CN113322436A - Nano composite WN-Cu coating and preparation method and application thereof - Google Patents
Nano composite WN-Cu coating and preparation method and application thereof Download PDFInfo
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- CN113322436A CN113322436A CN202110442823.XA CN202110442823A CN113322436A CN 113322436 A CN113322436 A CN 113322436A CN 202110442823 A CN202110442823 A CN 202110442823A CN 113322436 A CN113322436 A CN 113322436A
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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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/16—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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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
- C23C14/3464—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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
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Abstract
The invention belongs to the technical field of preparation of cutter coatings and surface lubricating coatings, and discloses a nano composite WN-Cu coating as well as a preparation method and application thereof. The atomic percentage contents of each element in the nano composite WN-Cu coating are respectively as follows: w25-35 at.%, Cu 0-30 at.%, N45-65 at.%. The nano composite WN-Cu coating prepared by adopting the double-target magnetron sputtering has the advantages of smooth surface, compact structure and good self-lubricating property, and can effectively reduce the friction coefficient and improve the wear resistance of the self-lubricating coating.
Description
Technical Field
The invention belongs to the technical field of preparation of cutter coatings and surface lubricating coatings, and particularly relates to a nano composite WN-Cu coating as well as a preparation method and application thereof.
Background
In recent years, the use of liquid lubricants has led to environmental pollution, and the development of cutting tool coatings and wear-resistant protective coatings is gradually heading for dry solid lubricating materials. Compared with a liquid lubricant, the dry solid lubricating material is environment-friendly and is an effective way for reducing the frictional wear of the cutter coating. Compared with the traditional transition group nitrides (TiN, CrN, ZrN and the like), the tungsten nitride (WN) coating has the advantages of high hardness, high melting point, good corrosion resistance and the like. Meanwhile, as a magneli phase representative element, the metal W can be used as a high-temperature lubricating phase and oxidized to form a magneli phase lubricating oxide WO3And the friction coefficient is effectively reduced. In addition, the soft metal Cu is usually added into the hard coating as a second phase or a lubricating phase to form a nitride/soft metal amorphous phase nano composite structure, and on one hand, the hardness of the nano composite film can be improved through grain refinement; on the other hand, the friction coefficient can be effectively reduced by adding the soft metal phase. Therefore, how to improve the wear resistance and self-lubricity of the cutter coating is a technical problem to be solved by the invention.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention mainly aims to provide a nano composite WN-Cu coating, which further improves the tribological performance of a self-lubricating coating by combining the respective advantages of a soft metal and an oxide lubricating phase.
The invention also aims to provide a preparation method of the nano composite WN-Cu coating.
The invention also aims to provide application of the nano composite WN-Cu coating.
The purpose of the invention is realized by the following technical scheme:
a nano composite WN-Cu coating comprises the following elements in atomic percentage: w25-35 at.%, Cu 0-30 at.%, N45-65 at.%, and the total amount of each element is 100 at.%.
The preparation method of the nano composite WN-Cu coating comprises the following steps:
(1) putting the substrate base body after mirror polishing into ultrasonic waves, sequentially carrying out ultrasonic cleaning for 10-20 min by using a metal detergent and alcohol, drying, fixing on a sample platform in a coating cavity, keeping the target base distance to be 50-150 mm, adjusting the rotation speed of the sample platform to be 0-20 rpm, opening a temperature control heater, heating to 25-500 ℃, pre-vacuumizing to the background vacuum of 3.0-5.0 multiplied by 10-3Pa；
(2) Opening Ar, N2And the gas flow valve is used for adjusting Ar: n is a radical of2Setting the flow ratio of 1: 1-10: 1, setting the rotation speed of a molecular pump to be 30000-90000 rpm, and adjusting the total air pressure to be 0.5-2.0 Pa;
(3) turning on a direct-current and radio-frequency magnetron sputtering power supply, adjusting the power of a direct-current sputtering Cu target to 0-100W, adjusting the power of a radio-frequency sputtering W target to 0-500W, adjusting the duty ratio to 10-100%, and carrying out composite deposition for 0-600 min to obtain a nano composite WN-Cu coating with the thickness of 1.0-4.0 microns;
(4) after deposition is finished, the direct current and radio frequency magnetron sputtering power supply is turned off, and Ar and N are turned off2And closing the molecular pump and the mechanical pump, opening the furnace door after the temperature of the chamber is reduced to room temperature, and taking out the sample to finish coating.
The nano composite WN-Cu coating is applied to the field of cutter coatings and surface lubricating coatings.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention organically combines the self-lubricating effect of the oxide lubricating phase and the soft metal phase, effectively reduces the friction coefficient, and can prepare the nano composite self-lubricating coating with good self-lubricating performance;
(2) the nano composite WN-Cu coating prepared by the invention has the advantages of smooth surface, low friction, high wear resistance and the like, and can realize good self-lubricating effect at medium and low temperature.
Drawings
FIG. 1 is a schematic illustration of the dual target magnetron sputtering deposition in the examples;
FIG. 2 is a surface topography of the nanocomposite WN-Cu coatings at different Cu target power depositions in the examples: (a)0W, (b)3W, (c)7W, (d) 9W;
FIG. 3 is a cross-sectional profile of the nano-composite WN-Cu coating deposited at different Cu target powers in the examples: (a)0W, (b)3W, (c)7W, (d) 9W.
Detailed Description
The present invention is further illustrated by the following examples, which are provided only for illustrating the present invention, but the scope of the present invention is not limited thereto.
A schematic of the dual target magnetron sputtering deposition used in the following examples is shown in fig. 1.
Example 1:
(1) putting the substrate base bodies of the monocrystalline Si piece, the stainless steel, the hard alloy and the like after mirror surface polishing into ultrasonic waves, sequentially carrying out ultrasonic cleaning for 10min by using a metal detergent and alcohol, drying, fixing on a sample platform in a coating chamber, keeping the target base distance of 100mm, adjusting the rotation speed of the sample platform to 10rpm, opening a temperature control heater to heat to 300 ℃, pre-vacuumizing the base to 5.0 multiplied by 10 for vacuum-3Pa；
(2) Opening Ar, N2Air flow valve, regulation A, N2Setting the flow ratio to be 8:1, setting the rotating speed of a molecular pump to be 63000rpm, and adjusting the total air pressure to be 1.0 Pa;
(3) turning on a direct current and radio frequency magnetron sputtering power supply, adjusting the power of a direct current sputtering Cu target to 0W, adjusting the power of a radio frequency sputtering W target to 100W, performing composite deposition for 500min at a duty ratio of 50%, and obtaining a nano composite WN-Cu coating with the thickness of 2.0 mu m;
(4) after deposition is finished, the direct current and radio frequency magnetron sputtering power supply is turned off, and Ar and N are turned off2And closing the molecular pump and the mechanical pump, opening the furnace door after the temperature of the chamber is reduced to room temperature, and taking out the sample to finish coating.
In this example, the atomic percentage contents of each element in the prepared nanocomposite WN-Cu coating are respectively: w64.6 at.%, Cu 0 at.%, N35.4 at.%.
FIG. 2 (a) is a surface topography of the nano-composite WN-Cu coating prepared by the process parameters, and the surface is smooth and flat; fig. 3 (a) is a cross-sectional profile of the nano-composite WN-Cu coating prepared by the process parameters, which has a dense structure and a columnar crystal morphology.
Example 2:
(1) putting the substrate base bodies of the monocrystalline Si piece, the stainless steel, the hard alloy and the like after mirror surface polishing into ultrasonic waves, sequentially carrying out ultrasonic cleaning for 10min by using a metal detergent and alcohol, drying, fixing on a sample platform in a coating chamber, keeping the target base distance of 100mm, adjusting the rotation speed of the sample platform to 10rpm, opening a temperature control heater to heat to 300 ℃, pre-vacuumizing the base to 5.0 multiplied by 10 for vacuum-3Pa；
(2) Opening Ar, N2Air flow valve, regulation A, N2Setting the flow ratio to be 8:1, setting the rotating speed of a molecular pump to be 63000rpm, and adjusting the total air pressure to be 1.0 Pa;
(3) turning on a direct current and radio frequency magnetron sputtering power supply, adjusting the power of a direct current sputtering Cu target to 3W, adjusting the power of a radio frequency sputtering W target to 100W, performing composite deposition for 500min at a duty ratio of 50%, and obtaining a nano composite WN-Cu coating with the thickness of 2.0 mu m;
(4) after deposition is finished, the direct current and radio frequency magnetron sputtering power supply is turned off, and Ar and N are turned off2And closing the molecular pump and the mechanical pump, opening the furnace door after the temperature of the chamber is reduced to room temperature, and taking out the sample to finish coating.
In this example, the atomic percentage contents of each element in the prepared nanocomposite WN-Cu coating are respectively: w30.9 at.%, Cu 10.9 at.%, N58.2 at.%.
FIG. 2 (b) is a surface topography of the nano-composite WN-Cu coating prepared by the process parameters, and the surface is smooth and flat; FIG. 3 (b) is a cross-sectional view of the nano-composite WN-Cu coating prepared by the process parameters, which has a dense structure and a columnar crystal morphology.
Example 3:
(1) putting the substrate base bodies of the monocrystalline Si piece, the stainless steel, the hard alloy and the like after mirror surface polishing into ultrasonic waves, sequentially carrying out ultrasonic cleaning for 10min by using a metal detergent and alcohol, drying, fixing on a sample platform in a coating chamber, keeping the target base distance of 100mm, adjusting the autorotation speed of the sample platform to be 10rpm, and opening the temperatureThe heater is controlled to be heated to 300 ℃, and the pre-vacuum background is pumped to 5.0 multiplied by 10-3Pa；
(2) Opening Ar, N2Air flow valve, regulation A, N2Setting the flow ratio to be 8:1, setting the rotating speed of a molecular pump to be 63000rpm, and adjusting the total air pressure to be 1.0 Pa;
(3) turning on a direct current and radio frequency magnetron sputtering power supply, adjusting the power of a direct current sputtering Cu target to 7W, adjusting the power of a radio frequency sputtering W target to 100W, performing composite deposition for 500min at a duty ratio of 50%, and obtaining a nano composite WN-Cu coating with the thickness of 2.1 mu m;
(4) after deposition is finished, the direct current and radio frequency magnetron sputtering power supply is turned off, and Ar and N are turned off2And closing the molecular pump and the mechanical pump, opening the furnace door after the temperature of the chamber is reduced to room temperature, and taking out the sample to finish coating.
In this example, the atomic percentage contents of each element in the prepared nanocomposite WN-Cu coating are respectively: w30.0 at.%, Cu 16.3 at.%, N53.7 at.%.
FIG. 2 (c) is a surface topography of the nano-composite WN-Cu coating prepared by the process parameters, and the surface is smooth and flat; fig. 3 (c) is a cross-sectional profile of the nano-composite WN-Cu coating prepared by the process parameters, which has a dense structure and a disappearance of the columnar crystal morphology.
Example 4:
(1) putting the substrate base bodies of the monocrystalline Si piece, the stainless steel, the hard alloy and the like after mirror surface polishing into ultrasonic waves, sequentially carrying out ultrasonic cleaning for 10min by using a metal detergent and alcohol, drying, fixing on a sample platform in a coating chamber, keeping the target base distance of 100mm, adjusting the rotation speed of the sample platform to 10rpm, opening a temperature control heater to heat to 300 ℃, pre-vacuumizing the base to 5.0 multiplied by 10 for vacuum-3Pa；
(2) Opening Ar, N2Air flow valve, regulation A, N2Setting the flow ratio to be 8:1, setting the rotating speed of a molecular pump to be 63000rpm, and adjusting the total air pressure to be 1.0 Pa;
(3) turning on a direct current and radio frequency magnetron sputtering power supply, adjusting the power of a direct current sputtering Cu target to 9W, adjusting the power of a radio frequency sputtering W target to 100W, performing composite deposition for 500min at a duty ratio of 50%, and obtaining a nano composite WN-Cu coating with the thickness of 2.1 mu m;
(4) after deposition is finished, the direct current and radio frequency magnetron sputtering power supply is turned off, and Ar and N are turned off2And closing the molecular pump and the mechanical pump, opening the furnace door after the temperature of the chamber is reduced to room temperature, and taking out the sample to finish coating.
In this example, the atomic percentage contents of each element in the prepared nanocomposite WN-Cu coating are respectively: w25.7 at.%, Cu 28.8 at.%, N45.5 at.%.
FIG. 2 (d) is a surface topography of the nanocomposite WN-Cu coating prepared by the process parameters, with particles appearing on the surface; fig. 3 (d) is a cross-sectional profile of the nano-composite WN-Cu coating prepared by the process parameters, which has a loose structure and a disappearance of the columnar crystal morphology.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (4)
1. A nano-composite WN-Cu coating is characterized in that: the atomic percentage contents of each element in the nano composite WN-Cu coating are respectively as follows: w25-35 at.%, Cu 0-30 at.%, N45-65 at.%, and the total amount of each element is 100 at.%.
2. The nano-composite WN-Cu coating as claimed in claim 1, wherein the preparation method of the nano-composite WN-Cu coating comprises the following steps:
(1) putting the substrate base body after mirror polishing into ultrasonic waves, sequentially carrying out ultrasonic cleaning for 10-20 min by using a metal detergent and alcohol, drying, fixing on a sample platform in a coating cavity, keeping the target base distance to be 50-150 mm, adjusting the rotation speed of the sample platform to be 0-20 rpm, opening a temperature control heater, heating to 25-500 ℃, pre-vacuumizing to the background vacuum of 3.0-5.0 multiplied by 10-3Pa；
(2) Opening Ar, N2And the gas flow valve is used for adjusting Ar: n is a radical of2The flow rate ratio is 1: 1-10: 1, and the device is divided intoThe rotation speed of the sub-pump is 30000-90000 rpm, and the total air pressure is adjusted to 0.5-2.0 Pa;
(3) turning on a direct-current and radio-frequency magnetron sputtering power supply, adjusting the power of a direct-current sputtering Cu target to 0-100W, adjusting the power of a radio-frequency sputtering W target to 0-500W, adjusting the duty ratio to 10-100%, and carrying out composite deposition for 0-600 min to obtain a nano composite WN-Cu coating with the thickness of 1.0-4.0 microns;
(4) after deposition is finished, the direct current and radio frequency magnetron sputtering power supply is turned off, and Ar and N are turned off2And closing the molecular pump and the mechanical pump, opening the furnace door after the temperature of the chamber is reduced to room temperature, and taking out the sample to finish coating.
3. The method for preparing the nano-composite WN-Cu coating of claim 2, wherein the substrate base in step (1) comprises single crystal Si wafer, stainless steel, or hard alloy.
4. The nano-composite WN-Cu coating of claim 1, wherein the nano-composite WN-Cu coating is applied to the fields of tool coating and surface lubrication coating.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103255366A (en) * | 2011-09-09 | 2013-08-21 | 伊威斯发动机***有限责任两合公司 | Articulated chain with hard coated chain links |
| CN104032269A (en) * | 2014-06-04 | 2014-09-10 | 江苏科技大学 | NbN-Ag hard thin film and preparation method thereof |
| CN104099576A (en) * | 2014-07-02 | 2014-10-15 | 江苏科技大学 | Hard film and preparation method thereof |
| CN104494229A (en) * | 2014-12-08 | 2015-04-08 | 中国人民解放军装甲兵工程学院 | Antibacterial and wear-resistant nano-composite coating and preparation method thereof |
-
2021
- 2021-04-23 CN CN202110442823.XA patent/CN113322436A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103255366A (en) * | 2011-09-09 | 2013-08-21 | 伊威斯发动机***有限责任两合公司 | Articulated chain with hard coated chain links |
| CN104032269A (en) * | 2014-06-04 | 2014-09-10 | 江苏科技大学 | NbN-Ag hard thin film and preparation method thereof |
| CN104099576A (en) * | 2014-07-02 | 2014-10-15 | 江苏科技大学 | Hard film and preparation method thereof |
| CN104494229A (en) * | 2014-12-08 | 2015-04-08 | 中国人民解放军装甲兵工程学院 | Antibacterial and wear-resistant nano-composite coating and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 赵洪舰 等: ""磁控溅射法制备W1−xAlxN薄膜的微结构与性能"", 《粉末冶金材料科学与工程》 * |
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