CN115074684B - 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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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 86
- 239000000956 alloy Substances 0.000 title claims abstract description 86
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 83
- 239000004332 silver Substances 0.000 title claims abstract description 83
- 239000000463 material Substances 0.000 title claims abstract description 77
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 63
- 239000011651 chromium Substances 0.000 claims abstract description 63
- 230000007704 transition Effects 0.000 claims abstract description 39
- KMCVQCJLAZSHCL-UHFFFAOYSA-N [Nb].[Mo].[Cr].[Ni] Chemical compound [Nb].[Mo].[Cr].[Ni] KMCVQCJLAZSHCL-UHFFFAOYSA-N 0.000 claims description 28
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 27
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 24
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 14
- 229910052750 molybdenum Inorganic materials 0.000 claims description 14
- 239000011733 molybdenum Substances 0.000 claims description 14
- 229910052758 niobium Inorganic materials 0.000 claims description 14
- 239000010955 niobium Substances 0.000 claims description 14
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 14
- 229910052759 nickel Inorganic materials 0.000 claims description 13
- 238000004544 sputter deposition Methods 0.000 claims description 13
- 238000005516 engineering process Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 238000005137 deposition process Methods 0.000 abstract description 5
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 230000002401 inhibitory effect Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 61
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 22
- 229910052786 argon Inorganic materials 0.000 description 11
- 238000000151 deposition Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910001026 inconel Inorganic materials 0.000 description 2
- 229910000816 inconels 718 Inorganic materials 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- -1 chromium-nickel-molybdenum-niobium-silver Chemical compound 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
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- 230000009977 dual effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 231100000719 pollutant Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- 239000002344 surface layer Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
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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
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- 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
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- 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
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- C23C14/505—Substrate holders for rotation of the substrates
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Abstract
The invention provides a silver-containing high-entropy alloy wide-temperature-range lubricating film material and a preparation method thereof, and relates to the technical field of lubricating materials. The silver-containing high-entropy alloy wide-temperature-range lubricating film material provided by the invention comprises a chromium transition layer and a CrNiMoNbAg high-entropy alloy layer which are sequentially arranged on the surface of a base material. The invention adopts chromium as the transition layer, solves the problems that the silver-containing film is difficult to combine with a base material in the deposition process and the film is peeled off under the high temperature condition; the invention adopts the CrNiMoNbAg high-entropy alloy layer as the lubricating layer, plays the advantages of good lubricating property of silver, excellent mechanical property and high-temperature stability of high-entropy alloy and inhibiting silver diffusion at high temperature, reduces the friction coefficient of the film material and prolongs the service life of the film material.
Description
Technical Field
The invention relates to the technical field of lubricating materials, in particular to a silver-containing high-entropy alloy wide-temperature-range lubricating film material and a preparation method thereof.
Background
In the industrial and aerospace fields, material, workpiece failures and equipment failures often occur due to frictional wear, resulting in significant economic losses. Therefore, the development of lubricating materials 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 has better lubricating performance in high and 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 binding force of the silver film and the base material, a method for forming a silver-containing multi-element composite film by compounding and doping silver with other metals is often adopted. However, the existing composite film is easy to peel off under the high temperature condition, and the service life is short.
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 silver-containing high-entropy alloy wide-temperature-range lubricating film material which comprises a chromium transition layer and a CrNiMoNbAg high-entropy alloy layer which are sequentially arranged on the surface of a base material.
Preferably, the thickness of the chromium transition layer is 0.2-0.3 mu m; the thickness of the CrNiMoNbAg high-entropy alloy layer is 0.8-1.2 mu m.
Preferably, the crnimonag high-entropy alloy layer comprises the following elements in atom percent: 20 to 30 percent of chromium, 20 to 30 percent of nickel, 10 to 20 percent of molybdenum, 5 to 15 percent of niobium and 20 to 25 percent of silver.
The invention provides a preparation method of the silver-containing high-entropy alloy wide-temperature-range lubricating film material, which comprises the following steps:
taking a chromium target as a magnetron sputtering target, and adopting a magnetron sputtering technology to prepare a chromium transition layer on the surface of the substrate;
and preparing a CrNiMoNbAg high-entropy alloy layer on the surface of the chromium transition layer by taking a chromium nickel molybdenum niobium target and a silver target as magnetron sputtering targets and adopting a magnetron sputtering technology to obtain the silver-containing high-entropy alloy wide-temperature-range lubricating film material.
Preferably, when preparing the chromium transition layer, sputtering a chromium target by adopting a direct current power supply, wherein the power of the direct current power supply is 100-300W; the sputtering time is 10-15 min.
Preferably, when preparing the chromium transition layer, a bias of-50 to-150V is applied 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 power of the direct current power supply 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-50 to-100V is applied to the substrate.
Preferably, the chromium-nickel-molybdenum-niobium target is formed by splicing chromium, nickel, molybdenum and niobium pure metal targets; the area ratio of chromium, nickel, molybdenum and niobium pure metals in the chromium-nickel-molybdenum-niobium target is 1-2:1-2:1:1.
Preferably, in the process of preparing the silver-containing high-entropy alloy wide-temperature-range lubricating film material, the substrate keeps rotating at a speed of 2.5-10 r/min.
The invention provides a silver-containing high-entropy alloy wide-temperature-range lubricating film material which comprises a chromium transition layer and a CrNiMoNbAg high-entropy alloy layer which are sequentially arranged on the surface of a base material. The invention adopts 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-nickel-molybdenum-niobium-silver high-entropy alloy as the transition layer, thereby solving the problems that the silver-containing film is difficult to combine with the base materials in the deposition process and the film is peeled off under the high-temperature condition; the invention adopts the CrNiMoNbAg high-entropy alloy layer as the lubricating layer, plays the advantages of good lubricating property of silver, excellent mechanical property and high-temperature stability of high-entropy alloy and inhibiting silver diffusion at high temperature, reduces the friction coefficient of the film material and prolongs the service life of the film material. 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, which is simple in preparation process, easy to obtain target materials, accurate and controllable in film thickness and element content, low in production cost and capable of mass 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 graph showing the friction coefficient of the silver-containing high-entropy alloy wide-temperature-range lubricating film material prepared in example 1 of the present invention at 25-600 ℃;
FIG. 3 is a graph showing the abrasion rate of the silver-containing high-entropy alloy wide-temperature-range lubricating film material prepared in example 1 at 25-600 ℃;
FIG. 4 is a graph showing the friction coefficient of the silver-containing high-entropy alloy wide-temperature-range lubricating film material prepared in example 2 of the present invention at 25-600 ℃;
FIG. 5 is a graph showing the abrasion rate of the silver-containing high-entropy alloy wide-temperature-range lubricating film material prepared in example 2 of the present invention at 25-600 ℃.
Detailed Description
The invention provides a silver-containing high-entropy alloy wide-temperature-range lubricating film material which comprises a chromium transition layer and a CrNiMoNbAg high-entropy alloy layer which are sequentially arranged on the surface of a base material.
The silver-containing high-entropy alloy wide-temperature-range lubricating film material provided by the invention comprises a chromium transition layer arranged on the surface of a base material. In the present invention, the thickness of the chromium transition layer is preferably 0.2 to 0.3 μm.
The silver-containing high-entropy alloy wide-temperature-range lubricating film material provided by the invention comprises a CrNiMoNbAg high-entropy alloy layer arranged on the surface of the chromium transition layer. In the present invention, the thickness of the crnimonag high-entropy alloy layer is preferably 0.8 to 1.2 μm, more preferably 1.0 μm. In the invention, the content of each element in the CrNiMoNbAg high-entropy alloy layer is preferably as follows in atom percent: 20 to 30 percent of chromium, 20 to 30 percent of nickel, 10 to 20 percent of molybdenum, 5 to 15 percent of niobium and 20 to 25 percent of silver. In a specific embodiment of the invention, the crnimonag high-entropy alloy layer comprises the following elements in percentage by atom: 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 friction coefficient of the silver-containing high-entropy alloy wide-temperature-range lubricating film material is preferably 0.2-0.45 under the atmospheric environment at the temperature of room temperature to 600 ℃; the abrasion ratio is preferably (9-25). Times.10 -5 mm 3 N -1 m -1 . In the present invention, the film-base bonding force of the silver-containing high-entropy alloy wide-temperature-range lubricating film material and the substrate is preferably more than 30N, more preferably 35 to 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:
taking a chromium target as a magnetron sputtering target, and adopting a magnetron sputtering technology to prepare a chromium transition layer on the surface of the substrate;
and preparing a CrNiMoNbAg high-entropy alloy layer on the surface of the chromium transition layer by taking a chromium nickel molybdenum niobium target and a silver target as magnetron sputtering targets and 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 the 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 Inconel series high temperature alloy. In the present invention, the purity of the chromium target is preferably >99.99%.
The present invention preferably further comprises, prior to the preparation of the chromium transition layer: and preheating and surface cleaning are sequentially carried out on the base material. In the present invention, the preheating temperature is preferably 100 to 200 ℃, 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 1.5x10 -3 Pa. In the present invention, the surface cleaning preferably includes: introducing 40sccm argon, adjusting the pressure of the cavity to 3-5 Pa, and exciting argon plasma to etch the surface of the substrate by using-400 to-500V bias. In the present invention, the time for the surface cleaning is preferably 10 minutes. The invention removes the oxide layer and the pollutant on the surface of the substrate through 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 2.5r/min.
In the invention, when preparing the chromium transition layer, a direct current power supply is preferably used for sputtering a chromium target, and the power of the direct current power supply is preferably 100-300W, more preferably 200W; the sputtering time is preferably 10 to 15 minutes.
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 is preferably 40sccm. When the chromium transition layer is prepared by the invention, the air pressure of the magnetron sputtering chamber is preferably 0.6-0.8 Pa, more preferably 0.65-0.7 Pa.
After the chromium transition layer is obtained, a chromium nickel molybdenum niobium target and a silver target are used as magnetron sputtering targets, and a CrNiMoNbAg high-entropy alloy layer is prepared on the surface of the chromium transition layer by adopting a magnetron sputtering technology, so that the silver-containing high-entropy alloy wide-temperature-range lubricating film material is obtained. In the invention, the chromium-nickel-molybdenum-niobium target is preferably formed by splicing chromium, nickel, molybdenum and niobium pure metal targets; the area ratio of each of the molybdenum target and the niobium target is not less than 15%; the area ratio of chromium, nickel, molybdenum and niobium pure metals in the chromium-nickel-molybdenum-niobium target is preferably 1-2:1-2:1:1. In the present invention, the purity of the chromium nickel molybdenum niobium target and silver target is preferably >99.99%.
In the invention, when preparing the CrNiMoNbAg high-entropy alloy layer, a direct-current power supply is preferably adopted to sputter a chromium-nickel-molybdenum-niobium target and a silver target simultaneously. In the invention, the chromium nickel molybdenum niobium target and the silver target are respectively connected with independent direct current power supplies. In the invention, the direct current power of the chromium-nickel-molybdenum-niobium target is preferably 100-300W, more preferably 200W; the direct current power of the silver target is preferably 13-40W, 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 preparing the CrNiMoNbAg high-entropy alloy layer, it is preferable to apply a bias of-50 to-150V, and more preferably-100V, to the base material.
In the invention, the CrNiMoNbAg high-entropy alloy layer is preferably prepared in an argon atmosphere; the flow rate of argon is preferably 40sccm. 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 present invention, it is preferable to cool the material in a vacuum environment to a substrate temperature of <50 ℃ after the sputtering is completed, and then take out the material.
The silver-containing high-entropy alloy wide-temperature-range lubricating film material prepared by the invention has excellent lubricating performance in the atmospheric environment at normal temperature to 600 ℃, and has the advantages of simple preparation method, high process controllability and reproducibility and wide application range.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The substrate used in the examples was W18Cr4V steel; argon purity >99.999%; in the film coating process, the argon flow is fixed, and the cavity air pressure is regulated by using a turbomolecular pump valve.
Example 1
Magnetron sputtering equipment: device ultimate vacuum<2×10 -4 Pa; the heatable temperature range of the equipment is 10-300 ℃, and the equipment has a temperature control function; 3 strong magnetic target heads are arranged above the equipment and used for installing targets, and each target is provided with an independent direct current sputtering power supply; when coating, the base material is placed on a rotatable sample tray at the bottom of the equipment; the apparatus is provided with a bias power source connected to the sample tray.
Preparing a base material: and cleaning the W18Cr4V substrate in absolute ethyl alcohol for three times by using an ultrasonic cleaner for 15 minutes each time, taking out and drying.
Preparing a target: the chromium target, the silver target and the chromium-nickel-molybdenum-niobium spliced target are respectively arranged at 3 ferromagnetic targets, wherein the area ratio of each pure metal of the chromium-nickel-molybdenum-niobium spliced target is 1:1:1:1.
The film deposition process sequentially comprises the following steps: (1) Placing the substrate on 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, starting a sample tray for heating; (2) After the sample plate is heated to 200 ℃, 40sccm of high-purity argon is introduced, the air pressure of the cavity is regulated to 5Pa, the rotation of the sample plate (2.5 r/min) is started, a bias power supply (-450V) is started, and argon plasma is excited to bombard the surface of the substrate; (3) Maintaining 40sccm argon gas to be introduced, adjusting the air pressure of the cavity to be 0.65Pa, applying 200W power on a chromium target by using a direct current power supply, depositing a chromium transition layer on a substrate, wherein the bias voltage of a sample tray in the deposition process is-150V, and the deposition time is 10min; (4) Closing the sputtering of the chromium target, keeping the argon of 40sccm to be 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 (Ag-containing high-entropy alloy layer), wherein the bias voltage is-100V, and the deposition time is 60min, so that the silver-containing high-entropy alloy wide-temperature-range lubricating film material is finally obtained.
In the silver-containing high-entropy alloy wide-temperature-range lubricating film material prepared in the embodiment, the thickness of the chromium transition layer is 0.2 mu m, the thickness of the CrNiMoNbAg high-entropy alloy layer is 1.0 mu m, and the content of each element in the CrNiMoNbAg high-entropy alloy layer is 24% of chromium, 24% of nickel, 16% of molybdenum, 12% of niobium and 24% of silver in terms of atomic percentage. The structure of the silver-containing high-entropy alloy wide-temperature-range lubricating film material prepared by the embodiment is shown in fig. 1, and as can be seen from fig. 1, the film material prepared by the invention has a double-layer structure, the bottom layer is a chromium transition layer, and the surface layer is a CrNiMoNbAg high-entropy alloy layer (Ag-containing high-entropy alloy layer).
Friction and wear properties: the frictional wear performance of the film material is evaluated by using an HT-2000 type high-temperature frictional wear testing machine, and the dual ball is Si with the diameter of 5mm 3 N 4 The ball, the 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 range is 0.23-0.32, and the wear rate range 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 in the same manner as in example 1.
Preparing a target: the chromium target, the silver target and the chromium-nickel-molybdenum-niobium spliced target are respectively arranged at 3 strong magnetic targets, wherein the pure metal areas of chromium, nickel, molybdenum and niobium in the chromium-nickel-molybdenum-niobium spliced target are in a ratio of 2:2:1:1.
Film deposition process: wherein steps (1) to (3) are the same as in example 1; (4) Closing the sputtering of the chromium target, keeping the argon of 40sccm to be 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 depositing a CrNiMoNbAg high-entropy alloy layer, wherein the bias voltage is-100V, and the deposition time is 60min, so that the silver-containing high-entropy alloy wide-temperature-range lubricating film material is finally obtained.
In the silver-containing high-entropy alloy wide-temperature-range lubricating film material prepared in the embodiment, the thickness of the chromium transition layer is 0.2 mu m, the thickness of the CrNiMoNbAg high-entropy alloy layer is 1.2 mu m, and the content of each element in the CrNiMoNbAg high-entropy alloy layer is 29% of chromium, 29% of nickel, 11% of molybdenum, 8% of niobium and 23% of silver in terms of atomic percentage.
Friction and wear Performance evaluation apparatus and test conditions were the same as in example 1, and the results obtained are shown in FIGS. 4 to 5 and tables 1 to 2, and the friction was measuredThe coefficient of friction is 0.22-0.42, and the abrasion rate is (12-24) x 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 35N.
Comparative example 1
The preparation process of the base material and the transition layer is the same as that of the embodiment 1, the Inconel-718 is used as the transition layer, a silver film is deposited on the Inconel-718 which is used as the transition layer, and the thickness of the silver film is 1200nm and is recorded as a pure silver film.
Film properties: the film-base bonding force of the pure silver film and the substrate is 8.5N. The frictional wear performance evaluation apparatus and test conditions were the same as in 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 wear Rate of films prepared in examples 1-2 and comparative example 1
As can be seen from the test results of the examples and the comparative examples, the silver-containing high-entropy alloy wide-temperature-range lubricating film material prepared by the invention has high film-base binding force, low friction coefficient and wear rate and excellent lubricating performance.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (9)
1. A silver-containing high-entropy alloy wide-temperature-range lubricating film material comprises a chromium transition layer and a CrNiMoNbAg high-entropy alloy layer which are sequentially arranged on the surface of a base material; the CrNiMoNbAg high-entropy alloy layer comprises the following elements in percentage by atom: 20-30% of chromium, 20-30% of nickel, 10-20% of molybdenum, 5-15% of niobium and 20-25% of silver;
the preparation method of the silver-containing high-entropy alloy wide-temperature-range lubricating film material comprises the following steps:
taking a chromium target as a magnetron sputtering target, and adopting a magnetron sputtering technology to prepare a chromium transition layer on the surface of the substrate;
and preparing a CrNiMoNbAg high-entropy alloy layer on the surface of the chromium transition layer by taking a chromium nickel molybdenum niobium target and a silver target as magnetron sputtering targets and adopting a magnetron sputtering technology to obtain the silver-containing high-entropy alloy wide-temperature-range lubricating film material.
2. The silver-containing high-entropy alloy wide-temperature-range lubricating film material according to 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 preparation method of the silver-containing high-entropy alloy wide-temperature-range lubricating film material according to any one of claims 1-2, comprising the following steps:
taking a chromium target as a magnetron sputtering target, and adopting a magnetron sputtering technology to prepare a chromium transition layer on the surface of the substrate;
and preparing a CrNiMoNbAg high-entropy alloy layer on the surface of the chromium transition layer by taking a chromium nickel molybdenum niobium target and a silver target as magnetron sputtering targets and adopting a magnetron sputtering technology to obtain the silver-containing high-entropy alloy wide-temperature-range lubricating film material.
4. The method for preparing the chromium transition layer according to claim 3, wherein a direct current power supply is used for sputtering a chromium target, and the power of the direct current power supply is 100-300W; the sputtering time is 10-15 min.
5. The method according to claim 3 or 4, wherein the chromium transition layer is prepared by applying a bias voltage of-50 to-150V to the substrate.
6. The preparation method of claim 3, wherein 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 direct-current power supply of the chromium-nickel-molybdenum-niobium target is 100-300W; the power of the direct current power supply of the silver target is 13-40W; and the sputtering time of the chromium-nickel-molybdenum-niobium target and the silver target is 40-60 min.
7. The method according to claim 3 or 6, wherein the crnimonag high-entropy alloy layer is prepared by applying a bias voltage of-50 to-100V to the substrate.
8. The method according to claim 3, wherein the chromium-nickel-molybdenum-niobium target is formed by splicing chromium, nickel, molybdenum and niobium pure metal targets; the area ratio of chromium, nickel, molybdenum and niobium in the chromium-nickel-molybdenum-niobium target is 1-2:1-2:1:1.
9. The method according to claim 3, wherein the substrate is kept rotating at a rate 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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