CN115110030B - Cerium doped high-entropy alloy nitride coating and preparation method thereof - Google Patents

Cerium doped high-entropy alloy nitride coating and preparation method thereof Download PDF

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CN115110030B
CN115110030B CN202210787585.0A CN202210787585A CN115110030B CN 115110030 B CN115110030 B CN 115110030B CN 202210787585 A CN202210787585 A CN 202210787585A CN 115110030 B CN115110030 B CN 115110030B
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entropy alloy
nitride coating
cerium
alloy nitride
coating
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CN115110030A (en
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蔡海潮
薛玉君
叶军
王景华
畅为航
李航
余永健
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Henan University of Science and Technology
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Henan 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
    • 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
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target

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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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Abstract

The invention relates to a cerium doped high-entropy alloy nitride coating and a preparation method thereof, belonging to the technical field of high-entropy alloy coatings. The cerium-doped high-entropy alloy nitride coating provided by the invention comprises the following elements in percentage by mass: 7 to 10 percent of Ti, 5 to 13 percent of Al, 10 to 14 percent of Cr, 14 to 22 percent of Nb, 8 to 11 percent of V, 0.7 to 1.5 percent of Ag, 10 to 31 percent of Ce and 19 to 23 percent of N. The cerium doped high-entropy alloy nitride coating contains cerium element Ce, and the cerium element Ce can change the positions of element atoms in the high-entropy alloy in crystal lattices due to active physical and chemical properties, so that the high-entropy alloy coating can exert thermodynamic high-entropy effect, kinetic slow diffusion effect, serious distortion effect of crystal lattice structure and performance cocktail effect to a greater extent, and the high-entropy alloy coating can be promoted to show higher hardness and elastic modulus and better tribological performance.

Description

Cerium doped high-entropy alloy nitride coating and preparation method thereof
Technical Field
The invention relates to a cerium doped high-entropy alloy nitride coating and a preparation method thereof, belonging to the technical field of high-entropy alloy coatings.
Background
The bearing is a key component in the aerospace equipment, and the dry running performance of the bearing under the oil-loss lubrication working condition is an important guarantee for the safe operation of the aerospace equipment. Over the past decades, the successful application of sulfide solid self-lubricating coatings to mechanical components such as bearings has become an important approach to improving the service performance of mechanical moving parts. However, sulfide coatings suffer from the disadvantage of being susceptible to oxidative failure, which limits their use in aerospace applications.
The high-entropy alloy coating is one of the potential important functional materials in the 21 st century because of the advantages of high strength and hardness, excellent oxidation resistance, corrosion resistance, friction resistance and other mechanical, physical and electrical aspects. The atoms of each element of the high-entropy alloy randomly occupy lattice positions, so that the high-entropy alloy has thermodynamic high-entropy effect, kinetic slow diffusion effect, serious distortion effect of a lattice structure and cocktail effect on performance, and has a plurality of color-developing performances under the synergistic action of a plurality of mechanisms. The potential engineering application of high entropy alloy coatings on precision bearing surfaces has received close attention from many scholars internationally. Chinese patent application CN108411272a discloses a preparation method of AlCrCuFeNi series high entropy alloy coating for bearing, comprising the following steps: and forming a high-entropy alloy coating on the surface of the bearing by using AlCrCuFeNi-series high-entropy alloy as a target material and adopting a magnetron sputtering process. The friction and wear properties of the coating prepared by the method still cannot meet the use requirements of the bearing field.
Disclosure of Invention
The invention aims to provide a cerium doped high-entropy alloy nitride coating, which is used for solving the problem that the friction and wear performance of the existing high-entropy alloy coating cannot meet the use requirements in the field of bearings.
The invention further aims at providing a preparation method of the cerium-doped high-entropy alloy nitride coating.
In order to achieve the above purpose, the technical scheme adopted by the cerium doped high-entropy alloy nitride coating of the invention is as follows:
A cerium-doped high-entropy alloy nitride coating, which consists of the following elements in mass percent: 7 to 10 percent of Ti, 5 to 13 percent of Al, 10 to 14 percent of Cr, 14 to 22 percent of Nb, 8 to 11 percent of V, 0.7 to 1.5 percent of Ag, 10 to 31 percent of Ce and 19 to 23 percent of N.
The cerium doped high-entropy alloy nitride coating contains cerium element Ce, and the cerium element Ce can change the positions of element atoms in the high-entropy alloy in crystal lattices due to active physical and chemical properties, so that the high-entropy alloy coating can exert thermodynamic high-entropy effect, kinetic slow diffusion effect, serious distortion effect of crystal lattice structure and performance cocktail effect to a greater extent, and the high-entropy alloy coating can be promoted to show higher hardness and elastic modulus and better tribological performance; in addition, ag has a self-lubricating effect and is beneficial to improving the mechanical and tribological properties of the cerium-doped high-entropy alloy nitride coating.
Preferably, the cerium-doped high-entropy alloy nitride coating consists of the following elements in percentage by mass ：Ti 7.82～9.97％,Al 5.87～12.55％,Cr 10.81～13.16％,Nb 14.34～21.32％,V 8.28～10.78％,Ag 0.76～1.29％,Ce 10.25～30.42％,N 19.39～22.61％.
Preferably, the cerium-doped high-entropy alloy nitride coating is deposited by a magnetron sputtering method.
Preferably, the cerium doped high entropy alloy nitride coating is deposited on the coated substrate; the coating substrate comprises a matrix material and a transition layer coated on the matrix material; the cerium doped high entropy alloy nitride coating is deposited on the transition layer of the coated substrate. The cerium doped high-entropy alloy nitride coating is deposited on the transition layer, so that the binding force between the cerium doped high-entropy alloy nitride coating and the matrix material can be improved.
Preferably, the matrix material is a metal matrix or a Si matrix. Preferably, the metal matrix is 9Cr18 or GCr15.
Preferably, the transition layer is a chromium layer. Preferably, the transition layer is deposited on the substrate material by magnetron sputtering.
Preferably, the thickness of the transition layer is 100-200 nm. When the thickness of the transition layer is 100-200 nm, the bonding force between the substrate material and the cerium doped high-entropy alloy nitride coating can be improved.
Preferably, the thickness of the cerium doped high entropy alloy nitride coating is 1-2.5 μm. When the thickness of the cerium doped high-entropy alloy nitride coating is 1-2.5 mu m, the compactness of the coating can be improved, and the coating is ensured to have good performance.
The preparation method of the cerium doped high-entropy alloy nitride coating adopts the following technical scheme:
The preparation method of the cerium doped high-entropy alloy nitride coating comprises the following steps:
(1) Providing a coated substrate; the coating substrate comprises a matrix material and a transition layer coated on the matrix material;
(2) Depositing a cerium doped high entropy alloy nitride coating on the transition layer of the coated substrate; the cerium-doped high-entropy alloy nitride coating consists of the following elements in percentage by mass: 7 to 10 percent of Ti, 5 to 13 percent of Al, 10 to 14 percent of Cr, 14 to 22 percent of Nb, 8 to 11 percent of V, 0.7 to 1.5 percent of Ag, 10 to 31 percent of Ce and 19 to 23 percent of N.
The cerium-doped high-entropy alloy nitride coating prepared by the preparation method of the cerium-doped high-entropy alloy nitride coating has higher hardness, elastic modulus and excellent wear resistance. The hardness and the elastic modulus of the cerium doped high-entropy alloy nitride coating prepared by the invention can reach 18.8GPa and 162.9GPa at maximum respectively, and the ratio (H/E value) of the hardness and the elastic modulus is between 0.09 and 0.12, so that the cerium doped high-entropy alloy nitride coating has excellent wear resistance.
Preferably, in the preparation method of the cerium doped high-entropy alloy nitride coating, the cerium doped high-entropy alloy nitride coating consists of the following elements in percentage by mass ：Ti 7.82～9.97％,Al 5.87～12.55％,Cr 10.81～13.16％,Nb 14.34～21.32％,V 8.28～10.78％,Ag 0.76～1.29％,Ce 10.25～30.42％,N 19.39～22.61％.
Preferably, in the preparation method of the cerium doped high-entropy alloy nitride coating, the transition layer is a chromium layer. Preferably, in the preparation method of the cerium doped high-entropy alloy nitride coating, the thickness of the transition layer is 100-200 nm.
Preferably, in the preparation method of the cerium doped high-entropy alloy nitride coating, the transition layer is formed by depositing on a base material in a magnetron sputtering mode.
Preferably, in the preparation method of the cerium doped high-entropy alloy nitride coating, the matrix material is a metal matrix or a Si matrix. Preferably, in the preparation method of the cerium doped high-entropy alloy nitride coating, the metal matrix is 9Cr18 or GCr15.
Preferably, before depositing the transition layer on the base material, ethanol and acetone are sequentially adopted to carry out ultrasonic cleaning on the base material, and then the transition layer is deposited on the base material after ultrasonic cleaning. Preferably, the ultrasonic cleaning of the substrate with ethanol takes place for 30 minutes. Preferably, the time for ultrasonic cleaning of the base material with acetone is 20min.
Preferably, the method for depositing and forming the transition layer on the substrate material by adopting a magnetron sputtering mode comprises the following steps: and placing the substrate material into a vacuum reaction cavity, taking a metal target as a target material, taking inert gas as a sputtering atmosphere, depositing a transition layer on the substrate material, and obtaining the substrate material deposited with the transition layer as a coating substrate.
Preferably, in the method of forming the transition layer on the substrate material by deposition in a magnetron sputtering mode, the temperature of the substrate material is 200-350 ℃. For example, in a method of forming a transition layer by deposition on a base material by magnetron sputtering, the temperature of the base material is 300 ℃. Preferably, in the method of forming the transition layer on the base material by deposition using the magnetron sputtering method, the bias voltage of the base material is 0-50V. For example, in a method of forming a transition layer by deposition on a base material by magnetron sputtering, the bias voltage of the base material is 0V.
Preferably, after the matrix material is placed in the vacuum reaction cavity, the vacuum reaction cavity is vacuumized, so that the vacuum degree in the vacuum reaction cavity reaches 5×10 -4 Pa, then inert gas is introduced into the vacuum reaction cavity, and then a transition layer is formed by deposition on the matrix material.
Preferably, the metal target is a chromium target. Preferably, in the method of forming the transition layer on the substrate material by deposition using a magnetron sputtering method, the inert gas is argon. Preferably, in the method of depositing the transition layer on the substrate material by using a magnetron sputtering method, the flow rate of the inert gas is 10-30 sccm. For example, in the method of depositing the transition layer on the substrate by using the magnetron sputtering method, the flow rate of the inert gas is 20sccm. Preferably, in the method of forming the transition layer on the base material by deposition using the magnetron sputtering method, the sputtering deposition pressure is 0.2 to 0.6Pa. For example, in a method of depositing a transition layer on a base material by magnetron sputtering, the sputtering deposition pressure is 0.3Pa. Preferably, the sputtering power of the metal target is 150 to 200W. For example, the sputtering power of the metal target is 200W. Preferably, the sputtering time taken to deposit the transition layer on the substrate material is 20-30 min. For example, the sputtering time taken to deposit the transition layer on the substrate material is 20 minutes.
Preferably, in the preparation method of the cerium doped high-entropy alloy nitride coating, the cerium doped high-entropy alloy nitride coating is deposited on the transition layer by a magnetron sputtering method.
It can be understood that after the transition layer is deposited on the substrate material by adopting the magnetron sputtering method, the cerium doped high-entropy alloy nitride coating can be continuously deposited on the transition layer by adopting the same magnetron sputtering equipment, or the substrate material deposited with the transition layer can be stored for standby, and the cerium doped high-entropy alloy nitride coating can be deposited on the transition layer by adopting the magnetron sputtering method when required at the later stage.
Preferably, in the preparation method of the cerium doped high-entropy alloy nitride coating, the magnetron sputtering method comprises the following steps: the coating substrate is placed in a vacuum reaction cavity, and a metal-based target is sputtered to deposit a cerium-doped high-entropy alloy nitride coating on a transition layer by taking N 2 -containing gas as sputtering atmosphere; the N 2 -containing gas consists of N 2 and an inert gas.
Preferably, in the method for depositing the cerium doped high entropy alloy nitride coating on the transition layer by using the magnetron sputtering method, the temperature of the coating substrate is 200-350 ℃. For example, in a method of depositing a cerium doped high entropy alloy nitride coating on a transition layer using a magnetron sputtering method, the temperature of the coated substrate is 300 ℃.
Preferably, the metal-based targets are Ce-Ag alloy targets and TiAlCrNbV high-entropy alloy targets. The Ce-Ag alloy target and TiAlCrNbV high-entropy alloy target are used as deposition sources, so that the preparation process can be simplified, and uniformity of Ti, al, cr, nb, V in the prepared coating can be improved.
Preferably, the atomic number ratio of Ce to Ag in the Ce-Ag alloy target is (0.9-1.1): 0.9-1.1. For example, the atomic number ratio of Ce to Ag in the Ce-Ag alloy target is 1:1. The Ce-Ag alloy target is used as a Ce source, so that the Ce can be prevented from being oxidized.
Preferably, the atomic number ratio of Ti, al, cr, nb to V in the TiAlCrNbV high-entropy alloy target is (0.9-1.1): (0.9-1.1). For example, the atomic number ratio of Ti, al, cr, nb to V in the TiAlCrNbV high-entropy alloy target is 1:1:1:1:1. When the atomic number ratio of Ti, al, cr, nb to V in TiAlCrNbV high-entropy alloy target is 1:1:1:1, the uniformity of Ti, al, cr, nb and V in the prepared high-entropy alloy nitride coating is improved.
Preferably, the purity of the Ce-Ag alloy target is 99.99%. Preferably, the TiAlCrNbV high-entropy alloy target has a purity of 99.99%.
Preferably, the sputtering power of the Ce-Ag alloy target is 50-180W. Preferably, the sputtering power of TiAlCrNbV high-entropy alloy target is 120-180W. Preferably, the sputtering power of the Ce-Ag alloy target is 50-150W. Further preferably, the sputtering power of the ce—ag alloy target is 100W. Further preferably, the sputtering power of TiCrNbAlV alloy targets is 150W.
Preferably, the Ce-Ag alloy is sputtered using a dc power supply. Preferably, the TiAlCrNbV alloy is sputtered using a radio frequency power source.
Preferably, in the method for depositing the cerium-doped high-entropy alloy nitride coating on the transition layer, the sputtering time is 120-180 min. For example, in the method of depositing a cerium doped high entropy alloy nitride coating on a transition layer, a sputtering time of 180min is used.
Preferably, in the method for depositing the cerium-doped high-entropy alloy nitride coating on the transition layer, a sputter deposition pressure of 0.2 to 0.6Pa is used. Further preferably, in the method of depositing the cerium-doped high-entropy alloy nitride coating on the transition layer, a sputter deposition pressure of 0.3 to 0.5Pa is used. For example, in the method of depositing a cerium doped high entropy alloy nitride coating on a transition layer, a sputter deposition pressure of 0.3Pa is used.
Preferably, the flow rate of the N 2 -containing gas is 25-70 sccm. Preferably, the flow rate of N 2 in the N 2 -containing gas is 15-40 sccm. For example, the flow rate of N 2 in the N 2 -containing gas is 20sccm. Preferably, the inert gas in the N 2 -containing gas is argon. Preferably, the flow rate of the inert gas in the N 2 -containing gas is 10-30 sccm. For example, the flow rate of the inert gas in the N 2 -containing gas is 20sccm.
Preferably, in the preparation method of the cerium doped high-entropy alloy nitride coating, the thickness of the cerium doped high-entropy alloy nitride coating is 1-2.5 mu m. Preferably, in the preparation method of the cerium doped high-entropy alloy nitride coating, the thickness of the cerium doped high-entropy alloy nitride coating is 2-2.4 mu m. For example, in the preparation method of the cerium-doped high-entropy alloy nitride coating, the thickness of the cerium-doped high-entropy alloy nitride coating is 2.0 μm.
Drawings
FIG. 1 is an XRD spectrum of the high entropy alloy nitride coating prepared in example 5 and comparative example in experimental example 1;
FIG. 2 is a schematic diagram showing the appearance of the cerium-doped high-entropy alloy nitride coating prepared in example 4 of experimental example 2 after friction test at room temperature;
FIG. 3 is a schematic view of the appearance of the cerium-doped high-entropy alloy nitride coating prepared in example 5 of experimental example 2 after friction test at room temperature;
FIG. 4 is a schematic view of the appearance of the cerium-doped high-entropy alloy nitride coating prepared in example 6 of experimental example 2 after friction test at room temperature;
FIG. 5 is a schematic diagram showing the appearance of the cerium-doped high-entropy alloy nitride coating prepared in Experimental example 2 after friction test at 500 ℃;
FIG. 6 is an XPS spectrum of the high-entropy alloy nitride coating prepared in example 5.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
The purity of the Ce-Ag alloy target used in the examples and the comparative examples is 99.99%, and the atomic number ratio of Ce to Ag in the Ce-Ag alloy target is 1:1; the purity of the TiAlCrNbV high-entropy alloy target material is 99.99%, and the atomic number ratio of Ti, al, cr, nb to V in the TiAlCrNbV high-entropy alloy target material is 1:1:1:1:1.TiAlCrNbV alloy is prepared from Ti, al, cr, nb and V by adopting a powder metallurgy method. The preparation method of the Ce-Ag alloy comprises the following steps: ce and Ag with the atomic ratio of 1:1 are prepared by adopting a smelting method.
1. Specific examples of cerium-doped high-entropy alloy nitride coatings of the present invention are as follows:
Example 1
The cerium-doped high-entropy alloy nitride coating of the embodiment comprises the following elements in percentage by mass: 9.97% of Ti, 12.55% of Al, 13.16% of Cr, 21.32% of Nb, 10.78% of V, 0.76% of Ag, 10.25% of Ce and 21.21% of N. The thickness of the cerium-doped high-entropy alloy nitride coating of this example was 2.4 μm.
Example 2
The cerium-doped high-entropy alloy nitride coating of the embodiment comprises the following elements in percentage by mass: ti7.82%, al 5.87%, cr 10.81%, nb 16.43%, V8.43%, ag 0.82%, ce 30.42%, N19.39%. The thickness of the cerium-doped high-entropy alloy nitride coating of this example was 2.0 μm.
Example 3
The cerium-doped high-entropy alloy nitride coating of the embodiment comprises the following elements in percentage by mass: 8.12% of Ti, 6.34% of Al, 12.41% of Cr, 14.34% of Nb, 8.28% of V, 1.29% of Ag, 26.61% of Ce and 22.61% of N. The thickness of the cerium-doped high-entropy alloy nitride coating of this example was 2.2 μm.
2. The specific examples of the preparation method of the cerium-doped high-entropy alloy nitride coating of the invention are as follows:
Example 4
The preparation method of the cerium-doped high-entropy alloy nitride coating of the embodiment is the preparation method of the cerium-doped high-entropy alloy nitride coating of embodiment 1, and specifically comprises the following steps:
(1) The method comprises the steps of firstly carrying out ultrasonic cleaning on a metal matrix material and a monocrystalline silicon piece (Si matrix material) which are made of 9Cr18 by adopting ethanol in an ultrasonic cleaner for 30min, then carrying out ultrasonic cleaning by adopting acetone in the ultrasonic cleaner for 20min, and then drying the metal matrix material and the Si matrix material after ultrasonic cleaning to obtain a pretreated metal matrix material and a pretreated Si matrix material.
(2) Placing the pretreated metal matrix material and the Si matrix material into a vacuum reaction cavity of a magnetron sputtering machine, vacuumizing the vacuum reaction cavity to ensure that the pressure of the vacuum reaction cavity is 5 multiplied by 10 -4 Pa, then introducing working gas argon with the flow of 20sccm, controlling the pressure of the vacuum reaction cavity to be 0.3Pa, heating the pretreated metal matrix material and the Si matrix material to 300 ℃, opening a chromium target baffle, taking the chromium target as a target material, applying no matrix bias voltage, exciting the chromium target by using a direct current power supply with the power of 200W, forming stable glow, sputtering and depositing on the surfaces of the pretreated metal matrix material and the Si matrix material to form a chromium transition layer, wherein the sputtering and depositing time is 20min, and the thickness of the transition layer formed on the surfaces of the pretreated metal matrix material and the Si matrix material is 200nm. The obtained metal matrix material and Si matrix material deposited with the chromium transition layer are the coating substrate.
Then simultaneously opening a Ce-Ag alloy target baffle and a TiAlCrNbV high-entropy alloy target baffle, introducing nitrogen with the flow of 20sccm, controlling the pressure of a vacuum reaction cavity to be 0.3Pa, then using a radio frequency power supply to excite the Ce-Ag alloy target and using a direct current power supply to excite the TiAlCrNbV high-entropy alloy target, controlling the sputtering power of the Ce-Ag alloy target to be 50W and the sputtering power of the TiAlCrNbV high-entropy alloy target to be 150W, keeping the temperature of a coating substrate to be 300 ℃, forming a cerium doped high-entropy alloy nitride coating on a chromium transition layer through co-sputtering of the Ce-Ag alloy target and the TiAlCrNbV high-entropy alloy target, wherein the co-sputtering time is 180min, and the thicknesses of the cerium doped high-entropy alloy nitride coating deposited on the transition layer on the surface of the metal matrix material and the transition layer on the surface of the Si matrix material are both 2.4 mu m.
Example 5
The preparation method of the cerium-doped high-entropy alloy nitride coating of the embodiment is the preparation method of the cerium-doped high-entropy alloy nitride coating of embodiment 2, and specifically comprises the following steps:
(1) The method comprises the steps of firstly carrying out ultrasonic cleaning on a metal matrix material and a monocrystalline silicon piece (Si matrix material) which are made of 9Cr18 by adopting ethanol in an ultrasonic cleaner for 30min, then carrying out ultrasonic cleaning by adopting acetone in the ultrasonic cleaner for 20min, and then drying the metal matrix material and the Si matrix material after ultrasonic cleaning to obtain a pretreated metal matrix material and a pretreated Si matrix material.
(2) Placing the pretreated metal matrix material and the Si matrix material into a vacuum reaction cavity of a magnetron sputtering machine, vacuumizing the vacuum reaction cavity to ensure that the pressure of the vacuum reaction cavity is 5 multiplied by 10 -4 Pa, then introducing working gas argon with the flow of 20sccm, controlling the pressure of the vacuum reaction cavity to be 0.3Pa, heating the pretreated metal matrix material and the Si matrix material to 300 ℃, opening a chromium target baffle, taking the chromium target as a target material, applying no matrix bias voltage, exciting the chromium target by using a direct current power supply with the power of 200W, forming stable glow, sputtering and depositing on the surfaces of the pretreated metal matrix material and the Si matrix material to form a chromium transition layer, wherein the sputtering and depositing time is 20min, and the thickness of the transition layer formed on the surfaces of the pretreated metal matrix material and the Si matrix material is 200nm. The obtained metal matrix material and Si matrix material deposited with the chromium transition layer are the coating substrate.
Then simultaneously opening a Ce-Ag alloy target baffle and a TiAlCrNbV high-entropy alloy target baffle, introducing nitrogen with the flow of 20sccm, controlling the pressure of a vacuum reaction cavity to be 0.3Pa, then using a radio frequency power supply to excite the Ce-Ag alloy target and using a direct current power supply to excite the TiAlCrNbV high-entropy alloy target, controlling the sputtering power of the Ce-Ag alloy target to be 100W and the sputtering power of the TiAlCrNbV high-entropy alloy target to be 150W, keeping the temperature of a coating substrate to be 300 ℃, forming a cerium doped high-entropy alloy nitride coating on a chromium transition layer through co-sputtering of the Ce-Ag alloy target and the TiAlCrNbV high-entropy alloy target, wherein the co-sputtering time is 180min, and the thicknesses of the cerium doped high-entropy alloy nitride coating deposited on the transition layer on the surface of the metal matrix material and the transition layer on the surface of the Si matrix material are both 2.0 mu m.
Example 6
The preparation method of the cerium-doped high-entropy alloy nitride coating of the embodiment is the preparation method of the cerium-doped high-entropy alloy nitride coating of embodiment 3, and specifically comprises the following steps:
(1) The method comprises the steps of firstly carrying out ultrasonic cleaning on a metal matrix material and a monocrystalline silicon piece (Si matrix material) which are made of 9Cr18 by adopting ethanol in an ultrasonic cleaner for 30min, then carrying out ultrasonic cleaning by adopting acetone in the ultrasonic cleaner for 20min, and then drying the metal matrix material and the Si matrix material after ultrasonic cleaning to obtain a pretreated metal matrix material and a pretreated Si matrix material.
(2) Placing the pretreated metal matrix material and the Si matrix material into a vacuum reaction cavity of a magnetron sputtering machine, vacuumizing the vacuum reaction cavity to ensure that the pressure of the vacuum reaction cavity is 5 multiplied by 10 -4 Pa, then introducing working gas argon with the flow of 20sccm, controlling the pressure of the vacuum reaction cavity to be 0.3Pa, heating the pretreated metal matrix material and the Si matrix material to 300 ℃, opening a chromium target baffle, taking the chromium target as a target material, applying no matrix bias voltage, exciting the chromium target by using a direct current power supply with the power of 200W, forming stable glow, sputtering and depositing on the surfaces of the pretreated metal matrix material and the Si matrix material to form a chromium transition layer, wherein the sputtering and depositing time is 20min, and the thickness of the transition layer formed on the surfaces of the pretreated metal matrix material and the Si matrix material is 200nm. The obtained metal matrix material and Si matrix material deposited with the chromium transition layer are the coating substrate.
Then simultaneously opening a Ce-Ag alloy target baffle and a TiAlCrNbV high-entropy alloy target baffle, introducing nitrogen with the flow of 20sccm, controlling the pressure of a vacuum reaction cavity to be 0.3Pa, then using a radio frequency power supply to excite the Ce-Ag alloy target and using a direct current power supply to excite the TiAlCrNbV high-entropy alloy target, controlling the sputtering power of the Ce-Ag alloy target to be 150W and the sputtering power of the TiAlCrNbV high-entropy alloy target to be 150W, keeping the temperature of a coating substrate to be 300 ℃, forming a cerium doped high-entropy alloy nitride coating on a chromium transition layer through co-sputtering of the Ce-Ag alloy target and the TiAlCrNbV high-entropy alloy target, wherein the co-sputtering time is 180min, and the thicknesses of the cerium doped high-entropy alloy nitride coating deposited on the transition layer on the surface of the metal matrix material and the transition layer on the surface of the Si matrix material are both 2.2 mu m.
Comparative example 1
The preparation method of the high-entropy alloy nitride coating of the comparative example specifically comprises the following steps:
(1) The method comprises the steps of firstly carrying out ultrasonic cleaning on a metal matrix material and a monocrystalline silicon piece (Si matrix material) which are made of 9Cr18 by adopting ethanol in an ultrasonic cleaner for 30min, then carrying out ultrasonic cleaning by adopting acetone in the ultrasonic cleaner for 20min, and then drying the metal matrix material and the Si matrix material after ultrasonic cleaning to obtain a pretreated metal matrix material and a pretreated Si matrix material.
(2) Placing the pretreated metal matrix material and the Si matrix material into a vacuum reaction cavity of a magnetron sputtering machine, vacuumizing the vacuum reaction cavity to ensure that the pressure of the vacuum reaction cavity is 5 multiplied by 10 -4 Pa, then introducing working gas argon with the flow of 20sccm, controlling the pressure of the vacuum reaction cavity to be 0.3Pa, heating the pretreated metal matrix material and the Si matrix material to 300 ℃, opening a chromium target baffle, taking the chromium target as a target material, applying no matrix bias voltage, exciting the chromium target by using a direct current power supply with the power of 200W, forming stable glow, sputtering and depositing on the surfaces of the pretreated metal matrix material and the Si matrix material to form a chromium transition layer, wherein the sputtering and depositing time is 20min, and the thickness of the transition layer formed on the surfaces of the pretreated metal matrix material and the Si matrix material is 200nm. The obtained metal matrix material and Si matrix material deposited with the chromium transition layer are the coating substrate.
Then simultaneously opening an Ag target baffle and a TiAlCrNbV high-entropy alloy target baffle, introducing nitrogen with the flow of 20sccm, controlling the pressure of a vacuum reaction cavity to be 0.3Pa, then using a radio frequency power supply to excite the Ag target and using a direct current power supply to excite the TiAlCrNbV high-entropy alloy target, controlling the sputtering power of the Ag alloy target to be 100W and the sputtering power of the TiAlCrNbV high-entropy alloy target to be 150W, keeping the temperature of a coating substrate to be 300 ℃, forming a high-entropy alloy nitride coating by co-sputtering the Ag target and the TiAlCrNbV high-entropy alloy target on a chromium transition layer, wherein the co-sputtering time is 180min, and the thickness of the high-entropy alloy nitride coating deposited on the transition layer on the surface of the metal matrix material and the transition layer on the surface of the Si matrix material is 2.1 mu m.
The high-entropy alloy nitride coating prepared by the comparative example consists of the following elements in percentage by mass: 12.45% of Ti, 5.26% of Al, 9.98% of Cr, 19.34% of Nb, 6.81% of V, 6.7% of Ag and 39.47% of N.
Comparative example 2
The preparation method of the high-entropy alloy nitride coating of the present comparative example differs from that of example 5 only in that the Ce-Ag alloy target is replaced with the La-Ag alloy target in step (2) of the present comparative example.
Comparative example 3
The preparation method of the high-entropy alloy nitride coating of the comparative example specifically comprises the following steps:
(1) And (3) firstly ultrasonically cleaning the metal matrix material with GCr15 and the monocrystalline silicon piece (Si matrix material) in an ultrasonic cleaner for 10min by adopting acetone, and then drying the ultrasonically cleaned metal matrix material and Si matrix material to obtain a pretreated metal matrix material and Si matrix material.
(2) Placing the pretreated metal matrix material and the Si matrix material into a vacuum reaction cavity of a magnetron sputtering machine, vacuumizing the vacuum reaction cavity to ensure that the pressure of the vacuum reaction cavity is 3.2 multiplied by 10 -3 Pa, then introducing working gas argon with the flow of 20sccm, controlling the pressure of the vacuum reaction cavity to be 0.1Pa, and then performing back sputtering cleaning on a matrix and a target material for 30min, wherein the target current is 1.25A and the matrix bias voltage is-400V. And opening a chromium target baffle, taking the chromium target as a target material, applying a base bias voltage of-110V, exciting the chromium target by using a direct current power supply with a target current of 1.25A, forming stable glow, and performing sputter deposition on the surfaces of the pretreated metal base material and the Si base material to form a chromium bottom layer, wherein the sputter deposition time is 20min. The obtained metal matrix material and Si matrix material deposited with the chromium transition layer are the coating substrate. Then introducing nitrogen with the flow of 6sccm, and continuing to bombard the surface of the matrix for 20min to form the CrN transition layer.
Then opening AlCrCuFeNi a high-entropy alloy target baffle plate, introducing nitrogen with the flow of 6sccm, controlling the pressure of a vacuum reaction cavity to be 0.1Pa, exciting AlCrCuFeNi the high-entropy alloy target by using a direct current power supply, controlling the sputtering current of the high-entropy alloy target to be 1.25A, forming a high-entropy alloy nitride coating by sputtering and depositing on a CrN transition layer through co-sputtering of the AlCrCuFeNi high-entropy alloy target, wherein the co-sputtering time is 60min, and the thickness of the high-entropy alloy nitride coating deposited on the transition layer on the surface of the metal matrix material and the transition layer on the surface of the Si matrix material is 1.2 mu m.
Comparative example 4
The preparation method of the high-entropy alloy nitride coating of the present comparative example is different from the preparation method of the high-entropy alloy nitride coating of comparative example 3 only in that in the step (2) of the preparation method of the high-entropy alloy nitride coating of the present comparative example, after forming the CrN transition layer on the metal base material and the Si base material, the Ce-Ag target baffle and the AlCrCuFeNi high-entropy alloy target baffle are simultaneously opened and the nitrogen gas with the flow rate of 6sccm is introduced, the pressure of the vacuum reaction chamber is controlled to be 0.1Pa, the Ce-Ag target is excited by the radio frequency power supply and the AlCrCuFeNi high-entropy alloy target is excited by the direct current power supply, the target current of the Ce-Ag alloy target is controlled to be 1A and the sputtering current of the AlCrCuFeNi high-entropy alloy target is controlled to be 1.25A, the high-entropy alloy nitride coating is formed on the CrN transition layer by co-sputtering of the Ce-Ag target and the AlCrCuFeNi high-entropy alloy target, the co-sputtering time is 60min, and the thickness of the high-entropy alloy nitride coating deposited on the transition layer on the surface of the metal base material and the Si base material is 1.02 μm.
Experimental example 1
To determine the microstructure of the prepared coating, the structure of the high entropy alloy nitride coating prepared in example 5 and comparative example 1 was characterized using an XRD scanner, and the results are shown in fig. 1. As can be seen from fig. 1, in combination with the existing studies, it is shown that the high-entropy alloy crystals form a single disordered BCC (body centered cubic) or FCC (face centered cubic) structure by mutual solutionizing of various elements in the absence of main elements. The high entropy alloy nitride coatings prepared in comparative example 1 and example 5 have a single FCC solid solution structure, since AlN, crN, nbN, tiN, agN and VN are both FCC structures. The high-entropy alloy nitride coating prepared in comparative example 1 has a wide bulge diffraction peak similar to steamed bread at the left side of 43 degrees, and has an amorphous structure, which shows that the crystallinity is low; the (111) crystal plane diffraction peak of the high-entropy alloy nitride coating prepared in example 5 is shifted leftwards and widened, which shows that with the addition of Ce or CeAg, particle bombardment is enhanced, crystallinity is improved, and preferential growth along the (111) crystal plane is obvious. The diffraction peak of the (200) crystal plane appears at 43 deg. for both coatings, and the diffraction peak of the (200) crystal plane of the high-entropy alloy nitride coating prepared in example 5 is enhanced compared with the XRD pattern of the high-entropy alloy nitride coating prepared in comparative example 1, which indicates that the preferred orientation of the coating is gradually changed from the (111) crystal plane to the (200) crystal plane. The analytical reasons are that this is related to the lowest strain energy of the (111) crystal plane and the lowest surface energy of the (200) crystal plane, and the increase of the surface adsorption atom mobility results in the growth of the coating along the crystal plane with the lowest surface energy of the (200) due to the difference of the Ce atom radius and other elements, thus improving the microstructure of the coating.
Experimental example 2
To evaluate the mechanical properties of the high-entropy alloy nitride coatings prepared in examples 4 to 6 and comparative examples 1 to 4, the hardness, elastic modulus, and abrasion resistance of the high-entropy alloy nitride coatings prepared in examples 4 to 6 and comparative examples 1 to 4, respectively, were tested. Wherein, adopt iNano nanometer indentation appearance analysis coating hardness and elastic modulus, select Berkovich pressure head to carry out hardness test. The test load adopted during iNano nanometer indentation instrument test is 50mN, and the maximum indentation depth is not more than 1/10 of the film thickness. The wear resistance is characterized by a friction coefficient and a wear rate, wherein the friction coefficient is obtained by testing a high-temperature friction and wear testing machine, and the friction test adopts the following parameters: the friction radius is 5mm, the diameter of the grinding ball is 6mm, the rotating speed is 336r/min, and the normal load is 10N; the wear rate is calculated according to the formula w=v/f×l (where V is the wear scar wear volume, F is the normal load applied by the friction test, and L is the friction stroke length). The friction test is dry friction, the temperature adopted in the friction test is room temperature or 500 ℃, and after the friction test, the appearance of the high-entropy alloy nitride coating prepared in the examples 4-6 after the friction test is observed by adopting a scanning electron microscope.
In order to ensure the accuracy of the test results of the wear resistance, the hardness and the elastic modulus, the high-entropy alloy nitride coating deposited on the surface of the metal matrix material is used for testing the wear resistance, and the high-entropy alloy nitride coating deposited on the surface of the Si matrix material is used for testing the hardness and the elastic modulus, and the accuracy of the hardness test of the coating can be ensured by adopting the Si matrix as the hardness test because the nano indentation instrument is calibrated by the Si matrix.
The test results of hardness, elastic modulus and abrasion resistance of the high-entropy alloy nitride coatings prepared in examples 4 to 6 and comparative examples 1 to 4 are shown in tables 1 to 2, and the appearance of the high-entropy alloy nitride coatings prepared in examples 4 to 6 after the friction test is shown in fig. 2 to 5, wherein fig. 2 to 4 is the appearance of the high-entropy alloy nitride coatings prepared in examples 4 to 6 after the friction test at room temperature, and fig. 5 is the appearance of the high-entropy alloy nitride coating prepared in example 5 after the friction test at 500 ℃.
TABLE 1 hardness, elastic modulus of high entropy alloy nitride coatings prepared in examples 4-6 and comparative examples 1-4
Note that: H/E represents the ratio of hardness to elastic modulus of the high entropy alloy nitride coating.
Table 2 wear resistance at room temperature and 500 c of the high entropy alloy nitride coatings prepared in examples 4-6 and comparative examples 1-4
The results show that the ratio (H/E value) of the hardness and the elastic modulus of the high-entropy alloy nitride coatings prepared in examples 4-6 and comparative example 4 is greater than the ratio of the hardness and the elastic modulus of the high-entropy alloy nitride coatings prepared in comparative examples 1-3, indicating that the high-entropy alloy nitride coatings doped with rare earth element Ce have higher plastic deformation resistance. In addition, the abrasion loss of the high-entropy alloy nitride coatings prepared in examples 4-6 at room temperature is smaller than that of the high-entropy alloy nitride coatings prepared in comparative examples 1-4, which shows that the high-entropy alloy nitride coatings can have better tribological properties by doping rare earth elements. Further comparing the tribological properties at high temperature and high temperature, it is found that the friction coefficient and the abrasion loss of the coating at high temperature are reduced, especially the friction coefficient and the abrasion loss of the high-entropy alloy nitride coating prepared in example 5 are minimum, and analysis shows that the mechanism for improving the friction performance of the coating is that the oxide formed in friction generates a synergistic lubrication effect with cerium oxide and Ag, the oxide formed at high temperature and the lubrication phase thereof effectively reduce the friction abrasion of the coating, and the friction abrasion is relatively large due to insufficient oxide generated in the friction process at room temperature.
When the metal matrix material of 9Cr18 in the preparation method of the cerium-doped high-entropy alloy nitride coating of example 5 was replaced with the metal matrix material of GCr15, the friction coefficient and the wear amount of the prepared cerium-doped high-entropy alloy nitride coating at room temperature and 500 ℃ were the same as those of the cerium-doped high-entropy alloy nitride coating prepared in example 5, respectively.
Experimental example 3
Since the high-entropy alloy nitride coating prepared in example 5 has better tribological properties at high temperature than at room temperature, to further confirm the excellent high-temperature tribological properties of the high-entropy alloy nitride coating prepared in example 5, the valence state was characterized by XPS, and the result is shown in fig. 6, where the XPS spectrum of Ce in fig. 6 shows the presence of CeO 2 in the high-entropy alloy nitride coating prepared in example 5. Therefore, during the abrasion test, ceO 2、Ce2O3 with a layered structure formed on the surface of the high-entropy alloy nitride coating prepared in example 5 and the soft metal Ag present on the surface together form a synergistic lubrication effect, so that the frictional abrasion of the coating is reduced, and the synergistic lubrication effect of Ag, ceO 2、Ce2O3 and other oxides is generated.

Claims (6)

1. The preparation method of the cerium-doped high-entropy alloy nitride coating is characterized by comprising the following elements in percentage by mass ：Ti 7.82～8.12％,Al 5.87～6.34％,Cr10.81～12.41％,Nb 14.34～16.43％,V 8.28～8.43％,Ag 0.82～1.29％,Ce26.61～30.42％,N 19.39～22.61％;: providing a coated substrate comprising a base material and a transition layer coated on the base material; the method comprises the steps of depositing a cerium doped high-entropy alloy nitride coating on a transition layer of a coating substrate by a magnetron sputtering method, wherein N 2 -containing gas is used as a sputtering atmosphere, N 2 -containing gas consists of N 2 and inert gas, the temperature of the coating substrate is 200-350 ℃, metal-based targets used in the deposition are Ce-Ag alloy targets and TiAlCrNbV high-entropy alloy targets, the atomic number ratio of Ce and Ag in the Ce-Ag alloy targets is (0.9-1.1) to (0.9-1.1), the atomic number ratio of Ti, al, cr, nb and V in the TiAlCrNbV high-entropy alloy targets is (0.9-1.1) to (0.9-1.1), the sputtering power of the Ce-Ag alloy targets is 50-180W, the sputtering power of the TiAlBv high-entropy alloy targets is 120-180W, the sputtering pressure of the sputtering targets is 0.2-6 Pa, and the flow of N in the coating substrate is (62.40 cm).
2. The cerium doped high entropy alloy nitride coating according to claim 1, wherein the cerium doped high entropy alloy nitride coating has a thickness of 1 to 2.5 μm.
3. The preparation method of the cerium doped high-entropy alloy nitride coating is characterized by comprising the following steps of: (1) providing a coated substrate; the coating substrate comprises a matrix material and a transition layer coated on the matrix material; (2) The method comprises the steps of depositing a cerium doped high-entropy alloy nitride coating on a transition layer of a coating substrate by a magnetron sputtering method, wherein during deposition, N-containing 2 gas is used as a sputtering atmosphere, N-containing 2 gas consists of N 2 and inert gas, the temperature of the coating substrate is 200-350 ℃, metal base targets used during deposition are Ce-Ag alloy targets and TiAlCrNbV high-entropy alloy targets, the atomic number ratio of Ce to Ag in the Ce-Ag alloy targets is (0.9-1.1) and (0.9-1.1), the atomic number ratio of Ti, al, cr, nb to V in the TiAlCrNbV high-entropy alloy targets is (0.9-1.1) and (0.9-1.1), the sputtering power of the Ce-Ag alloy targets is 50-180W, the sputtering power of the TiAlCrNbV high-entropy alloy targets is 120-180W, the sputtering deposition pressure is 0.2 Pa and the flow rate of N-containing N in the atmosphere is (62.40 cm); the cerium doped high-entropy alloy nitride coating consists of the following elements in percentage by mass ：Ti 7.82～8.12％,Al 5.87～6.34％,Cr10.81～12.41％,Nb 14.34～16.43％,V 8.28～8.43％,Ag 0.82～1.29％,Ce26.61～30.42％,N 19.39～22.61％.
4. The method for preparing a cerium-doped high-entropy alloy nitride coating according to claim 3, wherein the transition layer is a chromium layer; the thickness of the transition layer is 100-200 nm; the thickness of the cerium doped high-entropy alloy nitride coating is 1-2.5 mu m.
5. The method for preparing a cerium-doped high-entropy alloy nitride coating according to claim 4, wherein the thickness of the transition layer is 200nm; the thickness of the cerium doped high-entropy alloy nitride coating is 2-2.4 mu m.
6. The method for preparing a cerium-doped high-entropy alloy nitride coating according to claim 3, wherein the atomic number ratio of Ce to Ag in the Ce-Ag alloy target is 1:1; the atomic number ratio of Ti, al, cr, nb to V in the TiAlCrNbV high-entropy alloy target is 1:1:1:1:1; sputtering power of TiAlCrNbV high-entropy alloy target is 150W; the flow of N 2 in the N 2 -containing gas is 20sccm; and the sputtering deposition pressure adopted for depositing the cerium doped high-entropy alloy nitride coating on the transition layer is 0.3Pa.
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