CN108930022B - Nano multilayer AlTiN/MoVCuN coating and preparation method and application thereof - Google Patents

Nano multilayer AlTiN/MoVCuN coating and preparation method and application thereof Download PDF

Info

Publication number
CN108930022B
CN108930022B CN201810576281.3A CN201810576281A CN108930022B CN 108930022 B CN108930022 B CN 108930022B CN 201810576281 A CN201810576281 A CN 201810576281A CN 108930022 B CN108930022 B CN 108930022B
Authority
CN
China
Prior art keywords
coating
altin
movcun
target
multilayer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201810576281.3A
Other languages
Chinese (zh)
Other versions
CN108930022A (en
Inventor
王启民
梅海娟
王瑞
张腾飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangdong University of Technology
Original Assignee
Guangdong University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangdong University of Technology filed Critical Guangdong University of Technology
Priority to CN201810576281.3A priority Critical patent/CN108930022B/en
Publication of CN108930022A publication Critical patent/CN108930022A/en
Application granted granted Critical
Publication of CN108930022B publication Critical patent/CN108930022B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • 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
    • 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
    • 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
    • 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
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)

Abstract

The invention belongs to the technical field of preparation of cutter coatings and surface protection coatings, and discloses a nano multilayer AlTiN/MoVCuN coating as well as a preparation method and application thereof. The coating comprises a substrate base body, a Cr bombardment implantation layer, a CrN transition layer and a nano multilayer AlTiN/MoVCuN coating from bottom to top; the nano multilayer AlTiN/MoVCuN coating is formed by alternately depositing an AlTiN intermediate layer and a MoVCuN intermediate layer with the modulation ratio of 3:2, and the modulation period is 0.6-2.4 nm. The invention designs the nano multilayer self-lubricating hard coating by combining the nano multilayer and the nano composite structure, and adopts the anode layer ion source assisted bipolar pulse magnetron sputtering deposition technology to prepare the multilayer multi-element nano composite coating which has the effects of smooth surface, compact structure and low friction coefficient self-lubricating.

Description

Nano multilayer AlTiN/MoVCuN coating and preparation method and application thereof
Technical Field
The invention belongs to the technical field of preparation of cutter coatings and surface protection coatings, and particularly relates to a nano multilayer AlTiN/MoVCuN coating as well as a preparation method and application thereof.
Background
By adding the reinforcing phase into the matrix phase and forming the ternary or multicomponent transition metal nitride coating by virtue of nano-compounding, the hardness, high-temperature oxidation resistance and other properties of the coating are improved, and the hard coating with good wear resistance is prepared. If the reinforced TiAlN coating is developed on the basis of a binary TiN coating, the hardness of the coating is greatly improved due to the solid solution strengthening effect of Al, and a compact layer of Al is easily formed on the surface of the TiAlN coating at high temperature2O3The protective film inhibits the internal diffusion of O and the external diffusion of Ti, thereby improving the high-temperature oxidation resistance and the wear resistance of the TiAlN coating. The lubricating phase is a material which improves the lubricity and wear resistance of the coating by reducing the friction coefficient between the self-lubricating coating and the friction pair-grinding pair. Oxides MoO of, for example, Mo and V3And V2O5Belongs to magneli phase oxides and has certain self-lubricating effect during friction. However, the low tribological properties of the MoN coatings are essentially limited to a temperature range below 500 ℃, due to MoO at high temperatures3Unstable oxide phaseAnd is liable to volatilization, resulting in a decrease in high-temperature wear resistance. And V2O5The melting point temperature of the alloy is lower between 670 ℃ and 685 ℃, and the wear resistance at high temperature is greatly reduced. In addition, a nitride/soft metal amorphous phase nano composite structure is formed by adding soft metal Cu into the hard coating, so that grain refinement and hardness improvement occur, and lower friction coefficient and better wear resistance are obtained, such as TiN-Cu, CrN-Cu and Mo-N/Cu.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention mainly aims to provide a nano multilayer AlTiN/MoVCuN coating which realizes a self-lubricating coating within a certain temperature range.
The invention further aims to provide a preparation method of the nano multilayer AlTiN/MoVCuN coating.
The invention further aims to provide application of the nano multilayer AlTiN/MoVCuN coating.
The purpose of the invention is realized by the following technical scheme:
a nanometer multilayer AlTiN/MoVCuN coating comprises a substrate base body, a Cr bombardment implantation layer, a CrN transition layer and a nanometer multilayer AlTiN/MoVCuN coating from bottom to top; the nano multilayer AlTiN/MoVCuN coating is formed by alternately depositing an AlTiN intermediate layer and a MoVCuN intermediate layer with the modulation ratio of 3:2, and the modulation period is 0.6-2.4 nm; the atomic percentage of each element in the nanometer multilayer AlTiN/MoVCuN coating is as follows: 10-11 at.% of Al, 6-7 at.% of Ti, 27-29 at.% of Mo, 5-6 at.% of V, 0.1-1 at.% of Cu, and 46-49 at.% of N.
The thickness of the CrN transition layer is 100-300 nm, and the thickness of the nano multilayer AlTiN/MoVCuN coating is 1.0-2.0 mu m.
The substrate base body is a hard alloy or high-speed steel cutter base body.
The preparation method of the nano multilayer AlTiN/MoVCuN coating comprises the following steps:
(1) fixing the pretreated substrate base body on a workpiece rotating stand in a coating cavity, enabling the base body to face the surface of a target material, enabling the target base distance to be 50-150 cm, and adjusting the rotation speed of the workpiece rotating stand to be 1-4 rpm, the revolution speed is 1-4 rpm, a heater is turned on, the temperature is raised to 100-300 ℃, and the pre-vacuumizing background is 1.0-5.0 × 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the air pressure to be 1.0-2.0 Pa, starting a direct current pulse bias power supply, adjusting the bias voltage of a matrix to-800-1000V, the duty ratio to be 40-80 percent and the frequency to be 40-80 kHz, and carrying out glow sputtering cleaning on the cavity for 10-30 min;
(3) reducing the bias voltage of the substrate to-600 to-800V, adjusting the Ar gas pressure to 0.5 to 1.0Pa, opening a Cr arc target, adjusting the target current to 60 to 120A, and bombarding the substrate with Cr ions for 1 to 3min at high energy to generate a Cr bombardment implantation layer;
(4) reducing the bias voltage of the substrate to-50 to-250V, closing Ar and opening N2The air flow valve is used for adjusting the air pressure to 0.5-1.0 Pa, and depositing for 3-9 min to obtain a CrN transition layer;
(5) closing the Cr arc target, and opening Ar and N2Gas flow valve, regulating Ar/N2Adjusting the total air pressure to 0.5-1.0 Pa, the substrate bias to-50-250V, adjusting the anode layer ion source power to 0.5-2.0 kW, simultaneously opening bipolar pulse magnetron sputtering alloy target AlTi and splicing target Mo-V-Cu, adjusting the target power to 1.0-4.0 kW, the frequency to 40-80 kHz, the duty ratio to 25-75%, depositing for 300-600 min, and alternately depositing an AlTiN intermediate layer and a MoVCuN intermediate layer on a CrN transition layer through the revolution of a turntable to form a nano multilayer AlTiN/MoVCuN coating;
(6) after deposition is finished, turning off the ion source power supply, the target power supply and the bias power supply, and turning off Ar and N2And the gas flow valve is opened to take out the sample after the temperature of the chamber is reduced to room temperature, and coating is finished.
The atomic ratio of the alloy target AlTi in the step (5) is 67: 33; the spliced target Mo-V-Cu is a planar target formed by splicing a pure Mo target, a pure V target and a pure Cu target in a geometric shape.
The nano multilayer AlTiN/MoVCuN coating is applied to the fields of cutter cutting and surface protection coating.
The invention designs the nano multilayer self-lubricating coating by combining the nano multilayer and the nano composite structure, and prepares the nano multilayer coating by adopting ion source assisted bipolar pulse magnetron sputtering alternate deposition, thereby realizing the low-friction self-lubricating coating in a certain temperature range.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the invention designs a multi-layer multi-element nano composite coating by combining a nano multilayer and a nano composite structure, adopts an anode layer ion source assisted bipolar pulse magnetron sputtering deposition technology, deposits nano multilayer AlTiN/MoVCuN coatings with different element contents and good comprehensive performance by freely adjusting the relative position of a substrate matrix and a splicing target and changing process parameters, has smooth surface and compact structure, and realizes a low-friction self-lubricating coating in a certain temperature range.
Drawings
FIG. 1 is a schematic diagram of anode layer ion source assisted bipolar pulse magnetron sputtering alternate deposition of nano multilayer coating AlTiN/MoVCuN;
FIG. 2 is a schematic diagram of the target base distance of the MoVCuN planar splicing target and the sample position in the horizontal and vertical directions in the example;
FIG. 3 is a surface and cross-sectional profile of the nano-multilayer AlTiN/MoVCuN coating in the example: (a) revolution speed 1rpm, (b), (f) revolution speed 2rpm, (c), (j) revolution speed 3rpm, (d) and (h) revolution speed 4 rpm;
FIG. 4 is a graph showing the variation of the binding force of the nano multi-layered AlTiN/MoVCuN coating with the revolution speed of the turntable in the embodiment;
FIG. 5 is a friction curve diagram of the nano multilayer AlTiN/MoVCuN coating and a friction pair SiC ball at normal temperature in the embodiment.
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.
The schematic diagram of the following example of depositing nano multilayer coating AlTiN/movcu alternately by anode layer ion source assisted bipolar pulse magnetron sputtering is shown in fig. 1; in the embodiment, a schematic diagram of the target base distance between the spliced target Mo-V-Cu (a planar target formed by splicing a pure Mo target, a pure V target and a pure Cu target in a geometric shape) and the position of a sample in the horizontal and vertical directions is shown in FIG. 2; the structural schematic diagram of the obtained nano multilayer AlTiN/MoVCuN coating is shown in figure 3.
Example 1:
a nanometer multilayer AlTiN/MoVCuN coating comprises a substrate base body, a Cr bombardment implantation layer, a CrN transition layer and a nanometer multilayer AlTiN/MoVCuN coating from bottom to top; the nano multilayer AlTiN/MoVCuN coating is formed by alternately depositing an AlTiN intermediate layer and a MoVCuN intermediate layer with the modulation ratio of 3:2, and the modulation period is 0.6-2.4 nm; the atomic percentage of each element in the nano multilayer AlTiN/MoVCuN coating is as follows: al 10.6 at.%, Ti 7.0 at.%, Mo 28.8 at.%, v5.8 at.%, Cu 1.4 at.%, N46.4 at.%.
The preparation method comprises the following steps:
(1) fixing the pretreated substrate base body on a workpiece rotating frame in a coating cavity, enabling the base body to face the surface of a target material, enabling the distance between the target base and the base to be 120cm, adjusting the rotation speed of the rotating frame to be 3rpm and the revolution speed to be 1rpm, turning on a heater, heating to 200 ℃, and pre-vacuumizing to the background vacuum of 5.0 × 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the air pressure to 1.8Pa, starting a direct current pulse bias power supply, adjusting the bias voltage of a matrix to-1000V, adjusting the duty ratio to 40 percent and the frequency to 80kHz, and carrying out glow sputtering cleaning on the cavity for 15 min;
(3) reducing the bias voltage of the substrate to-800V, adjusting the Ar gas pressure to 0.5Pa, opening a Cr arc target, adjusting the target current to 100A, and bombarding the substrate with Cr ions for 2min at high energy to form a Cr bombardment implantation layer;
(4) reducing the substrate bias to-150V, turning off Ar, turning on N2The air flow valve is used for adjusting the air pressure to 0.5Pa, and depositing is carried out for 5min to obtain a CrN transition layer with the thickness of 200 nm;
(5) closing the Cr arc target, and opening Ar and N2Gas flow valve, regulating Ar/N2The flow ratio is 3.5:1, the total air pressure is adjusted to 0.5Pa, the matrix bias voltage is-150V, the anode layer ion source power is adjusted to 0.6kW, meanwhile, the bipolar pulse magnetron sputtering columnar alloy target AlTi and the planar splicing target Mo-V-Cu are opened, the target power is adjusted to 1.5kW, the frequency is 40kHz, the duty ratio is 50 percent, the deposition is carried out for 500min, and the AlTiN intermediate layer and the MoVCuN are alternately deposited on the CrN transition layer through the revolution of a turntableThe interlayer forms a nano multilayer AlTiN/MoVCuN coating with the thickness of 1.3 mu m;
(6) after deposition is finished, turning off the ion source power supply, the target power supply and the bias power supply, and turning off Ar and N2And the gas flow valve is opened to take out the sample after the temperature of the chamber is reduced to room temperature, and coating is finished.
FIGS. 3 (a) and (e) are respectively a surface and cross-sectional profile of the nano-multilayer AlTiN/MoVCuN coating prepared by the process parameters of the present embodiment, which shows that the surface of the coating is smooth and flat, and the cross-section presents a micro-columnar crystal structure; the nano multilayer AlTiN/AlTiVCuN coating prepared by the embodiment in the figure 4 has the bonding force reaching the maximum value of 135N and shows excellent film-based bonding force; the nano-multilayer AlTiN/AlTiVCuN coating prepared in this example in fig. 5 had an average coefficient of friction of 0.57.
Example 2:
a nanometer multilayer AlTiN/MoVCuN coating comprises a substrate base body, a Cr bombardment implantation layer, a CrN transition layer and a nanometer multilayer AlTiN/MoVCuN coating from bottom to top; the nano multilayer AlTiN/MoVCuN coating is formed by alternately depositing an AlTiN intermediate layer and a MoVCuN intermediate layer with the modulation ratio of 3:2, and the modulation period is 0.6-2.4 nm; the atomic percentage of each element in the nano multilayer AlTiN/MoVCuN coating is as follows: al 10.9 at.%, Ti 6.7 at.%, Mo 29.2 at.%, v5.6 at.%, Cu 1.0 at.%, N46.6 at.%.
The preparation method comprises the following steps:
(1) fixing the pretreated substrate base body on a workpiece rotating frame in a coating cavity, enabling the base body to face the surface of a target material, enabling the distance between the target base and the base to be 120cm, adjusting the rotation speed of the rotating frame to be 3rpm and the revolution speed to be 2rpm, turning on a heater, heating to 200 ℃, and pre-vacuumizing to the background vacuum of 5.0 × 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the air pressure to 1.8Pa, starting a direct current pulse bias power supply, adjusting the bias voltage of a matrix to-1000V, adjusting the duty ratio to 40 percent and the frequency to 80kHz, and carrying out glow sputtering cleaning on the cavity for 15 min;
(3) reducing the bias voltage of the substrate to-800V, adjusting the Ar gas pressure to 0.5Pa, opening a Cr arc target, adjusting the target current to 100A, and bombarding the substrate with Cr ions for 2min at high energy to form a Cr bombardment implantation layer;
(4) reducing the substrate bias to-150V, turning off Ar, turning on N2The air flow valve is used for adjusting the air pressure to 0.5Pa, and depositing is carried out for 5min to obtain a CrN transition layer with the thickness of 200 nm;
(5) closing the Cr arc target, and opening Ar and N2Gas flow valve, regulating Ar/N2The flow ratio is 3.5:1, the total air pressure is adjusted to 0.5Pa, the matrix bias voltage is-150V, the anode layer ion source power is adjusted to 0.6kW, meanwhile, a bipolar pulse magnetron sputtering columnar alloy target AlTi and a planar splicing target Mo-V-Cu are opened, the target power is adjusted to 1.5kW, the frequency is 40kHz, the duty ratio is 50 percent, the deposition is carried out for 500min, and an AlTiN intermediate layer and a MoVCuN intermediate layer are alternately deposited on a CrN transition layer through the revolution of a turntable to form a nano multilayer AlTiN/MoVCuN coating with the thickness of 1.4 mu m;
(6) after deposition is finished, turning off the ion source power supply, the target power supply and the bias power supply, and turning off Ar and N2And the gas flow valve is opened to take out the sample after the temperature of the chamber is reduced to room temperature, and coating is finished.
FIGS. 3 (b) and (f) are the surface and cross-sectional profiles of the nano-multilayer AlTiN/MoVCuN coating prepared by the process parameters of the present example, respectively, wherein the cross section shows a relatively dense structure; the bonding force of the nano multilayer AlTiN/AlTiVCuN coating prepared by the embodiment in the figure 4 reaches the minimum value of 66N; the friction coefficient of the nano-multilayer AlTiN/AlTiVCuN coating prepared by the embodiment in FIG. 5 is reduced.
Example 3:
a nanometer multilayer AlTiN/MoVCuN coating comprises a substrate base body, a Cr bombardment implantation layer, a CrN transition layer and a nanometer multilayer AlTiN/MoVCuN coating from bottom to top; the nano multilayer AlTiN/MoVCuN coating is formed by alternately depositing an AlTiN intermediate layer and a MoVCuN intermediate layer with the modulation ratio of 3:2, and the modulation period is 0.6-2.4 nm; the atomic percentage of each element in the nano multilayer AlTiN/MoVCuN coating is as follows: al 11.4 at.%, Ti 6.7 at.%, Mo 27.3 at.%, v5.8 at.%, Cu 0.4 at.%, N48.4 at.%.
The preparation method comprises the following steps:
(1) fixing the pretreated substrate matrix on a workpiece rotating stand in a coating chamber to ensure that the matrix is opposite to the surface of the target material,the distance between the target base and the target base is 120cm, the autorotation speed of the rotating frame is adjusted to be 3rpm, the revolution speed is adjusted to be 3rpm, the heater is switched on, the temperature is raised to 200 ℃, and the background vacuum is pre-pumped to 5.0 × 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the air pressure to 1.8Pa, starting a direct current pulse bias power supply, adjusting the bias voltage of a matrix to-1000V, adjusting the duty ratio to 40 percent and the frequency to 80kHz, and carrying out glow sputtering cleaning on the cavity for 15 min;
(3) reducing the bias voltage of the substrate to-800V, adjusting the Ar gas pressure to 0.5Pa, opening a Cr arc target, adjusting the target current to 100A, and bombarding the substrate with Cr ions for 2min at high energy to form a Cr bombardment implantation layer;
(4) reducing the substrate bias to-150V, turning off Ar, turning on N2The air flow valve is used for adjusting the air pressure to 0.5Pa, and depositing is carried out for 5min to obtain a CrN transition layer with the thickness of 200 nm;
(5) closing the Cr arc target, and opening Ar and N2Gas flow valve, regulating Ar/N2The flow ratio is 3.5:1, the total air pressure is adjusted to 0.5Pa, the matrix bias voltage is-150V, the anode layer ion source power is adjusted to 0.6kW, meanwhile, a bipolar pulse magnetron sputtering columnar alloy target AlTi and a planar splicing target Mo-V-Cu are opened, the target power is adjusted to 1.5kW, the frequency is 40kHz, the duty ratio is 50 percent, the deposition is carried out for 500min, and an AlTiN intermediate layer and a MoVCuN intermediate layer are alternately deposited on a CrN transition layer through the revolution of a turntable to form a nano multilayer AlTiN/MoVCuN coating with the thickness of 1.3 mu m;
(6) after deposition is finished, turning off the ion source power supply, the target power supply and the bias power supply, and turning off Ar and N2And the gas flow valve is opened to take out the sample after the temperature of the chamber is reduced to room temperature, and coating is finished.
FIGS. 3 (c) and (j) are the surface and cross-sectional topography diagrams of the nano-multilayer AlTiN/MoVCuN coating prepared by the process parameters of the present embodiment, respectively, which has a compact cross-section and a structure without obvious features; the bonding force of the nano multilayer AlTiN/AlTiVCuN coating prepared by the embodiment in the figure 4 is improved compared with that of the coating prepared by the embodiment 2; the average friction coefficient of the nano multilayer AlTiN/AlTiVCuN coating prepared by the embodiment in the figure 5 reaches a minimum of 0.47.
Example 4:
a nanometer multilayer AlTiN/MoVCuN coating comprises a substrate base body, a Cr bombardment implantation layer, a CrN transition layer and a nanometer multilayer AlTiN/MoVCuN coating from bottom to top; the nano multilayer AlTiN/MoVCuN coating is formed by alternately depositing an AlTiN intermediate layer and a MoVCuN intermediate layer with the modulation ratio of 3:2, and the modulation period is 0.6-2.4 nm; the atomic percentage of each element in the nano multilayer AlTiN/MoVCuN coating is as follows: al 10.4 at.%, Ti 7.1 at.%, Mo 27.6 at.%, v5.7 at.%, Cu 0.5 at.%, N48.7 at.%.
The preparation method comprises the following steps:
(1) fixing the pretreated substrate base body on a workpiece rotating frame in a coating cavity, enabling the base body to face the surface of a target material, enabling the distance between the target base and the base to be 120cm, adjusting the rotation speed of the rotating frame to be 3rpm and the revolution speed to be 4rpm, turning on a heater, heating to 200 ℃, and pre-vacuumizing to the background vacuum of 5.0 × 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the air pressure to 1.8Pa, starting a direct current pulse bias power supply, adjusting the bias voltage of a matrix to-1000V, adjusting the duty ratio to 40 percent and the frequency to 80kHz, and carrying out glow sputtering cleaning on the cavity for 15 min;
(3) reducing the bias voltage of the substrate to-800V, adjusting the Ar gas pressure to 0.5Pa, opening a Cr arc target, adjusting the target current to 100A, and bombarding the substrate with Cr ions for 2min at high energy to form a Cr bombardment implantation layer;
(4) reducing the substrate bias to-150V, turning off Ar, turning on N2The air flow valve is used for adjusting the air pressure to 0.5Pa, and depositing is carried out for 5min to obtain a CrN transition layer with the thickness of 200 nm;
(5) closing the Cr arc target, and opening Ar and N2Gas flow valve, regulating Ar/N2The flow ratio is 3.5:1, the total air pressure is adjusted to 0.5Pa, the matrix bias voltage is-150V, the anode layer ion source power is adjusted to 0.6kW, meanwhile, a bipolar pulse magnetron sputtering columnar alloy target AlTi and a planar splicing target Mo-V-Cu are opened, the target power is adjusted to 1.5kW, the frequency is 40kHz, the duty ratio is 50 percent, the deposition is carried out for 500min, and an AlTiN intermediate layer and a MoVCuN intermediate layer are alternately deposited on a CrN transition layer through the revolution of a turntable to form a nano multilayer AlTiN/MoVCuN coating with the thickness of 1.4 mu m;
(6) after deposition is finished, turning off the ion source power supply, the target power supply and the bias power supply, and turning off Ar and N2A gas flow valve, which can be opened after the temperature of the chamber is reduced to room temperatureAnd taking out the sample through the door to finish film coating.
FIGS. 3 (d) and (h) are the surface and cross-sectional profiles of the nano-multilayer AlTiN/MoVCuN coating prepared by the process parameters of the present example, respectively, and the cross section is also denser; the nano multilayer AlTiN/AlTiVCuN coating prepared by the embodiment in the figure 4 has the bonding force reaching 106N and better film-substrate bonding force; the friction coefficient of the nano-multilayer AlTiN/AlTiVCuN coating prepared by the embodiment in FIG. 5 is also lower.
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 (6)

1. A nanometer multilayer AlTiN/MoVCuN coating is characterized in that: the coating comprises a substrate base body, a Cr bombardment implantation layer, a CrN transition layer and a nano multilayer AlTiN/MoVCuN coating from bottom to top; the nano multilayer AlTiN/MoVCuN coating is formed by alternately depositing an AlTiN intermediate layer and a MoVCuN intermediate layer with the modulation ratio of 3:2, and the modulation period is 0.6-2.4 nm; the nanometer multilayer AlTiN/MoVCuN coating comprises the following elements in percentage by atom: 10-11 at.% of Al, 6-7 at.% of Ti, 27-29 at.% of Mo, 5-6 at.% of V, 0.1-1 at.% of Cu, and 46-49 at.% of N.
2. The nano-multilayer AlTiN/movcu coating of claim 1, wherein: the thickness of the CrN transition layer is 100-300 nm, and the thickness of the nano multilayer AlTiN/MoVCuN coating is 1.0-2.0 mu m.
3. The nano-multilayer AlTiN/movcu coating of claim 1, wherein: the substrate base body is a hard alloy or high-speed steel cutter base body.
4. The method for preparing nano multilayer AlTiN/MoVCuN coating according to claim 1, characterized by comprising the following steps:
(1) fixing the pretreated substrate base body on a workpiece rotating frame in a coating cavity, enabling the base body to face the surface of a target material, enabling the distance between the target base and the target to be 50-150 cm, adjusting the rotation speed of the workpiece rotating frame to be 1-4 rpm and the revolution speed to be 1-4 rpm, turning on a heater, heating to 100-300 ℃, pre-vacuumizing to the background vacuum of 1.0-5.0 × 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the air pressure to be 1.0-2.0 Pa, starting a direct current pulse bias power supply, adjusting the bias voltage of a matrix to-800-1000V, the duty ratio to be 40-80 percent and the frequency to be 40-80 kHz, and carrying out glow sputtering cleaning on the cavity for 10-30 min;
(3) reducing the bias voltage of the substrate to-600 to-800V, adjusting the Ar gas pressure to 0.5 to 1.0Pa, opening a Cr arc target, adjusting the target current to 60 to 120A, and bombarding the substrate with Cr ions for 1 to 3min at high energy to generate a Cr bombardment implantation layer;
(4) reducing the bias voltage of the substrate to-50 to-250V, closing Ar and opening N2The air flow valve is used for adjusting the air pressure to 0.5-1.0 Pa, and depositing for 3-9 min to obtain a CrN transition layer with the thickness of 100-300 nm;
(5) closing the Cr arc target, and opening Ar and N2Gas flow valve, regulating Ar/N2Adjusting the total air pressure to 0.5-1.0 Pa, the substrate bias to-50-250V, adjusting the anode layer ion source power to 0.5-2.0 kW, simultaneously opening bipolar pulse magnetron sputtering alloy target AlTi and splicing target Mo-V-Cu, adjusting the target power to 1.0-4.0 kW, the frequency to 40-80 kHz, the duty ratio to 25-75%, depositing for 300-600 min, and alternately depositing an AlTiN intermediate layer and a MoVCuN intermediate layer on a CrN transition layer through the revolution of a turntable to form a nano multilayer AlTiN/MoVCuN coating;
(6) after deposition is finished, turning off the ion source power supply, the target power supply and the bias power supply, and turning off Ar and N2And the gas flow valve is opened to take out the sample after the temperature of the chamber is reduced to room temperature, and coating is finished.
5. The method of claim 4, wherein: the atomic ratio of the alloy target AlTi in the step (5) is 67: 33; the spliced target Mo-V-Cu is a planar target formed by splicing a pure Mo target, a pure V target and a pure Cu target in a geometric shape.
6. Use of a nanolayered multilayer AlTiN/movcu coating according to claim 1 in the field of tool cutting and surface protective coatings.
CN201810576281.3A 2018-06-06 2018-06-06 Nano multilayer AlTiN/MoVCuN coating and preparation method and application thereof Active CN108930022B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810576281.3A CN108930022B (en) 2018-06-06 2018-06-06 Nano multilayer AlTiN/MoVCuN coating and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810576281.3A CN108930022B (en) 2018-06-06 2018-06-06 Nano multilayer AlTiN/MoVCuN coating and preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN108930022A CN108930022A (en) 2018-12-04
CN108930022B true CN108930022B (en) 2020-07-28

Family

ID=64449486

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810576281.3A Active CN108930022B (en) 2018-06-06 2018-06-06 Nano multilayer AlTiN/MoVCuN coating and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN108930022B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111962029A (en) * 2020-08-14 2020-11-20 中国科学院宁波材料技术与工程研究所 High-temperature self-lubricating (Cr, V)2AlC MAX phase coating and preparation method and application thereof
CN112853261A (en) * 2020-12-15 2021-05-28 东南大学 Temperature self-adaptive lubricating bearing and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107034465A (en) * 2009-02-27 2017-08-11 欧瑞康表面解决方案股份公司，普费菲孔 Coating systems and the painting method for manufacturing coating systems

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103469154B (en) * 2013-09-05 2016-01-20 江西稀有稀土金属钨业集团有限公司 A kind of TiAlN compound coating and be provided with the preparation method of cutter of this coating
CN107604329A (en) * 2017-08-11 2018-01-19 广东工业大学 A kind of wear-resistant self-lubricating Mo Cu V N composite coatings and its preparation method and application

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107034465A (en) * 2009-02-27 2017-08-11 欧瑞康表面解决方案股份公司，普费菲孔 Coating systems and the painting method for manufacturing coating systems

Also Published As

Publication number Publication date
CN108930022A (en) 2018-12-04

Similar Documents

Publication Publication Date Title
CN108866480B (en) Multilayer multi-element nano composite self-lubricating hard coating and preparation method and application thereof
CN102011090B (en) TiAlN/TiAlCN multilayer coating of substrate surface and preparing method thereof
CN103273687B (en) TiSiN+ZrSiN composite nanometer coated cutting tool and preparation method thereof
CN108396292A (en) A kind of die casting composite coating and preparation method thereof
CN105112858B (en) A kind of nano combined cutter coat of sandwich construction
CN107130213B (en) Multicomponent alloy laminated film Preparation equipment and preparation method
CN109295425B (en) Cr/CrN/CrAlSiN/CrAlTiSiN nano multilayer gradient film and preparation method thereof
CN109207938B (en) Ti/TiN/TiAlSiN/TiAlCrSiN nano multilayer gradient film and preparation method thereof
CN102115883B (en) Surface compound strengthening process for aluminum alloy material
CN103160781B (en) Manufacture method of multilayer gradient nano-composite diamond film of surface of die steel
CN108930021B (en) Nano multilayer AlTiN/AlTiVCuN coating and preparation method and application thereof
WO2019072084A1 (en) Hard composite coating with high temperature resistance and method for preparing same, and coated tool
CN103143761B (en) AlTiN-MoN nano multi-layer composite coating milling cutter and preparation method thereof
CN108930022B (en) Nano multilayer AlTiN/MoVCuN coating and preparation method and application thereof
CN108517487B (en) TiAlN/W with high hardness and high wear resistance2N-multilayer coating and method for producing same
CN103789726B (en) AlTiCrN/MoN nano laminated coating being firmly combined with tool surfaces and preparation method thereof
CN101698362A (en) Self-lubricating hard nanocomposite laminated coating and preparation method thereof
CN110129741A (en) A kind of polynary nanometer laminated coating cutter and preparation method thereof
CN106567074A (en) Preparation method for AlTiSiN-AlCrSiN nanocrystalline-amorphous multilayer composite coating
CN107740053B (en) A kind of AlCrSiN/VSiN nano laminated coating and preparation method thereof
CN108866481B (en) Nano composite Al-Ti-V-Cu-N coating and preparation method and application thereof
CN110670029A (en) High-hardness wear-resistant TiN/TiAlSiN composite coating on surface of aluminum alloy and preparation method thereof
CN104278235B (en) Cutter with titanium nitride ceramic membrane and preparation method of cutter
CN106676470B (en) A kind of AlTiON hot die steel complex gradient coating and preparation method thereof
CN107190229A (en) A kind of self-assembled nanometer oxynitride high-temperaure coating and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant