CN111304619A - Preparation method and application of wide-temperature-range self-lubricating MoN-VN multilayer coating - Google Patents
Preparation method and application of wide-temperature-range self-lubricating MoN-VN multilayer coating Download PDFInfo
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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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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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
- 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
Abstract
The invention discloses a preparation method and application of a wide-temperature-range self-lubricating MoN-VN multilayer coating, wherein the multilayer coating is formed by alternately superposing MoN and VN, the preparation method is characterized in that a magnetron sputtering technology is utilized in a nitrogen environment, and the rotating speed of a substrate sample is regulated to prepare the MoN/VN multilayer coating with different modulation cycles.
Description
Technical Field
The invention relates to the technical field of low-lubrication nitride coatings, in particular to a preparation method and application of a wide-temperature-range self-lubricating MoN-VN multilayer coating, and belongs to the technical field of surface treatment.
Background
Under the wide temperature range environment, metal parts such as turbine blades of aero-engines and the like are easy to deform, so that the friction surfaces of the parts are seriously abraded, and the reliability and service life of space equipment are seriously reduced. Under the working condition of low temperature, the metal mechanical parts are lubricated mainly by using lubricating oil and solid lubricants such as molybdenum disulfide and carbon. However, as the service temperature increases, the lubricating grease is easily volatilized, molybdenum disulfide, carbon and the like are oxidized to form abrasive grains, and the excellent lubricating effect cannot be exerted. The hard nitride coating has good chemical stability and wear resistance, can play a good lubricating role in low-temperature and high-temperature environments, and is increasingly applied to reducing the frictional wear performance of parts. VN and MoN are subjected to oxidation reaction in the high-temperature friction process to generate an easily-sheared phase V2O5And MoO3And the lubricant can well play a role in lubrication in a high-temperature environment. However, since the general pure VN coating has a higher room temperature friction coefficient and a higher high temperature friction coefficient of the pure MoN coating, and cannot meet the requirement of wide temperature range lubricating performance, an improved technology is urgently needed to solve the problem existing in the prior art
Disclosure of Invention
The common methods for preparing the hard coating mainly comprise magnetron sputtering and arc ion plating, but because the surface of the coating prepared by the arc ion plating is rough, the wide-temperature-range self-lubricating MoN/VN multilayer coating is prepared by adopting a magnetron sputtering method. The method has low requirements, and the coating with small surface roughness and good bonding strength can be prepared at a lower temperature. The MoN/VN multilayer coating is prepared by using a non-equilibrium magnetron sputtering system, the preparation method can reduce the roughness of the coating, and the coating has great application prospect in the high-precision surface protection field of aeroengine turbine blades and the like.
The invention aims to provide a preparation method and application of a wide-temperature-range self-lubricating MoN-VN multilayer coating, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a wide-temperature-range self-lubricating MoN-VN multilayer coating comprises the following steps:
the method comprises the following steps: adopting a magnetron sputtering technology, selecting a Mo target and a V target, and depositing a MoN/VN multilayer coating on the surface of the pretreated substrate by using high-purity nitrogen as a working gas;
step two: carrying out ion etching on the surface of the matrix;
step three: firstly, depositing a Mo transition layer on the surface of the pretreated substrate, and then depositing a plurality of layers of coatings.
Preferably, the three steps are composed of alternating deposition of a plurality of coating layers MoN and VN, wherein the ratio of the thickness of the MoN layer to the VN layer is about 2: 1.
Preferably, the MoN layer and the VN layer in the multilayer coating in the third step are mainly in single crystal form respectively from the MoN phase and the VN phase.
Preferably, the friction coefficient of the multilayer coating in the third step is 0.32-0.4 at room temperature, the friction coefficient at a high temperature of 300 ℃ is 0.65-0.73, the friction coefficient at a high temperature of 500 ℃ is 0.55-0.59, and the friction coefficient at a high temperature of 700 ℃ is 0.28-0.32.
Preferably, the parameter settings of the Mo transition layer in step three are: mo target current of 3A, V target current of 0A, bias voltage of-70V, matrix rotation speed of 5rpm, and vacuum degree of cavity lower than 3.0 × 10-5Pa。
Preferably, the conditions required for depositing the MoN/VN multilayer coating in the first step include: is provided with a Mo targetThe current is 5A, the target current is 5A, the bias voltage is-50V, the rotating speeds of the substrates are 0.5rpm, 1.5rpm and 2.5rpm respectively, and the vacuum degree of the cavity is pumped to be lower than 3.0 multiplied by 10-5Pa。
Preferably, the material of the matrix in the second step comprises 718 high-temperature alloy steel and GH4169 alloy steel.
Compared with the prior art, the invention has the beneficial effects that:
the wide-temperature-range self-lubricating MoN/VN multilayer coating provided by the invention has long service life and good self-lubricating property in a high-temperature environment, can be used for matrix protection in a wide-temperature-range environment, and is simple and controllable in preparation process, and the wide-temperature-range self-lubricating property of the multilayer coating can be regulated and controlled by controlling the Mo target and the V target to be constant in current and regulating the substrate rotating speed and controlling the modulation period in the multilayer coating.
Drawings
FIG. 1 is a schematic structural view of the MoN/VN multilayer coating of example 1.
FIG. 2 is a TEM cross-sectional topography of the MoN/VN multilayer coating of example 1.
FIG. 3 is an XRD diffraction pattern of the MoN/VN multilayer coating of example 1.
FIG. 4 is a graph of the coefficient of friction of the MoN/VN multilayer coating of example 1 at various temperatures.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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 invention provides a technical scheme that: a preparation method of a wide-temperature-range self-lubricating MoN-VN multilayer coating comprises the following steps:
the method comprises the following steps: adopting a magnetron sputtering technology, selecting a Mo target and a V target, and depositing a MoN/VN multilayer coating on the surface of the pretreated substrate by using high-purity nitrogen as a working gas;
step two: carrying out ion etching on the surface of the matrix;
step three: firstly, depositing a Mo transition layer on the surface of the pretreated substrate, and then depositing a plurality of layers of coatings.
Further, the multilayer coating has a composition of alternating MoN and VN layers deposited, wherein the ratio of the MoN layers to the VN layer thickness is about 2: 1.
Further, in the multilayer coating, through adjusting the substrate rotating speed, MoN/VN multilayer coatings with different modulation cycles are prepared.
Further, the MoN layer and the VN layer in the multilayer coating mainly exist in a single crystal form from the MoN phase and the VN phase respectively.
In the embodiment of the invention, a multilayer structure with different modulation periods is formed by adopting the MoN layer and the VN layer, wherein the friction coefficient of the coating under a wide temperature range environment is obviously reduced by introducing a proper modulation period into the MoN/VN multilayer coating, for example, the friction coefficient of the MoN/VN multilayer coating with the modulation period of 22.66nm is respectively lower than the friction coefficient of the MoN/VN multilayer coating with the modulation period of 4.77nm by 20.2%, 10.9%, 6.79% and 9.36% under the conditions of room temperature, 300 ℃, 500 ℃ and 700 ℃.
In the embodiment of the invention, the friction coefficient of the MoN/VN multilayer coating with the modulation period of 22.66nm (the thickness of the MoN layer is 15.11nm, and the thickness of the VN layer is 7.55nm) in the multilayer coating is particularly good under four different temperature environments.
The multilayer coating provided by the embodiment of the invention has good wide-temperature-range self-lubricating property while ensuring the hardness, and can be used for matrix protection in a wide-temperature-range environment.
One aspect of the embodiments of the present invention provides a method for preparing the wide temperature range self-lubricating MoN/VN multilayer coating, including: and depositing the MoN/VN multilayer coating on the surface of the pretreated substrate by adopting a magnetron sputtering technology, selecting a Mo target and a V target, and taking high-purity nitrogen as a working gas.
Further, the preparation method can also comprise the following steps: firstly, depositing a Mo transition layer on the surface of the pretreated substrate, and then depositing the multilayer coating. The bonding force between the multilayer coating and the substrate can be improved by combining the Mo transition layer with the MoN/VN multilayer coating.
In some more specific embodiments, the preparation method comprises: the method comprises the steps of adopting a magnetron sputtering technology, respectively selecting two adjacent Mo targets and two adjacent V targets, taking high-purity nitrogen as working gas, depositing the MoN/VN multilayer coating on the surface of a cleaned substrate, controlling the currents of the Mo targets and the V targets to be unchanged, controlling the modulation in the multilayer coating by regulating and controlling the rotating speed of the substrate, and further researching the wide-temperature-range self-lubricating property of the multilayer coating.
Further, the pretreatment may include: and carrying out ion etching on the surface of the substrate.
As an implementation, the preprocessing may further include: cleaning to remove impurities such as oil stain and water on the surface of the substrate, wherein the cleaning method is not limited, and can comprise ultrasonic cleaning, for example; further, after the cleaning is completed, the surface of the substrate may be blow-dried with flowing nitrogen gas.
As an implementation, the preprocessing may further include: and etching and cleaning the surface of the substrate by utilizing a glow discharge principle before depositing the Mo transition layer and the MoN/VN multilayer coating so as to remove an oxide layer or pollutants on the surface of the substrate.
As an implementation, the preprocessing may further include: before the Mo transition layer and the MoN/VN multilayer coating are deposited, the magnetron sputtering cavity is vacuumized to the vacuum degree lower than 3.0 multiplied by 10-5Pa。
Further, in the preparation method, the conditions required for depositing and forming the Mo transition layer include: the Mo target current was set at 3A, the V target current at 0A, the bias at-70V, and the substrate rotation speed at 5 rpm.
Further, in the preparation method, the conditions required for depositing and forming the MoN/VN multilayer coating include: the Mo target current was set at 5A, the V target current at 5A, the bias voltage at-50V, and the substrate rotation speeds were set at 0.5rpm, 1.5rpm, and 2.5rpm, respectively.
In another aspect of an embodiment of the present invention, there is provided a device comprising a coating disposed on a substrate, the coating comprising any one of the wide temperature range self-lubricating MoN/VN multilayer coatings described above.
Further, the coating comprises a Mo transition layer and a wide-temperature-range self-lubricating MoN/VN multilayer coating which are sequentially arranged on the substrate.
Further, the material of the substrate includes, but is not limited to, high temperature alloys such as 718 high temperature alloy steel and GH4169 alloy steel.
The device may be an aircraft component or the like, such as an aircraft engine, but is not limited thereto.
The technical solution of the present invention will be explained in more detail with reference to several embodiments.
Example 1:
in this example, the base material was 718 high-temperature alloy steel. A magnetron sputtering technology is adopted to prepare a MoN/VN multilayer coating on the surface of a substrate, and the method mainly comprises the following steps:
(1) and (3) mechanically polishing the surface of the matrix, ultrasonically cleaning the surface of the matrix for 3 times by using petroleum ether, acetone and alcohol respectively, and then drying the surface of the matrix by using flowing nitrogen.
(2) Putting the cleaned substrate into a magnetron sputtering cavity, and vacuumizing until the vacuum degree is 3.0 multiplied by 10–5Pa; then, the target material is sputter cleaned for 120s, and the substrate sample is ion etched for 1800 s.
(3) Sputtering Mo target (purity is 99.99 at.%) for 600s, and depositing Mo transition layer on the surface of the substrate. The deposition parameters of the transition layer are as follows: the Mo target current was 3A, the V target current was 0A, the bias was-70V, and the substrate rotation speed was 5 rpm.
(4) Prepare a deposited MoN/VN multilayer coating.
High-purity nitrogen (with the purity of 99.99 at.%) is filled into the magnetron sputtering cavity, the flow rate is set to 30sccm, a Mo target (with the purity of 99.99 at.%) and a V target (with the purity of 99.99 at.%) are adopted to deposit the MoN/VN multilayer coating on the surface of the substrate, and the deposition parameters are as follows: the Mo target and the V target have the current of 5A, the Ag target current is regulated to be 1A, 1.5A and 2A respectively, the bias voltage is-50V, the matrix rotating speed is 0.5rpm, 1.5rpm and 2.5rpm respectively, the deposition time is 12000s, and 3 groups of MoN/VN multilayer coating samples with different modulation periods are prepared, wherein the specific parameters are shown in Table 1:
table 1: preparation parameter table of MoN/VN multilayer coating samples at substrate rotation speeds of 0.5rpm, 1.5rpm and 2.5rpm respectively
FIG. 1 is a schematic structural diagram of the obtained MoN/VN multilayer coating, and it can be seen that the multilayer coating is composed of two different phase structures of MoN and VN which are alternately deposited.
Fig. 2 is a TEM cross-sectional topography of the resulting MoN/VN multilayer coating from which the MoN and VN layer thicknesses of the multilayer thin film for three different modulation periods can be seen, fig. 2 (a) is a multilayer coating at a spin speed of 0.5rpm from which it can be seen that the ratio of the MoN and VN layer thicknesses is about 2: 1. The modulation period of the multilayer film gradually decreases as the rotation speed increases.
FIG. 3 is an XRD pattern at room temperature of the prepared MoN/VN multilayer coating sample, and it can be seen that the phase structures of the MoN/VN multilayer coatings with three different modulation periods are not very different.
FIG. 4 is a graph of the coefficient of friction of the obtained MoN/VN multilayer coating at different temperatures, and it can be seen that the MoN/VN multilayer coating shows lower coefficient of friction at four different temperatures at a modulation period of 22.66 nm. The MoN/VN multilayer coatings at this time had coefficients of friction of 0.32, 0.65, 0.55 and 0.28 at room temperature, 300 ℃, 500 ℃ and 700 ℃ test temperatures, respectively. All exhibit a low coefficient of friction.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A preparation method of a wide-temperature-range self-lubricating MoN-VN multilayer coating is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: adopting a magnetron sputtering technology, selecting a Mo target and a V target, and depositing a MoN/VN multilayer coating on the surface of the pretreated substrate by using high-purity nitrogen as a working gas;
step two: carrying out ion etching on the surface of the matrix;
step three: firstly, depositing a Mo transition layer on the surface of the pretreated substrate, and then depositing a plurality of layers of coatings.
2. The method for preparing the wide-temperature-range self-lubricating MoN-VN multilayer coating according to claim 1, wherein the wide-temperature-range self-lubricating MoN-VN multilayer coating comprises the following steps: the three steps are composed of alternately depositing a plurality of coating layers MoN and VN layers, wherein the thickness ratio of the MoN layers to the VN layers is about 2: 1.
3. The method for preparing the wide-temperature-range self-lubricating MoN-VN multilayer coating according to claim 1, wherein the wide-temperature-range self-lubricating MoN-VN multilayer coating comprises the following steps: in the third step, the MoN layer and the VN layer in the multilayer coating mainly exist in a single crystal form respectively from the MoN phase and the VN phase.
4. The method for preparing the wide-temperature-range self-lubricating MoN-VN multilayer coating according to claim 1, wherein the wide-temperature-range self-lubricating MoN-VN multilayer coating comprises the following steps: the friction coefficient of the multilayer coating in the third step is 0.32-0.4 at room temperature, the friction coefficient at high temperature of 300 ℃ is 0.65-0.73, the friction coefficient at high temperature of 500 ℃ is 0.55-0.59, and the friction coefficient at high temperature of 700 ℃ is 0.28-0.32.
5. The method for preparing the wide-temperature-range self-lubricating MoN-VN multilayer coating according to claim 1, wherein the wide-temperature-range self-lubricating MoN-VN multilayer coating comprises the following steps: the parameter setting of the Mo transition layer in the third step is as follows: mo target current of 3A, V target current of 0A, bias voltage of-70V, matrix rotation speed of 5rpm, and vacuum degree of cavity lower than 3.0 × 10-5Pa。
6. The method for preparing the wide-temperature-range self-lubricating MoN-VN multilayer coating according to claim 1, wherein the wide-temperature-range self-lubricating MoN-VN multilayer coating comprises the following steps: the conditions required for depositing and forming the MoN/VN multilayer coating in the first step comprise the following steps: setting Mo target current at 5A, V target current at 5A, bias voltage at-50V, substrate rotation speed at 0.5rpm, 1.5rpm and 2.5rpm, respectively, and pumping the vacuum degree of the cavity to be lower than 3.0 × 10-5Pa。
7. The method for preparing the wide-temperature-range self-lubricating MoN-VN multilayer coating according to claim 1, wherein the wide-temperature-range self-lubricating MoN-VN multilayer coating comprises the following steps: and in the second step, the material of the matrix comprises 718 high-temperature alloy steel and GH4169 alloy steel.
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Application publication date: 20200619 |