CN118164783A - High-performance high-entropy ceramic-based nano multilayer coating and preparation method thereof - Google Patents
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- 238000000576 coating method Methods 0.000 title claims abstract description 46
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
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Abstract
The invention provides a preparation method of a high-performance high-entropy ceramic-based nano multilayer coating, which is characterized by comprising the steps of cleaning a substrate and preparing a (TiZrTaWVNb) N/MoS 2 nano multilayer structure coating, and belongs to the technical field of novel hard protective coatings. In the preparation of the (TiZrTaWVNb) N/MoS 2 nanometer multilayer structure coating, the thickness of the modulation layer MoS 2 is controlled, so that the modulation layer is converted into the same lattice structure as the template layer, and the coating interface forms a coherent epitaxial growth morphology.
Description
Technical Field
The invention relates to a high-performance high-entropy ceramic-based nano multilayer coating and a preparation method thereof, belonging to the technical field of novel hard protective coatings.
Background
High entropy ceramics are widely used as superhard coatings, tool surface protection and mechanical friction parts due to their high hardness, high wear resistance and excellent corrosion resistance. However, with the rapid development of the mechanical industry, for the traditional tool coating, only improving the hardness of the tool surface cannot meet the requirements of people on the service life of a workpiece, so that the friction and abrasion of the workpiece surface are effectively reduced, and the abrasion resistance of the workpiece surface is improved, so that the method is one of the important research directions of the current material disciplines.
The proposal and discovery of nano multi-layer films largely solves the high performance requirements of the manufacturing industry, especially the knife coating, on hard films. The concept of nano-multilayer films was originally proposed in 1970 by Koehler first in theory, which is a multilayer structure formed by the alternate deposition of two or more materials having different compositions or structures with each other in the nano-scale in the direction of film growth. In nanomultilayer films deposited alternately from two layers, typically one film is thicker than the other, with the thicker layer being referred to as the bulk layer, also referred to as the template layer, and the thinner layer being referred to as the modulating layer, also referred to as the intervening layer. Wherein each adjacent two layers form a basic repeating unit whose thickness is the modulation period (≡) of the multilayer film. Typically, the a is no more than 100nm. The ratio of the thicknesses of modulation layers a and B is referred to as the modulation ratio. There are a large number of phase interfaces in the nano-multilayer film, so the toughness of the film layer can be increased, thereby improving the wear resistance of the multilayer film. The aim of improving the wear resistance can be achieved by selecting a proper deposition material or solid lubricating material.
Therefore, there is a need in the art for a high performance high entropy ceramic-based nano-multilayer coating that can improve the wear resistance of tool coatings and methods of making the same.
Disclosure of Invention
The invention aims to solve the problem of large friction and abrasion on the surface of a workpiece in the prior art.
In order to solve the problems, the technical scheme adopted by the invention is to provide the high-performance high-entropy ceramic-based nano multilayer coating and the preparation method thereof.
The invention provides a preparation method of a high-performance high-entropy ceramic-based nano multilayer coating, which comprises the following steps:
step 1, cleaning a substrate: firstly, carrying out ultrasonic cleaning on a polished substrate, and then carrying out ion cleaning;
Step 2, (TiZrTaWVNb) preparation of N/MoS 2 nano multilayer structure coating:
Placing a substrate into a reaction magnetron sputtering instrument and respectively staying on a TiZrTaWVNb high-entropy alloy target material and a MoS 2 target material, obtaining (TiZrTaWVNb) N/MoS 2 nanometer multilayer structure coating through reaction magnetron sputtering deposition, and controlling the thickness of a MoS 2 layer by controlling the stay time on the MoS 2 target material to obtain the high-performance high-entropy ceramic-based nanometer multilayer coating.
Wherein the template layer is (TiZrTaWVNb) N and the modulation layer is MoS 2.
Preferably, in the step 1, the substrate is metal, cemented carbide, ceramic or monocrystalline Si.
Preferably, in the ultrasonic cleaning in the step 1, the ultrasonic cleaning is performed by using 15-30 kHz ultrasonic waves in analytically pure absolute alcohol and acetone for 15min.
Preferably, in the step 1, the ion cleaning is to put the substrate into a vacuum chamber, vacuum the substrate to 4× - 3 Pa, then introduce argon, maintain the vacuum degree at 2-4Pa, bombard the target material with argon ions for 10min.
Preferably, in the step 2, the TiZrTaWVNb high-entropy alloy target is a direct current target, the MoS 2 target is a radio frequency target, and the diameter of the target is 75mm and the thickness of the target is 3mm.
Preferably, in the step 2, the dc sputtering power of the reactive magnetron sputtering apparatus is 180W, and the rf sputtering power is 100W.
Preferably, in the step 2, the residence time of the substrate on the TiZrTaWVNb high-entropy alloy target is 15s, and the residence time of the substrate on the MoS 2 target is 2s, 4s, 6s, 8s or 10s, which is 180r; the distance between the target substrate is 50mm; the total air pressure was in the range of 0.5Pa.
In a second aspect of the invention, a high-performance high-entropy ceramic-based nano multilayer coating prepared by the method is provided, wherein the hardness and the elastic modulus of the coating reach 18.6GPa and 202.6GPa respectively, the friction coefficient is 0.43, and the fracture toughness value reaches 1.561 MPa-m 1/2.
Compared with the prior art, the invention has the following beneficial effects:
According to the high-performance high-entropy ceramic-based nano multilayer coating, when the thickness of a modulation layer MoS 2 is 0.6nm according to a deformation mechanism of the nano coating, the modulation layer and a template layer are grown in a coherent epitaxial mode. In the preparation of the (TiZrTaWVNb) N/MoS 2 nanometer multilayer structure coating, the thickness of the modulation layer MoS 2 is controlled, so that the modulation layer is converted into the same lattice structure as the template layer, and the coating interface forms a coherent epitaxial growth morphology.
In addition, the preparation method of the high-performance high-entropy ceramic-based nano multilayer coating has the advantages of high production efficiency, low energy consumption, lower equipment requirements and the like in the preparation process, and is suitable for large-scale production.
Drawings
FIG. 1 is an XRD pattern of (TiZrTaWVNb) N/MoS 2 nm multilayer films with different MoS 2 layer thicknesses.
FIG. 2 is a cross section of (TiZrTaWVNb) N/MoS 2 nm multilayer films with different MoS 2 layer thicknesses SEM,(a)tMoS2＝0nm;(b)tMoS2＝0.2nm;(c)tMoS2＝0.4nm;(d)tMoS2＝0.6nm;(e)tMoS2＝0.8nm;(f)tMoS2＝1.0nm.
FIG. 3 is a cross-sectional HRTEM image of a (TiZrTaWVNb) N/MoS 2 nm multilayer film with a MoS 2 layer thickness of 0.6nm, (a) a low-power HRTEM image; (b) a medium-magnification HRTEM image; (c) HRTEM images with enlarged area selection in panel b; (d) selected area electron diffraction pattern.
FIG. 4 is the hardness and elastic modulus of (TiZrTaWVNb) N/MoS 2 nm multilayer films with different MoS 2 layer thicknesses.
FIG. 5 is a plot of (TiZrTaWVNb) N/MoS 2 nm multilayer film fracture toughness as a function of modulating layer thickness.
FIG. 6 is the coefficient of friction of (TiZrTaWVNb) N/MoS 2 nm multilayer films with different MoS 2 layer thicknesses.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments accompanied with the accompanying drawings are described in detail as follows:
the preparation, characterization and measurement instrument used in the present invention:
JGP-450 type magnetron sputtering system, shenyang scientific instrument development center Co., ltd
D8 Advance type X-ray diffractometer, bruker, germany
Bruker TI-980 nanoindenter, bruker, germany
Tecnai G2 high resolution transmission electron microscope, FEI Co., U.S.A
Quanta FEG450 type scanning electron microscope, FEI Co., U.S.A
MFT-5000 multifunctional friction and wear testing machine, rtec company
Example 1
The high-performance high-entropy ceramic-based nano multilayer coating and the preparation method thereof are characterized in that a reaction magnetron sputtering instrument is adopted, and TiZrTaWVNb high-entropy alloy targets are subjected to reaction magnetron sputtering deposition on a substrate to form the high-entropy ceramic-based nano multilayer coating; the substrate is monocrystalline Si.
Adopting TiZrTaWVNb high-entropy alloy target material as direct current target, wherein the diameter of the target material is 75mm, and the thickness is 3mm;
Ar gas flow: 25sccm, N 2 air flow rate: 5sccm;
The DC sputtering power is 180W;
the deposition time of the substrate on TiZrTaWVNb high-entropy alloy target is 1h;
the distance between the target substrate and the target substrate is 50mm, and the total air pressure is 0.5Pa.
The hardness of the obtained (TiZrTaWVNb) N coating is 20.6GPa, the elastic modulus is 213.0GPa, the friction coefficient is 0.88, and the fracture toughness is 1.129MPa m 1/2.
Example 2
The high-performance high-entropy ceramic-based nano multilayer coating and the preparation method thereof are characterized in that a reaction magnetron sputtering instrument is adopted, and a TiZrTaWVNb high-entropy alloy target material is a direct current target and a MoS 2 target material is a radio frequency target to perform reaction magnetron sputtering deposition on a substrate; the substrate is monocrystalline Si.
Adopting TiZrTaWVNb high-entropy alloy target as a direct current target and MoS 2 target as a radio frequency target, wherein the diameter of the target is 75mm, and the thickness of the target is 3mm;
Ar gas flow: 25sccm, N 2 air flow rate: 5sccm;
the direct-current sputtering power is 180W, and the radio-frequency sputtering power is 100W;
the residence time of the substrate on the two targets is 15s and 2s respectively, and the deposition circle number is 180r;
the distance between the target substrate and the target substrate is 50mm, and the total air pressure is 0.5Pa.
The hardness of the obtained (TiZrTaWVNb) N/MoS 2 nanometer multilayer structure coating is 16.7GPa, the elastic modulus is 189.0GPa, the friction coefficient is 0.33, and the fracture toughness is 1.227MPa m 1/2.
Example 3
The high-performance high-entropy ceramic-based nano multilayer coating and the preparation method thereof are characterized in that a reaction magnetron sputtering instrument is adopted, and a TiZrTaWVNb high-entropy alloy target material is a direct current target and a MoS 2 target material is a radio frequency target to perform reaction magnetron sputtering deposition on a substrate; the substrate is monocrystalline Si.
Adopting TiZrTaWVNb high-entropy alloy target as a direct current target and MoS 2 target as a radio frequency target, wherein the diameter of the target is 75mm, and the thickness of the target is 3mm;
Ar gas flow: 25sccm, N 2 air flow rate: 5sccm;
the direct-current sputtering power is 180W, and the radio-frequency sputtering power is 100W;
The residence time of the substrate on the two targets is 15s and 4s respectively, and the deposition circle number is 180r;
the distance between the target substrate and the target substrate is 50mm, and the total air pressure is 0.5Pa.
The hardness of the obtained (TiZrTaWVNb) N/MoS 2 nanometer multilayer structure coating is 18.0GPa, the elastic modulus is 196.6GPa, the friction coefficient is 0.36, and the fracture toughness is 1.384MPa m 1/2.
Example 4
The high-performance high-entropy ceramic-based nano multilayer coating and the preparation method thereof are characterized in that a reaction magnetron sputtering instrument is adopted, and a TiZrTaWVNb high-entropy alloy target material is a direct current target and a MoS 2 target material is a radio frequency target to perform reaction magnetron sputtering deposition on a substrate; the substrate is monocrystalline Si.
Adopting TiZrTaWVNb high-entropy alloy target as a direct current target and MoS 2 target as a radio frequency target, wherein the diameter of the target is 75mm, and the thickness of the target is 3mm;
Ar gas flow: 25sccm, N 2 air flow rate: 5sccm;
the direct-current sputtering power is 180W, and the radio-frequency sputtering power is 100W;
The residence time of the substrate on the two targets is 15s and 6s respectively, and the deposition circle number is 180r;
the distance between the target substrate and the target substrate is 50mm, and the total air pressure is 0.5Pa.
The hardness of the obtained (TiZrTaWVNb) N/MoS 2 nanometer multilayer structure coating is 18.6GPa, the elastic modulus is 202.6GPa, the friction coefficient is 0.43, and the fracture toughness is 1.561MPa m 1/2.
Example 5
The high-performance high-entropy ceramic-based nano multilayer coating and the preparation method thereof are characterized in that a reaction magnetron sputtering instrument is adopted, and a TiZrTaWVNb high-entropy alloy target material is a direct current target and a MoS 2 target material is a radio frequency target to perform reaction magnetron sputtering deposition on a substrate; the substrate is monocrystalline Si.
Adopting TiZrTaWVNb high-entropy alloy target as a direct current target and MoS 2 target as a radio frequency target, wherein the diameter of the target is 75mm, and the thickness of the target is 3mm;
Ar gas flow: 25sccm, N 2 air flow rate: 5sccm;
the direct-current sputtering power is 180W, and the radio-frequency sputtering power is 100W;
the residence time of the substrate on the two targets is 15s and 8s respectively, and the deposition circle number is 180r;
the distance between the target substrate and the target substrate is 50mm, and the total air pressure is 0.5Pa.
The hardness of the (TiZrTaWVNb) N/MoS 2 nanometer multilayer structure coating is 16.3GPa, the elastic modulus is 183.0GPa, the friction coefficient is 0.37, and the fracture toughness is 1.437MPa m 1/2.
Example 6
The high-performance high-entropy ceramic-based nano multilayer coating and the preparation method thereof are characterized in that a reaction magnetron sputtering instrument is adopted, and a TiZrTaWVNb high-entropy alloy target material is a direct current target and a MoS 2 target material is a radio frequency target to perform reaction magnetron sputtering deposition on a substrate; the substrate is monocrystalline Si.
Adopting TiZrTaWVNb high-entropy alloy target as a direct current target and MoS 2 target as a radio frequency target, wherein the diameter of the target is 75mm, and the thickness of the target is 3mm;
Ar gas flow: 25sccm, N 2 air flow rate: 5sccm;
the direct-current sputtering power is 180W, and the radio-frequency sputtering power is 100W;
the residence time of the substrate on the two targets is 15s and 10s respectively, and the deposition circle number is 180r;
the distance between the target substrate and the target substrate is 50mm, and the total air pressure is 0.5Pa.
The hardness of the obtained (TiZrTaWVNb) N/MoS 2 nanometer multilayer structure coating is 15.3GPa, the elastic modulus is 181.1GPa, the friction coefficient is 0.37, and the fracture toughness is 1.327MPa m 1/2.
XRD measurements were performed on the N/MoS 2 nano-multilayer films of examples 1-6, respectively, i.e., the MoS 2 intercalating layers having thicknesses of 0nm, 0.2nm, 0.4nm, 0.6nm, 0.8nm, and 1.0nm, respectively, as shown in FIG. 1. It can be seen that as MoS 2 increases in thickness, (TiZrTaWVNb) N/MoS 2, both (111) and (220) show a tendency to increase and decrease before one another, with the crystallinity reaching a maximum when MoS 2 is 0.6nm thick.
SEM observations were made of cross-sections of N/MoS 2 nm multilayer films of examples 1-6, respectively, during magnetron sputtering, i.e., moS 2 intercalating layers having thicknesses of 0nm, 0.2nm, 0.4nm, 0.6nm, 0.8nm, 1.0nm, respectively, as shown in FIG. 2. As can be seen from the figure, the film is tightly combined with the substrate, the interface is clear, the cross-sectional shape is smooth, and cracks and other internal defects are not generated. In fig. 2 (a), no distinct columnar crystal structure was observed when MoS 2 was 0nm thick, and in fig. 2 (b) and (c), the (TiZrTaWVNb) N/MoS 2 nm multilayer film showed similar columnar growth structures when MoS 2 was 0.2nm and 0.4nm thick. As the thickness of MoS 2 increases, moS 2 gradually changes from a hexagonal structure to an FCC structure under the template of (TiZrTaWVNb) N. Thus, crystallinity is improved. When the thickness of the MoS 2 layer of the nano-multilayer film in fig. 2 (d) is 0.6nm, the nano-multilayer film columnar crystal growth is completed. However, when the thickness of MoS 2 is greater than 0.6nm, the metastable MoS 2 layer cannot continue to maintain the cubic structure and is converted into its own hexagonal structure, resulting in the destruction of the coherent epitaxial growth structure of the nano-multilayer film, the decrease of the crystallinity of the thin film, and the deterioration of the compactness.
HRTEM observations were performed on cross-sections of the multilayer film of example 4, i.e. MoS 2 insert layer thickness 0.6nm (TiZrTaWVNb) N/MoS 2 nm, and the results are shown in fig. 3. As can be seen from the low magnification image of fig. 3 (a), the nano-multilayer film has a definite layer structure, and the interface is smooth and clear. According to comparison, dark and light stripes in fig. 3 (b) correspond to (TiZrTaWVNb) N and MoS 2 layers, respectively. (111) Diffraction rings of the FCC structures (200), (220) appear in the inserted Selected Area Electron Diffraction (SAED) patterns, consistent with the results in the XRD patterns.
Hardness and elastic modulus were measured on sections of the (TiZrTaWVNb) N/MoS 2 nm multilayer films of examples 1-6, respectively, during magnetron sputtering, i.e., moS 2 insert layers having thicknesses of 0nm, 0.2nm, 0.4nm, 0.6nm, 0.8nm, and 1.0nm, respectively, as shown in FIG. 4. From the graph, the variation of the hardness and the elastic modulus with increasing layer thickness of the MoS 2 can be divided into three phases. The first stage is a stage from no insertion of MoS 2 to insertion of MoS 2 with an insertion layer thickness of 0.2nm, and the hardness and elastic modulus of the (TiZrTaWVNb) N monolayer film are 20.6GPa and 213.0GPa, respectively; after insertion of the 0.2nm thick MoS 2, the hardness and elastic modulus of the film decreased to 16.7GPa and 189.0GPa; the second stage is that the hardness and the elastic modulus of the film rise along with the gradual increase of the thickness of the MoS 2 layer, and the hardness and the elastic modulus respectively reach higher values of 18.6GPa and 202.6GPa when the thickness of the MoS 2 insert layer is 0.6 nm; the third stage is that the hardness and elastic modulus decrease rapidly again to 15.3GPa and 181.1GPa as the MoS 2 layer thickness increases further.
Fracture toughness was measured on sections of the (TiZrTaWVNb) N/MoS 2 nm multilayer films of examples 1-6, respectively, during magnetron sputtering, i.e., moS 2 insert layers having thicknesses of 0nm, 0.2nm, 0.4nm, 0.6nm, 0.8nm, and 1.0nm, respectively, as shown in FIG. 5. The fracture toughness value of the nano multi-layer film is increased with the thickness MoS 2 of the modulation layer and is displayed as being increased and then decreased. The nano multilayer film has the optimal toughness at the thickness of MoS 2 of 0.6nm, and the value of the nano multilayer film is 1.561MPa m 1/2.
The results of the frictional wear measurements of the (TiZrTaWVNb) N/MoS 2 nano-multilayer films of examples 1-6, respectively, during magnetron sputtering, i.e., moS 2 insert layers having thicknesses of 0nm, 0.2nm, 0.4nm, 0.6nm, 0.8nm, 1.0nm, respectively, are shown in FIG. 6. As can be seen from this figure, the coefficient of friction of (TiZrTaWVNb) N is 0.88. The coefficient of friction after insertion of the lubricating layer is reduced by between 0.32 and 0.43 compared to that without insertion of the lubricating layer. As the thickness of the MoS 2 layer increases, the friction coefficient of the nano-multilayer film generally tends to increase and then decrease.
While the invention has been described with respect to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. Equivalent embodiments of the present invention will be apparent to those skilled in the art having the benefit of the teachings disclosed herein, when considered in the light of the foregoing disclosure, and without departing from the spirit and scope of the invention; meanwhile, any equivalent changes, modifications and evolution of the above embodiments according to the essential technology of the present invention still fall within the scope of the technical solution of the present invention.
Claims (8)
1. The preparation method of the high-performance high-entropy ceramic-based nano multilayer coating is characterized by comprising the following steps of:
step 1, cleaning a substrate: firstly, carrying out ultrasonic cleaning on a polished substrate, and then carrying out ion cleaning;
Step 2, (TiZrTaWVNb) preparation of N/MoS 2 nano multilayer structure coating: placing a substrate into a reaction magnetron sputtering instrument and respectively staying on a TiZrTaWVNb high-entropy alloy target material and a MoS 2 target material, obtaining (TiZrTaWVNb) N/MoS 2 nanometer multilayer structure coating through reaction magnetron sputtering deposition, and controlling the thickness of a MoS 2 layer by controlling the stay time on the MoS 2 target material to obtain the high-performance high-entropy ceramic-based nanometer multilayer coating.
2. The method for preparing a high-performance high-entropy ceramic-based nano multi-layer coating according to claim 1, wherein in the step 1, the substrate is metal, cemented carbide, ceramic or monocrystalline Si.
3. The method for preparing a high-performance high-entropy ceramic-based nano multilayer coating according to claim 1, wherein in the step 1, ultrasonic cleaning is performed by using analytically pure absolute alcohol and acetone and using 15-30 kHz ultrasonic waves for 15min.
4. The method for preparing the high-performance high-entropy ceramic-based nano multilayer coating according to claim 1, wherein in the step 1, the substrate is put into a vacuum chamber, the vacuum is pumped to 4 x 10 -3 Pa, argon is introduced, the vacuum degree is maintained at 2-4Pa, and the target is bombarded by argon ions for 10min.
5. The method for preparing the high-performance high-entropy ceramic-based nano multilayer coating according to claim 1, wherein in the step 2, tiZrTaWVNb high-entropy alloy target is a direct current target, moS 2 target is a radio frequency target, and the diameter of the target is 75mm and the thickness of the target is 3mm.
6. The method for preparing a high-performance high-entropy ceramic-based nano multilayer coating according to claim 1, wherein in the step 2, the direct-current sputtering power of the reaction magnetron sputtering instrument is 180W, and the radio-frequency sputtering power is 100W.
7. The method for preparing the high-performance high-entropy ceramic-based nano multilayer coating according to claim 1, wherein in the step 2, the residence time of the substrate on the TiZrTaWVNb high-entropy alloy target is 15s, and the residence time on the MoS 2 target is 2s, 4s, 6s, 8s or 10s, which is 180r in total; the distance between the target substrate is 50mm; the total air pressure was in the range of 0.5Pa.
8. A high performance high entropy ceramic matrix nano multilayer coating obtained by the preparation method of any one of claims 1 to 7, characterized in that its hardness and elastic modulus reach at most 18.6GPa and 202.6GPa, respectively, friction coefficient 0.43, fracture toughness value 1.561mpa·m 1/2.
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