CN108866481B - Nano composite Al-Ti-V-Cu-N coating and preparation method and application thereof - Google Patents

Nano composite Al-Ti-V-Cu-N coating and preparation method and application thereof Download PDF

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CN108866481B
CN108866481B CN201810575978.9A CN201810575978A CN108866481B CN 108866481 B CN108866481 B CN 108866481B CN 201810575978 A CN201810575978 A CN 201810575978A CN 108866481 B CN108866481 B CN 108866481B
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CN108866481A (en
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王启民
梅海娟
张腾飞
王瑞
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Guangdong University of Technology
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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
    • C23C14/24—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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
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    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/347—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with layers adapted for cutting tools or wear applications

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Abstract

The invention belongs to the technical field of preparation of cutter coatings and surface protection coatings, and discloses a nano composite Al-Ti-V-Cu-N coating and a preparation method thereof. The coating comprises a Cr metal bonding layer, a CrN transition layer and an Al-Ti-V-Cu-N nano composite layer which are deposited on a substrate base body; the Al-Ti-V-Cu-N nano composite layer comprises the following elements in atomic percentage: 18-20 at.% of Al, 8-10 at.% of Ti, 10-12 at.% of V, 6-12 at.% of Cu, and 50-54 at.% of N. The invention can also deposit Al-Ti-V-Cu-N nano composite coatings with different element contents by freely adjusting the relative position of the substrate matrix and the splicing target and changing process parameters so as to meet different processing objects and cutting conditions, and has the advantages of strong controllability, simple process and the like.

Description

Nano composite Al-Ti-V-Cu-N 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 composite Al-Ti-V-Cu-N coating as well as a preparation method and application thereof.
Background
At present, arc ion plating and magnetron sputtering deposition are the mainstream PVD techniques for preparing cutter coatings. The arc ion plating technology has the advantages of high ion energy, high metal ionization rate, compact film layer, strong adhesive force and the like, but the prepared coating has poor surface quality and large stress in the film; the coating prepared by the magnetron sputtering deposition technology has a smooth and compact surface, no obvious holes and large particles, but low ionization rate, poor film-substrate binding force, uneven target etching and low utilization rate. With the continuous development of a novel coating preparation technology, a high-power pulse magnetron sputtering technology (HIPIMS) realizes high metal ionization rate by utilizing higher pulse peak power and lower pulse duty ratio, and has remarkable technical advantages in the aspects of obtaining excellent film-substrate binding force, reducing residual internal stress and the like. The HIPIMS technology integrates the advantages of magnetron sputtering low-temperature deposition, smooth surface, no particle defect, high ionization rate of arc ion plating metal, strong film-substrate binding force, compact coating and the like, and can prepare the hard coating with more excellent structure and performance.
With the development of modern high-speed cutting technology and difficult-to-machine materials, the conventional hard coating cutter can not meet the requirement of high-speed cutting machining. Particularly, as the hardness of hardened steel and high-strength steel is increased, diffusion wear and oxidation wear are increased due to increase of cutting force and increase of cutting temperature, and the coating is locally peeled off in a short time, resulting in rapid wear and failure of the tool coating.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention mainly aims to provide the nano composite Al-Ti-V-Cu-N coating, which greatly improves the high-temperature wear resistance of the hard coating and solves the problem of easy abrasion of the existing PVD hard coating cutter for cutting the difficult-to-machine materials at high speed.
The invention also aims to provide a preparation method of the nano composite Al-Ti-V-Cu-N coating.
The invention further aims to provide application of the nano composite Al-Ti-V-Cu-N coating.
The purpose of the invention is realized by the following technical scheme:
a nano composite Al-Ti-V-Cu-N coating comprises a substrate matrix, a Cr metal bonding layer, a CrN transition layer and an Al-Ti-V-Cu-N nano composite layer from bottom to top; wherein the Al-Ti-V-Cu-N nano composite layer comprises the following elements in atomic percentage: 18-20 at.% of Al, 8-10 at.% of Ti, 10-12 at.% of V, 6-12 at.% of Cu, and 50-54 at.% of N.
The thickness of the CrN transition layer is 100-500 nm, and the thickness of the Al-Ti-V-Cu-N nano composite layer is 0.5-1.5 mu m.
The substrate base body is a WC-Co hard alloy or a high-speed steel cutter base body.
The preparation method of the nano composite Al-Ti-V-Cu-N coating comprises the following steps:
(1) putting the polished substrate base body into an ultrasonic cleaning machine, sequentially and respectively carrying out ultrasonic cleaning for 10-20 min by using acetone and alcohol, then blowing the substrate base body to dry by using dry compressed air, fixing the substrate base body on a workpiece rotating frame in a coating cavity, adjusting the rotation speed of the workpiece rotating frame to be 2-5 rpm, enabling the base body to be opposite to the surface of a target material, keeping the target base distance to be 60-120 cm, starting a heater to heat to 100-300 ℃, pre-vacuumizing the base to be 1.0-5.0 multiplied by 10 and vacuumizing the base to be 1.0-5.0 multiplied by 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the air pressure to be 1.0-2.0 Pa, biasing the substrate to be-800-1000V, and carrying out glow sputtering cleaning on the cavity for 10-30 min;
(3) reducing the bias voltage of the matrix to-400 to-600V, adjusting the Ar gas pressure to 0.5 to 1.0Pa, opening a Cr arc target, adjusting the target current to 60 to 120A, bombarding the matrix with Cr ions at high energy for 3 to 5min, and activating the surface of the matrix to improve the film-substrate binding force to form a Cr metal bonding layer;
(4) reducing the bias voltage of the substrate to-50 to-200V, closing Ar and opening N2The air flow valve is used for adjusting the air pressure to be 0.5-1.0 Pa, and depositing is carried out for 3-15 min to obtain a CrN transition layer with the thickness of 100-500 nm so as to reduce the residual internal stress of the coating and improve the toughness;
(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, biasing the substrate to-50-200V, turning on a high-power pulse magnetron sputtering power supply, starting a splicing target Al-Ti-V-Cu, adjusting the target power to 0.5-3.0 kW, the target voltage to 600-900V, the pulse width to 50-250 mu s, the frequency to 160-500 Hz, and depositing for 100-300 min to obtain an Al-Ti-V-Cu-N nano composite layer with the thickness of 0.5-1.5 mu m according to the flow ratio of 1: 1-5: 1;
(6) after the deposition is finished, the target power supply and the bias power supply are turned off, and Ar and N are turned off2And 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.
And (5) the Al-Ti-V-Cu spliced target is a planar target formed by splicing an Al67Ti33 alloy target, a pure V target and a pure Cu target in a geometric shape.
The application of the nano composite Al-Ti-V-Cu-N coating in the fields of cutter cutting and surface protection coating.
The research of the invention finds that the lubricating phase V can form Ti-Al-V-N solid solution when added into the TiAlN coating, realizes the solid solution strengthening effect and effectively improves the hardness of the coating. On the other hand, the V can diffuse to the outer surface to realize the oxidation lubrication effect, and the wear resistance of the coating is improved. In addition, soft metal Cu can be added into the hard coating to form a nitride/soft metal amorphous phase nano composite structure, so that the crystal grain is refined, the hardness is improved, and a lower friction coefficient and higher wear resistance are obtained.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention organically combines the advantages of high-power pulse magnetron sputtering, can prepare the Al-Ti-V-Cu-N nano composite coating with good comprehensive performance, has smooth surface, high hardness and excellent high-temperature wear resistance, can greatly prolong the service life of the coated cutter during high-speed cutting, and has great application prospect in the fields of cutter cutting and surface protection coating;
(2) the Al-Ti-V-Cu-N nano composite coating with different element contents can be deposited by freely adjusting the relative position of the substrate matrix and the splicing target and changing the process parameters so as to meet different processing objects and cutting conditions, and the method has the advantages of strong controllability, simple process and the like.
Drawings
FIG. 1 is a schematic illustration of a spliced target in the example, in which the atomic percent of the AlTi alloy target is 67: 33;
FIG. 2 is a surface topography diagram of the Al-Ti-V-Cu-N nanocomposite coating in the embodiment with different duty ratios: (a) 1.6%, (b) 2%, (c) 3%, (d) 4%, (e) 5%;
FIG. 3 is a sectional view of the Al-Ti-V-Cu-N nanocomposite coating in the embodiment with different duty ratios: (a) 1.6%, (b) 2%, (c) 3%, (d) 4%, (e) 5%;
FIG. 4 is an XRD pattern of the Al-Ti-V-Cu-N nanocomposite coating at different duty ratios in the example;
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 spliced target Al-Ti-V-Cu used in the following examples is shown in FIG. 1, which is a planar target geometrically spliced from an Al67Ti33 alloy target, a pure V target, and a pure Cu target with the sample substrate facing the center of the V target.
Example 1:
(1) putting the polished substrate base body (WC-Co hard alloy) into an ultrasonic cleaning machine, sequentially and respectively carrying out ultrasonic cleaning for 15min by using acetone and alcohol, then drying the substrate base body by using dry compressed air, fixing the substrate base body on a workpiece rotating frame in a coating cavity, adjusting the rotation speed of the workpiece rotating frame to be 3rpm, enabling the base body to be opposite to the surface of a target material, keeping the target base distance to be 120cm, starting a heater to heat to 200 ℃, pre-vacuumizing the base to be 5.0 multiplied by 10 and vacuumizing the base to be 5.0 multiplied by 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the gas pressure to 1.8Pa, applying bias voltage to the substrate to 1000V, and carrying out glow sputtering cleaning on the cavity for 30 min;
(3) reducing the bias voltage of the substrate to-600V, adjusting the Ar gas pressure to 0.5Pa, opening a Cr arc target, adjusting the target current to 100A, bombarding the substrate with Cr ions at high energy for 5min, and activating the surface of the substrate to improve the film-substrate binding force to form a Cr metal bonding layer;
(4) reducing the substrate bias to-120V, turning off Ar, turning on N2The air flow valve is used for adjusting the air pressure to 0.5Pa, and depositing the CrN transition layer for 10min to obtain the CrN transition layer with the thickness of 400nm so as to reduce the residual internal stress of the coating and improve the toughness;
(5) closing the Cr arc target, and opening Ar and N2Gas flow valve, regulating Ar/N2Regulating the total air pressure to 0.6Pa, reducing the bias voltage of the matrix to-100V, starting a high-power pulse magnetron sputtering power supply, starting a spliced target Al-Ti-V-Cu, regulating the target power to 1.0kW, the target voltage to 800V, the pulse width to 100 mu s, the frequency to 160Hz, and depositing for 180min to obtain an Al-Ti-V-Cu-N nano composite layer with the thickness of 0.7 mu m;
(6) after the deposition is finished, the target power supply and the bias power supply are turned off, and Ar and N are turned off2The gas flow valve is opened to take out the sample after the temperature of the chamber is reduced to the room temperatureForming a coating film.
In this embodiment, the atomic percentage content of each element in the prepared Al-Ti-V-Cu-N nano composite layer is: 19.9 at.% Al, 9.9 at.% Ti, 10.3 at.% V, 6.2 at.% Cu, 53.7 at.% N.
FIG. 2 (a) and FIG. 3 (a) are surface and cross-sectional topography views of the nanocomposite Al-Ti-V-Cu-N coating, respectively, and it can be seen that the surface is relatively smooth, the cross-section is very dense, and the film-substrate interface is flat and smooth; FIG. 4 is an XRD pattern of the nanocomposite Al-Ti-V-Cu-N coating, forming a TiAlVN solid solution structure.
Example 2:
(1) putting the polished substrate base body (WC-Co hard alloy) into an ultrasonic cleaning machine, sequentially and respectively carrying out ultrasonic cleaning for 15min by using acetone and alcohol, then drying the substrate base body by using dry compressed air, fixing the substrate base body on a workpiece rotating frame in a coating cavity, adjusting the rotation speed of the workpiece rotating frame to be 3rpm, enabling the base body to be opposite to the surface of a target material, keeping the target base distance to be 120cm, starting a heater to heat to 200 ℃, pre-vacuumizing the base to be 5.0 multiplied by 10 and vacuumizing the base to be 5.0 multiplied by 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the gas pressure to 1.8Pa, applying bias voltage to the substrate to 1000V, and carrying out glow sputtering cleaning on the cavity for 30 min;
(3) reducing the bias voltage of the substrate to-600V, adjusting the Ar gas pressure to 0.5Pa, opening a Cr arc target, adjusting the target current to 100A, bombarding the substrate with Cr ions at high energy for 5min, and activating the surface of the substrate to improve the film-substrate binding force to form a Cr metal bonding layer;
(4) reducing the substrate bias to-120V, turning off Ar, turning on N2The air flow valve is used for adjusting the air pressure to 0.5Pa, and depositing the CrN transition layer for 10min to obtain the CrN transition layer with the thickness of 400nm so as to reduce the residual internal stress of the coating and improve the toughness;
(5) closing the Cr arc target, and opening Ar and N2Gas flow valve, regulating Ar/N2Regulating the total air pressure to 0.6Pa, reducing the bias voltage of the matrix to-100V, starting a high-power pulse magnetron sputtering power supply, starting a spliced target Al-Ti-V-Cu, regulating the target power to 1.0kW, the target voltage to 800V, the pulse width to 100 mu s, the frequency to 200Hz, and depositing for 180min to obtain an Al-Ti-V-Cu-N nano composite layer with the thickness of 0.9 mu m;
(6) after the deposition is finished, the target power supply and the bias power supply are turned off, and Ar and N are turned off2And 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.
In this embodiment, the atomic percentage content of each element in the prepared Al-Ti-V-Cu-N nano composite layer is: al 19.4 at.%, Ti 9.4 at.%, V11.6 at.%, Cu 7.9 at.%, N51.7 at.%.
FIG. 2 (b) and FIG. 3 (b) are surface and cross-sectional topography views of the nanocomposite Al-Ti-V-Cu-N coating, respectively, the surface is also relatively smooth, and the cross-section presents a relatively dense double-layer structure; in the XRD chart of fig. 4, in addition to the diffraction peak of the TiAlVN solid solution, the (111) peak of the weaker Cu simple substance appears.
Example 3:
(1) putting the polished substrate base body (WC-Co hard alloy) into an ultrasonic cleaning machine, sequentially and respectively carrying out ultrasonic cleaning for 15min by using acetone and alcohol, then drying the substrate base body by using dry compressed air, fixing the substrate base body on a workpiece rotating frame in a coating cavity, adjusting the rotation speed of the workpiece rotating frame to be 3rpm, enabling the base body to be opposite to the surface of a target material, keeping the target base distance to be 120cm, starting a heater to heat to 200 ℃, pre-vacuumizing the base to be 5.0 multiplied by 10 and vacuumizing the base to be 5.0 multiplied by 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the gas pressure to 1.8Pa, applying bias voltage to the substrate to 1000V, and carrying out glow sputtering cleaning on the cavity for 30 min;
(3) reducing the bias voltage of the substrate to-600V, adjusting the Ar gas pressure to 0.5Pa, opening a Cr arc target, adjusting the target current to 100A, bombarding the substrate with Cr ions at high energy for 5min, and activating the surface of the substrate to improve the film-substrate binding force to form a Cr metal bonding layer;
(4) reducing the substrate bias to-120V, turning off Ar, turning on N2The air flow valve is used for adjusting the air pressure to 0.5Pa, and depositing the CrN transition layer for 10min to obtain the CrN transition layer with the thickness of 400nm so as to reduce the residual internal stress of the coating and improve the toughness;
(5) closing the Cr arc target, and opening Ar and N2Gas flow valve, regulating Ar/N2The flow ratio is 4:1, the total air pressure is adjusted to 0.6Pa, the substrate bias voltage is reduced to-100V, the high-power pulse magnetron sputtering power supply is turned on, and the substrate is turned onSplicing a target Al-Ti-V-Cu, adjusting the target power to be 1.0kW, the target voltage to be 800V, the pulse width to be 100 mu s and the frequency to be 300Hz, and depositing for 180min to obtain an Al-Ti-V-Cu-N nano composite layer with the thickness of 1.0 mu m;
(6) after the deposition is finished, the target power supply and the bias power supply are turned off, and Ar and N are turned off2And 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.
In this embodiment, the atomic percentage content of each element in the prepared Al-Ti-V-Cu-N nano composite layer is: 19.4 at.% Al, 8.9 at.% Ti, 10.6 at.% V, 10.2 at.% Cu, and 50.9 at.% N.
FIG. 2 (c) and FIG. 3 (c) are surface and cross-sectional topography views of the nanocomposite Al-Ti-V-Cu-N coating, respectively, with increased surface particles and a cross-section exhibiting a micro-columnar crystal structure; in the XRD pattern of fig. 4, the (111) peak of the Cu simple substance is significantly enhanced, indicating that the content of Cu in the coating layer is increased.
Example 4:
(1) putting the polished substrate (high-speed steel cutter substrate) into an ultrasonic cleaning machine, sequentially and respectively carrying out ultrasonic cleaning for 15min by using acetone and alcohol, then drying the substrate by using dry compressed air, fixing the substrate on a workpiece rotating stand in a coating cavity, adjusting the rotation speed of the workpiece rotating stand to 3rpm to ensure that the substrate is just opposite to the surface of a target material, keeping the target base distance to be 120cm, starting a heater to heat to 200 ℃, pre-vacuumizing the base to 5.0 x 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the gas pressure to 1.8Pa, applying bias voltage to the substrate to 1000V, and carrying out glow sputtering cleaning on the cavity for 30 min;
(3) reducing the bias voltage of the substrate to-600V, adjusting the Ar gas pressure to 0.5Pa, opening a Cr arc target, adjusting the target current to 100A, bombarding the substrate with Cr ions at high energy for 5min, and activating the surface of the substrate to improve the film-substrate binding force to form a Cr metal bonding layer;
(4) reducing the substrate bias to-120V, turning off Ar, turning on N2The air flow valve is used for adjusting the air pressure to 0.5Pa, and depositing the CrN transition layer for 10min to obtain the CrN transition layer with the thickness of 400nm so as to reduce the residual internal stress of the coating and improve the toughness;
(5) closing the Cr arc target, and opening Ar and N2Gas flow valve, regulating Ar/N2Regulating the total air pressure to 0.6Pa, reducing the bias voltage of the matrix to-100V, starting a high-power pulse magnetron sputtering power supply, starting a spliced target Al-Ti-V-Cu, regulating the target power to 1.0kW, the target voltage to 800V, the pulse width to 100 mu s and the frequency to 400Hz, and depositing for 180min to obtain an Al-Ti-V-Cu-N nano composite layer with the thickness of 1.1 mu m;
(6) after the deposition is finished, the target power supply and the bias power supply are turned off, and Ar and N are turned off2And 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.
In this embodiment, the atomic percentage content of each element in the prepared Al-Ti-V-Cu-N nano composite layer is: 18.5 at.% Al, 8.1 at.% Ti, 11.2 at.% V, 10.7 at.% Cu, and 51.5 at.% N.
FIG. 2 (d) and FIG. 3 (d) are surface and cross-sectional topography views of the nanocomposite Al-Ti-V-Cu-N coating, respectively, the surface being relatively rough and the cross-section exhibiting a loose columnar crystal structure; in the XRD pattern of fig. 4, the intensity of the diffraction peak of the TiAlVN solid solution is reduced.
Example 5:
(1) putting the polished substrate (high-speed steel cutter substrate) into an ultrasonic cleaning machine, sequentially and respectively carrying out ultrasonic cleaning for 15min by using acetone and alcohol, then drying the substrate by using dry compressed air, fixing the substrate on a workpiece rotating stand in a coating cavity, adjusting the rotation speed of the workpiece rotating stand to 3rpm to ensure that the substrate is just opposite to the surface of a target material, keeping the target base distance to be 120cm, starting a heater to heat to 200 ℃, pre-vacuumizing the base to 5.0 x 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the gas pressure to 1.8Pa, applying bias voltage to the substrate to 1000V, and carrying out glow sputtering cleaning on the cavity for 30 min;
(3) reducing the bias voltage of the substrate to-600V, adjusting the Ar gas pressure to 0.5Pa, opening a Cr arc target, adjusting the target current to 100A, bombarding the substrate with Cr ions at high energy for 5min, and activating the surface of the substrate to improve the film-substrate binding force to form a Cr metal bonding layer;
(4) reducing the substrate bias to-120V, turning off Ar, turning on N2Adjusting the air pressure to 0.5Pa by using an air flow valve, and depositing a CrN transition layer for 10min to obtain a CrN transition layer with the thickness of 400nmThe CrN transition layer is used for reducing the residual internal stress of the coating and improving the toughness;
(5) closing the Cr arc target, and opening Ar and N2Gas flow valve, regulating Ar/N2Regulating the total air pressure to 0.6Pa, reducing the bias voltage of the matrix to-100V, starting a high-power pulse magnetron sputtering power supply, starting a spliced target Al-Ti-V-Cu, regulating the target power to 1.0kW, the target voltage to 800V, the pulse width to 100 mu s and the frequency to 500Hz, and depositing for 180min to obtain an Al-Ti-V-Cu-N nano composite layer with the thickness of 1.1 mu m;
(6) after the deposition is finished, the target power supply and the bias power supply are turned off, and Ar and N are turned off2And 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.
In this embodiment, the atomic percentage content of each element in the prepared Al-Ti-V-Cu-N nano composite layer is: al 17.9 at.%, Ti 8.3 at.%, V10.3 at.%, Cu 11.7 at.%, N51.8 at.%.
FIG. 2 (e) and FIG. 3 (e) are surface and cross-sectional topography views of the nanocomposite Al-Ti-V-Cu-N coating, respectively, with a relatively rough surface and a cross-section exhibiting a pronounced columnar grain structure; in the XRD pattern of fig. 4, the intensity of the diffraction peak of the TiAlVN solid solution is greatly reduced, and the (111) peak of the Cu simple substance is further enhanced, indicating that the content of Cu in the coating layer is further increased.
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 nano composite Al-Ti-V-Cu-N coating is characterized in that: the coating comprises a substrate matrix, a Cr metal bonding layer, a CrN transition layer and an Al-Ti-V-Cu-N nano composite layer from bottom to top; wherein the Al-Ti-V-Cu-N nano composite layer comprises the following elements in atomic percentage: 18-20 at.% of Al, 8-10 at.% of Ti, 10-12 at.% of V, 6-12 at.% of Cu, and 50-54 at.% of N.
2. The nanocomposite Al-Ti-V-Cu-N coating of claim 1, wherein: the thickness of the CrN transition layer is 100-500 nm, and the thickness of the Al-Ti-V-Cu-N nano composite layer is 0.5-1.5 mu m.
3. The nanocomposite Al-Ti-V-Cu-N coating of claim 1, wherein: the substrate base body is a WC-Co hard alloy or a high-speed steel cutter base body.
4. The method for preparing a nanocomposite Al-Ti-V-Cu-N coating according to claim 1, comprising the steps of:
(1) putting the polished substrate base body into an ultrasonic cleaning machine, sequentially and respectively carrying out ultrasonic cleaning for 10-20 min by using acetone and alcohol, then blowing the substrate base body to dry by using dry compressed air, fixing the substrate base body on a workpiece rotating frame in a coating cavity, adjusting the rotation speed of the workpiece rotating frame to be 2-5 rpm, enabling the base body to be opposite to the surface of a target material, keeping the target base distance to be 60-120 cm, starting a heater to heat to 100-300 ℃, pre-vacuumizing the base to be 1.0-5.0 multiplied by 10 and vacuumizing the base to be 1.0-5.0 multiplied by 10-3Pa；
(2) Opening an Ar gas flow valve, adjusting the air pressure to be 1.0-2.0 Pa, biasing the substrate to be-800-1000V, and carrying out glow sputtering cleaning on the cavity for 10-30 min;
(3) reducing the bias voltage of the matrix to-400 to-600V, adjusting the Ar gas pressure to 0.5 to 1.0Pa, opening a Cr arc target, adjusting the target current to 60 to 120A, bombarding the matrix with Cr ions at high energy for 3 to 5min, and activating the surface of the matrix to improve the film-substrate binding force to form a Cr metal bonding layer;
(4) reducing the bias voltage of the substrate to-50 to-200V, closing Ar and opening N2The air flow valve is used for adjusting the air pressure to be 0.5-1.0 Pa, and depositing is carried out for 3-15 min to obtain a CrN transition layer with the thickness of 100-500 nm so as to reduce the residual internal stress of the coating and improve the toughness;
(5) closing the Cr arc target, and opening Ar and N2Gas flow valve, regulating Ar/N2The flow ratio is 1: 1-5: 1, the total air pressure is adjusted to 0.5-1.0 Pa, the substrate is biased to-50 to-200V, a high-power pulse magnetron sputtering power supply is turned on, the spliced target Al-Ti-V-Cu is turned on, and the target power is adjusted0.5-3.0 kW, target voltage of 600-900V, pulse width of 50-250 mus and frequency of 160-500 Hz, and depositing for 100-300 min to obtain an Al-Ti-V-Cu-N nano composite layer with thickness of 0.5-1.5 mu m;
(6) after the deposition is finished, the target power supply and the bias power supply are turned off, and Ar and N are turned off2And 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: and (5) the Al-Ti-V-Cu spliced target is a planar target formed by splicing an Al67Ti33 alloy target, a pure V target and a pure Cu target in a geometric shape.
6. Use of a nanocomposite Al-Ti-V-Cu-N coating according to claim 1 in the field of tool cutting and surface protective coatings.
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