CN109402590B - Method for preparing high-entropy alloy coating through magnetron sputtering - Google Patents

Method for preparing high-entropy alloy coating through magnetron sputtering Download PDF

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CN109402590B
CN109402590B CN201910017561.5A CN201910017561A CN109402590B CN 109402590 B CN109402590 B CN 109402590B CN 201910017561 A CN201910017561 A CN 201910017561A CN 109402590 B CN109402590 B CN 109402590B
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entropy alloy
metal powder
magnetron sputtering
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workpiece
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CN109402590A (en
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卢金斌
马振武
冯杰
张明敏
王志新
马明星
殷振
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Bai Xuanyu
Hefei Jiuzhou Longteng Scientific And Technological Achievement Transformation Co ltd
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Suzhou University of Science and 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive 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
    • C23C14/06—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
    • 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
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a method for preparing a high-entropy alloy coating by magnetron sputtering, which comprises the steps of firstly carrying out ball milling alloying on Cr, Mn, Fe, Ni-B, Al-Si according to a proportion, preparing a high-entropy alloy target by pressure sintering, then carrying out magnetron sputtering on the surface of a steel substrate to form a high-entropy alloy coating, and finally carrying out nitriding in a nitriding furnace.

Description

Method for preparing high-entropy alloy coating through magnetron sputtering
Technical Field
The invention belongs to the field of surface treatment of metal materials, and particularly relates to a method for preparing a high-entropy alloy coating by adopting a magnetron sputtering technology.
Background
With the increasing application of advanced cutting technologies such as high-speed cutting and dry cutting, higher requirements are also put forward on the comprehensive properties of the cutter coating, such as toughness, hardness, wear resistance and the like. The high-entropy alloy contains a plurality of main elements, and the content of each element is between 5 and 35 percent. Therefore, the high-entropy alloy subverts the traditional alloy preparation method. Compared with the traditional alloy, the high-entropy alloy has higher strength, hardness, wear resistance, corrosion resistance and the like, but the action mechanism and the scientific problem of the high-entropy alloy are not well explained. The current high-entropy alloy system is mainly prepared by a test method, and a theory of selecting alloy elements forming a scientific system does not exist. The high-entropy alloy has high comprehensive performance and price, so the method for preparing the high-entropy alloy coating is one of the methods for realizing the high-performance coating. The coating is prepared on the surface of the metal material by adopting methods such as thermal spraying, thermal spray welding, cladding and the like, so that the wear resistance and hardness of the material can be improved, but the heating temperature of a steel matrix in the preparation process of cladding, thermal spray welding and the like is too high, even partial melting easily causes uneven components and deteriorated tissues of high-speed steel and serious deformation of the matrix, magnetron sputtering can be used for preparing various materials such as metal, ceramics, composite coatings and the like, and the method has the advantages of simple equipment, easy control, large coating area and the like. During the deposition process, the temperature of the steel substrate is low, so that the method can be used in occasions with high precision requirements.
The high-speed steel cutter has good toughness, but the surface wear resistance is low, the influence on a steel matrix by adopting a magnetron sputtering method is small, and the method can be used for manufacturing a high-precision cutter coating. The nitride reinforced high-entropy alloy coating is deposited on a high-speed steel substrate, the characteristics of high hardness, high wear resistance and high toughness of the high-entropy alloy can be fully utilized, wherein the reinforced phase nitrides CrN, AlN and steel are inert in the cutting process, the adhesion and wear of the coating are favorably reduced, the compatibility of Cr, Ni and Fe elements and the steel is good, and the bonding force between the coating and the high-speed steel can be well improved through mutual diffusion in the deposition process. In addition, the coating contains small amount of Si and B to raise the smoothness of the coating and form small amount of compound to raise the hardness and wear resistance.
Disclosure of Invention
Aiming at the defect of poor wear resistance of high-speed steel, the invention improves the wear resistance and hardness of the surface of the high-speed steel by preparing the coating, can be used for efficiently cutting stainless steel and other materials which are difficult to process, and mainly comprises the following process steps:
the method comprises the following steps of firstly, preprocessing the surface of a precoated workpiece, wherein the workpiece is made of high-speed steel, polishing the surface by using a grinding wheel or abrasive paper to remove rust, burrs and flashes, and removing oil stains on the surface by using acetone;
and secondly, alloying the Cr, Mn, Fe and Ni-B, Al-Si metal powder by ball milling according to a certain proportion, wherein the purity of the Cr, Mn and Fe metal powder is 99.5-100%, and the particle size of the powder is 30-120 mu m. B, Ni mass percent of the Ni-B metal powder is respectively 3-4% and 96-97%; the mass percentages of Si and Al in the Al-Si metal powder are respectively 3-4% and 96-97%; the mass ratio of the Cr metal powder to the Mn metal powder to the Fe metal powder to the Ni-B, Al-Si metal powder is 1-1.1: 1.2-1.3: 1.2-1.4: 0.6-0.7. Ball-milling and mixing are carried out by adopting a steel ball-milling tank, the mass ratio of the grinding balls to the metal powder is 2.7-3.3: 1, the vacuum valve is opened after sealing, vacuum pumping is carried out for 20-30 minutes, the ball-milling tank is placed into a planetary ball mill, the rotating speed is 260-300 r/min, the inversion frequency is 32-45 Hz, and the ball-milling and mixing time is 40-50 minutes. The high-entropy alloy target is prepared by adopting the mixed powder through pressure sintering, namely the high-entropy alloy target is pressurized in a pressure sintering furnace under the protection of argon at 200-320 MPa, the sintering temperature is 860-970 ℃, and the temperature is kept for 4-7 minutes.
Step three,Placing the high-entropy alloy target on a DC cathode, closing a vacuum chamber, and vacuumizing to 2 x 10-2Pa~2×10- 3And Pa, introducing the flow of the Ar gas-regulated gas flowmeter to stabilize the gas pressure at 2-6 Pa, turning on a negative bias power supply, regulating the negative bias to a range of 400-900V, and performing ion bombardment glow cleaning on the pre-coated workpiece for 10-20 minutes.
And step four, after the ion cleaning is finished, starting a heater to heat the precoated workpiece for magnetron sputtering. The process comprises the steps of firstly introducing 10-50 liters/minute of argon-nitrogen mixed gas into a vacuum chamber, wherein the flow ratio of the argon to the nitrogen is 1: 2-3, the working air pressure is kept at 0.5-1.7 Pa, the target spacing is kept at 30-80 mm, the reactive magnetron sputtering is carried out under the conditions that the workpiece temperature is kept at 150-190 ℃, the substrate bias voltage is 0.3-0.4 kV, and the current is 0.1-0.75A, and the sputtering time is controlled for 4-8 minutes.
And step five, obtaining the AlN and CrN enhanced AlCrFeMnNi high-entropy alloy coating after the magnetron sputtering is finished.
The invention has the beneficial effects that:
(1) the process method adopts the high-entropy alloy as the wear-resistant coating, and has higher wear resistance, hardness and strength.
(2) The coating is reacted in magnetron sputtering to form nitride-enhanced high-entropy alloy, and the nitride has inertia to common metal materials, so that the adhesion of the manufactured high-speed steel cutter to ferrous metal during cutting processing can be reduced, the abrasion is reduced, and the service life of the cutter is prolonged.
(3) The small amount of Si and B contained in the coating can improve the smoothness of the coating, and the small amount of compound formed can enhance the hardness and the wear resistance of the coating.
Detailed Description
Example 1:
step one, selecting high-speed steel W18Cr4V as a substrate, polishing the surface by using sand paper to remove rust, burrs and fins, and removing oil stains on the surface by using acetone.
Secondly, alloying Cr, Mn, Fe and Ni-B, Al-Si metal powder by ball milling according to a proportion, wherein the purity of the Cr, Mn and Fe metal powder is 99.5-100%, and the particle size of the powder is 30-120 mu m; the mass percent of B in the Ni-B metal powder is 3-4%, and the mass percent of Ni is 96-97%; the mass percent of Si in the Al-Si metal powder is 3-4%, and the mass percent of Al is 96-97%; the mass ratio of Cr, Mn, Fe and Ni-B, Al-Si metal powder is 1:1.2:1.2:1.2: 0.6. Ball milling and mixing are carried out by adopting a steel ball milling tank, wherein the mass ratio of the grinding balls to the metal powder is 2.7: 1, a vacuum valve is opened after sealing, vacuum pumping is carried out for 20 minutes, the ball milling tank is placed into a planetary ball mill, the rotating speed is 260 r/min, the inversion frequency is 32 Hz, and the ball milling and mixing time is 40 minutes. And after mixing, pressurizing 200 MPa in a pressurizing sintering furnace under the protection of argon, wherein the sintering temperature range is 860 ℃, and preserving heat for 4 minutes to prepare the high-entropy alloy target.
Step three, placing the high-entropy alloy target on a direct current cathode, closing a vacuum chamber, and vacuumizing to 2 x 10-3And Pa, introducing Ar gas, adjusting the flow of the gas flowmeter to stabilize the gas pressure at 2-2.5 Pa, turning on a negative bias power supply, adjusting the negative bias to 400V, and performing ion bombardment glow cleaning on the pre-coated workpiece for 20 minutes.
And step four, after the ion cleaning is finished, starting a heater to heat the precoated workpiece for magnetron sputtering. The process comprises introducing 10L/min mixed gas of argon and nitrogen into a vacuum chamber, wherein the flow ratio of argon to nitrogen is 1:2, the working pressure is kept at 0.5 Pa, the target spacing is kept at 30mm, the temperature of a workpiece is kept at 150 ℃, the bias voltage of a matrix is 0.3kV, and the sputtering time is controlled for 8 minutes.
And step five, obtaining the AlN and CrN enhanced AlCrFeMnNi high-entropy alloy coating after the magnetron sputtering is finished.
Experiments show that the coating formed by magnetron sputtering is smooth in appearance and basically free of defects such as air holes and cracks, the coating structure is fine in crystal grains and uniform in components, and fine AlN, CrN and CrB are distributed in an FCC (fluid catalytic cracking) high-entropy alloy matrix, so that the wear resistance of the coating is 2.3 times that of W18Cr4V steel. In addition, the nitride has good inertia to the iron-based alloy, and is beneficial to improving the cutting processing performance of the high-speed steel.
Example 2:
step one, selecting high-speed steel W6Mo5Cr4V2 as a substrate, polishing the surface by using sand paper to remove rust, burrs and fins, and removing oil stains on the surface by using acetone.
Secondly, alloying Cr, Mn, Fe and Ni-B, Al-Si metal powder by ball milling according to a proportion, wherein the purity of the Cr, Mn and Fe metal powder is 99.5-100%, and the particle size of the powder is 30-120 mu m; the mass percent of B in the Ni-B metal powder is 3-4%, and the mass percent of Ni is 96-97%; the mass percent of Si in the Al-Si metal powder is 3-4%, and the mass percent of Al is 96-97%; the mass ratio of Cr, Mn, Fe and Ni-B, Al-Si metal powder is 1.1:1.2:1.2:1.4: 0.7. The ball milling and mixing are carried out by adopting a steel ball milling tank, wherein the mass ratio of the milling balls to the metal powder is 3.3: 1, the vacuum valve is opened after the sealing and the vacuum pumping is carried out for 30 minutes, the ball milling tank is placed into a planetary ball mill, the rotating speed is 300 r/min, the inversion frequency is 45 Hz, and the ball milling and mixing time is 50 minutes. After mixing, the mixture is pressurized in a pressurized sintering furnace under the protection of argon at 320 MPa, the sintering temperature range is 970 ℃, and the temperature is kept for 7 minutes, so that the high-entropy alloy target is prepared.
Step three, placing the high-entropy alloy target on a direct current cathode, closing a vacuum chamber, and vacuumizing to 5 multiplied by 10-3And Pa, introducing Ar gas, adjusting the flow of the gas flowmeter to stabilize the gas pressure at 5.5-6 Pa, turning on a negative bias power supply, adjusting the negative bias to 900V, and performing ion bombardment glow cleaning on the pre-coated workpiece for 20 minutes.
And step four, after the ion cleaning is finished, starting a heater to heat the precoated workpiece for magnetron sputtering. Introducing a mixed gas of argon and nitrogen with the flow ratio of 1:3 into a vacuum chamber of 35 liters/minute, keeping the working pressure at 1.7 Pa, keeping the target spacing between 80mm, keeping the temperature of a workpiece at 190 ℃, keeping the bias voltage of a matrix at 0.4kV, and controlling the sputtering time to be 4 minutes.
And step five, obtaining the AlN and CrN enhanced AlCrFeMnNi high-entropy alloy coating after the magnetron sputtering is finished.
Experiments show that the coating formed on the surface of the high-speed steel by adopting magnetron sputtering has smooth appearance and basically has no defects of air holes, cracks and the like, because the deposition temperature is not high, the matrix deformation of the high-speed steel is small, the structure of the coating is a structure with fine grains and uniform components, fine CrB, AlN and CrN are distributed in the FCC high-entropy alloy matrix, the wear resistance of the coating is 1.9 times that of W6Mo5Cr4V2 high-speed steel, and the coating can be used for cutting difficult-to-process materials such as stainless steel and the like.
Example 3:
selecting high-speed steel W6Mo5Cr4V3 as a substrate, polishing the surface of the workpiece, which is usually high-speed steel, by using a grinding wheel to remove rust, burrs and fins, and removing oil stains on the surface by using acetone;
secondly, alloying Cr, Mn, Fe and Ni-B, Al-Si metal powder by ball milling according to a certain proportion, wherein the purity of the Cr, Mn and Fe metal powder is 99.5-100%, and the particle size of the powder is 30-120 mu m; the mass percent of B in the Ni-B metal powder is 3-4%, and the mass percent of Ni is 96-97%; the mass percent of Si in the Al-Si metal powder is 3-4%, and the mass percent of Al is 96-97%; the mass ratio of Cr, Mn, Fe and Ni-B, Al-Si metal powder is 1:1.2:1.3:1.3: 0.7. The ball milling and mixing are carried out by adopting a steel ball milling tank, wherein the mass ratio of the milling balls to the metal powder is 3:1, the vacuum valve is opened after the sealing and the vacuum pumping is carried out for 25 minutes, the ball milling tank is put into a planetary ball mill, the rotating speed is 280 r/min, the inversion frequency is 37 Hz, and the ball milling and mixing time is 45 minutes. And after mixing, pressurizing in a pressure sintering furnace under the protection of argon at 280 MPa, wherein the sintering temperature range is 900 ℃, and preserving heat for 6 minutes to prepare the high-entropy alloy target.
Step three, placing the high-entropy alloy target on a direct current cathode, closing a vacuum chamber, and vacuumizing to 1 × 10-2And Pa, introducing Ar gas, adjusting the flow of the gas flowmeter to stabilize the gas pressure at 3.5-4 Pa, turning on a negative bias power supply, adjusting the negative bias to 650V, and performing ion bombardment glow cleaning on the pre-coated workpiece for 15 minutes.
And step four, after the ion cleaning is finished, starting a heater to heat the precoated workpiece for magnetron sputtering. The process comprises introducing 30L/min mixed gas of argon and nitrogen into a vacuum chamber, wherein the flow ratio of argon to nitrogen is 1:2.5, the working pressure is kept at 1.3Pa, the target spacing is kept between 50mm, the temperature of a workpiece is kept at 170 ℃, the substrate bias voltage is 0.35kV, and the sputtering time is controlled for 6 minutes.
And step five, obtaining the AlN and CrN enhanced AlCrFeMnNi high-entropy alloy coating after the magnetron sputtering is finished.
Experiments show that the coating formed on the surface of the high-speed steel through magnetron sputtering has smooth appearance and basically has no defects of pores, cracks and the like, the coating structure is a structure with fine grains and uniform components, and fine AlN and CrN are distributed in an FCC high-entropy alloy matrix. The deformation of a high-speed steel matrix is small, the wear resistance of the coating is 2.1 times that of W6Mo5Cr4V3, the tolerance size of the cutter can be met, and turning of stainless steel parts shows that the increase of the surface coating of the cutter improves the wear resistance of the cutter, so that the service life of the cutter is prolonged.
Example 4:
selecting high-speed steel W6Mo5Cr4V3 as a substrate, polishing the surface by using sand paper to remove rust, burrs and fins, and removing oil stains on the surface by using acetone;
and secondly, alloying the Cr, Mn, Fe and Ni-B, Al-Si metal powder by ball milling according to a certain proportion, wherein the purity of the Cr, Mn and Fe metal powder is 99.5-100%, and the particle size of the powder is 30-120 mu m. B, Ni mass percent of the Ni-B metal powder is respectively 3-4% and 96-97%; the mass percentages of Si and Al in the Al-Si metal powder are respectively 3-4% and 96-97%; the mass ratio of Cr, Mn, Fe and Ni-B, Al-Si metal powder is 1.1:1.3:1.4:1.3: 0.65. Ball-milling and mixing by adopting a steel ball-milling tank, wherein the mass ratio of the milling balls to the metal powder is 2.9: 1, sealing, opening a vacuum valve, vacuumizing for 20-30 minutes, putting the ball-milling tank into a planetary ball mill, rotating at 280 r/min, inverting at 38 Hz, and ball-milling and mixing for 43 minutes. The high-entropy alloy target is prepared by adopting the mixed powder through pressure sintering, namely, the high-entropy alloy target is pressurized in a pressure sintering furnace under the protection of argon at 270 MPa, the sintering temperature is 890 ℃, and the high-entropy alloy target is kept warm for 5 minutes.
Step three, placing the high-entropy alloy target on a direct current cathode, closing a vacuum chamber, and vacuumizing to 9 x 10-3Introducing Ar gas to regulate the flow rate of gas flowmeter to make the gas pressure stable at 5Pa,and turning on a negative bias power supply, adjusting the negative bias to a range of 400-900V, and carrying out ion bombardment glow cleaning on the pre-coated workpiece for 18 minutes.
And step four, after the ion cleaning is finished, starting a heater to heat the precoated workpiece for magnetron sputtering. The process comprises introducing 28L/min mixed gas of argon and nitrogen into a vacuum chamber, wherein the flow ratio of argon to nitrogen is 1:2.5, the working pressure is kept at 1.2 Pa, the target spacing is kept between 50mm, the temperature of a workpiece is kept at 170 ℃, the bias voltage of a matrix is 0.35kV, the current is 0.5A, and the sputtering time is controlled for 6 minutes.
And step five, obtaining the AlN and CrN enhanced AlCrFeMnNi high-entropy alloy coating after the magnetron sputtering is finished.
Experiments show that the coating formed on the surface of the high-speed steel by adopting magnetron sputtering has smooth appearance and is basically free of defects such as air holes, cracks and the like, the deposition temperature is not high, the matrix deformation of the high-speed steel is small, the structure of the coating is an FCC (fluid catalytic cracking) high-entropy alloy matrix, the crystal grains are fine, the components are uniform, fine CrB, AlN and CrN are dispersed and distributed, the wear resistance of the coating is 1.8 times that of W6Mo5Cr4V3 high-speed steel, and the coating can be used for cutting difficult-to-process materials such as stainless steel.

Claims (3)

1. A method for preparing a high-entropy alloy coating by magnetron sputtering is characterized by comprising the following process steps:
the method comprises the following steps of firstly, pretreating the surface of a precoated workpiece, namely polishing the surface by using a grinding wheel or abrasive paper to remove rust, burrs and flashes, and removing oil stains on the surface by using acetone;
secondly, ball-milling and mixing metal powder of Cr, Mn, Fe and Ni-B, Al-Si according to a certain proportion to carry out alloying, and then preparing the high-entropy alloy target by adopting pressure sintering, wherein the purity of the metal powder of Cr, Mn and Fe is 99.5-100%, and the particle size of the metal powder is 30-120 mu m; the mass percent of B in the Ni-B metal powder is 3-4%, and the mass percent of Ni is 96-97%; the mass percent of Si in the Al-Si metal powder is 3-4%, and the mass percent of Al is 96-97%; the mass ratio of Cr, Mn, Fe and Ni-B, Al-Si metal powder is 1-1.1: 1.2-1.3: 1.2-1.4: 0.6-0.7; the pressure sintering process comprises the following steps: pressurizing 200-320 MPa in a pressure sintering furnace under the protection of argon, wherein the sintering temperature is 860-970 ℃, and preserving heat for 4-7 minutes;
step three, placing the high-entropy alloy target on a direct current cathode, closing a vacuum chamber, vacuumizing and filling argon, and then performing ion cleaning, wherein the process comprises the following steps: vacuum-pumping to 2 × 10-2 Pa ~ 2×10 -3Pa, introducing the flow of an Ar gas-regulated gas flowmeter to stabilize the gas pressure at 2-6 Pa, turning on a negative bias power supply, regulating the negative bias to a range of 400-900V, performing ion bombardment glow cleaning on the pre-coated workpiece for 10-20 minutes, and starting a heater to heat the pre-coated workpiece;
and step four, after the ion cleaning is finished, starting a heater to heat the precoated workpiece for magnetron sputtering, wherein the process comprises the following steps of firstly introducing 10-50 liters/minute of mixed gas of argon and nitrogen into a vacuum chamber, wherein the argon: the flow ratio of nitrogen is 1: 2-3, the working air pressure is kept at 0.5-1.7 Pa, the target spacing is kept at 30-80 mm, the temperature of a workpiece is kept at 150-190 ℃, the bias voltage of a matrix is 0.3-0.4 kV, and reactive magnetron sputtering is carried out under the current of 0.1-0.75A, and the sputtering time is controlled for 4-8 minutes;
and step five, obtaining the AlN and CrN enhanced AlCrFeMnNi high-entropy alloy coating after the magnetron sputtering is finished.
2. The method for preparing the high-entropy alloy coating by magnetron sputtering according to claim 1, characterized in that: the precoated workpiece is made of high-speed steel.
3. The method for preparing the high-entropy alloy coating by magnetron sputtering according to claim 1, characterized in that: the ball milling and mixing are carried out by adopting a steel ball milling tank, wherein the mass ratio of milling balls to metal powder is 2.7-3.3: 1, a vacuum valve is opened after sealing, vacuum pumping is carried out for 20-30 minutes, the ball milling tank is placed into a planetary ball mill, the rotating speed is 260-300 r/min, the inversion frequency is 32-45 Hz, and the ball milling and mixing time is 40-50 minutes.
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CN113308675B (en) * 2021-05-10 2023-04-25 西安工业大学 High-entropy alloy nitride cutter coating and preparation method thereof
CN114250441B (en) * 2021-12-23 2023-12-08 黑龙江省原子能研究院 Method for preparing bismuth-antimony alloy coating with uniform surface and stable combination by utilizing magnetron sputtering
CN116496760A (en) * 2022-01-19 2023-07-28 中南大学 Superhard material abrasive particles with multi-principal element medium/high entropy alloy coating layer and preparation method thereof
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