CN105839054A - CrAlTiSiN cutter protective coating and preparation method thereof - Google Patents
CrAlTiSiN cutter protective coating and preparation method thereof Download PDFInfo
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- CN105839054A CN105839054A CN201610347127.XA CN201610347127A CN105839054A CN 105839054 A CN105839054 A CN 105839054A CN 201610347127 A CN201610347127 A CN 201610347127A CN 105839054 A CN105839054 A CN 105839054A
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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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3464—Sputtering using more than one target
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C28/04—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 only coatings of inorganic non-metallic material
- C23C28/044—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 only coatings of inorganic non-metallic material coatings specially adapted for cutting tools or wear applications
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Abstract
The invention discloses a CrAlTiSiN cutter protective coating. The CrAlTiSiN cutter protective coating comprises the following elements according to atomic ratio: 12-16% of Cr, 20-24% of Al, 4-8% of Ti, 6-10% of Si and 48-52% of N. The invention also provides a preparation method of the cutter protective coating. The preparation method of the cutter protective coating comprises the following steps: firstly carrying out ultrasonic washing and ionic washing on a substrate; conveying the washed substrate to a sputtering chamber and depositing a CrN transition layer on the substrate; depositing a CrAlN transition layer on the substrate on which the CrN transition layer is deposited; and depositing a CrAlTiSi nano composite coating on the substrate on which the CrAlN transition layer is deposited by using a CrAlTiSi composite target controlled by a radio frequency cathode. According to the CrAlTiSiN cutter protective coating and the preparation method thereof, the CrAlTiSi coating has hardness being higher than 40GPa; the CrAlTiSi coating has excellent high-temperature service performance and can be applied to high-speed cutting tools subjected to service at 1000 DEG C.
Description
Technical field
The invention belongs to materialogy field, relate to consistent process for modifying surface, specifically a kind of CrAlTiSiN cutter protection
Property coating and preparation method thereof.
Background technology
Along with the development of modern mechanical processing industry, people propose the highest requirement to cutting tool.In cutting
In processing, cutting performance has the impact of decision to the efficiency of machining, precision, surface quality.Two passes of cutting performance
Key index hardness and intensity, always also exist contradiction between them, the strength of materials that hardness is high is low, and improve intensity often with
Hardness be reduced to cost.In order to solve this contradiction present in Hardmetal materials, preferably improve the machinability of cutter
Can, a kind of relatively effective method is to use various coating technologies, coats last layer high rigidity, high wear resistance on tool matrix
The coating material of performance, combines tool matrix with hard coat, so that the performance of cutter is greatly improved.On tool surface
Coating as a chemical barrier and thermodynamic barrier, decrease the crescent hollow abrasion of cutter, can significantly increase and add work efficiency
Rate, raising machining accuracy, tool life, reduction processing cost.
But, along with the development of the technology such as high accuracy, high-speed cutting, DRY CUTTING, the deterioration of cutter Service Environment, to painting
Overlay on the coating performance on its surface and it is also proposed higher requirement, high rigidity to be possessed, high elastic modulus, wearability and tough
The mechanical performances such as property, the mechanical behavior under high temperature of high temperature oxidation resistance to be possessed, corrosion resistance and excellence.Traditional coating,
As TiN, CrN even TiAlN coating the most gradually can not meet the performance requirement of harshness.In recent years, based on Cr, Al, Ti, Si, N five
The CrAlTiSiN protective coating that kind of essential element is formed is owing to having nano composite structure so that it is have the hardness of superelevation, excellent
Different wearability, corrosion resistance and high-temperature stability, CrAlTiSi coating not only has the hardness higher than 40GPa, and has
Excellent high-temperature service performance, can meet the high speed cutting tool carrying out being on active service at 1000 DEG C, and this coating material has become new one
For the representative of high-performance protective coating, can be coated with as the protection of high-speed cutting, the cutter coat of DRY CUTTING and other field
Layer.
At present, understand CrAlTiSiN coating by inquiry document and report seldom in the patent literature, by update search, with
Coating that CrAlTiSiN coating composition is close and preparation method thereof has a following Patents:
The patent of Application No. 201310132567.X relates to a kind of NC cutting tool with CrAlTiN superlattice coating and system thereof
Preparation Method, including ultra-fine cemented carbide cutter body, cutter body outside deposition includes Ti metal adhesion layers, TiN
Supporting the multi-layer wear-resistant layer that layer, CrAlN layer are alternately constituted with TiN layer, it is resistance to that the present invention can solve NC cutting tool of the prior art
Mill poor performance, the problem that coefficient of friction is higher, there is the advantage that hardness is higher and anti-wear performance good, coefficient of friction is relatively low, can
To significantly improve the life-span of cutter, improve the surface quality of processing component.
The patent of Application No. 201410152265.3 discloses a kind of matrix protective coating with ultrahigh hardness and system
Preparation Method.The described layer structure that matrix protective coating is two layers with ultrahigh hardness, the coating near matrix is TiAlN mistake
Crossing layer, the surface of TiAlN transition zone is fine and close CrAlTiN quaternary ceramic coating.Its preparation method is first by surface clean
After matrix use multi-arc ion coating reactive deposition TiAlN transition zone, CrAlTiN quaternary ceramic coating successively on its surface.This
The preparation method of the matrix protective coating with ultrahigh hardness of invention has stable preparation process, deposition velocity is fast, be prepared as
This is low, and finally CrAlTiN coating and the bond strength advantages of higher of matrix.
The patent of Application No. 201510253841.8 discloses a kind of high rigidity CrAlSiN nano composite structure protectiveness
Coating and preparation method thereof, preparation comprises the steps: that (1) matrix cleans, then carries out Ion Cleaning；(2) CrN transition zone system
Standby: the matrix after step (1) being processed is delivered to sputtering chamber and carried out depositing CrN transition zone, and Cr target is by DC cathode control, deposition
The CrN transition zone of 200-300nm；(3) prepared by CrAlSiN layer: CrAlSi composite target material is by radio frequency cathodic control, in CrN transition
The CrAlSiN nano-composite coating of layer surface deposition 2～4 μm.Coating of the present invention not only has high rigidity 43.6GPa, and
And there is excellent high temperature oxidation resistance and corrosion resistance.
The patent of Application No. 201410436236.X discloses a kind of containing CrAlVN layer with the composite coating of CrAlSiN layer
Cutter and preparation method thereof.This composite coating layer cutter includes tool matrix and the composite coating being deposited on tool matrix, compound
Coating includes the periodicity coating of CrAlVN layer and CrAlSiN layer described in an alternating deposit, CrAlVN layer and CrAlSiN layer altogether
Lattice are epitaxially grown to superstructure.Preparation method includes pre-processing tool matrix, then selectively deposits transition zone,
Redeposited CrAlVN layer and the periodicity coating of CrAlSiN layer, obtain composite coating layer cutter.The composite coating layer cutter tool of the present invention
There are the advantages such as self lubricity, high rigidity, high-heat performance and low-friction coefficient.
The patent of Application No. 201110344681.X discloses a kind of high temperature oxidation corrosion resistance performance and excellent mechanical
The CrAlSiN gradient coating new technology of energy.Many target reaction magnetocontrol sputterings method is used to be coated with in substrate surface deposition CrAlSiN gradient
Layer, its preparation process is divided into continuous four-stage and carries out: the first stage prepares Cr gradient coating；Second stage prepares CrAl gradient
Coating；Phase III prepares CrAlN gradient coating；Fourth stage prepares CrAlSiN gradient coating, more annealed processes.
The present invention changes micro-structural in gradient by each elemental composition of appropriate design, makes coating oxidation resistance temperature reach 950 DEG C, and hardness number reaches
More than 37GPa, with base material adhesive force higher than 34N, and coating also has the anti-thermal shock of excellence, the performance such as wear-resistant.
The patent of Application No. 201410044737.3 discloses a kind of TiN/CrAlSiN nanocomposite laminated coating and system
Preparation Method.Described TiN/CrAlSiN nanocomposite laminated coating is the most heavy by CrAlSiN layer and the TiN layer of nano composite structure
Amassing and formed on matrix, one layer of close matrix is TiN layer, and the superiors are the CrAlSiN layer of nano composite structure；Described TiN/
CrAlSiN nanocomposite laminated coating thickness is 2.0-3.2 μm, and the CrAlSiN layer thickness of described nano composite structure is
1.2nm, described TiN layer thickness is 6.0nm.Its preparation method includes cleaning matrix and alternating sputtering CrAlSiN layer and TiN layer
Deng 2 steps.This TiN/CrAlSiN nanocomposite laminated coating hardness is higher, when the atomic ratio of Si Yu CrAl, i.e. Si:CrAl
During for 5:20, its hardness is up to 39.7GPa.
From patent documents above analysis, in the prior art, not open be applicable to high-speed cutting high rigidity,
The CrAlTiSiN protective coating of high antioxygenic property and preparation method, and prepared by the preparation method of prior art
In journey, energy consumption is relatively big, the shortcomings such as cost is high and inefficient.
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of CrAlTiSiN cutter protection coating
And preparation method thereof, described this CrAlTiSiN cutter protection coating and preparation method thereof to solve of the prior art
The cutting of cutter protection coating improper high temperature and high speed, the technical problem of DRY CUTTING, and in preparation process, energy consumption is relatively big, becomes
This high and inefficient technical problem.
The invention provides a kind of CrAlTiSiN cutter protection coating, described coating is by Cr, Al, Ti, Si and N element
Composition, wherein the atomic ratio of Cr, Al, Ti, Si, N is 12-16%, 20-24%, 4-8%, 6-10% and 48-52%.
Present invention also offers the preparation method of above-mentioned a kind of CrAlTiSiN cutter protection coating, including walking as follows
Rapid:
1) step cleaning matrix, utilizes super by the matrix after polishing mirror finish processes in absolute ethyl alcohol and acetone
Sound wave cleans 5-10min；Then carry out Ion Cleaning: load Sample Room after being installed by sample, after vacuumizing, open Ar gas, remain true
Reciprocal of duty cycle, at 2-4Pa, carries out the Ions Bombardment of 20 ~ 40min to described matrix, and power is 100-120W；
2) step preparing CrN transition zone, the matrix after step 1) being processed is delivered to sputtering chamber, is passed through DC power control
Cr target, the background vacuum of vacuum chamber is less than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power is
80-120W, sputtering time is 5-10min, carries out depositing the CrN transition zone of 100-200nm；
3) step preparing CrAlN transition zone, by step 2) process after matrix by DC power control CrAl target, its
The atomic ratio of middle Cr:Al is 50%:50%, and the background vacuum of vacuum chamber is less than 510-3Pa, sputtering atmosphere uses Ar and N2's
Mixed gas, sputtering power is 80-120W, and sputtering time is 5-10min, carries out depositing the CrAlN transition zone of 100-200nm；
4) step preparing CrAlTiSiN main body coating, the matrix after step 3) being processed deposits, radio frequency negative electrode control
CrAlTiSi composite target material processed, wherein the atomic ratio of Cr, Al, Ti and Si is 28%:44%:12%:16%, the base vacuum of vacuum chamber
Degree is less than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power is 240-300W, and sputtering time is 60-
120min, heats during matrix deposition, the CrAlTiSiN main body coating of deposition 2-5 μm.
Further, described matrix is metal, hard alloy or pottery.
Further, described CrAlN transition zone is the CrAl alloy target material system that the atomic ratio utilizing Cr and Al is 50%:50%
Standby.
Further, described CrAlTiSiN main body coating be the atomic ratio utilizing Cr, Al, Ti and Si be 28%:44%:
Prepared by the CrAlTiSi composite target material of 12%:16%.
Further, step 2), 3) and 4) in, N2/ Ar flow-rate ratio scope is 1/2-1.
Further, step 2), 3) and 4) in, the air pressure range of coating deposition is 0.2-0.6Pa.
Further, in described step 1), the cleaning frequency of ultrasonic wave is 15-30kHz, described step 2) and 3) in argon
Throughput is 30-50sccm, and nitrogen flow is 15-25sccm.
Further, in step 4), heating temperature range during matrix deposition 200-400 DEG C.
The coated body that the present invention proposes is the CrAlTiSiN coating with five kinds of element compositions of Cr, Al, Ti, Si, N, should
Coating has Si3N4The nano composite structure of nanocrystal phase is wrapped up at interface mutually, and the addition of Cr, Al, Ti simultaneously makes nanocrystal phase
There is higher solution strengthening effect, therefore, this coating not only has the hardness higher than 40GPa, and has excellent height
Warmly take labour performance, the high speed cutting tool carrying out being on active service at 1000 DEG C can be met, the coating production that simultaneously the present invention relates to
Have that technique is simple, deposition velocity fast, low cost, bond strength high, can cut as high temperature and high speed, DRY CUTTING
Cutter coat and the protective coating of other field.
Detailed description of the invention
Below by specific embodiment, the present invention will be described in detail, but is not limited to present invention.
Instrument used in the preparation method of the present invention is respectively as follows:
JGP-450 type many targets dual chamber magnetic control sputtering system；
M308457 supersonic wave cleaning machine；
Method of testing of the present invention:
EDAX energy disperse spectroscopy (EDS) analysis ingredient；
D/MAX 2550 VB/PC type X-ray diffractometer (XRD) measures thing phase composition；
NANO Indenter G200 type nano-hardness tester measures consistency and elasticity modulus.
Floating coat of the present invention uses reactive sputtering to prepare on JGP-450 type multi-target magnetic control sputtering instrument.Employing high-speed steel,
Hard alloy etc. are as matrix, and the ion carrying out 30min in loading vacuum chamber after acetone and absolute ethyl alcohol Ultrasonic Cleaning is clear
Wash, then use direct current or RF-reactively sputtered titanium method deposition.
Embodiment 1
The preparation method of a kind of CrAlTiSiN cutter protection coating being suitable for high-speed cutting that the present invention proposes, including such as
Lower step:
(1) matrix cleans
Matrix after polishing mirror finish processes is utilized Ultrasonic Cleaning 5min in absolute ethyl alcohol and acetone；Then carry out
Ion Cleaning, opens Ar gas after vacuumizing, maintain vacuum at 2Pa, described matrix carries out the Ions Bombardment of 30min, and power is
100W；
(2) prepared by CrN transition zone
Matrix after step 1) being processed delivers to sputtering chamber, and by DC power control Cr target, the background vacuum of vacuum chamber is excellent
In 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, d.c. sputtering power is 80W, and sputtering time is 5min, carries out
The CrN transition zone of deposition 100nm；
(3) prepared by CrAlN transition zone
By step 2) process after matrix by DC power control CrAl target, wherein the atomic ratio of Cr:Al is 50%:50%, very
The background vacuum of empty room is less than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power is 120W, sputtering
Time is 10min, carries out depositing the CrAlN transition zone of 200nm；
(4) prepared by CrAlTiSiN main body coating
Matrix after step 3) being processed deposits, and controls CrAlTiSi target, N by radio-frequency power supply2Throughput: 15sccm；
Ar throughput: 30sccm；Total gas pressure: 0.4Pa；Temperature: 200 DEG C；Radio-frequency power supply power: 300W, sedimentation time: 120min.Warp
Analyzing test, in CrAlTiSiN coating, the atomic ratio of Cr, Al, Ti, Si, N is 12%, 23%, 8%, 7% and 50%, it is thus achieved that coating is hard
Degree is 44.6GPa, and coating layer thickness is 4.6 μm.
Embodiment 2
The preparation method of a kind of CrAlTiSiN cutter protection coating being suitable for high-speed cutting that the present invention proposes, including such as
Lower step:
(1) matrix cleans
Matrix after polishing mirror finish processes is utilized Ultrasonic Cleaning 10min in absolute ethyl alcohol and acetone；Then enter
Row Ion Cleaning, opens Ar gas after vacuumizing, maintain vacuum at 2Pa, described matrix carries out the Ions Bombardment of 30min, power
For 120W；
(2) prepared by CrN transition zone
Matrix after step 1) being processed delivers to sputtering chamber, and by DC power control Cr target, the background vacuum of vacuum chamber is excellent
In 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, d.c. sputtering power is 100W, and sputtering time is 10min, enters
The CrN transition zone of row deposition 200nm；
(3) prepared by CrAlN transition zone
By step 2) process after matrix by DC power control CrAl target, wherein the atomic ratio of Cr:Al is 50%:50%, very
The background vacuum of empty room is less than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power is 100W, sputtering
Time is 10min, carries out depositing the CrAlN transition zone of 180nm；
(4) prepared by CrAlTiSiN main body coating
Matrix after step 3) being processed deposits, and controls CrAlTiSi target, N by radio-frequency power supply2Throughput: 20sccm；
Ar throughput: 40sccm；Total gas pressure: 0.6Pa；Temperature: 300 DEG C；Radio-frequency power supply power: 240W, sedimentation time: 60min.Through dividing
Analysis test, in CrAlTiSiN coating, the atomic ratio of Cr, Al, Ti, Si, N is 16%, 22%, 7%, 7% and 48%, it is thus achieved that coating hardness
For 41.5GPa, coating layer thickness is 2.4 μm.
Embodiment 3
The preparation method of a kind of CrAlTiSiN cutter protection coating being suitable for high-speed cutting that the present invention proposes, including such as
Lower step:
(1) matrix cleans
Matrix after polishing mirror finish processes is utilized Ultrasonic Cleaning 10min in absolute ethyl alcohol and acetone；Then enter
Row Ion Cleaning, opens Ar gas after vacuumizing, maintain vacuum at 2Pa, described matrix carries out the Ions Bombardment of 30min, power
For 100W；
(2) prepared by CrN transition zone
Matrix after step 1) being processed delivers to sputtering chamber, and by DC power control Cr target, the background vacuum of vacuum chamber is excellent
In 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, d.c. sputtering power is 90W, and sputtering time is 5min, carries out
The CrN transition zone of deposition 100nm；
(3) prepared by CrAlN transition zone
By step 2) process after matrix by DC power control CrAl target, wherein the atomic ratio of Cr:Al is 50%:50%, very
The background vacuum of empty room is less than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power is 90W, sputtering
Time is 10min, carries out depositing the CrAlN transition zone of 120nm；
(4) prepared by CrAlTiSiN main body coating
Matrix after step 3) being processed deposits, and controls CrAlTiSi target, N by radio-frequency power supply2Throughput: 25sccm；
Ar throughput: 60sccm；Total gas pressure: 0.6Pa；Temperature: 400 DEG C；Radio-frequency power supply power: 280W, sedimentation time: 90min.Through dividing
Analysis test, in CrAlTiSiN coating, the atomic ratio of Cr, Al, Ti, Si, N is 12%, 20%, 8%, 9% and 51%, it is thus achieved that coating hardness
For 42.9GPa, coating layer thickness is 3.9 μm.
Embodiment 4
The preparation method of a kind of CrAlTiSiN cutter protection coating being suitable for high-speed cutting that the present invention proposes, including such as
Lower step:
(1) matrix cleans
Matrix after polishing mirror finish processes is utilized Ultrasonic Cleaning 10min in absolute ethyl alcohol and acetone；Then enter
Row Ion Cleaning, opens Ar gas after vacuumizing, maintain vacuum at 2Pa, described matrix carries out the Ions Bombardment of 30min, power
For 100W；
(2) prepared by CrN transition zone
Matrix after step 1) being processed delivers to sputtering chamber, and by DC power control Cr target, the background vacuum of vacuum chamber is excellent
In 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, d.c. sputtering power is 120W, and sputtering time is 10min, enters
The CrN transition zone of row deposition 200nm；
(3) prepared by CrAlN transition zone
By step 2) process after matrix by DC power control CrAl target, wherein the atomic ratio of Cr:Al is 50%:50%, very
The background vacuum of empty room is less than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power is 120W, sputtering
Time is 10min, carries out depositing the CrAlN transition zone of 200nm；
(4) prepared by CrAlTiSiN main body coating
Matrix after step 3) being processed deposits, and controls CrAlTiSi target, N by radio-frequency power supply2Throughput: 15sccm；
Ar throughput: 50sccm；Total gas pressure: 0.5Pa；Temperature: 350 DEG C；Radio-frequency power supply power: 260W, sedimentation time: 100min.Warp
Analyzing test, in CrAlTiSiN coating, the atomic ratio of Cr, Al, Ti, Si, N is 15%, 21%, 8%, 8% and 48%, it is thus achieved that coating is hard
Degree is 40.8GPa, and coating layer thickness is 3.5 μm.
Embodiment 5
The preparation method of a kind of CrAlTiSiN cutter protection coating being suitable for high-speed cutting that the present invention proposes, including such as
Lower step:
(1) matrix cleans
Matrix after polishing mirror finish processes is utilized Ultrasonic Cleaning 5min in absolute ethyl alcohol and acetone；Then carry out
Ion Cleaning, opens Ar gas after vacuumizing, maintain vacuum at 2Pa, described matrix carries out the Ions Bombardment of 30min, and power is
100W；
(2) prepared by CrN transition zone
Matrix after step 1) being processed delivers to sputtering chamber, and by DC power control Cr target, the background vacuum of vacuum chamber is excellent
In 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, d.c. sputtering power is 100W, and sputtering time is 10min, enters
The CrN transition zone of row deposition 200nm；
(3) prepared by CrAlN transition zone
By step 2) process after matrix by DC power control CrAl target, wherein the atomic ratio of Cr:Al is 50%:50%, very
The background vacuum of empty room is less than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power is 100W, sputtering
Time is 5min, carries out depositing the CrAlN transition zone of 120nm；
(4) prepared by CrAlTiSiN main body coating
Matrix after step 3) being processed deposits, and controls CrAlTiSi target, N by radio-frequency power supply2Throughput: 25sccm；
Ar throughput: 40sccm；Total gas pressure: 0.2Pa；Temperature: 250 DEG C；Radio-frequency power supply power: 240W, sedimentation time: 120min.Warp
Analyzing test, in CrAlTiSiN coating, the atomic ratio of Cr, Al, Ti, Si, N is 12%, 22%, 8%, 8% and 50%, it is thus achieved that coating is hard
Degree is 43.1GPa, and coating layer thickness is 2.9 μm.
Embodiment 6
The preparation method of a kind of CrAlTiSiN cutter protection coating being suitable for high-speed cutting that the present invention proposes, including such as
Lower step:
(1) matrix cleans
Matrix after polishing mirror finish processes is utilized Ultrasonic Cleaning 10min in absolute ethyl alcohol and acetone；Then enter
Row Ion Cleaning, opens Ar gas after vacuumizing, maintain vacuum at 2Pa, described matrix carries out the Ions Bombardment of 30min, power
For 100W；
(2) prepared by CrN transition zone
Matrix after step 1) being processed delivers to sputtering chamber, and by DC power control Cr target, the background vacuum of vacuum chamber is excellent
In 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, d.c. sputtering power is 80W, and sputtering time is 5min, carries out
The CrN transition zone of deposition 100nm；
(3) prepared by CrAlN transition zone
By DC power control CrAl target, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power is 100W, during sputtering
Between be 5min, carry out deposit 100nm CrAlN transition zone；
(4) prepared by CrAlTiSiN main body coating
Matrix after step 3) being processed deposits, and controls CrAlTiSi target, N by radio-frequency power supply2Throughput: 20sccm；
Ar throughput: 50sccm；Total gas pressure: 0.6Pa；Temperature: 200 DEG C；Radio-frequency power supply power: 280W, sedimentation time: 100min.Warp
Analyzing test, in CrAlTiSiN coating, the atomic ratio of Cr, Al, Ti, Si, N is 13%, 21%, 7%, 8% and 51%, it is thus achieved that coating is hard
Degree is 40.8GPa, and coating layer thickness is 4.1 μm.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a CrAlTiSiN cutter protection coating, it is characterised in that: described coating is by Cr, Al, Ti, Si and N element group
Becoming, wherein the atomic ratio of Cr, Al, Ti, Si, N is 12-16%, 20-24%, 4-8%, 6-10% and 48-52%.
2. the preparation method of a kind of CrAlTiSiN cutter protection coating described in claim 1, it is characterised in that include as follows
Step:
1) step cleaning matrix, utilizes super by the matrix after polishing mirror finish processes in absolute ethyl alcohol and acetone
Sound wave cleans 5-10min；Then carry out Ion Cleaning: load Sample Room after being installed by sample, after vacuumizing, open Ar gas, remain true
Reciprocal of duty cycle, at 2-4Pa, carries out the Ions Bombardment of 20 ~ 40min to described matrix, and power is 100-120W；
2) step preparing CrN transition zone, the matrix after step 1) being processed is delivered to sputtering chamber, is passed through DC power control
Cr target, the background vacuum of vacuum chamber is less than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power is
80-120W, sputtering time is 5-10min, carries out depositing the CrN transition zone of 100-200nm；
3) step preparing CrAlN transition zone, by step 2) process after matrix by DC power control CrAl target, its
The atomic ratio of middle Cr:Al is 50%:50%, and the background vacuum of vacuum chamber is less than 510-3Pa, sputtering atmosphere uses Ar and N2's
Mixed gas, sputtering power is 80-120W, and sputtering time is 5-10min, carries out depositing the CrAlN transition zone of 100-200nm；
4) step preparing CrAlTiSiN main body coating, the matrix after step 3) being processed deposits, radio frequency negative electrode control
CrAlTiSi composite target material processed, wherein the atomic ratio of Cr, Al, Ti and Si is 28%:44%:12%:16%, the base vacuum of vacuum chamber
Degree is less than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power is 240-300W, and sputtering time is 60-
120min, heats during matrix deposition, the CrAlTiSiN main body coating of deposition 2-5 μm.
The preparation method of a kind of CrAlTiSiN cutter protection coating the most as claimed in claim 1, it is characterised in that: described
Matrix is metal, hard alloy or pottery.
The preparation method of a kind of CrAlTiSiN cutter protection coating the most as claimed in claim 1, it is characterised in that: described
CrAlN transition zone is prepared by the CrAl alloy target material that the atomic ratio utilizing Cr and Al is 50%:50%.
The preparation method of a kind of CrAlTiSiN cutter protection coating the most as claimed in claim 1, it is characterised in that: described
CrAlTiSiN main body coating is the CrAlTiSi composition target that the atomic ratio utilizing Cr, Al, Ti and Si is 28%:44%:12%:16%
Prepared by material.
The preparation method of a kind of CrAlTiSiN cutter protection coating the most as claimed in claim 1, it is characterised in that: step
2), 3) and 4) in, N2/ Ar flow-rate ratio scope is 1/2-1.
The preparation method of a kind of CrAlTiSiN cutter protection coating the most as claimed in claim 1, it is characterised in that: step
2), 3) and 4) in, coating deposition air pressure range be 0.2-0.6Pa.
The preparation method of a kind of CrAlTiSiN cutter protection coating the most as claimed in claim 1, it is characterised in that: described
In step 1), the cleaning frequency of ultrasonic wave is 15-30kHz, described step 2) and 3) in argon flow amount be 30-50sccm, nitrogen
Throughput is 15-25sccm.
The preparation method of a kind of CrAlTiSiN cutter protection coating the most as claimed in claim 1, it is characterised in that: step
4) in, heating temperature range during matrix deposition 200-400 DEG C.
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| CN108103465A (en) * | 2017-12-20 | 2018-06-01 | 富耐克超硬材料股份有限公司 | Processing stainless steel special-purpose coat cutter and preparation method thereof |
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| CN108950480A (en) * | 2018-08-22 | 2018-12-07 | 中国科学院力学研究所 | It a kind of high-ductility abrasion-proof composite coating and is deposited onto heat and makees method in convex mold |
| CN109295425A (en) * | 2018-09-28 | 2019-02-01 | 深圳市奥美特纳米科技有限公司 | Cr/CrN/CrAlSiN/CrAlTiSiN nanometer multilayer Gradient Film and preparation method thereof |
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| CN108103465A (en) * | 2017-12-20 | 2018-06-01 | 富耐克超硬材料股份有限公司 | Processing stainless steel special-purpose coat cutter and preparation method thereof |
| CN108220880B (en) * | 2018-01-30 | 2019-11-15 | 上海新弧源涂层技术有限公司 | A kind of high rigidity high corrosion-resistant high-entropy alloy nitride coatings and preparation method thereof |
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| CN108866481A (en) * | 2018-06-06 | 2018-11-23 | 广东工业大学 | A kind of nano combined Al-Ti-V-Cu-N coating and its preparation method and application |
| CN108866481B (en) * | 2018-06-06 | 2021-01-19 | 广东工业大学 | Nano composite Al-Ti-V-Cu-N coating and preparation method and application thereof |
| CN108950480A (en) * | 2018-08-22 | 2018-12-07 | 中国科学院力学研究所 | It a kind of high-ductility abrasion-proof composite coating and is deposited onto heat and makees method in convex mold |
| CN109295425B (en) * | 2018-09-28 | 2020-07-14 | 深圳市奥美特纳米科技有限公司 | Cr/CrN/CrAlSiN/CrAlTiSiN nano multilayer gradient film and preparation method thereof |
| CN109295425A (en) * | 2018-09-28 | 2019-02-01 | 深圳市奥美特纳米科技有限公司 | Cr/CrN/CrAlSiN/CrAlTiSiN nanometer multilayer Gradient Film and preparation method thereof |
| CN109440064A (en) * | 2018-11-14 | 2019-03-08 | 广东工业大学 | A kind of Thermal Conductivity Varying With Temperature cutter coat and preparation method thereof |
| CN110408903A (en) * | 2019-09-16 | 2019-11-05 | 济南大学 | Tool surface multi-component multi-layer coating production |
| CN111304618A (en) * | 2020-04-14 | 2020-06-19 | 上海工具厂有限公司 | Nano composite coating and preparation method thereof |
| CN113737144A (en) * | 2021-08-27 | 2021-12-03 | 西安交通大学 | Al for high-frequency electrotome2O3/CrN composite insulating coating and preparation method thereof |
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