CN112501569B - Surface gradient high-entropy alloy layer and preparation method thereof - Google Patents

Surface gradient high-entropy alloy layer and preparation method thereof Download PDF

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CN112501569B
CN112501569B CN202011511244.8A CN202011511244A CN112501569B CN 112501569 B CN112501569 B CN 112501569B CN 202011511244 A CN202011511244 A CN 202011511244A CN 112501569 B CN112501569 B CN 112501569B
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base material
source electrode
power supply
pulse power
entropy alloy
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CN112501569A (en
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刘兴军
王成磊
黄超
姚志富
杨木金
杨智杰
贾雪
成东旭
王彤彤
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Shenzhen Graduate School Harbin Institute of Technology
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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
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • C23C14/5806—Thermal treatment
    • 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
    • C23C14/5893—Mixing of deposited material

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  • Chemical Kinetics & Catalysis (AREA)
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  • Mechanical Engineering (AREA)
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Abstract

The invention discloses a surface gradient high-entropy alloy layer and a preparation method thereof, wherein rod-shaped metal source materials such as Cr, Ni, Fe, Cu, Ti, W, Mo and Nb are inserted into small holes of an auxiliary source barrel, the auxiliary source barrel inserted with the rod-shaped source materials is placed on a working disc connected with a source pulse power supply, a pre-permeation substrate is suspended in the auxiliary source barrel through a workpiece cathode frame and a hook connected with the workpiece pulse power supply, a double-cathode plasma solid-state metallurgy method is adopted to infiltrate and plate pre-permeation elements on the surface of the substrate to form the surface gradient high-entropy alloy layer, the alloy layer comprises a surface deposition layer and a diffusion layer from top to bottom, the surface deposition layer and the substrate are metallurgically bonded, the components are in gradient distribution, and the bonding force is strong; the thickness of the deposition layer can be as high as 60 mu m, the thickness of the diffusion layer can be as high as 100 mu m, and the thicknesses of the deposition layer and the diffusion layer can be adjusted by adjusting process parameters according to requirements; the high-entropy alloy layer can be prepared on the surfaces of workpieces with various complex shapes, the components are controllable, and the organizational structure characteristics are good.

Description

Surface gradient high-entropy alloy layer and preparation method thereof
Technical Field
The invention relates to the technical field of surface modification, in particular to a surface gradient high-entropy alloy layer and a preparation method thereof.
Background
The high-entropy alloy is defined as that the alloy is composed of 5 and more than 5 main elements, and the atomic percentage of each main element is between 5 and 35 percent. Although high entropy alloys possess multiple principal elements with a tendency to form complex phases, the "high entropy effect" results in the alloy actually forming a solid solution structure with simple fcc or bcc or a composite of both, rather than forming complex phases such as intermetallic compounds. The excellent performance of the high-entropy alloy determines the wide application space of the high-entropy alloy. Potential application areas include: the material comprises a mould, a cutter, an electronic component, an engine, an abrasion-resistant coating, a high-frequency alternating-current material, a nuclear structure material, a light transmission material, a biomedical material, a thermal barrier material, a hydrogen storage material, a ship and ocean engineering material, a chemical material, a corrosion-resistant material, an abrasion-resistant material, a thermoelectric material, a superconducting material, an electromagnetic material and the like.
Metal materials themselves suffer from some unexpected performance deficiencies and inadequacies during the manufacturing process, so that the surface film (coating) is used as an important protection means and is mainly applied to improving the performance of the material. A film (coating) with excellent performance can play a great role in enhancing the protection performance and the service life of the material. As a new alloy film material, the high-entropy alloy film (coating) has excellent performance, so that the high-entropy alloy film has wide application range in practical production and life, such as high-temperature protective materials, cutting tool coatings, micro-nano electronic devices, radiation-proof materials, soft magnetic functional materials, hydrogen storage materials and the like.
With the improvement of the technological level, the research on the high-entropy alloy film (coating) is continuously deepened, and more, convenient and innovative film (coating) preparation methods emerge. So far, the preparation of high-entropy alloy thin films (coatings) mainly adopts the following methods: (1) physical Vapor Deposition (PVD): vacuum sputtering, vacuum evaporation and ion plating; (2) a cladding method: thermal spraying, laser cladding; (3) an electrodeposition method; (4) chemical Vapor Deposition (CVD), and the like. However, the preparation methods of the high-entropy alloy thin films (coatings) have certain disadvantages, such as: the high-entropy alloy film (coating) prepared by Physical Vapor Deposition (PVD) is thin, metallurgical bonding is not realized, and the bonding force is poor; although the thickness of the high-entropy alloy film (coating) prepared by the cladding method is thicker, cracks and holes are easy to generate, the defects are more, and the composition segregation exists; chemical Vapor Deposition (CVD) processes are difficult to control and pollute the environment.
Disclosure of Invention
The present invention aims to overcome the defects of the prior art and provide a surface gradient high-entropy alloy layer and a preparation method thereof.
The technical scheme for realizing the purpose of the invention is as follows:
a preparation method of a surface gradient high-entropy alloy layer comprises the following steps:
1) inserting a rod-shaped metal source electrode material into small holes around a self-made auxiliary source electrode barrel;
2) cleaning a base material: firstly, polishing the surface of a base material to be smooth by adopting a manual polishing machine, then soaking the base material for 30-50 min by adopting a hydrochloric acid solution with the mass percent of 10-20%, then adding acetone into an ultrasonic cleaning machine for cleaning for 10-30 min, and finally drying the base material for later use;
3) adopting double-cathode plasma solid-state metallurgical equipment, placing the auxiliary source electrode barrel inserted with the rod-shaped source electrode material in the step 1) on a working disc connected with a source electrode pulse power supply, and supporting the auxiliary source electrode barrel by using a metal gasket; the base material is suspended in the auxiliary source electrode barrel through a workpiece cathode frame and a hook which are connected with a workpiece pulse power supply and is not contacted with the rod-shaped metal source electrode material;
4) vacuumizing the inside of the double-cathode plasma solid-state metallurgical equipment to less than 500Pa, respectively starting a source electrode pulse power supply and a workpiece pulse power supply, gradually increasing the voltage and the current of the two power supplies, generating glow discharge and arc striking phenomena on the auxiliary source electrode barrel and the base material at the moment, and performing primary bombardment cleaning on the rod-shaped metal source electrode material and the base material;
5) when the rod-shaped metal source electrode material and the base material are not arcing, the source electrode pulse power supply and the workpiece pulse power supply are closed, and the vacuum degree is pumped to less than 5.0 multiplied by 10 0 When Pa, closing the front valve, starting the molecular pump and opening the baffle valve;
6) when the vacuum degree is pumped to be less than 3.0 multiplied by 10 -3 When Pa is needed, the baffle valve is closed, the molecular pump is closed, argon is introduced into the furnace body, when the vacuum degree reaches 20-60 Pa, the front-stage valve is opened, the source pulse power supply and the workpiece pulse power supply are opened again, and the steps are carried out one by oneGradually increasing the voltage and current of the two power supplies, generating glow discharge and arc striking phenomena on the auxiliary source electrode barrel and the workpiece, and performing secondary bombardment cleaning on the rod-shaped metal source electrode material and the base material;
7) when the rod-shaped metal source electrode material and the base material do not have arcing, an infrared thermometer is adopted, a temperature measuring device is aligned to the surface of the base material through an observation window of the furnace body and an observation hole of the auxiliary cathode, and the temperature of the base material is tested;
8) gradually increasing the voltage and current of a source pulse power supply and a workpiece pulse power supply, rapidly heating the base material at the moment, adjusting the flow of argon to ensure that the vacuum degree is 20-60 Pa when the temperature reaches 800-1400 ℃, controlling the voltage of the source pulse power supply to-600V-1000V and the voltage of the workpiece pulse power supply to-200V-900V for heat preservation;
9) utilizing low-temperature plasma generated by gas discharge to combine the cathode sputtering phenomenon, the hollow cathode effect and the point discharge effect, applying a magnetic field and an electric field to the whole gas discharge working space, so that alloy elements to be infiltrated into a solid are sputtered out, bombarded, deposited and diffused to the surface of a workpiece by larger energy under the action of the electric field and the magnetic field, and forming a gradient high-entropy alloy layer with special physical, chemical and mechanical properties on the surface of a base material;
10) after the heat preservation time is finished, the argon flow is closed, the power supply is closed, and the mechanical pump is kept pumping until the base material is reduced to the room temperature;
11) homogenizing the base material in an atmosphere heat treatment furnace filled with argon protection, quickly putting the base material into an ice-water mixture or liquid nitrogen for primary quenching, then carrying out aging treatment on the base material in the atmosphere heat treatment furnace filled with argon protection, quickly putting the base material into the ice-water mixture or liquid nitrogen for secondary quenching, and forming a gradient high-entropy alloy layer on the surface of the base material.
In the step 1), the rod-shaped metal source electrode material is at least five of Cr, Ni, Fe, Cu, Ti, W, Mo and Nb metal rods with the diameter of phi 3 mm to phi 10 mm, the length of 20 mm to 80mm and the purity of more than or equal to 99.99%, and the number of each metal rod is 5 to 50.
In the step 2), the base material is a conductive metal material with a melting point of 900-3500 ℃.
In the step 3), the distance between the base material suspended in the auxiliary source electrode barrel and the rod-shaped metal source electrode material is 10-90 mm.
In the step 4), the time for the first bombardment cleaning is 5-50 min.
In the step 6), the purity of the argon is more than or equal to 99.99%, and the flow rate is 20-40 mL/min; and the time for the second bombardment cleaning is 5-30 min.
In the step 8), the heat preservation is carried out for 2-24 h.
In the step 11), the homogenization treatment is carried out at the temperature of 1000-1300 ℃ for 2-12 h; the aging treatment is carried out at the temperature of 700-900 ℃ for 4-24 h.
The surface gradient high-entropy alloy layer prepared by the preparation method of the surface gradient high-entropy alloy layer is embedded into a base material and is metallurgically bonded with the base material, the alloy layer comprises a surface deposition layer and a diffusion layer from top to bottom, the thickness of the deposition layer can reach 60 mu m, the thickness of the diffusion layer can reach 100 mu m, and the diffusion layer and the inner part of the base material form a phase change boundary line, which is a phenomenon of reaction diffusion when the surface is diffused, and the thicknesses of the surface deposition layer and the diffusion layer can be adjusted by adjusting process parameters according to needs, so that the thickness selection range of the diffusion layer is large; the base material and the diffusion-plated source electrode material are very wide, and both the base material and the diffusion-plated source electrode material can be conductive metal materials with the melting point of 900-3500 ℃; because the alloy layer and the base material are metallurgically bonded, the components are distributed in a gradient way, and the bonding force is strong; the diffusion plating uniformity is good, workpieces in various complex shapes can be processed, and the tissue structure characteristics are good; the components of the diffusion coating are easy to control, the technological parameters can be adjusted according to the requirements of the surface components, and the parameters can be randomly adjusted at any time in the whole technological process, so that the purpose of controlling the surface components is achieved.
The method for preparing the surface gradient high-entropy alloy layer can be used for preparing high-entropy alloy films or coatings on the surfaces of workpieces with various complex shapes, has controllable components, forms metallurgical bonding, ensures sufficient bonding strength and has high surface modification efficiency.
Drawings
FIG. 1 is a schematic structural diagram of a twin cathode plasma solid state metallurgical apparatus;
fig. 2 is a schematic view of a surface high entropy alloy layer.
Detailed Description
The invention will be further elucidated with reference to the drawings and examples, without however being limited thereto.
The embodiment is as follows:
in the embodiment, a pure iron sample with the size of 180 mm × 15 mm × 4 mm is selected as the pre-infiltration base material, an auxiliary source barrel with the size of 150 mm × 200 mm is adopted, and tungsten (W) with the size of 4 mm × 30 mm is selected as the source material: 26, molybdenum (Mo): 26, chromium (Cr): 26, titanium (Ti): 34, iron (Fe): 32, nickel (Ni): uniformly inserting 6 kinds of rod-shaped source electrode materials into the small holes of the auxiliary source electrode barrel; firstly, polishing the surface of a pre-infiltrated base material by adopting a manual polishing machine, soaking the surface of the pre-infiltrated base material for 30 minutes by using dilute hydrochloric acid with the mass fraction of 15%, then adding acetone into an ultrasonic cleaning agent for cleaning for 10 minutes, and then drying the surface of the pre-infiltrated base material for later use by using a blower; adopting a double-cathode plasma solid-state metallurgical device shown in figure 1, placing an auxiliary source electrode barrel inserted with a rod-shaped source electrode material on a working disc connected with a source electrode pulse power supply, and supporting the auxiliary source electrode barrel by using 3 self-made metal gaskets with the diameter of 10 mm and the height of 4 mm, wherein the metal gaskets are uniformly distributed on the circumference of the auxiliary source electrode barrel, and a pre-infiltration base material is suspended in the auxiliary source electrode barrel through a workpiece cathode frame connected with a workpiece pulse power supply and a hook, so that the distance between the rod-shaped metal source electrode material and the base material is ensured to be 50 mm; firstly, vacuumizing to 400 Pa by using a mechanical pump, respectively starting a source electrode pulse power supply and a workpiece pulse power supply, gradually increasing the voltage and the current of the two power supplies, generating glow discharge and arc striking phenomena on an auxiliary source electrode barrel and a workpiece at the moment, and bombarding and cleaning a source electrode and a base material for 40 minutes; when the source electrode and the substrate are not arcing, the source electrode pulse power supply and the workpiece pulse power supply are turned off, and the vacuum degree is pumped to 3.0 multiplied by 10 0 When Pa, closing the front valve, starting the molecular pump and opening the baffle valve; when the vacuum is pumped to 2.2X 10 -3 When Pa, close the baffle valve, close the molecular pump, and let in 3 from the furnace bodyHigh-purity argon (99.99%) with the flow rate of 0mL/min, when the vacuum degree reaches 40 Pa, opening a front-stage valve, opening a source pulse power supply and a workpiece pulse power supply again, gradually increasing the voltage and the current of the two power supplies, assisting the source barrel and the base material to generate glow discharge and arc striking phenomena at the moment, and performing bombardment cleaning on the source and the base material for 20 minutes; when the source electrode and the base material do not have arcing phenomenon, an infrared thermometer is adopted, a temperature measuring device is aligned to the surface of the base material through an observation window of the furnace body and an observation hole of the auxiliary cathode, and the temperature of the base material is tested; gradually increasing the voltage and current of the two power supplies, rapidly heating the base material at the moment, adjusting the argon flow to 40 Pa when the temperature reaches 1100 ℃, controlling the voltage of a source pulse power supply to-900V, controlling the voltage of a workpiece pulse power supply to-400V, and starting heat preservation for 10 h; after the heat preservation time is finished, the argon flow is closed, the power supply is closed, and the mechanical pump is kept pumping until the base material is reduced to the room temperature; the base material is homogenized in an atmosphere heat treatment furnace with argon protection at 1100 ℃ for 4 hours, and then quickly placed into an ice-water mixture or liquid nitrogen for quenching. Then, the base material is subjected to aging treatment in an atmosphere heat treatment furnace with argon protection at the temperature of 800 ℃ for 24 hours, and then is quickly put into an ice-water mixture or liquid nitrogen for quenching, and finally a gradient high-entropy alloy layer is formed on the surface of the base material, as shown in the schematic diagram of fig. 2, through detection, the thickness of a deposition layer is 15 micrometers, the thickness of a diffusion layer is 45 micrometers, an obvious phase change boundary line is arranged between the diffusion layer and a base body, the distribution of each element in the deposition layer is relatively uniform, and the atomic percentage content of each element in the deposition layer is respectively as follows: tungsten (W): 12%, molybdenum (Mo): 15%, chromium (Cr): 14%, titanium (Ti): 20%, iron (Fe): 19%, nickel (Ni): 20 percent, the surface high-entropy alloy is formed, and the content of each element of the diffusion layer is gradually reduced along with the increase of the depth.

Claims (4)

1. A preparation method of a surface gradient high-entropy alloy layer is characterized by comprising the following steps:
1) inserting a rod-shaped metal source electrode material into small holes around a self-made auxiliary source electrode barrel;
2) cleaning a base material: firstly, polishing the surface of a base material to be smooth by adopting a manual polishing machine, then soaking the base material for 30-50 min by adopting a hydrochloric acid solution with the mass percent of 10-20%, then adding acetone into an ultrasonic cleaning machine for cleaning for 10-30 min, and finally drying the base material for later use;
3) adopting double-cathode plasma solid-state metallurgical equipment, placing the auxiliary source barrel inserted with the rod-shaped source material in the step 1) on a working disc connected with a source pulse power supply, and supporting the auxiliary source barrel by using a metal gasket; the base material is suspended in the auxiliary source electrode barrel through a workpiece cathode frame and a hook which are connected with a workpiece pulse power supply and is not contacted with the rod-shaped metal source electrode material;
4) vacuumizing the inside of the double-cathode plasma solid-state metallurgical equipment to less than 500Pa, respectively starting a source electrode pulse power supply and a workpiece pulse power supply, gradually increasing the voltage and the current of the two power supplies, generating glow discharge and arc striking phenomena on the auxiliary source electrode barrel and the base material at the moment, and performing primary bombardment cleaning on the rod-shaped metal source electrode material and the base material;
5) when the rod-shaped metal source electrode material and the base material are not arcing, the source electrode pulse power supply and the workpiece pulse power supply are closed, and the vacuum degree is pumped to less than 5.0 multiplied by 10 0 When Pa, closing the front valve, starting the molecular pump and opening the baffle valve;
6) when the vacuum degree is pumped to be less than 3.0 multiplied by 10 -3 When the vacuum degree reaches 20-60 Pa, a front-stage valve is opened, a source electrode pulse power supply and a workpiece pulse power supply are opened again, the voltage and the current of the two power supplies are gradually increased, the auxiliary source electrode barrel and the workpiece generate glow discharge and arc striking phenomena at the moment, and the rod-shaped metal source electrode material and the base material are subjected to secondary bombardment cleaning;
7) when the rod-shaped metal source electrode material and the base material do not have arcing, an infrared thermometer is adopted, a temperature measuring device is aligned to the surface of the base material through an observation window of the furnace body and an observation hole of the auxiliary cathode, and the temperature of the base material is tested;
8) gradually increasing the voltage and current of a source pulse power supply and a workpiece pulse power supply, rapidly heating the base material at the moment, adjusting the flow of argon to ensure that the vacuum degree is 20-60 Pa when the temperature reaches 800-1400 ℃, controlling the voltage of the source pulse power supply to-600V-1000V and the voltage of the workpiece pulse power supply to-200V-900V for heat preservation;
9) utilizing low-temperature plasma generated by gas discharge to combine the cathode sputtering phenomenon, the hollow cathode effect and the point discharge effect, applying a magnetic field and an electric field to the whole gas discharge working space, so that alloy elements to be infiltrated into a solid are sputtered out, bombarded, deposited and diffused to the surface of a workpiece by larger energy under the action of the electric field and the magnetic field, and forming a gradient high-entropy alloy layer with special physical, chemical and mechanical properties on the surface of a base material;
10) after the heat preservation time is finished, the argon flow is closed, the power supply is closed, and the mechanical pump is kept pumping until the base material is reduced to the room temperature;
11) homogenizing a base material in an atmosphere heat treatment furnace filled with argon protection, quickly putting the base material into an ice-water mixture or liquid nitrogen for primary quenching, then carrying out aging treatment on the base material in the atmosphere heat treatment furnace filled with argon protection, quickly putting the base material into the ice-water mixture or liquid nitrogen for secondary quenching, and forming a gradient high-entropy alloy layer on the surface of the base material, wherein the high-entropy alloy layer comprises a surface deposition layer and a diffusion layer from top to bottom, is metallurgically bonded with the base material, has gradient distribution of components, and has uniform distribution of all elements in the deposition layer to form the surface high-entropy alloy, and the content of all elements in the diffusion layer is gradually reduced along with the increase of the depth; the thickness of the deposition layer is 60 μm, the thickness of the diffusion layer is 100 μm, and the thicknesses of the deposition layer and the diffusion layer are adjusted by adjusting process parameters according to requirements;
in the step 1), the rod-shaped metal source electrode material is at least five of Cr, Ni, Fe, Cu, Ti, W, Mo and Nb metal rods with the diameter of phi 3 mm to phi 10 mm, the length of 20 mm to 80mm and the purity of more than or equal to 99.99%, and the number of each metal rod is 5 to 50;
in the step 2), the base material is a conductive metal material with a melting point of 900-3500 ℃, and the conductive metal material is pure iron;
in the step 6), the purity of the argon is more than or equal to 99.99%, and the flow rate is 20-40 mL/min; the time for the second bombardment cleaning is 5-30 min;
in the step 11), the homogenization treatment is carried out at the temperature of 1000-1300 ℃ for 2-12 h; the aging treatment is carried out at the temperature of 700-900 ℃ for 4-24 h;
the atomic percentage of each element in the deposition layer is respectively as follows: 12% of tungsten, 15% of molybdenum, 14% of chromium, 20% of titanium, 19% of iron and 20% of nickel, wherein elements in the deposition layer are uniformly distributed to form a surface high-entropy alloy, and the content of each element in the diffusion layer is gradually reduced along with the increase of the depth.
2. The method for preparing a surface gradient high-entropy alloy layer according to claim 1, wherein in the step 3), the distance between the substrate suspended in the auxiliary source barrel and the rod-shaped metal source material is 10-90 mm.
3. The method for preparing a surface gradient high-entropy alloy layer according to claim 1, wherein in the step 4), the time for the first bombardment cleaning is 5-50 min.
4. The method for preparing a surface gradient high-entropy alloy-layer according to claim 1, wherein in the step 8), the heat preservation time is 2-24 hours.
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CN111876645B (en) * 2020-07-13 2021-10-29 中国兵器科学研究院宁波分院 Ta-W-Nb-Al-Cr-Ti-Si series high-entropy alloy infiltration coating for high-flux screening and preparation method thereof
CN112064024B (en) * 2020-09-23 2021-08-31 广东省科学院新材料研究所 Diffusion-resistant high-entropy alloy coating material, high-temperature-resistant coating material, and preparation method and application thereof

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