大学 | High-entropy alloy oxide coating and preparation method thereof |
| CN114606457B (en) * | 2022-03-15 | 2024-01-26 | 江苏科技大学 | High-entropy alloy oxide coating and preparation method thereof |
| CN116288219A (en) * | 2023-05-19 | 2023-06-23 | 西南交通大学 | FeCoNiCu high-entropy alloy doped amorphous carbon film, and preparation method and application thereof |
| CN116288219B (en) * | 2023-05-19 | 2023-08-11 | 西南交通大学 | FeCoNiCu high-entropy alloy doped amorphous carbon film, and preparation method and application thereof |
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