CN111455338A - Nano multilayer coating, preparation method thereof and cutter with nano multilayer coating coated on surface - Google Patents

Nano multilayer coating, preparation method thereof and cutter with nano multilayer coating coated on surface Download PDF

Info

Publication number
CN111455338A
CN111455338A CN202010381727.4A CN202010381727A CN111455338A CN 111455338 A CN111455338 A CN 111455338A CN 202010381727 A CN202010381727 A CN 202010381727A CN 111455338 A CN111455338 A CN 111455338A
Authority
CN
China
Prior art keywords
layer
multilayer coating
nano
sputtering
coating
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.)
Pending
Application number
CN202010381727.4A
Other languages
Chinese (zh)
Inventor
冯利民
李伟
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.)
Shanghai New Arc Coating Technology Co ltd
Original Assignee
Shanghai New Arc Coating Technology Co ltd
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 Shanghai New Arc Coating Technology Co ltd filed Critical Shanghai New Arc Coating Technology Co ltd
Priority to CN202010381727.4A priority Critical patent/CN111455338A/en
Publication of CN111455338A publication Critical patent/CN111455338A/en
Pending legal-status Critical Current

Links

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
    • C23C14/0021—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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • C23C14/0623—Sulfides, selenides or tellurides
    • 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
    • C23C14/0682—Silicides
    • 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

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)

Abstract

The invention provides a nano multilayer coating, a preparation method thereof and a cutter with the surface coated with the nano multilayer coating, belonging to the technical field of protective coatings. The nano multilayer coating provided by the invention comprises a TiN layer and a nano composite alternate layer which are sequentially stacked on the surface of a substrate; the nano-composite alternating layer comprises TiAlSiN layers and MoS layers which are alternately stacked2A layer; the TiN layer and the TiAlSiN layer are in contact. In the nano multilayer coating provided by the invention, the TiN layer is a transition layer to improve the bonding strength; the multilayer structure of the TiN layer and the nano composite alternate layer improves the hardness of the coating and reduces the friction coefficient of the coating, so that the nano multilayer coating has high hardness and low friction coefficient and better lubricating property at the same timeThe shortages in the use of the layer broadens the research range of the cutter coating, and the cutter coating can work in the environment of bearing load and requiring low friction.

Description

Nano multilayer coating, preparation method thereof and cutter with nano multilayer coating coated on surface
Technical Field
The invention relates to the technical field of protective coatings, in particular to a nano multilayer coating, a preparation method thereof and a cutter with the surface coated with the nano multilayer coating.
Background
In cutting machining, the tool properties have a decisive influence on the efficiency, accuracy and surface quality of the cutting machining. One method that is more effective in order to better improve the cutting performance of the tool is to coat the substrate with one or more layers of high hardness, high wear resistance material using various coating techniques. The coating on the surface of the cutter is used as a chemical barrier and a thermal barrier, so that the crater abrasion of the cutter is reduced, the processing efficiency can be obviously improved, the processing precision is improved, the service life of the cutter is prolonged, and the processing cost is reduced. The coating is characterized in that the coating film is combined with the cutter base body, so that the wear resistance of the cutter is improved without reducing the toughness of the base body, the friction factor between the cutter and a workpiece is reduced, and the service life of the cutter is prolonged. However, as the use conditions of the cutting tool become more and more severe, not only higher requirements on the hardness of the coating of the cutting tool are provided, but also the coating material is required to have good self-lubricating performance, so that the use performance of the cutting tool can be effectively improved.
The nano multilayer coating is a multilayer film formed by alternately depositing two materials in a nano level, and has attracted extensive attention due to the abnormal performance of physical properties and mechanical properties. In particular, in the aspect of mechanical property, as the nano multilayer coating materials can be randomly cut and selected, some nano multilayer coatings with the modulation period less than 100nm show the supermode effect and the superhard effect of abnormally increased elastic modulus and hardness, so that the nano multilayer coatings have a larger application prospect in the field of advanced coating materials.
Chinese patent 201010176320.4 relates to a nano-composite titanium-chromium-silicon nitride cutter coating, which comprises a titanium-chromium-silicon nitride coating with a transition layer, wherein the grain size is 5-15 nm, the coating thickness is 1-4 μm, the coating microhardness is 26Gpa, the high-temperature stability is above 1068 ℃, the nano-composite titanium-chromium-silicon nitride cutter coating is suitable for cutting high-hardness steel materials under high-speed conditions, and the friction coefficient is 0.45. Chinese patent 200910055595.X relates to TiC/Si3N4A nano multilayer coating consisting of a TiC layer and Si3N4The layers are alternately deposited on a metal, cemented carbide or ceramic substrate, the coating having excellent high temperature oxidation resistance and having a hardness of more than 40GPa with a coefficient of friction of 0.4. However, the conventional coating layer still has a problem that both high hardness and low friction coefficient cannot be achieved, and cannot satisfy performance requirements of high-speed cutting and dry cutting.
Disclosure of Invention
The invention aims to provide a nano multilayer coating, a preparation method thereof and a cutter with the surface coated with the nano multilayer coating. The nano multilayer coating provided by the invention has high hardness and low friction coefficient.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a nano multilayer coating, which comprises a TiN layer and a nano composite alternate layer which are sequentially stacked on the surface of a substrate; the nano-composite alternating layer comprises TiAlSiN layers and MoS layers which are alternately stacked2A layer; the TiN layer and the TiAlSiN layer are in contact.
Preferably, the thickness of the TiN layer is 300-500 nm.
Preferably, the thickness of the TiAlSiN layer is 6-8 nm.
Preferably, the MoS2The thickness of the single layer of the layer is 0.3 to 1.5 nm.
Preferably, the thickness of the nano multilayer coating is 1-4 μm.
The invention provides a preparation method of the nano multilayer coating, which comprises the following steps:
in a nitrogen atmosphere and a protective atmosphere, performing single-target magnetron sputtering on the surface of the substrate by using a Ti target to obtain a TiN layer;
alternating TiAlSi targets and MoS2Target, carrying out multi-target magnetron sputtering on the surface of the TiN layer to alternately and circularly deposit TiAlSi layer and MoS2A nano composite alternate layer is formed on the surface of the TiN layer to obtain a nano multilayer coating; the TiN layer and the TiAlSiN layer are in contact.
Preferably, the working conditions of the single-target magnetron sputtering include: the sputtering target is obtained by direct current sputtering, the sputtering power is 100-150W, the sputtering time is 20-30 min, the Ar gas flow is 20-40 sccm, and N is2The gas flow is 5-20 sccm, and the total gas pressure is 0.2-0.6 Pa.
Preferably, the working conditions of the multi-target magnetron sputtering include: ar gas flow of 20-40 sccm, N2The gas flow is 5-20 sccm, and the total gas pressure is 0.2-0.8 Pa.
Preferably, the TiAlSi layer is obtained by direct current sputtering, the power of the direct current sputtering is 100-200W, and the time is 10-20 s;
the MoS2The layer is obtained by radio frequency sputtering, the power of the radio frequency sputtering is 80-160W, and the time is 2-10 s.
The invention also provides a cutter with the surface coated with the nano multilayer coating or the nano multilayer coating prepared by the preparation method in the technical scheme.
The invention provides a nano multilayer coating, which comprises a TiN layer and a nano composite alternate layer which are sequentially stacked on the surface of a substrate; the nano-composite alternating layer comprises TiAlSiN layers and MoS layers which are alternately stacked2A layer; the TiN layer and the TiAlSiN layer are in contact. In the nano multilayer coating provided by the invention, the TiN layer is a transition layer to improve the bonding strength; in the nano composite alternate layer, the TiN layer and the multilayer structure of the nano composite alternate layer improve the hardness of the coating and reduce the friction coefficient of the coating, so that the nano multilayer coating has high hardness, low friction coefficient and better lubricating property. The nano multilayer coating provided by the invention can make up for the defects in the use of the traditional cutter coating, broadens the research range of the cutter coating and can work in the environment of bearing load and requiring low friction. As shown by the results of the embodiment of the invention, the hardness of the nano multilayer coating provided by the invention is 35.7-38.2 GPa, and the friction coefficient is 0.22-0.28.
The preparation method provided by the invention has the advantages of simple process, low cost and high efficiency, and can realize batch production.
Detailed Description
The invention provides a nano multilayer coating, which comprises a TiN layer and a nano composite alternate layer which are sequentially stacked on the surface of a substrate; the nano-composite alternating layer comprises TiAlSiN layers and MoS layers which are alternately stacked2A layer; the TiN layer and the TiAlSiN layer are in contact.
In the present invention, all the raw material components 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 substrate, and more preferably a cemented carbide, and the present invention is not particularly limited to a specific kind of the cemented carbide, and a cemented carbide known to those skilled in the art, specifically, a high-speed steel, may be used.
In the invention, the thickness of the nano multilayer coating is preferably 1-4 μm, more preferably 1.5-3.5 μm, and most preferably 2-3 μm.
In the present invention, the thickness of the TiN layer is preferably 300 to 500nm, more preferably 350 to 450nm, and most preferably 400 to 450 nm. In the invention, if the TiAlSiN layer is directly contacted with the substrate, the TiAlSiN layer is easy to fall off due to stress generated by different lattice constants and thermal expansion coefficients between the TiAlSiN layer and the substrate.
In the invention, the thickness of the nano composite alternating layer is preferably 0.5-3.7 μm, more preferably 1-3.5 μm, and most preferably 1.5-3 μm. In the invention, the thickness of the TiAlSiN layer is preferably 6-8 nm, more preferably 6.5-7.5 nm, and most preferably 7.0-7.5 nm. In the present invention, the MoS2The thickness of the single layer of the layer is preferably 0.3 to 1.5nm, more preferably 0.5 to 1.2nm, and most preferably 0.5 to 1 nm. In the invention, the TiAlSiN layer and the MoS layer in the nano composite alternating layer2The number of layers is independently preferably 52 to 570, more preferably 100 to 500, and most preferably 200 to 400. In the present invention, the TiAlSiN layer and MoS2The alternating multilayer structure of the layers improves the hardness of the coating and reduces the friction coefficient of the coating, so that the nano multilayer coating has high hardness and low friction coefficient and better lubricating property.
The invention provides a preparation method of the nano multilayer coating, which comprises the following steps:
in a nitrogen atmosphere and a protective atmosphere, performing single-target magnetron sputtering on the surface of the substrate by using a Ti target to obtain a TiN layer;
alternating TiAlSi targets and MoS2Target, carrying out multi-target magnetron sputtering on the surface of the TiN layer to alternately and circularly deposit TiAlSi layer and MoS2A nano composite alternate layer is formed on the surface of the TiN layer to obtain a nano multilayer coating; the TiN layer and the TiAlSiN layer are in contact.
In the invention, in a nitrogen atmosphere and a protective atmosphere, a Ti target is used for carrying out single-target magnetron sputtering on the surface of a substrate to obtain a TiN layer.
In the present invention, the substrate is preferably subjected to a pretreatment before use, and the pretreatment preferably includes polishing, organic solvent washing and vacuum ion washing, which are sequentially performed. The polishing method of the present invention is not particularly limited, and may be any polishing method known to those skilled in the art, such as mechanical polishing. In the present invention, the organic solvent washing preferably includes absolute ethanol washing and acetone washing which are sequentially performed, and the amount of the absolute ethanol and the acetone used in the present invention is not particularly limited, and the substrate can be immersed. In the invention, the absolute ethyl alcohol washing and the acetone washing are preferably carried out under the ultrasonic condition, the power of the ultrasonic of the absolute ethyl alcohol washing and the ultrasonic of the acetone washing are preferably 15-30 kHz independently, more preferably 20-25 kHz independently, and the time is preferably 10-15 min independently, more preferably 12-14 min independently. In the present invention, the organic solvent washing is intended to remove impurities such as oil from the surface of the substrate.
In the present invention, the vacuum ion cleaning preferably comprises evacuating to 6 × 10-4And introducing Ar as an ion source after Pa, and performing intermediate frequency ion bombardment on the substrate washed by the organic solvent. In the invention, the pressure after Ar filling is preferably 0.4-1.0 Pa, more preferably 0.5-0.8 Pa, and most preferably 0.6-0.7 Pa; the power of the medium-frequency ion bombardment is preferably 80-100W, more preferably 85-95W, and most preferably 90W, and the time of the medium-frequency ion bombardment is preferably 20-40 min, more preferably 25-35 min, and most preferably 30 min.
In the present invention, the Ti targets each preferably have a diameter of 75 mm.
In the invention, the working conditions of the single-target magnetron sputtering include: preferably straightFlow sputtering to obtain; the sputtering power is preferably 100-150W, more preferably 110-140W, and most preferably 120-130W; the sputtering time is preferably 20-30 min, more preferably 22-28 min, and most preferably 25 min; the Ar gas flow is preferably 20-40 sccm, more preferably 25-35 sccm, and most preferably 30-35 sccm; n is a radical of2The gas flow is preferably 5 to 20sccm, more preferably 8 to 18sccm, and most preferably 10 to 15 sccm; the total air pressure is preferably 0.2 to 0.6Pa, more preferably 0.3 to 0.5Pa, and most preferably 0.4 to 0.5 Pa; the target base distance is preferably 3-7 cm, and more preferably 4-6 cm.
The equipment adopted by the magnetron sputtering is not particularly limited, and the magnetron sputtering equipment well known by the technicians in the field can be adopted; in the embodiment of the present invention, the magnetron sputtering apparatus is preferably a JGP-450 type magnetron sputtering system (Shenyang scientific instruments research center, Inc., of Chinese academy of sciences).
After obtaining the TiN layer, the invention alternately uses the TiAlSi target and the MoS2Target, carrying out multi-target magnetron sputtering on the surface of the TiN layer to alternately and circularly deposit TiAlSi layer and MoS2A nano composite alternate layer is formed on the surface of the TiN layer to obtain a nano multilayer coating; the TiN layer and the TiAlSiN layer are in contact.
In the present invention, the TiAlSi target and MoS2The purity of the target is independently preferably 99.99% or more, more preferably 99.99%; the TiAlSi target and MoS2The diameter of the target is preferably 75 mm; the target base distance is preferably 3-7 cm, more preferably 4-6 cm, and most preferably 5-6 cm.
In the invention, the TiAlSi layer is preferably obtained by direct current sputtering, and the power of the direct current sputtering is preferably 100-200W, more preferably 120-180W, and most preferably 150-170W; the time of the direct current sputtering is preferably 10-20 s, more preferably 12-18 s, and most preferably 14-16 s.
In the present invention, the MoS2The layer is preferably obtained by radio frequency sputtering, and the power of the radio frequency sputtering is preferably 80-160W, more preferably 100-150W, and most preferably 120-150W; the time of the radio frequency sputtering is preferably 2-10 s, more preferably 3-8 s, and most preferably 4-7 s.
In the present invention, the operating conditions of the multi-target magnetron sputtering preferably further include: the Ar gas flow is preferably 20-40 sccm, more preferably 25-35 sccm, and most preferably 30-35 sccm; n is a radical of2The gas flow is preferably 5 to 20sccm, more preferably 8 to 18sccm, and most preferably 10 to 15 sccm; the total pressure is preferably 0.2 to 0.8Pa, more preferably 0.3 to 0.7Pa, and most preferably 0.4 to 0.6 Pa.
The equipment adopted by the multi-target magnetron sputtering is not particularly limited, and magnetron sputtering equipment well known by the technicians in the field can be adopted; in the embodiment of the present invention, the apparatus for multi-target magnetron sputtering is preferably a JGP-450 type magnetron sputtering system (Shenyang scientific instruments research center, Inc., of Chinese academy of sciences).
The preparation method provided by the invention has the advantages of simple process, low cost and high efficiency, and can realize batch production.
The invention also provides a cutter with the surface coated with the nano multilayer coating or the nano multilayer coating prepared by the preparation method in the technical scheme.
The invention comprehensively utilizes the high hardness and MoS of the TiAlSiN layer2The coating that nanometer multilayer coating has had both high rigidity and low friction has been obtained to the low coefficient of friction on layer, can make up traditional alloy not enough in the cutter coating use, and the cutter hardness that obtains is high and coefficient of friction is low, can bear load and work under the environment that low friction required.
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 the examples was a magnetron sputtering system of the JGP-450 type (Shenyang scientific instruments research center, Inc., of Chinese academy of sciences).
Example 1
(1) Base high speed steelPolishing, respectively ultrasonic cleaning with anhydrous ethanol and acetone at 30kHz for 5min, placing in a vacuum chamber, and vacuumizing to 6 × 10-4Introducing Ar as an ion source after Pa, maintaining the vacuum degree at 0.4Pa, and bombarding the acetone-washed high-speed steel matrix with medium-frequency ions for 30min under the condition of 80W to obtain the pretreated high-speed steel matrix.
(2) Performing magnetron sputtering on the surface of the high-speed steel substrate obtained in the step (1) by using a Ti target to obtain a TiN layer;
wherein, the working conditions of magnetron sputtering are as follows: obtained by direct current sputtering with sputtering power of 120W for 25min, Ar gas flow of 30sccm, N2The gas flow rate was 10sccm and the total gas pressure was 0.4 Pa.
(3) TiAlSi targets (purity 99.99%, diameter 75mm) and MoS were used alternately2Target (purity is 99.99%, diameter is 75mm), and multiple targets magnetron sputtering is carried out on the surface of the TiN layer to alternately and circularly deposit TiAlSi layer and MoS2A nano composite alternating layer is formed on the surface of the TiN layer to obtain a nano multilayer coating, wherein the TiN layer is in contact with the TiAlSi layer;
among them, TiAlSi target and MoS2The purity of the target is 99.99 percent, the diameter is 75mm, and the target base distance is 5 cm; the TiAlSi layer is obtained by direct current sputtering, the power of the direct current sputtering is 100W, and the time is 10 s; the MoS2The layer is obtained by radio frequency sputtering, the power of the radio frequency sputtering is 80W, and the time is 2 s; the working conditions of the multi-target magnetron sputtering preferably comprise: ar gas flow of 20sccm, N2The gas flow rate was 5sccm and the total gas pressure was 0.2 Pa.
The thickness of the nano multilayer coating prepared in this example was 1.8 μm, the thickness of the TiN layer was 300nm, the single layer thickness of the TiAlSiN layer was 6.5nm, and MoS2The monolayer thickness of the layer is 0.3 nm; the hardness of the nano multilayer coating is 35.9GPa, and the friction coefficient is 0.28;
wherein, the hardness measurement: NanoindenterG200 nanoindenter (Agilent, USA);
and (3) measuring the friction coefficient: model HRS-2M reciprocating friction wear tester (zhongkeh wachitech development ltd).
Example 2
A nano-multilayer coating was prepared according to the method of example 1, differing from example 1 in that: in the step (3), the power of the direct current sputtering of the TiAlSi layer is 150W, and the time is 18 s; MoS2The power of the radio frequency sputtering of the layer is 100W, and the time is 4 s; the total gas pressure was 0.2 Pa.
The thickness of the nano multilayer coating prepared in this example was 2.4 μm, the thickness of the TiN layer was 400nm, the single layer thickness of the TiAlSiN layer was 8nm, and MoS2The monolayer thickness of the layer is 0.6 nm; the hardness of the nano multilayer coating is 36.1GPa, and the friction coefficient is 0.24.
Example 3
A nano-multilayer coating was prepared according to the method of example 1, differing from example 1 in that: in the step (3), the flow rate of Ar gas is 30sccm, N2The gas flow is 20sccm, the total gas pressure is 0.6Pa, the power of the direct-current sputtering of the TiAlSi layer is 200W, and the time is 10 s; MoS2The power of the RF sputtering of the layer was 120W for 6 s.
The thickness of the nano multilayer coating prepared in this example was 3.2 μm, the thickness of the TiN layer was 500nm, the single layer thickness of the TiAlSiN layer was 8.5m, and MoS2The monolayer thickness of the layer is 0.9 nm; the hardness of the nano multilayer coating is 37.5GPa, and the friction coefficient is 0.27.
Example 4
A nano-multilayer coating was prepared according to the method of example 1, differing from example 1 in that: in the step (3), the flow rate of Ar gas is 35sccm, N2The gas flow is 15sccm, the total gas pressure is 0.7Pa, the power of the direct-current sputtering of the TiAlSi layer is 180W, and the time is 16 s; MoS2The power of the RF sputtering of the layer was 140W for 8 s.
The thickness of the nano multilayer coating prepared in this example was 3.4 μm, the thickness of the TiN layer was 350nm, the single layer thickness of the TiAlSiN layer was 7.5m, and MoS2The monolayer thickness of the layer is 1.2 nm; the hardness of the nano multilayer coating is 38.2GPa, and the friction coefficient is 0.28.
Example 5
A nano-multilayer coating was prepared according to the method of example 1, differing from example 1 in that: in the step (3), the flow rate of Ar gas is 40sccm, N2The gas flow is 20sccm, the total gas pressure is 0.8Pa, the power of the direct-current sputtering of the TiAlSi layer is 160W, and the time is 12 s; MoS2The power of the RF sputtering of the layer was 160W for 10 s.
The thickness of the nano multilayer coating prepared in this example was 2.9 μm, the thickness of the TiN layer was 450nm, the single layer thickness of the TiAlSiN layer was 7nm, and MoS2The monolayer thickness of the layer is 1.5 nm; the hardness of the nano multilayer coating is 35.7GPa, and the friction coefficient is 0.22.
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. A nanometer multilayer coating is characterized by comprising a TiN layer and a nanometer composite alternate layer which are sequentially stacked on the surface of a matrix; the nano-composite alternating layer comprises TiAlSiN layers and MoS layers which are alternately stacked2A layer; the TiN layer and the TiAlSiN layer are in contact.
2. The nanolayered multilayer coating of claim 1, wherein the TiN layer has a thickness of 300 to 500 nm.
3. The nanolayered multilayer coating of claim 1, wherein the TiAlSiN layer is a single layer 6 to 8nm thick.
4. The nanolayered multilayer coating of claim 1, wherein the MoS is2The thickness of the single layer of the layer is 0.3 to 1.5 nm.
5. The nanolayered multilayer coating of any one of claims 1 to 4, wherein the nanolayered multilayer coating has a thickness of 1 to 4 μm.
6. A method for preparing a nano-multilayer coating according to any one of claims 1 to 5, characterized by comprising the following steps:
in a nitrogen atmosphere and a protective atmosphere, performing single-target magnetron sputtering on the surface of the substrate by using a Ti target to obtain a TiN layer;
alternating TiAlSi targets and MoS2Target, carrying out multi-target magnetron sputtering on the surface of the TiN layer to alternately and circularly deposit TiAlSi layer and MoS2A nano composite alternate layer is formed on the surface of the TiN layer to obtain a nano multilayer coating; the TiN layer and the TiAlSiN layer are in contact.
7. The method according to claim 6, wherein the operating conditions of the single-target magnetron sputtering include: adopting direct current sputtering with the sputtering power of 100-150W, the sputtering time of 20-30 min, the Ar gas flow of 20-40 sccm, N2The gas flow is 5-20 sccm, and the total gas pressure is 0.2-0.6 Pa.
8. The method for preparing the magnetic material according to the claim 6, wherein the working conditions of the multi-target magnetron sputtering include: ar gas flow of 20-40 sccm, N2The gas flow is 5-20 sccm, and the total gas pressure is 0.2-0.8 Pa.
9. The preparation method according to claim 6 or 8, wherein the TiAlSi layer is obtained by direct current sputtering, the power of the direct current sputtering is 100-200W, and the time is 10-20 s;
the MoS2The layer is obtained by radio frequency sputtering, the power of the radio frequency sputtering is 80-160W, and the time is 2-10 s.
10. A cutting tool coated with the nano multi-layer coating prepared by the preparation method of any one of claims 1 to 5 or 6 to 9.
CN202010381727.4A 2020-05-08 2020-05-08 Nano multilayer coating, preparation method thereof and cutter with nano multilayer coating coated on surface Pending CN111455338A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010381727.4A CN111455338A (en) 2020-05-08 2020-05-08 Nano multilayer coating, preparation method thereof and cutter with nano multilayer coating coated on surface

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010381727.4A CN111455338A (en) 2020-05-08 2020-05-08 Nano multilayer coating, preparation method thereof and cutter with nano multilayer coating coated on surface

Publications (1)

Publication Number Publication Date
CN111455338A true CN111455338A (en) 2020-07-28

Family

ID=71678695

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010381727.4A Pending CN111455338A (en) 2020-05-08 2020-05-08 Nano multilayer coating, preparation method thereof and cutter with nano multilayer coating coated on surface

Country Status (1)

Country Link
CN (1) CN111455338A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112628381A (en) * 2020-12-02 2021-04-09 东南大学 Temperature self-adaptive lubricating gear and preparation method thereof
CN114371047A (en) * 2020-10-14 2022-04-19 石家庄铁道大学 Single-layer MoS2Band gap regulating method

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030091851A (en) * 2003-09-26 2003-12-03 학교법인 울산공업학원 Tool steel having a complex coating layer and method of the same
CN104002516A (en) * 2014-06-10 2014-08-27 上海理工大学 CrAlN/MoS2 multi-layered coating layer with high rigidity and low friction coefficient and preparation method thereof
CN104131256A (en) * 2014-07-25 2014-11-05 广东工业大学 Multilayer nanometer composite cutting tool coating and preparation method thereof
CN105256273A (en) * 2015-11-08 2016-01-20 宜昌后皇真空科技有限公司 Nitrogen boron titanium/ nitrogen silicon aluminum titanium nanometer composite multilayer coating cutter and preparation method thereof
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
EP3404126A1 (en) * 2017-05-19 2018-11-21 Walter Ag Metal cutting tool with multi-layer coating

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030091851A (en) * 2003-09-26 2003-12-03 학교법인 울산공업학원 Tool steel having a complex coating layer and method of the same
CN104002516A (en) * 2014-06-10 2014-08-27 上海理工大学 CrAlN/MoS2 multi-layered coating layer with high rigidity and low friction coefficient and preparation method thereof
CN104131256A (en) * 2014-07-25 2014-11-05 广东工业大学 Multilayer nanometer composite cutting tool coating and preparation method thereof
CN105256273A (en) * 2015-11-08 2016-01-20 宜昌后皇真空科技有限公司 Nitrogen boron titanium/ nitrogen silicon aluminum titanium nanometer composite multilayer coating cutter and preparation method thereof
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
EP3404126A1 (en) * 2017-05-19 2018-11-21 Walter Ag Metal cutting tool with multi-layer coating

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114371047A (en) * 2020-10-14 2022-04-19 石家庄铁道大学 Single-layer MoS2Band gap regulating method
CN112628381A (en) * 2020-12-02 2021-04-09 东南大学 Temperature self-adaptive lubricating gear and preparation method thereof

Similar Documents

Publication Publication Date Title
CN114411037B (en) High-entropy alloy and preparation method thereof, and wear-resistant and oxidation-resistant coating and preparation method thereof
US8741111B2 (en) Coated article and method for making said article
CN111455338A (en) Nano multilayer coating, preparation method thereof and cutter with nano multilayer coating coated on surface
CN115044867B (en) TiAlWN coating and preparation method and application thereof
CN108977775A (en) A kind of TiAlSiN coated cutting tool preparation process
CN113235041A (en) AlCrTiSiWMoN high-entropy alloy nitride coating and preparation method and application thereof
CN112359327A (en) Preparation method of titanium alloy cutting tool coating, coating and tool
CN111778485B (en) Coating and preparation method thereof
CN111304612B (en) CrAlN/AlN nano multilayer coating with high hardness and high oxidation resistance and preparation method thereof
CN105441945B (en) A kind of nano coating of high rigidity low-friction coefficient and preparation method thereof
CN107354429A (en) The composite coating that a kind of physical vaporous deposition is prepared on saw blade
CN107354437A (en) A kind of multi-layer composite coatings for improving saw blade cutting speed
KR20150116523A (en) Coating layer of zirconium composite material and method of forming the coating layer
CN111962036B (en) Nano multilayer coating, preparation method thereof and cutter with nano multilayer coating coated on surface
CN106756833A (en) A kind of high rigidity TiCrN/TiSiN nano-multilayered structures coatings and preparation method thereof
CN113564526B (en) Composite coating film and preparation method and application thereof
CN115198233A (en) Preparation method of PVD (physical vapor deposition) nano coating for die milling blade
CN114774857A (en) TiAlCrN micro-nano coating and preparation method thereof
US8722180B2 (en) Coated article and method for making said article
CN113913746A (en) Coating, method for producing the same and device
CN109338312B (en) Silver-containing chromium nitride-based hard nano-structure composite film and preparation method thereof
CN1661132A (en) Hard coat and fabricating method
CN115261774B (en) Gradient superhard composite film layer for cutting edge of high-speed blanking die of aluminum alloy pop can cover and preparation method of gradient superhard composite film layer
CN117026148B (en) Corrosion-resistant wear-resistant high-temperature-resistant coating material for PVD (physical vapor deposition) and preparation method thereof
RU2780078C1 (en) Method for obtaining multilayer nanocomposite coating

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
RJ01 Rejection of invention patent application after publication

Application publication date: 20200728

RJ01 Rejection of invention patent application after publication