CN117187766A - High-temperature oxidation-resistant high-entropy nitride film and preparation and application thereof - Google Patents
High-temperature oxidation-resistant high-entropy nitride film and preparation and application thereof Download PDFInfo
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- CN117187766A CN117187766A CN202311221943.2A CN202311221943A CN117187766A CN 117187766 A CN117187766 A CN 117187766A CN 202311221943 A CN202311221943 A CN 202311221943A CN 117187766 A CN117187766 A CN 117187766A
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- 150000004767 nitrides Chemical class 0.000 title claims abstract description 50
- 230000003647 oxidation Effects 0.000 title claims abstract description 35
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000758 substrate Substances 0.000 claims abstract description 36
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 22
- 238000004544 sputter deposition Methods 0.000 claims abstract description 14
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 6
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims description 26
- 239000011248 coating agent Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 11
- 238000000151 deposition Methods 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000007769 metal material Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- VTPDTRDBFKXCRO-UHFFFAOYSA-N B([O-])([O-])[O-].B(O)(O)O.B(O)(O)O.B([O-])([O-])O.[Ta+5] Chemical compound B([O-])([O-])[O-].B(O)(O)O.B(O)(O)O.B([O-])([O-])O.[Ta+5] VTPDTRDBFKXCRO-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 2
- 239000011241 protective layer Substances 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 2
- 239000013077 target material Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 description 33
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 238000000137 annealing Methods 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 9
- UPMLURQYCFPZHO-UHFFFAOYSA-N molybdenum niobium tantalum tungsten Chemical compound [Nb][Mo][Ta][W] UPMLURQYCFPZHO-UHFFFAOYSA-N 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- -1 Transition Metal Nitride Chemical class 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 238000005280 amorphization Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000003678 scratch resistant effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
The invention discloses a high-temperature oxidation-resistant high-entropy nitride film and preparation and application thereof, wherein the high-entropy nitride film comprises Nb, mo, ta, W, al, N, and the atomic percentage of Nb, mo, ta, W elements is 2:2:1:1, the doping amount of Al element is 0-30% of the total number of atoms of the high-entropy nitride film, the content of nitrogen element is 40-45% of the total number of atoms of the high-entropy nitride film, and high-entropy nitride films with different Al contents are deposited on a substrate by a magnetron co-sputtering method. The high-temperature oxidation-resistant high-entropy nitride film and the preparation and application thereof are adopted, and the addition of a proper amount of Al not only keeps the intrinsic hardness of the film, but also improves the high-temperature oxidation resistance of the film.
Description
Technical Field
The invention relates to the technical field of alloy films, in particular to a high-temperature oxidation-resistant high-entropy nitride film and preparation and application thereof.
Background
As technology continues to develop, there is a growing demand for protective properties of materials from which cutting tools, turbine blades, reactor walls, etc. are made. The increased hardness and oxidation resistance at high temperatures are one of the most basic properties that such materials must possess. Transition Metal Nitride (TMN) coatings are widely used for cutting protective coatings, scratch resistant devices, hard parts of metal matrix composites and corrosion resistant coatings due to their superior properties including high melting point, high hardness, high chemical and thermal stability, excellent wear resistance and electrical conductivity. However, the TMN material is subject to the problems of hardness reduction and oxidation failure when in service under a high-temperature environment, so that the design of TMN with enhanced performance is important.
Much research is currently focused on further improving the mechanical and oxidation resistance properties of TMN coatings by tailoring the microstructure of the TMN coating. The most common of these methods is two main ones, one of which is the formation of nanocomposite structures by doping, also known as nanoscale alloying, the alloying of Al to transition metal nitrides (MeN) being considered as a popular strategy to increase the hardness (H) and oxidation resistance widely required by the modern industry. Another way is to obtain a high entropy material by multi-component solid solution.
In recent years, high-entropy nitride has been published about 70 times since 2004 as a high-entropy ceramic that has been studied more widely. Among them, the high entropy nitrides based on early transition group metals, which have been reported, are generally solid solutions having FCC structures, and have exhibited many excellent properties such as high hardness, good corrosion resistance and thermal stability. Meanwhile, compared with the traditional TMN, the mechanical, friction and corrosion performances of HEN are improved to a certain extent. However, as the number of components increases, the difficulty of successful preparation of materials increases, and in particular, how the structure evolves due to the addition of elements which are difficult to dissolve, such as Al, is not clear.
Disclosure of Invention
The invention aims to provide a high-temperature oxidation-resistant high-entropy nitride film and preparation and application thereof, so as to solve the problems that the high-entropy nitride film is subjected to hardness reduction and oxidation failure in service in a high-temperature environment.
To achieve the above object, the first aspect of the present invention provides a high-temperature oxidation-resistant high-entropy nitride film, which comprises Nb, mo, ta, W, al, N, wherein the atomic percentage of Nb, mo, ta, W elements is 2:2:1: the doping amount of the Al element is 0-30% of the total number of atoms of the high-entropy nitride film, and the nitrogen element content is 40-45% of the total number of atoms of the high-entropy nitride film.
Preferably, the nitrogen element content is 43-45% of the total number of atoms of the high-entropy nitride film.
Preferably, the thickness of the high-entropy nitride film is 1-1.2 μm.
The second aspect of the invention provides a method for preparing a high-temperature oxidation-resistant high-entropy nitride film, which is to deposit high-entropy nitride films with different Al contents on a substrate by a magnetron co-sputtering method.
Preferably, the method comprises the following steps:
(1) Preparation work
The substrate is single-sided polished monocrystalline silicon, the crystal face orientation of the polished surface is (100), and the target materials are an Al target and an NbMoTaW target;
(2) Coating operation
High-purity Ar gas is introduced into the cavity to perform pre-sputtering, then a direct current power supply for connecting a tantalum target and a tantalum tetraborate target is started, and Ar/N is carried out 2 And carrying out a deposition reaction in the gas mixture to obtain the high-entropy nitride film.
Preferably, the volume ratio of nitrogen to argon in the gas mixture is 8:80.
Preferably, the preparation in the step (1) comprises mounting an Al target and an NbMoTaW target on a horizontal target position, both targets being connected to a dc power supply; cutting a substrate into a proper size, sequentially ultrasonically cleaning the substrate with absolute ethyl alcohol and acetone for 15min, drying the substrate with nitrogen, and mounting the substrate on a sample stage; the cleaning of the coating chamber is ensured before deposition, and all sealing parts are wiped clean by alcohol dust-free cloth to ensure the sealing performance of the coating chamber.
Preferably, the Al target and NbMoTaW target in step (1) have a diameter of 60mm, a thickness of 3mm and a purity of 99.999%.
Preferably, the sum of the power of the Al target and the power of the NbMoTaW target in step (2) is 80W.
Preferably, the power of the Al target in step (2) is 20W, 30W and 40W.
Preferably, the deposition pressure in step (2) is lower than 4X 10 -4 Pa, the distance between the target and the substrate is 6.5cm, the bias voltage of the substrate is-80V, and the rotating speed is 10r/min.
The third aspect of the invention provides an application of the high-temperature oxidation-resistant high-entropy nitride film, wherein the high-entropy nitride film is applied to a protective layer on the surface of a metal material.
Therefore, the high-temperature oxidation-resistant high-entropy nitride film adopting the structure and the preparation and application thereof have the following beneficial effects:
(1) The parameters of the magnetron sputtering process are regulated so that Al element can be dissolved in the high-entropy nitride film and different structures can be induced to appear.
(2) The advantages of the Al element and the high-entropy structure under the high-temperature condition can be simultaneously exerted, so that the film has better high-temperature performance.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is XRD patterns of examples and comparative examples;
FIG. 2 is a cross-sectional SEM image of a comparative example;
FIG. 3 is a cross-sectional SEM image of examples 1-3;
FIG. 4 is XRD patterns of examples and comparative examples after annealing;
FIG. 5 is a cross-sectional SEM image of a comparative example after annealing in air;
FIG. 6 is a cross-sectional SEM image of examples 1-3 after annealing in air;
FIG. 7 is a comparison of hardness of examples and comparative examples before and after annealing in air.
Detailed Description
The present invention will be further described below, and it should be noted that the present embodiment provides a detailed implementation manner and a specific operation procedure on the premise of the present technical solution, but the present invention is not limited to the present embodiment.
Example 1
The preparation method of the high-temperature oxidation-resistant high-entropy nitride film comprises the following steps:
(1) Preparation:
the aluminum target and the niobium molybdenum tantalum tungsten target are arranged on the target position in the horizontal direction, the two targets are connected with a direct current power supply, the substrate is cut into a proper size, and then the substrate is ultrasonically cleaned for 15min by using absolute ethyl alcohol and acetone in sequence, and then the substrate is dried by nitrogen and arranged on a sample table.
Ensuring the cleaning of the coating chamber before deposition, wiping all sealing parts with alcohol dust-free cloth to ensure the tightness of the coating chamber, and vacuumizing the coating chamber by a vacuum system consisting of a mechanical pump and a molecular pump to ensure that the vacuum degree is 4 multiplied by 10 -4 Pa or below.
(2) Coating operation:
and (3) introducing high-purity argon and nitrogen into the cavity, wherein the volume ratio of the nitrogen to the argon is 8:80, controlling the total pressure to be 0.8Pa by using a regulating valve, and applying negative bias of-80V to the substrate.
And switching on a direct current power supply for connecting the two targets, setting the power of the niobium-molybdenum-tantalum-tungsten target to be 60W, setting the power of the aluminum target to be 20W, and performing pre-sputtering.
After 5min, sputtering was started for 2 hours to control the film thickness to 1.2 μm or less, thereby obtaining a high-entropy nitride thin film.
Example 2
The preparation method of the high-temperature oxidation-resistant high-entropy nitride film comprises the following steps:
(1) Preparation:
the aluminum target and the niobium molybdenum tantalum tungsten target are arranged on the target position in the horizontal direction, and both targets are connected with a direct current power supply; cutting the substrate into proper size, ultrasonically cleaning the substrate for 15min by using absolute ethyl alcohol and acetone in sequence, drying the substrate by using nitrogen, and mounting the substrate on a sample stage.
Ensuring the cleaning of the coating chamber before deposition, wiping all sealing parts with alcohol dust-free cloth to ensure the tightness of the coating chamber, and vacuumizing the coating chamber by a vacuum system consisting of a mechanical pump and a molecular pump to ensure that the vacuum degree is 4 multiplied by 10 -4 Pa or below.
(2) Coating operation:
and (3) introducing high-purity argon and nitrogen into the cavity, wherein the volume ratio of the nitrogen to the argon is 8:80, and controlling the total pressure to be 0.8Pa by using a regulating valve. And applies a negative bias of-80V to the substrate.
And switching on a direct current power supply for connecting the two targets, setting the power of the niobium-molybdenum-tantalum-tungsten target to be 50W, setting the power of the aluminum target to be 30W, and performing pre-sputtering.
After 5min, sputtering was started for 2 hours to control the film thickness to 1.2 μm or less, thereby obtaining a high-entropy nitride thin film.
Example 3
The preparation method of the high-temperature oxidation-resistant high-entropy nitride film comprises the following steps:
(1) Preparation:
the aluminum target and the niobium molybdenum tantalum tungsten target are arranged on the target position in the horizontal direction, and both targets are connected with a direct current power supply; cutting the substrate into proper size, ultrasonically cleaning the substrate for 15min by using absolute ethyl alcohol and acetone in sequence, drying the substrate by using nitrogen, and mounting the substrate on a sample stage.
Ensuring the cleaning of the coating chamber before deposition, wiping all sealing parts with alcohol dust-free cloth to ensure the tightness of the coating chamber, and vacuumizing the coating chamber by a vacuum system consisting of a mechanical pump and a molecular pump to ensure that the vacuum degree is 4 multiplied by 10 -4 Pa or below.
(2) Coating operation:
and (3) introducing high-purity argon and nitrogen into the cavity, wherein the volume ratio of the nitrogen to the argon is 8:80, and controlling the total pressure to be 0.8Pa by using a regulating valve. And applies a negative bias of-80V to the substrate.
And switching on a direct current power supply for connecting the two targets, setting the power of the niobium-molybdenum-tantalum-tungsten target to be 40W, setting the power of the aluminum target to be 40W, and performing pre-sputtering.
After 5min, sputtering was started for 2 hours to control the film thickness to 1.2 μm or less, thereby obtaining a high-entropy nitride thin film.
Comparative example
The preparation method of the niobium-molybdenum-tantalum-tungsten-nitrogen film comprises the following steps:
(1) Preparation:
the niobium-molybdenum-tantalum-tungsten target is arranged on a target position in the horizontal direction and is connected with a direct current power supply; cutting the substrate into proper size, ultrasonically cleaning the substrate for 15min by using absolute ethyl alcohol and acetone in sequence, drying the substrate by using nitrogen, and mounting the substrate on a sample stage.
Ensuring the cleaning of the coating chamber before deposition, wiping all sealing parts with alcohol dust-free cloth to ensure the tightness of the coating chamber, and vacuumizing the coating chamber by a vacuum system consisting of a mechanical pump and a molecular pump to ensure that the vacuum degree is 4 multiplied by 10 -4 Pa or below.
(2) Coating operation:
and (3) introducing a high-purity mixed gas of argon and nitrogen into the cavity, wherein the volume ratio of the nitrogen to the argon is 8:80, controlling the total pressure to be 0.8Pa by using a regulating valve, and applying negative bias of-80V to the substrate.
And (3) starting a direct current power supply connected with the niobium-molybdenum-tantalum-tungsten target, setting the power to be 80W, and performing pre-sputtering.
And after 5min, formally sputtering, and controlling the sputtering time to be 2h to obtain the niobium-molybdenum-tantalum-tungsten-nitrogen film with the film thickness of about 1.2 um.
Test examples
Examples 1-3 and comparative examples were characterized and tested for hardness properties as follows.
The comparative examples are pure NbMoTaWN films without aluminum element, the aluminum target power of each example is different resulting in different film composition and structure, it can be seen from the XRD pattern of fig. 1 that the comparative examples have very strong face-centered cubic structure, examples 1 and 2 also retain better face-centered cubic structure, and example 3 shows significant amorphization. It can also be seen from the sectional SEM images of fig. 2 and 3 that comparative examples and examples 1 and 2 have a columnar crystalline structure, while example 3 exhibits a dense amorphous structure.
Fig. 4 shows XRD patterns of examples and comparative examples after annealing in air at 600 ℃ for half an hour, and it can be found that the comparative examples have been completely amorphized after the high temperature annealing for half an hour, that example 1 has a serious drop in crystallinity although the crystalline structure is still maintained, whereas example 2 has an excellent crystallinity, and that example 3 does not show a significant change due to the amorphous structure. The oxidation degree was also seen from the comparative examples and example cross-sectional SEM in fig. 5 and 6, and example 2 was found to have the best oxidation resistance.
Fig. 7 shows the hardness results obtained by nanoindentation test before and after annealing of the examples and comparative examples, and it was found that the hardness of example 2 was not greatly reduced by the addition of aluminum element, and the hardness after annealing in air was well maintained. Specifically, the initial hardness of example 2 is 22.2 GPa, the hardness after 600 ℃ air annealing is 21.9 GPa, the difference between the two is 0.3 GPa, the hardness is almost unchanged, which shows that the alloy has both oxidation resistance and higher hardness.
As can be seen from fig. 4 and 7, the nitride film prepared by the present invention has both good oxidation resistance and high hardness, which makes it possible to provide the surface of a metal material with a coating layer for protecting the metal material.
Therefore, the high-temperature oxidation-resistant high-entropy nitride film adopting the structure and the preparation and application thereof, and the addition of a proper amount of Al not only maintains the intrinsic hardness of the film, but also improves the high-temperature oxidation resistance of the film.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (10)
1. A high temperature oxidation resistant high entropy nitride film, characterized by: the high entropy nitride film comprises Nb, mo, ta, W, al, N, wherein the atomic percent of Nb, mo, ta, W elements is 2:2:1: the doping amount of the Al element is 0-30% of the total number of atoms of the high-entropy nitride film, and the nitrogen element content is 40-45% of the total number of atoms of the high-entropy nitride film.
2. The high-temperature oxidation-resistant high-entropy nitride film according to claim 1, wherein: the thickness of the high-entropy nitride film is 1-1.2 mu m.
3. The method for preparing a high-temperature oxidation-resistant high-entropy nitride film according to any one of claims 1 to 2, wherein: high entropy nitride films with different Al contents are deposited on a substrate by a magnetron co-sputtering method.
4. A method for preparing a high-temperature oxidation-resistant high-entropy nitride film according to claim 3, wherein: the method comprises the following steps:
(1) Preparation work
The substrate is single-sided polished monocrystalline silicon, the crystal face orientation of the polished surface is (100), and the target materials are an Al target and an NbMoTaW target;
(2) Coating operation
High-purity Ar gas is introduced into the cavity to perform pre-sputtering, then a direct current power supply for connecting a tantalum target and a tantalum tetraborate target is started, and Ar/N is carried out 2 And carrying out a deposition reaction in the gas mixture to obtain the high-entropy nitride film.
5. The method for preparing a high-temperature oxidation-resistant high-entropy nitride film according to claim 4, wherein the method comprises the following steps: the preparation work in the step (1) comprises the steps of installing an Al target and an NbMoTaW target on a target position in the horizontal direction, wherein the two targets are connected with a direct current power supply; cutting a substrate into a proper size, sequentially ultrasonically cleaning the substrate with absolute ethyl alcohol and acetone for 15min, drying the substrate with nitrogen, and mounting the substrate on a sample stage; the cleaning of the coating chamber is ensured before deposition, and all sealing parts are wiped clean by alcohol dust-free cloth to ensure the sealing performance of the coating chamber.
6. The method for preparing a high-temperature oxidation-resistant high-entropy nitride film according to claim 5, wherein the method comprises the following steps: the diameter of the Al target and the NbMoTaW target in the step (1) is 60mm, the thickness is 3mm, and the purity is 99.999%.
7. The method for preparing a high-temperature oxidation-resistant high-entropy nitride film according to claim 6, wherein the method comprises the following steps: the sum of the power of the Al target and the power of the NbMoTaW target in the step (2) is 80W.
8. The method for preparing a high-temperature oxidation-resistant high-entropy nitride film according to claim 7, wherein the method comprises the following steps: the power of the Al target in step (2) was 20W, 30W and 40W.
9. The method for preparing the high-temperature oxidation-resistant high-entropy nitride film according to claim 8, which is characterized in that: step (2) deposition pressure is lower than 4×10 -4 Pa, the distance between the target and the substrate is 6.5cm, the bias voltage of the substrate is-80V, and the rotating speed is 10r/min.
10. Use of a high temperature oxidation resistant high entropy nitride film according to any of claims 1-2, characterized in that: the high-entropy nitride film is applied to a protective layer on the surface of a metal material.
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