CN115074684A - Silver-containing high-entropy alloy wide-temperature-range lubricating film material and preparation method thereof - Google Patents
Silver-containing high-entropy alloy wide-temperature-range lubricating film material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a wide-temperature-range lubricating film material of a silver-containing high-entropy alloy and a preparation method thereof, and relates to the technical field of lubricating materials. The wide-temperature-range lubricating film material of the silver-containing high-entropy alloy comprises a chromium transition layer and a CrNiMoNbAg high-entropy alloy layer which are sequentially arranged on the surface of a substrate. The invention adopts chromium as the transition layer, solves the problems that the silver-containing film is difficult to combine with the substrate in the deposition process and the film is peeled off under the high-temperature condition; the CrNiMoNbAg high-entropy alloy layer is used as the lubricating layer, so that the advantages of good lubricating property of silver, excellent mechanical property and high-temperature stability of the high-entropy alloy and inhibition of silver diffusion at high temperature are exerted, the friction coefficient of the film material is reduced, and the service life of the film material is prolonged.
Description
Technical Field
The invention relates to the technical field of lubricating materials, in particular to a wide-temperature-range lubricating film material containing silver high-entropy alloy and a preparation method thereof.
Background
In the industrial and aerospace fields, material, workpiece failure and equipment failure often occur due to frictional wear, thereby causing huge economic loss. Therefore, the development of a lubricant having excellent properties is one of the research hotspots in the fields of materials science and tribology. As a classical solid lubricant, the soft metal film shows better lubricating performance in high-low temperature and vacuum environments, and is widely applied to lubricating materials of moving parts such as gears, bearings and the like. In order to improve the bearing capacity of the silver film and the bonding force between the silver film and the substrate, a method of forming a silver-containing multi-element composite film by compounding and doping silver and other metals is often adopted. However, the existing composite film is easy to peel off under the high-temperature condition and has short service life.
Disclosure of Invention
The invention aims to provide a silver-containing high-entropy alloy wide-temperature-range lubricating film material and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a wide-temperature-range lubricating film material of a silver-containing high-entropy alloy, which comprises a chromium transition layer and a CrNiMoNbAg high-entropy alloy layer which are sequentially arranged on the surface of a substrate.
Preferably, the thickness of the chromium transition layer is 0.2-0.3 μm; the thickness of the CrNiMoNbAg high-entropy alloy layer is 0.8-1.2 mu m.
Preferably, the crnimotnbag high-entropy alloy layer contains the following elements by atomic percentage: 20-30% of chromium, 20-30% of nickel, 10-20% of molybdenum, 5-15% of niobium and 20-25% of silver.
The invention provides a preparation method of a wide-temperature-range lubricating film material containing silver high-entropy alloy, which comprises the following steps:
preparing a chromium transition layer on the surface of a base material by using a chromium target as a magnetron sputtering target and adopting a magnetron sputtering technology;
and (3) taking the chromium-nickel-molybdenum-niobium target and the silver target as magnetron sputtering targets, and preparing a CrNiMoNbAg high-entropy alloy layer on the surface of the chromium transition layer by adopting a magnetron sputtering technology to obtain the silver-containing high-entropy alloy wide-temperature-range lubricating film material.
Preferably, when the chromium transition layer is prepared, a direct-current power supply is adopted to sputter a chromium target, and the power of the direct-current power supply is 100-300W; the sputtering time is 10-15 min.
Preferably, the chromium transition layer is prepared by applying a bias of-50 to-150V to the substrate.
Preferably, when the CrNiMoNbAg high-entropy alloy layer is prepared, a direct-current power supply is adopted to sputter a chromium-nickel-molybdenum-niobium target and a silver target at the same time, and the power of the direct-current power supply of the chromium-nickel-molybdenum-niobium target is 100-300W; the direct current power supply power of the silver target is 13-40W; the sputtering time of the chromium-nickel-molybdenum-niobium target and the silver target is 40-60 min.
Preferably, when the CrNiMoNbAg high-entropy alloy layer is prepared, a bias voltage of-50V to-100V is applied to the substrate.
Preferably, the chromium-nickel-molybdenum-niobium target is formed by splicing pure metal targets of chromium, nickel, molybdenum and niobium; the area ratio of pure metals of chromium, nickel, molybdenum and niobium in the chromium-nickel-molybdenum-niobium target is 1-2: 1: 1.
Preferably, in the process of preparing the silver-containing high-entropy alloy wide-temperature-range lubricating film material, the substrate keeps rotating at the speed of 2.5-10 r/min.
The invention provides a wide-temperature-range lubricating film material of a silver-containing high-entropy alloy, which comprises a chromium transition layer and a CrNiMoNbAg high-entropy alloy layer which are sequentially arranged on the surface of a substrate. According to the invention, chromium which has excellent compatibility and binding force with high-temperature resistant base materials such as W18Cr4V steel, Inconel series high-temperature alloy and the like and chromium which has excellent compatibility and binding force with chromium-nickel-molybdenum-niobium-silver high-entropy alloy is used as a transition layer, so that the problems that the silver-containing film is difficult to bind with the base materials in the deposition process and the film is peeled off under a high-temperature condition are solved; the CrNiMoNbAg high-entropy alloy layer is used as the lubricating layer, so that the advantages of good lubricating property of silver, excellent mechanical property and high-temperature stability of the high-entropy alloy and inhibition of silver diffusion at high temperature are exerted, the friction coefficient of the film material is reduced, and the service life of the film material is prolonged. In addition, the silver-containing high-entropy alloy wide-temperature-range lubricating film material provided by the invention has excellent conductivity, and can provide a lubricating scheme for the field of electric contact materials.
The invention also provides a preparation method of the silver-containing high-entropy alloy wide-temperature-range lubricating film material in the technical scheme, and the preparation method is simple in preparation process, easy in obtaining of target materials, accurate and controllable in film thickness and element content, low in production cost and capable of realizing batch production.
Drawings
FIG. 1 is a schematic structural diagram of a wide temperature range lubricating film material of a silver-containing high-entropy alloy prepared by the invention;
FIG. 2 is a friction coefficient curve of the wide temperature range lubricating film material containing the silver high-entropy alloy prepared in example 1 of the present invention at 25 ℃ -600 ℃;
FIG. 3 is a wear rate result graph of the wide temperature range lubricating film material of the silver-containing high-entropy alloy prepared in example 1 of the present invention at 25 ℃ -600 ℃;
FIG. 4 is a friction coefficient curve of the wide temperature range lubricating film material containing the silver high-entropy alloy prepared in example 2 of the present invention at 25 ℃ -600 ℃;
FIG. 5 is a wear rate result graph of the wide temperature range lubricating film material of the silver-containing high-entropy alloy prepared in example 2 of the present invention at 25 ℃ -600 ℃.
Detailed Description
The invention provides a wide-temperature-range lubricating film material of a silver-containing high-entropy alloy, which comprises a chromium transition layer and a CrNiMoNbAg high-entropy alloy layer which are sequentially arranged on the surface of a substrate.
The wide-temperature-range lubricating film material containing the silver high-entropy alloy comprises a chromium transition layer arranged on the surface of a base material. In the invention, the thickness of the chromium transition layer is preferably 0.2-0.3 μm.
The wide-temperature-range lubricating film material of the silver-containing high-entropy alloy comprises a CrNiMoNbAg high-entropy alloy layer arranged on the surface of the chromium transition layer. In the invention, the thickness of the CrNiMoNbAg high-entropy alloy layer is preferably 0.8-1.2 μm, and more preferably 1.0 μm. In the invention, the content of each element in the CrNiMoNbAg high-entropy alloy layer is preferably as follows by atomic percentage: 20-30% of chromium, 20-30% of nickel, 10-20% of molybdenum, 5-15% of niobium and 20-25% of silver. In a specific embodiment of the present invention, the crnimotnbag high-entropy alloy layer contains the following elements by atomic percentage: 24-29% of chromium, 24-29% of nickel, 11-16% of molybdenum, 8-12% of niobium and 23-24% of silver.
In the invention, the silver-containing high-entropy alloy wide-temperature-range lubricating film material is at room temperature up toThe friction coefficient under the atmospheric environment at the temperature of 600 ℃ is preferably 0.2-0.45; the wear rate is preferably (9-25) x 10 -5 mm 3 N -1 m -1 . In the invention, the film-base bonding force between the silver-containing high-entropy alloy wide-temperature-range lubricating film material and the base material is preferably greater than 30N, and more preferably 35-36N.
The invention also provides a preparation method of the silver-containing high-entropy alloy wide-temperature-range lubricating film material, which comprises the following steps:
preparing a chromium transition layer on the surface of a base material by using a chromium target as a magnetron sputtering target and adopting a magnetron sputtering technology;
and (3) taking the chromium-nickel-molybdenum-niobium target and the silver target as magnetron sputtering targets, and preparing a CrNiMoNbAg high-entropy alloy layer on the surface of the chromium transition layer by adopting a magnetron sputtering technology to obtain the silver-containing high-entropy alloy wide-temperature-range lubricating film material.
The invention takes a chromium target as a magnetron sputtering target and adopts magnetron sputtering technology to prepare a chromium transition layer on the surface of a substrate. In the present invention, the base material is preferably a high-temperature resistant material, more preferably a high-temperature alloy, and particularly preferably W18Cr4V steel or an Inconel-series high-temperature alloy. In the present invention, the purity of the chromium target is preferably > 99.99%.
Before preparing the chromium transition layer, the invention preferably further comprises: the substrate is preheated and surface cleaned in sequence. In the invention, the preheating temperature is preferably 100-200 ℃, and more preferably 200 ℃. In the present invention, the preheating is preferably performed in a magnetron sputtering chamber; the preheating is preferably carried out under vacuum conditions; the pressure of the magnetron sputtering chamber during preheating is preferably lower than 1.5X 10 -3 Pa. In the present invention, the surface cleaning preferably comprises: introducing 40sccm argon gas, adjusting the pressure of the cavity to 3-5 Pa, and exciting argon plasma by using a bias voltage of-400 to-500V to etch the surface of the substrate. In the present invention, the time for the surface cleaning is preferably 10 min. The invention removes the oxide layer and the pollutants on the surface of the substrate by surface cleaning.
In the process of preparing the silver-containing high-entropy alloy wide-temperature-range lubricating film material, the substrate keeps rotating, and the rotating speed is preferably 2.5-10 r/min, and more preferably 2.5 r/min.
In the invention, when the chromium transition layer is prepared, a direct current power supply is preferably adopted to sputter a chromium target, and the power of the direct current power supply is preferably 100-300W, and more preferably 200W; the sputtering time is preferably 10-15 min.
In the present invention, it is preferable to apply a bias of-50 to-150V to the substrate when preparing the chromium transition layer. In the present invention, the chromium transition layer is preferably prepared in an argon atmosphere; the flow rate of argon gas is preferably 40 sccm. When the chromium transition layer is prepared, the air pressure of the magnetron sputtering chamber is preferably 0.6-0.8 Pa, and more preferably 0.65-0.7 Pa.
After the chromium transition layer is obtained, the invention takes a chromium-nickel-molybdenum-niobium target and a silver target as magnetron sputtering targets, and prepares a CrNiMoNbAg high-entropy alloy layer on the surface of the chromium transition layer by adopting a magnetron sputtering technology, so as to obtain the silver-containing high-entropy alloy wide-temperature-range lubricating film material. In the invention, the chromium-nickel-molybdenum-niobium target is preferably formed by splicing pure metal targets of chromium, nickel, molybdenum and niobium; the area ratio of the molybdenum target to the niobium target is not less than 15%; the area ratio of pure metals of chromium, nickel, molybdenum and niobium in the chromium-nickel-molybdenum-niobium target is preferably 1-2: 1: 1. In the present invention, the purity of the chromium nickel molybdenum niobium target and the silver target is preferably > 99.99%.
In the invention, when the CrNiMoNbAg high-entropy alloy layer is prepared, a direct-current power supply is preferably adopted to sputter the chromium-nickel-molybdenum-niobium target and the silver target simultaneously. In the invention, the chromium-nickel-molybdenum-niobium target and the silver target are respectively connected with an independent direct current power supply. In the invention, the direct-current power supply power of the chromium-nickel-molybdenum-niobium target is preferably 100-300W, and more preferably 200W; the direct current power supply power of the silver target is preferably 13-40W, and more preferably 27-30W; the sputtering time of the chromium-nickel-molybdenum-niobium target and the silver target is preferably 40-60 min.
In the present invention, when the CrNiMoNbAg high-entropy alloy layer is prepared, a bias of-50 to-150V is preferably applied to the substrate, and a bias of-100V is more preferably applied.
In the invention, the CrNiMoNbAg high-entropy alloy layer is preferably prepared in an argon atmosphere; the flow rate of argon gas is preferably 40 sccm. When the CrNiMoNbAg high-entropy alloy layer is prepared, the air pressure of the magnetron sputtering chamber is preferably 0.6-0.8 Pa, and more preferably 0.65-0.7 Pa.
In the invention, after the sputtering is finished, the material is preferably taken out after being cooled to the temperature of the base material below 50 ℃ in a vacuum environment.
The wide-temperature-range lubricating film material containing the silver high-entropy alloy has excellent lubricating performance in the atmospheric environment from normal temperature to 600 ℃, and is simple in preparation method, high in process controllability and reproducibility and wide in application range.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The base material adopted in the examples is W18Cr4V steel; the purity of argon is more than 99.999 percent; in the coating process, the argon flow is fixed, and the air pressure of the cavity is adjusted by utilizing a turbomolecular pump valve.
Example 1
Magnetron sputtering equipment: ultimate vacuum of equipment<2×10 -4 Pa; the equipment can be heated to 10-300 ℃ and has a temperature control function; 3 strong magnetic target heads are arranged above the equipment and used for mounting target materials, and each target is provided with an independent direct-current sputtering power supply; during film coating, the base material is placed on a rotatable sample disc at the bottom of the device; the apparatus is provided with a bias power supply connected to the sample plate.
Preparing a base material: the W18Cr4V substrate was cleaned in absolute ethanol three times for 15 minutes each using an ultrasonic cleaner, taken out and dried.
Preparing a target material: the chromium target, the silver target and the chromium-nickel-molybdenum-niobium spliced target are respectively arranged on 3 strong magnetic target heads, wherein the area ratio of pure metals of the chromium-nickel-molybdenum-niobium spliced target is 1:1:1: 1.
The film deposition process comprises the following steps in sequence: (1) placing the substrate in a sample tray at the bottom of a magnetron sputtering device, vacuumizing the device, and waiting for the air pressure of a cavity of the device<1.5×10 -3 After Pa, opening the sample tray for heating; (2) after the sample plate is heated to 200 DEG CIntroducing 40sccm high-purity argon, adjusting the air pressure of the cavity to be 5Pa, starting the sample plate to rotate (2.5r/min), starting the bias voltage power supply (-450V), and exciting argon plasma to bombard the surface of the substrate; (3) keeping 40sccm argon gas to be introduced, adjusting the air pressure of the cavity to be 0.65Pa, applying 200W power to the chromium target by using a direct-current power supply, depositing a chromium transition layer on the base material, wherein the bias voltage of the sample plate is-150V in the deposition process, and the deposition time is 10 min; (4) closing the sputtering of the chromium target, keeping 40sccm argon gas introduced, keeping the air pressure of the cavity at 0.65Pa, respectively applying 200W and 27W power to the chromium-nickel-molybdenum-niobium target and the silver target by using a direct current power supply, and depositing a CrNiMoNbAg high-entropy alloy layer (containing an Ag high-entropy alloy layer), wherein the bias voltage of the process is-100V, the deposition time is 60min, and finally obtaining the silver-containing high-entropy alloy wide-temperature-range lubricating film material.
In the wide-temperature-range lubricating film material of the silver-containing high-entropy alloy prepared in this embodiment, the thickness of the chromium transition layer is 0.2 μm, the thickness of the crnimotnbag high-entropy alloy layer is 1.0 μm, and the content of each element in the crnimotnbag high-entropy alloy layer includes, in atomic percentage, 24% of chromium, 24% of nickel, 16% of molybdenum, 12% of niobium, and 24% of silver. The structure of the wide-temperature-range lubricating film material containing the silver high-entropy alloy prepared in the embodiment is shown in fig. 1, and as can be seen from fig. 1, the film material prepared in the invention is of a double-layer structure, the bottom layer is a chromium transition layer, and the surface layer is a CrNiMoNbAg high-entropy alloy layer (containing an Ag high-entropy alloy layer).
Frictional wear performance: the frictional wear performance of the film material is evaluated by using an HT-2000 type high-temperature frictional wear tester, and the dual ball is Si with the diameter of 5mm 3 N 4 The ball load is 2N, the friction radius is 5mm, the sliding linear velocity is 0.26m/s, the test temperature is 25 ℃, 100 ℃, 200 ℃, 300 ℃, 400 ℃, 500 ℃ and 600 ℃, the obtained results are shown in figures 2-3 and tables 1-2, the friction coefficient is 0.23-0.32, the wear rate is (9-18) × 10 -5 mm 3 N -1 m -1 。
The film-base bonding force between the silver-containing high-entropy alloy wide-temperature-range lubricating film material and the base material is 36N.
Example 2
The magnetron sputtering apparatus and the substrate were prepared as in example 1.
Preparing a target material: the chromium target, the silver target and the chromium-nickel-molybdenum-niobium spliced target are respectively arranged on 3 strong magnetic target heads, wherein the area ratio of pure metals of chromium, nickel, molybdenum and niobium in the chromium-nickel-molybdenum-niobium spliced target is 2:2:1: 1.
And (3) a film deposition process: wherein the steps (1) to (3) are the same as in example 1; (4) closing the sputtering of the chromium target, keeping 40sccm argon gas introduced, keeping the air pressure of the cavity at 0.65Pa, respectively applying 200W and 30W power to the chromium-nickel-molybdenum-niobium target and the silver target by using a direct current power supply, and carrying out CrNiMoNbAg high-entropy alloy layer deposition, wherein the bias voltage in the process is-100V, the deposition time is 60min, and finally obtaining the silver-containing high-entropy alloy wide-temperature-range lubricating film material.
In the wide-temperature-range lubricating film material of the silver-containing high-entropy alloy prepared in this embodiment, the thickness of the chromium transition layer is 0.2 μm, the thickness of the crnimotnbag high-entropy alloy layer is 1.2 μm, and the content of each element in the crnimotnbag high-entropy alloy layer includes, in atomic percentage, 29% of chromium, 29% of nickel, 11% of molybdenum, 8% of niobium, and 23% of silver.
The friction and wear performance evaluation equipment and test conditions are the same as those of example 1, and the obtained results are shown in FIGS. 4-5 and tables 1-2, wherein the friction coefficient ranges from 0.22 to 0.42, and the wear rate ranges from (12-24). times.10 -5 mm 3 N -1 m -1 . The film-based bonding force between the silver-containing high-entropy alloy wide-temperature-range lubricating film material and the base material is 35N.
Comparative example 1
The preparation process of the base material and the transition layer is the same as that of the example 1, the Inconel-718 is used as the transition layer, the silver film is deposited on the Inconel-718 used as the transition layer, the thickness of the silver film is 1200nm, and the silver film is marked as a pure silver film.
Film performance: the film-based bonding force between the pure silver film and the substrate is 8.5N. The frictional wear performance evaluation equipment and test conditions were the same as those of example 1, and the results are shown in tables 1 to 2.
TABLE 1 average coefficient of friction of films prepared in examples 1-2 and comparative example 1
TABLE 2 abrasion rates of the films prepared in examples 1-2 and comparative example 1
As can be seen from the test results of the above examples and comparative examples, the silver-containing high-entropy alloy wide-temperature-range lubricating film material prepared by the invention has the advantages of high film-base binding force, low friction coefficient and wear rate and excellent lubricating property.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A wide-temperature-range lubricating film material of silver-containing high-entropy alloy comprises a chromium transition layer and a CrNiMoNbAg high-entropy alloy layer which are sequentially arranged on the surface of a substrate.
2. The silver-containing high-entropy alloy wide-temperature-range lubricating film material as claimed in claim 1, wherein the thickness of the chromium transition layer is 0.2-0.3 μm; the thickness of the CrNiMoNbAg high-entropy alloy layer is 0.8-1.2 mu m.
3. The silver-containing high-entropy alloy wide-temperature-range lubricating film material as claimed in claim 1, wherein the CrNiMoNbAg high-entropy alloy layer contains the following elements in atomic percentage: 20-30% of chromium, 20-30% of nickel, 10-20% of molybdenum, 5-15% of niobium and 20-25% of silver.
4. The preparation method of the silver-containing high-entropy alloy wide-temperature-range lubricating film material as claimed in any one of claims 1 to 3, which comprises the following steps:
preparing a chromium transition layer on the surface of a base material by using a chromium target as a magnetron sputtering target and adopting a magnetron sputtering technology;
and (3) taking the chromium-nickel-molybdenum-niobium target and the silver target as magnetron sputtering targets, and preparing a CrNiMoNbAg high-entropy alloy layer on the surface of the chromium transition layer by adopting a magnetron sputtering technology to obtain the silver-containing high-entropy alloy wide-temperature-range lubricating film material.
5. The preparation method according to claim 4, wherein a direct current power supply is adopted to sputter a chromium target when the chromium transition layer is prepared, and the power of the direct current power supply is 100-300W; the sputtering time is 10-15 min.
6. The method according to claim 4 or 5, wherein a bias of-50 to-150V is applied to the substrate when the chromium transition layer is prepared.
7. The preparation method according to claim 4, wherein a direct current power supply is adopted to sputter a chromium-nickel-molybdenum-niobium target and a silver target simultaneously when the CrNiMoNbAg high-entropy alloy layer is prepared, and the direct current power supply power of the chromium-nickel-molybdenum-niobium target is 100-300W; the direct current power supply power of the silver target is 13-40W; the sputtering time of the chromium-nickel-molybdenum-niobium target and the silver target is 40-60 min.
8. The method according to claim 4 or 7, wherein a bias of-50 to-100V is applied to the substrate when the CrNiMoNbAg high-entropy alloy layer is prepared.
9. The method according to claim 4, wherein the NiMo niobium target is formed by splicing pure metal targets of Cr, Ni, Mo and Nb; the area ratio of pure metals of chromium, nickel, molybdenum and niobium in the chromium-nickel-molybdenum-niobium target is 1-2: 1: 1.
10. The preparation method according to claim 4, wherein the substrate is kept rotating at a speed of 2.5-10 r/min during the preparation of the silver-containing high-entropy alloy wide-temperature-range lubricating film material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN116479305A (en) * | 2023-04-27 | 2023-07-25 | 西北工业大学 | Wear-resistant codeposition refractory high-entropy alloy film and preparation method thereof |
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