CN111926292A - Composite coating and preparation method and application thereof - Google Patents
Composite coating and preparation method and application thereof Download PDFInfo
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- CN111926292A CN111926292A CN202010942973.2A CN202010942973A CN111926292A CN 111926292 A CN111926292 A CN 111926292A CN 202010942973 A CN202010942973 A CN 202010942973A CN 111926292 A CN111926292 A CN 111926292A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0617—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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Abstract
The invention relates to the technical field of protective coatings, in particular to a composite coating and a preparation method and application thereof. The composite coating provided by the invention comprises a TiN layer, an AlTiN layer, an AlTiSiN layer and a V-doped AlTiSiN layer which are sequentially stacked. According to the description of the embodiment, the hardness of the composite coating can reach 47.3GPa at most, and can be kept above 40GPa even if the annealing treatment is carried out in air at 900 ℃ for 30 min. Therefore, the composite coating can meet the requirement of working in a complex high-speed cutting environment.
Description
Technical Field
The invention relates to the technical field of protective coatings, in particular to a composite coating and a preparation method and application thereof.
Background
With the continuous development of the machining industry, the cutting tool not only needs to meet the requirements of high strength, long service life, high cutting and feeding speed, but also needs to be suitable for high-automation production. In addition, in consideration of small environmental pollution, green cutting such as high-speed cutting, dry cutting and micro-lubrication cutting increasingly becomes the mainstream of the development of cutting technology, which puts higher requirements on the development of the cutting tool. At present, the tool coating is also developed from the original single TiN and NbN film into NbSiN, TiSiN and other nano composite coatings and TiN/AlN, TiN/NbN and other nano multilayer coating structures, so that the comprehensive performance of the film tool is improved to a great extent.
The nano composite coating is a three-dimensional network structure coating formed by two materials, wherein an interface phase wraps a matrix phase, and the forming materials can be in a nano crystal/nano crystal form or a nano crystal/amorphous form. A large number of scientists research and explore the film and obtain a lot of results: for example, Chinese patent with application number of 201611164439.3 discloses a Ti-Ag-N nano composite coating and a preparation method thereof, which aims to solve the technical problem of nc-TiN/a-Si3N4The high friction coefficient of the nano composite coating causes a large amount of heat to be generated in the cutting process, and the front cutter face of the coated cutter still generates built-up edges. The nano composite coating of the invention: according to the distance from the matrix, the composite material sequentially comprises the following components from inside to outside: a transition layer formed by a Ti film on the surface of the substrate, an intermediate layer formed by a TiN film and a Ti-Ag-N layer. The preparation method is completed by adopting an arc ion plating technology, and the nano composite coating prepared by the method has the advantages of high hardness, high coating toughness, strong film-substrate bonding, small friction coefficient and the like. The Chinese patent with the application number of 201610310464.1 discloses a preparation process of a Zr-B-N nano composite coating, which adopts the high-power pulse and pulse direct current composite magnetron sputtering technology to deposit the Zr-B-N coating on a metal or alloy substrate, wherein the coating has higher toughness and strength, good wear resistance, compact structure and strong bonding force between the coating and the substrate; chinese patent application No. 201710155500.6 discloses a nano composite coating and a preparation technique thereof, which adopts an arc ion plating technique to prepare an AlCrN nano composite coating on a metal or hard alloy substrate, wherein the AlCrN nano composite coating has high hardness and strength, good high temperature oxidation resistance and corrosion resistance; the Chinese patent with the application number of 201320139896.2 relates to a TiCuN nano composite coating, and aims to solve the technical problem that nc-TiN/a-Si3N4The high friction coefficient of the nano composite coating causes a large amount of heat to be generated in the cutting process, and the front cutter face of the coated cutter still generates built-up edges. In order to solve the technical problem, a transition layer and a TiCuN layer which are formed by a TiCu film are sequentially arranged on the surface of a substrate. The preparation method is completed by adopting an arc ion plating technology, and the preparation method isThe nano composite coating has the advantages of high toughness, strong film-substrate bonding, small friction coefficient and the like besides high hardness; the application number 201410341995.8 discloses a TiSiCN nano composite coating with ultrahigh hardness and low friction coefficient and a preparation method thereof, wherein the TiSiCN nano composite coating with ultrahigh hardness and low friction coefficient is formed by adopting a multi-target magnetron sputtering instrument and carrying out magnetron sputtering reaction deposition on a substrate which is sequentially subjected to polishing, ultrasonic cleaning and ion cleaning by using a TiSiC composite target material, and the composite target material can be used for dry-type and high-speed cutting processing cutters and the surfaces of parts serving under frictional wear conditions, so that the surface properties and the service lives of the cutters and the parts are improved, and the preparation method has the advantages of simple process, high deposition speed, low cost, high bonding strength and the like; chinese patent with application number 201710505960.7 discloses NbN and NbB2The composite coating is prepared by utilizing a multi-target magnetron sputtering technology and firstly researching on N2Each process parameter pair NbN and NbB under the environment2Influence of monolayer film properties, the main factors found for hardness making were the influence of substrate bias and annealing temperature on the thin film coating. Then for NbN and NbB2The composite coating structure of (a) was designed and tested experimentally. The prepared Nb-B-N nano composite coating has the excellent mechanical characteristics of higher hardness, high film-substrate binding force, good friction resistance and thermal stability. NbN and NbB2The composite coating has important application prospect in the fields of cutting tools, mechanical parts and the like.
However, the conventional coating still has the problems that hardness, thermal stability and deposition efficiency cannot be simultaneously achieved, and the coating has the defects that the hardness, high-temperature oxidation resistance and production efficiency cannot meet the performance requirements of high-speed cutting and dry cutting, and the like.
Disclosure of Invention
The invention aims to provide a composite coating, and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a composite coating, which comprises a TiN layer, an AlTiN layer, an AlTiSiN layer and a V-doped AlTiSiN layer which are sequentially stacked.
Preferably, the doping amount of V in the V-doped AlTiSiN layer is 4-8 at.%.
Preferably, the thickness of the composite coating is 2.0-4.5 μm;
the TiN layer, the AlTiN layer and the AlTiSiN layer are 200-400 nm in thickness independently.
The invention also provides a preparation method of the composite coating, which comprises the following steps:
and sputtering a TiN layer, an AlTiN layer, an AlTiSiN layer and a V-doped AlTiSiN layer on the surface of the matrix in sequence to obtain the composite coating.
Preferably, the substrate is cleaned before the sputtering;
the cleaning comprises ultrasonic cleaning and ion cleaning which are sequentially carried out.
Preferably, the frequency of ultrasonic cleaning is 15-30 kHz, and the time is 5-10 min;
the ion cleaning is carried out under a vacuum condition, and the vacuum degree is 2-4 Pa;
the gas used for ion cleaning is Ar gas, and the power is 80-100W.
Preferably, the power for sputtering the TiN layer, the AlTiN layer and the AlTiSiN layer is independently 80-120W, and the time is independently 5-8 min.
Preferably, the power for sputtering the V-doped AlTiSiN layer is 180-200W, and the time is 60-120 min.
Preferably, when the TiN layer, the AlTiN layer, the AlTiSiN layer and the V-doped AlTiSiN layer are sputtered, the diameter of the target material is 75mm, and the total air pressure range is 0.4-0.8 Pa;
ar gas flow is independently 20-40 sccm, N2The flow rate is independently 20-40 sccm, and the target base distance is independently 4-8 cm.
The invention also provides the composite coating in the technical scheme or the application of the composite coating prepared by the preparation method in the technical scheme as a cutter coating in the field of cutters.
The invention provides a composite coating, which comprises a TiN layer, an AlTiN layer, an AlTiSiN layer and a V-doped AlTiSiN layer which are sequentially stacked. The TiN layer, the AlTiN layer and the AlTiSiN layer are used as transition layers between the base material and the V-doped AlTiSiN coating, so that internal stress generated between the base material and the coating due to different lattice constants and different thermal expansion systems can be relieved, and the bonding strength between the base material and the coating is improved. The composite coating can make up the defects of the traditional alloy in the use of the cutter coating, broadens the research range of the cutter coating, and has Si inside the coating3N4The interface phase is wrapped with a nano composite structure of AlTiVN nano crystal grains, and the doping of the V element can realize the strengthening of the AlTiVN nano matrix phase through solid solution strengthening, thereby further strengthening the coating. According to the description of the embodiment, the hardness of the composite coating can reach 47.3GPa at most, and can be kept above 40GPa even if the annealing treatment is carried out in air at 900 ℃ for 30 min. Therefore, the composite coating can meet the requirement of working in a complex high-speed cutting environment.
Drawings
FIG. 1 is a transmission electron microscope image of the cross section of the composite coating prepared in example 3.
Detailed Description
The invention provides a composite coating, which comprises a TiN layer, an AlTiN layer, an AlTiSiN layer and a V-doped AlTiSiN layer which are sequentially stacked.
In the invention, the thickness of the composite coating is preferably 2.0-4.5 μm, and more preferably 2.5-4.0 μm. The thickness of the TiN layer, the AlTiN layer, the AlTiSiN layer and the V-doped AlTiSiN layer is independent and preferably 200-400 nm, and more preferably 250-350 nm.
In the invention, the atomic number ratio of Al to Ti in the AlTiN layer is 1: 1; the atomic number ratio of Al, Ti and Si in the AlTiSiN layer is preferably 9:9: 2; the atomic number ratio of Al, Ti, V and Si in the V-doped AlTiSiN layer is preferably (45-x/2) to (45-x/2): x: 10, wherein the value range of x is 8-16.
In the invention, the doping amount of V in the V-doped AlTiSiN layer is preferably 4-8 at.%.
The invention also provides a preparation method of the composite coating, which comprises the following steps:
and sputtering a TiN layer, an AlTiN layer, an AlTiSiN layer and a V-doped AlTiSiN layer on the surface of the matrix in sequence to obtain the composite coating.
In the present invention, all the raw materials are commercially available products well known to those skilled in the art unless otherwise specified.
In the present invention, the substrate is preferably a metal, cemented carbide or ceramic; the present invention does not have any particular limitation on the types of the metal, cemented carbide, or ceramic, and those known to those skilled in the art may be used.
In the present invention, before the sputtering, it is preferable that the substrate is sequentially polished and cleaned; the polishing is not particularly limited in the present invention, and may be carried out by a procedure well known to those skilled in the art. In the present invention, the cleaning preferably includes ultrasonic cleaning and ion cleaning performed in this order; the ultrasonic cleaning is preferably carried out in absolute ethyl alcohol and acetone in sequence; in the invention, the frequency of the ultrasonic cleaning is preferably 15-30 kHz, and more preferably 18-25 kHz; the time is preferably 5 to 10min, and more preferably 6 to 8 min. After the ultrasonic cleaning is finished, the cleaned substrate is preferably placed in a vacuum chamber and vacuumized to 6 x 10-4And introducing Ar gas to carry out ion cleaning after Pa. In the invention, the ion cleaning is preferably carried out under a vacuum condition, and the vacuum degree is preferably 2-4 Pa; the ion cleaning power is preferably 80-100W, and preferably 85-95W; the time is preferably 30 min.
In the invention, the targets for sputtering the TiN layer, the AlTiN layer and the AlTiSiN layer are preferably Ti, AlTi and AlTiSi in sequence. In the present invention, the atomic ratio of Al and Ti in AlTi is preferably 1: 1; the atomic ratio of Al, Ti and Si in the AlTiSi is preferably 9:9: 2. In the invention, the power of the sputtering is preferably 80-120W independently, more preferably 90-110W, and most preferably 100W; the time is preferably 5-8 min independently, and more preferably 6-7 min independently. In the present invention, the sputtering is preferably performed in a multi-target magnetron sputtering apparatus, and each target is preferably controlled by a direct current power supply during the sputtering.
In the invention, the target material adopted for sputtering the V-doped AlTiSiN layer is preferably Al45-x/2Ti45-x/2VxSi10And in the target, the value range of x is 8-16. In the invention, the power for sputtering the V-doped AlTiSiN layer is preferably 180-200W, more preferably 185-195W, and most preferably 190W; the time is preferably 60 to 120min, and more preferably 80 to 100 min. In the present invention, the sputtering is preferably controlled by a radio frequency power supply.
In the invention, when the TiN layer, the AlTiN layer, the AlTiSiN layer and the V-doped AlTiSiN layer are sputtered, the diameter of the target material is preferably 75 mm; the total air pressure range is preferably 0.4-0.8 Pa, and more preferably 0.5-0.6 Pa; the Ar gas flow is preferably 20-40 sccm independently, more preferably 25-35 sccm, and most preferably 28-32 sccm; n is a radical of2The flow rate is preferably 20-40 sccm independently, more preferably 25-35 sccm, and most preferably 28-32 sccm; the target base distance is preferably 4-8 cm independently, and more preferably 5-6 cm independently.
The invention also provides the composite coating in the technical scheme or the application of the composite coating prepared by the preparation method in the technical scheme as a cutter coating in the field of cutters. The present invention is not limited to any particular application, and may be applied by application methods known to those skilled in the art.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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 apparatus used in examples 1 to 5 were as follows:
JGP-450 magnetron sputtering system, Shenyang scientific instruments research center, Inc., of Chinese academy of sciences;
NANO indentor model G200 NANO indentor, agilent technologies, usa;
Tecnai G2model 20 high resolution transmission electron microscope, FEI company, usa;
QuantaFEG model 450 scanning electron microscope, FEI USA.
Example 1
Polishing a high-speed steel substrate, putting the polished high-speed steel substrate into an ultrasonic cleaning machine, and sequentially performing ultrasonic cleaning in absolute ethyl alcohol and acetone for 10min, wherein the ultrasonic frequency is 20 kHz; then putting the cleaned substrate into a vacuum chamber, and vacuumizing to 6 x 10-4Introducing Ar gas after Pa, maintaining the vacuum degree at 4Pa and the power at 100W, and washing the substrate with neutral ions for 30min to obtain a pretreated substrate;
placing the pretreated substrate into a multi-target magnetron sputtering instrument, sequentially staying above Ti, AlTi (atomic ratio of 1:1) and AlTiSi (atomic ratio of 9:9: 2) targets, controlling each target by a direct current power supply, sputtering with the power of 100W, and after 5min, placing the substrate in AlTiV8Dwell over Si target, Al45-x/2Ti45-x/2VxSi10The (x is 8) target is controlled by a radio frequency power supply, the sputtering power is 180W, and the deposition time is 60 min; in the whole sputtering process, the flow rate of Ar gas is 20sccm, N2The flow rate of the composite coating is 20sccm, and the working air pressure is 0.4Pa, so that the composite coating is obtained.
The total thickness of the composite coating is 2.1 mu m, and the thicknesses of the layers are 0.2 mu m, 0.2 mu m and 1.5 mu m respectively through the test of a scanning electron microscope;
performing hardness test on the composite coating according to the national standard GB/T25898-2010 to obtain the hardness of the composite coating of 46.6 GPa;
and annealing the composite coating in 900 ℃ air for 30min, and then continuing to perform hardness test according to the standard to obtain the composite coating with the hardness of 40.5GPa after annealing treatment.
Example 2
Polishing the hard alloy matrix, putting the polished hard alloy matrix into an ultrasonic cleaning machine, and sequentially carrying out ultrasonic cleaning in absolute ethyl alcohol and acetone for 10min, wherein the ultrasonic frequency is 20 kHz; then putting the cleaned substrate into a vacuum chamberIn the middle, vacuum is pumped to 6 x 10-4Introducing Ar gas after Pa, maintaining the vacuum degree at 4Pa and the power at 100W, and washing the substrate with neutral ions for 30min to obtain a pretreated substrate;
placing the pretreated substrate into a multi-target magnetron sputtering instrument, sequentially staying above Ti, AlTi (atomic ratio of 1:1) and AlTiSi (atomic ratio of 9:9: 2) targets, controlling each target by a direct current power supply, sputtering with the power of 100W, and after 6min, placing the substrate in AlTiV10Dwell over Si target, Al45-x/2Ti45-x/2VxSi10The (x is 10) target is controlled by a radio frequency power supply, the sputtering power is 180W, and the deposition time is 80 min; in the whole sputtering process, the flow rate of Ar gas is 30sccm, N2The flow rate of the composite coating is 30sccm, and the working air pressure is 0.6Pa, so that the composite coating is obtained.
The total thickness of the composite coating is 3.2 mu m, and the thicknesses of the layers are 0.3 mu m, 0.2 mu m and 2.5 mu m respectively through the test of a scanning electron microscope;
performing a hardness test on the composite coating according to the national standard GB/T25898-2010 to obtain the hardness of the composite coating of 45.4 GPa;
and annealing the composite coating in the air at 900 ℃ for 30min, and then continuing to perform hardness test according to the standard to obtain the composite coating with the hardness of 40.7GPa after annealing treatment.
Example 3
Polishing a high-speed steel substrate, putting the polished high-speed steel substrate into an ultrasonic cleaning machine, and sequentially performing ultrasonic cleaning in absolute ethyl alcohol and acetone for 10min, wherein the ultrasonic frequency is 20 kHz; then putting the cleaned substrate into a vacuum chamber, and vacuumizing to 6 x 10-4Introducing Ar gas after Pa, maintaining the vacuum degree at 4Pa and the power at 100W, and washing the substrate with neutral ions for 30min to obtain a pretreated substrate;
placing the pretreated substrate into a multi-target magnetron sputtering instrument, sequentially staying above Ti, AlTi (atomic ratio of 1:1) and AlTiSi (atomic ratio of 9:9: 2) targets, controlling each target by a direct current power supply, sputtering with the power of 100W for 5min, and placing the substrate on Al45-x/2Ti45-x/2VxSi10(x-12) dwell over target, AlTiV12The Si target is controlled by a radio frequency power supply, the sputtering power is 180W, and the deposition time is 100 min; in the whole sputtering process, the flow rate of Ar gas is 40sccm, N2The flow rate of the composite coating is 40sccm, and the working air pressure is 0.8Pa, so that the composite coating is obtained.
The total thickness of the composite coating is 3.7 mu m, and the thicknesses of the layers are 0.3 mu m, 0.3 mu m and 2.8 mu m respectively through the test of a scanning electron microscope;
performing a hardness test on the composite coating according to the national standard GB/T25898-2010 to obtain the hardness of the composite coating of 47.3 GPa;
annealing the composite coating in air at 900 ℃ for 30min, and then continuing to perform hardness test according to the standard to obtain the hardness of the annealed composite coating of 41.4 GPa;
the composite coating described in example 3 was subjected to TEM test, and the test result is shown in fig. 1, and it can be seen from fig. 1 that a significant nanocomposite structure was formed inside the coating.
Example 4
Polishing the hard alloy matrix, putting the polished hard alloy matrix into an ultrasonic cleaning machine, and sequentially carrying out ultrasonic cleaning in absolute ethyl alcohol and acetone for 10min, wherein the ultrasonic frequency is 20 kHz; then putting the cleaned substrate into a vacuum chamber, and vacuumizing to 6 x 10-4Introducing Ar gas after Pa, maintaining the vacuum degree at 4Pa and the power at 100W, and washing the substrate with neutral ions for 30min to obtain a pretreated substrate;
placing the pretreated substrate into a multi-target magnetron sputtering instrument, sequentially staying above Ti, AlTi (atomic ratio of 1:1) and AlTiSi (atomic ratio of 9:9: 2) targets, controlling each target by a direct current power supply, sputtering with the power of 100W, and after 7min, placing the substrate on an Al target45-x/2Ti45-x/2VxSi10(x-12) dwell over target, AlTiV12The Si target is controlled by a radio frequency power supply, the sputtering power is 180W, and the deposition time is 110 min; in the whole sputtering process, the flow rate of Ar gas is 30sccm, N2The flow rate of the composite coating is 30sccm, and the working air pressure is 0.7Pa, so that the composite coating is obtained.
The total thickness of the composite coating is 3.9 mu m, and the thicknesses of the layers are 0.4 mu m, 0.3 mu m and 2.9 mu m respectively through the test of a scanning electron microscope;
performing hardness test on the composite coating according to the national standard GB/T25898-2010 to obtain the hardness of the composite coating of 46.8 GPa;
and annealing the composite coating in the air at 900 ℃ for 30min, and then continuing to perform hardness test according to the standard to obtain the composite coating with the hardness of 40.7GPa after annealing treatment.
Example 5
Polishing the hard alloy matrix, putting the polished hard alloy matrix into an ultrasonic cleaning machine, and sequentially carrying out ultrasonic cleaning in absolute ethyl alcohol and acetone for 10min, wherein the ultrasonic frequency is 20 kHz; then putting the cleaned substrate into a vacuum chamber, and vacuumizing to 6 x 10-4Introducing Ar gas after Pa, maintaining the vacuum degree at 4Pa and the power at 100W, and washing the substrate with neutral ions for 30min to obtain a pretreated substrate;
placing the pretreated substrate into a multi-target magnetron sputtering instrument, sequentially staying above Ti, AlTi (atomic ratio of 1:1) and AlTiSi (atomic ratio of 9:9: 2) targets, controlling each target by a direct current power supply, sputtering with the power of 100W, and after 8min, placing the substrate on an Al target45-x/2Ti45-x/2VxSi10(x ═ 16) dwell over target, AlTiV16The Si target is controlled by a radio frequency power supply, the sputtering power is 180W, and the deposition time is 120 min; in the whole sputtering process, the flow rate of Ar gas is 20sccm, N2The flow rate of the composite coating is 20sccm, and the working air pressure is 0.5Pa, so that the composite coating is obtained.
The total thickness of the composite coating is 4.5 mu m, and the thicknesses of the layers are 0.4 mu m, 0.4 mu m and 3.3 mu m respectively through the test of a scanning electron microscope;
performing a hardness test on the composite coating according to the national standard GB/T25898-2010 to obtain the hardness of the composite coating of 47.0 GPa;
and annealing the composite coating in the air at 900 ℃ for 30min, and then continuing to perform hardness test according to the standard to obtain the composite coating with the hardness of 41.1GPa after annealing treatment.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The composite coating is characterized by comprising a TiN layer, an AlTiN layer, an AlTiSiN layer and a V-doped AlTiSiN layer which are sequentially stacked.
2. The composite coating of claim 1, wherein the amount of V doped in the V doped AlTiSiN layer is from 4 to 8 at.%.
3. The composite coating of claim 1, wherein the composite coating has a thickness of 2.0 to 4.5 μ ι η;
the TiN layer, the AlTiN layer and the AlTiSiN layer are 200-400 nm in thickness independently.
4. A method for preparing a composite coating according to any one of claims 1 to 3, comprising the steps of:
and sputtering a TiN layer, an AlTiN layer, an AlTiSiN layer and a V-doped AlTiSiN layer on the surface of the matrix in sequence to obtain the composite coating.
5. The method according to claim 4, wherein the substrate is cleaned before the sputtering;
the cleaning comprises ultrasonic cleaning and ion cleaning which are sequentially carried out.
6. The method according to claim 5, wherein the ultrasonic cleaning is performed at a frequency of 15 to 30kHz for 5 to 10 min;
the ion cleaning is carried out under a vacuum condition, and the vacuum degree is 2-4 Pa;
the gas used for ion cleaning is Ar gas, and the power is 80-100W.
7. The method according to claim 4, wherein the TiN layer, AlTiN layer and AlTiSiN layer are sputtered independently at 80-120W for 5-8 min.
8. The method according to claim 4, wherein the power for sputtering the V-doped AlTiSiN layer is 180-200W for 60-120 min.
9. The method according to claim 4, 7 or 8, wherein the diameter of the target is 75mm and the total pressure range is independently 0.4 to 0.8Pa when the TiN layer, the AlTiN layer, the AlTiSiN layer and the V-doped AlTiSiN layer are sputtered;
ar gas flow is independently 20-40 sccm, N2The flow rate is independently 20-40 sccm, and the target base distance is independently 4-8 cm.
10. Use of the composite coating according to any one of claims 1 to 3 or the composite coating produced by the production method according to any one of claims 4 to 9 in a cutting tool.
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| CN202010942973.2A Pending CN111926292A (en) | 2020-09-09 | 2020-09-09 | Composite coating and preparation method and application thereof |
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Citations (4)
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| JP2000326108A (en) * | 1999-05-19 | 2000-11-28 | Hitachi Tool Engineering Ltd | Hard film coated tool |
| KR20100076281A (en) * | 2008-12-26 | 2010-07-06 | (주)보림시스템 | Multi-layer coating method |
| CN107190233A (en) * | 2016-05-25 | 2017-09-22 | 上海仟纳真空镀膜科技有限公司 | A kind of preparation technology of the Si dopen Nano composite coatings with ultrahigh hardness |
| CN110079766A (en) * | 2019-05-27 | 2019-08-02 | 国宏工具系统（无锡）股份有限公司 | A kind of highly-efficient processing high temperature alloy nano-composite coating technique |
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2020
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000326108A (en) * | 1999-05-19 | 2000-11-28 | Hitachi Tool Engineering Ltd | Hard film coated tool |
| KR20100076281A (en) * | 2008-12-26 | 2010-07-06 | (주)보림시스템 | Multi-layer coating method |
| CN107190233A (en) * | 2016-05-25 | 2017-09-22 | 上海仟纳真空镀膜科技有限公司 | A kind of preparation technology of the Si dopen Nano composite coatings with ultrahigh hardness |
| CN110079766A (en) * | 2019-05-27 | 2019-08-02 | 国宏工具系统（无锡）股份有限公司 | A kind of highly-efficient processing high temperature alloy nano-composite coating technique |
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Application publication date: 20201113 |