CN110484870A - A kind of multicomponent nitride hard coating and its preparation method and application - Google Patents
A kind of multicomponent nitride hard coating and its preparation method and application Download PDFInfo
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- CN110484870A CN110484870A CN201910754387.2A CN201910754387A CN110484870A CN 110484870 A CN110484870 A CN 110484870A CN 201910754387 A CN201910754387 A CN 201910754387A CN 110484870 A CN110484870 A CN 110484870A
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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
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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
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
Abstract
The invention belongs to surface protection coating Material Field, a kind of multicomponent nitride hard coating and its preparation method and application is disclosed.The hard coat includes N layer of (TiAlCrTaW), and N layers of (TiAlCrTaW) is in the form of a column crystals growth structure, and chemical molecular formula is (TiaAlbCrcTadWe) N, wherein a+b+c+d+e=1；0.2≤a≤0.5；0.2≤b≤0.5；0≤c≤0.2；0≤d≤0.2；0≤e≤0.2.The hard coat has excellent thermal structure, mechanical stability, inoxidizability and wear resistance；Hardness number when deposited is 30~40GPa, and elasticity modulus is 400~500GPa；Hardness number at 900 DEG C is 35~45GPa, and elasticity modulus is 450~550GPa.
Description
Technical field
The invention belongs to Materials Science and Engineering technical fields, apply more particularly, to a kind of multicomponent nitride hard
Layer and its preparation method and application.
Background technique
With the fast development of modern cutting technology, especially high-speed cutting and DRY CUTTING, performance to cutting tool and
More stringent requirements are proposed for Service Environment.And coated cutting tool combine surface covering high rigidity, high-wearing feature, low-friction coefficient and
Matrix high tenacity, high-intensitive advantage, greatly improve the cutting ability of cutter, improve processing efficiency, while coating material
As chemical barrier and thermodynamic barrier, reduce the diffusion and chemical reaction between cutter and workpiece, to reduce cutter mill
Damage, extends cutting-tool's used life, has become the center of gravity of modern cutting technology.
Al substitutes the metastable phase MeAlN coating tool that part Me is formed in magnesium-yttrium-transition metal nitride MeN (Me=Ti, Cr etc.)
There are high rigidity, high-melting-point and good inoxidizability to be widely used as cutting tool coating material, wherein TiAlN coating has good
Red hardness, and CrAlN is excellent in inoxidizability.With the continuous renewal of industrial materials, it is related specifically to some difficulties
The machining of rapidoprint forms, and local service temperature is higher than 900 DEG C.Severe high-temperature service environment will lead to MeAlN painting
The phase decomposition of layer, while antioxygenic property sharply declines, and finally causes the premature failure of coated cutting tool.This height to cutter coat
Especially more stringent requirements are proposed for thermal stability and inoxidizability and high temperature wear resistance for warm resistance.
By add alloying element (V, Cr, Y, W, Ta etc.) Lai Gaishan cutter coat (such as TiAlN coating) performance by
Gradually become the focus on research direction of cutter coat.As the introducing of Cr can improve the inoxidizability of TiAlN coating；The introducing of Ta is to it
Thermal stability influences significant；The addition of W can significantly improve its wear-resisting property.However single alloying element addition is to coating performance
Improvement there are certain limitations, such as the addition of excess Cr will lead to poor thermal stability.To realize cutter coat performance
It is comprehensive promoted, the multi-element alloyed method for improving coating performance starts to attract attention.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art and disadvantage, the primary purpose of the present invention is that providing a kind of multiple groups
First nitride hard coating.The coating has excellent high high-temp stability, high-temperature oxidation resistance and wear resistance.
Another object of the present invention is to provide the preparation method of above-mentioned multicomponent nitride hard coating.This method is based on yin
Polar arc vapor deposition techniques adjust coating composition by adjusting alloy target material component ratio.
Still a further object of the present invention is to provide the application of above-mentioned multicomponent nitride hard coating.
The purpose of the present invention is realized by following technical proposals:
A kind of multicomponent nitride hard coating, the hard coat includes N layers of (TiAlCrTaW), described
(TiAlCrTaW) N coating is in the form of a column crystals growth structure, and chemical molecular formula is (TiaAlbCrcTadWe) N, wherein a+b+c+d+e
=1；0.2≤a≤0.5；0.2≤b≤0.5；0≤c≤0.2；0≤d≤0.2；0≤e≤0.2.
Preferably, the hardness number when hard coat deposited is 30~40GPa, and elasticity modulus is 400~500GPa.
Preferably, hardness number of the hard coat at 900 DEG C be 35~45GPa, elasticity modulus be 450~
550GPa。
The multicomponent nitride hard coating, comprises the following specific steps that:
S1. the basis material after cleaning drying is put into PVD vacuum coating chamber, and is evacuated to 1~6 × 10-3Pa；
S2. heating cavity to 300~400 DEG C and keeps constant temperature, is passed through Ar controlled atmosphere section chamber pressure, carries out high energy to matrix
Beam ion etch cleaner；
S3. Ar air valve is closed, N is passed through2, chamber pressure is adjusted, corresponding target is lighted using cathodic arc evaporation sedimentation
And target current is set, under nitrogen atmosphere, bias is set as -80~-150V, deposits (TiaAlbCrcTadWe) N coating, it is made
Multicomponent nitride hard coating.
Preferably, basis material described in step S1 is hard alloy or high-speed steel.
It is further preferable that the hard alloy is WC-Co-TiC, WC-Co, WC-TiC-TaC (NbC)-Co alloy.
Preferably, chamber pressure described in step S2 is 0.5~1Pa.
Preferably, chamber pressure described in step S3 is 2~4Pa, and the target current is 65~95A.
Preferably, the time of deposition described in step S3 is 60~120min.
Application of the multicomponent nitride hard coating in turning, milling and drilling manufacture field.
The present invention is based on cathodic arc evaporation deposition techniques, realize ingredient regulation by multi-element alloyed approach, are had
There is (the Ti of excellent high high-temp stability, high-temperature oxidation resistance and wear resistanceaAlbCrcTadWe) N hard coat.Pass through target
The ingredient of material designs the regulation to realize coating composition, on the basis of TiAlN coating, introduces Cr alloying element, can promote
Coating surface densification (Al, Cr) under high temperature2O3The formation of oxide effectively prevents the further oxidation of coating；Introduce Ta alloy member
Element, the polymerization energy that can significantly improve coating system overcome list so that coating keeps good structural stability at high temperature
The poor disadvantage of thermal stability caused by one Cr alloying, while the introducing of Ta element can be with Cr element in terms of inoxidizability
Complementation is formed, (Ti is madeaAlbCrcTadWe) N in biggish temperature window keeps excellent inoxidizability, compensate for single Cr
Alloying is in high temperature section (especially temperature >=900 DEG C) antioxidative deterioration；W element can be on surface during friction
A kind of Magn é li phase is generated, the coefficient of friction of coating is significantly reduced, makes (TiaAlbCrcTadWe) N show it is excellent wear-resistant
Performance.By to (TiaAlbCrcTadWe) N coating composition design so that (TiaAlbCrcTadWe) N hard coat is being higher than
Excellent comprehensive performance, such as high-temperature stability, high-temperature oxidation resistance and wear resistance are shown at a temperature of 900 DEG C, into one
Step enriches cutter coat selective system, meets the needs of modern machining.
Compared with prior art, the invention has the following advantages:
1. (Ti of the inventionaAlbCrcTadWe) N hard coat, it shows polycrystalline structure and is in the form of a column crystals growth, which exists
Service temperature has excellent high high-temp stability, high-temperature oxidation resistance and wear resistance in the case of being higher than 900 DEG C.
2. multicomponent nitride hard coating of the invention at high temperature can relative to MeAlN (Me=Ti, Cr) coating
It is obvious to postpone coating phase transition temperature, the high high-temp stability of coating is improved, coating is made to show apparent ageing strengthening effect
Fruit；Good oxygen diffusion barrier layer is formed in coating surface simultaneously, slows down oxidation course under high temperature, coating is in wider temperature
Window shows excellent antioxygenic property；The generation that phase is lubricated in friction process significantly improves the wear resistance of coating.
3. preparation method of the invention is simple, strong operability, controllability is good, is suitable for component of machine, knife/mold etc.
The protection of product surface has preferable economic benefit.
Detailed description of the invention
Fig. 1 is the XRD spectrum of TiAlCrN, TiAlCrTaN and TiAlCrTaWN hard coat in embodiment 1-3.
Fig. 2 is the section secondary electron shape of TiAlCrN, TiAlCrTaN and TiAlCrTaWN hard coat in embodiment 1-3
Looks.
Fig. 3 is TiAlCrN, TiAlCrTaN and TiAlCrTaWN hard coat vacuum at different temperatures in embodiment 1-3
XRD spectrum after annealing.
Fig. 4 is TiAlCrN, TiAlCrTaN and TiAlCrTaWN hard coat vacuum at different temperatures in embodiment 1-3
(a) nano-indentation hardness and (b) elasticity modulus after annealing.
Fig. 5 is TiAlCrN, TiAlCrTaN and TiAlCrTaWN hard coat constant temperature at different temperatures in embodiment 1-3
Fracture cross-sectional scans sem image after aoxidizing 5h.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
The present invention is based on cathodic arc evaporation deposition techniques, using PVD vacuum coating equipment (GDUT-HAS500) in nitrogen ring
Different multicomponent alloy hard coats is prepared in border.Wherein the alloy target material of seven kinds of heterogeneity ratios is used to prepare
(TiAlCrTaW) N coating of tie element, target material composition is respectively Ti50Al50、Ti40Al50Cr10、Ti30Al50Cr10Ta10、
Ti30Al50Cr10W10、Ti20Al20Cr20Ta20W20、Ti30Al30Cr20Ta10W10、Ti25Al30Cr15Ta15W15。
Embodiment 1
Hard alloy substrate (WC-8wt.%Co-4wt.%TiC) is processed by shot blasting, it is super by acetone, dehydrated alcohol
Sound wave cleans 60min, is packed on vacuum chamber charging tray after being dried up with general nitrogen.It opens heater and is warming up to 350 DEG C, heating process is beaten
Vacuum system is opened, vacuum degree 5 × 10 is evacuated to chamber-3Pa or less.It is passed through Ar gas, adjusting chamber pressure is 0.55Pa, right
Matrix carries out energetic beam ions etch cleaner, closes Ar air valve, is passed through N2Gas velocity is 300sccm, and control chamber pressure is 3Pa.
Adjusting workpiece rotating frame bias is -100V, lights Ti40Al50Cr10Alloy target material, setting target current are 80A, deposit 60min, In
Cemented carbide substrate surfaces prepare Ti0.42Al0.47Cr0.11N hard coat (is labeled as TiAlCrN).
Embodiment 2
Difference from Example 1 is: the alloy target material is Ti30Al50Cr10Ta10Target, prepared coating are
Ti0.34Al0.48Cr0.11Ta0.07N (is labeled as TiAlCrTaN).
Embodiment 3
Difference from Example 1 is: the alloy target material is Ti20Al20Cr20Ta20W20Target, prepared coating are
Ti0.20Al0.20Cr0.20Ta0.20W0.20N (is labeled as TiAlCrTaWN).
Embodiment 4
Difference from Example 1 is: the alloy target material is Ti30Al50Cr10W10Target, prepared coating are
Ti0.34Al0.47Cr0.11W0.08N。
Embodiment 5
Difference from Example 1 is that the alloy target material is Ti30Al30Cr20Ta10W10Target, prepared coating are
Ti0.30Al0.30Cr0.20Ta0.10W0.10N。
Embodiment 6
Difference from Example 1 is that the alloy target material is Ti25Al30Cr15Ta15W15Target, prepared coating are
Ti0.25Al0.30Cr0.15Ta0.15W0.15N。
Comparative example 1
Difference from Example 1 is: the alloy target material is Ti50Al50Target, prepared coating are Ti0.50Al0.50N。
Chemical composition such as 1 institute of table of seven kinds of different target material compositions and corresponding coating in above-described embodiment 1~6 and comparative example 1
Show.
1 target material composition of table and corresponding coating chemical composition
Coating cross sections pattern is seen using scanning electron microscope (FEI Nova NanoSEM 430) in the present invention
Examine analysis；Carry out vacuum heat treatment experiment using high-temperature vacuum annealing furnace, to select heat treatment temperature be respectively 700 DEG C, 800 DEG C,
900 DEG C, 1000 DEG C, 1100 DEG C, heating rate 10K/min, soaking time 30min take the mode of furnace cooling, rear to utilize
X-ray diffractometer (BRUKER D8) characterizes the phase structure after coating deposited and annealing, and utilizes nano-hardness tester
The hardness and elastic modulus of annealed state sample is characterized using load modes are determined；850 DEG C and 900 DEG C are carried out to coating sample
Constant temperature oxidation experiment, constant temperature duration 5h characterize oxidation section using scanning electron microscope.
Fig. 1 is Ti in embodiment 1-30.42Al0.47Cr0.11N(TiAlCrN)、Ti0.34Al0.48Cr0.11Ta0.07N
(TiAlCrTaN) and Ti0.20Al0.20Cr0.20Ta0.20W0.20The XRD spectrum of N (TiAlCrTaWN) coating deposited, all coatings
Typical face-centred cubic structure is all shown, relative to TiAlN coating in comparative example 1, with solid after alloying elements cr, Ta, W introducing
The form of solution exists, and will lead to diffraction cutting edge of a knife or a sword position and deviates to high angle；Fig. 2 is Ti in embodiment 1-30.42Al0.47Cr0.11N、
Ti0.34Al0.48Cr0.11Ta0.07N and Ti0.20Al0.20Cr0.20Ta0.20W0.20The section secondary electron pattern of N coating, three kinds of coatings
All show apparent column crystal growth morphology.
Fig. 3 is Ti in embodiment 1-30.42Al0.47Cr0.11N、Ti0.34Al0.48Cr0.11Ta0.07N and
Ti0.20Al0.20Cr0.20Ta0.20W0.20N coating anneal at a temperature of 700 DEG C, 800 DEG C, 900 DEG C, 1000 DEG C, 1100 DEG C after XRD
Map.Relative to TiAlN coating in comparative example 1, Ti0.42Al0.47Cr0.11N and Ti0.34Al0.48Cr0.11Ta0.07N coating exists respectively
Start w-AlN occur at 900 DEG C and 1000 DEG C, and Ti0.20Al0.20Cr0.20Ta0.20W0.20N coating can obviously postpone w-AlN's
Temperature is generated to 1100 DEG C, wherein the generation of w-AlN can have an adverse effect to coating mechanical property.In addition,
Ti0.34Al0.48Cr0.11Ta0.07N and Ti0.20Al0.20Cr0.20Ta0.20W0.20The thermal decomposition process of N coating is also centainly inhibited,
It can be seen that and be reacted in mechanical property performance from the corresponding nano hardness of Fig. 4 and elasticity modulus characterization curve
Ti0.20Al0.20Cr0.20Ta0.20W0.20Hardness number of the N coating in deposited is 34.3GPa, and elasticity modulus 480GPa works as temperature
When degree is increased to 900 DEG C, the hardness number of 35.8GPa can still be maintained, and elasticity modulus is 497GPa.
Fig. 5 is Ti in embodiment 1-30.42Al0.47Cr0.11N、Ti0.34Al0.48Cr0.11Ta0.07N and
Ti0.20Al0.20Cr0.20Ta0.20W0.20Fracture cross-sectional scans electron microscope of the N coating at 850 DEG C and 900 DEG C after constant temperature oxidation 5h
Picture.Ti at 850 DEG C0.34Al0.48Cr0.11Ta0.07N and Ti0.20Al0.20Cr0.20Ta0.20W0.20The performance of N coating antioxygenic property is excellent
It is different, and at 850 DEG C vigorous oxidation can occur for TiAlN coating in comparative example 1；At 900 DEG C, Ti0.42Al0.47Cr0.11N complete oxidation,
Ti0.34Al0.48Cr0.11Ta0.07N coating largely aoxidizes, and Ti0.20Al0.20Cr0.20Ta0.20W0.20N coating still maintains higher
Inoxidizability, and surface oxides compact structure, to being diffused with certain barrier effect in oxygen.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of multicomponent nitride hard coating, which is characterized in that the hard coat includes N layers of (TiAlCrTaW), described
(TiAlCrTaW) N coating is in the form of a column crystals growth structure, and chemical molecular formula is (TiaAlbCrcTadWe) N, wherein a+b+c+d+e
=1；0.2≤a≤0.5；0.2≤b≤0.5；0≤c≤0.2；0≤d≤0.2；0≤e≤0.2.
2. multicomponent nitride hard coating according to claim 1, which is characterized in that when the hard coat deposited
Hardness number be 30~40GPa, elasticity modulus be 400~500GPa.
3. multicomponent nitride hard coating according to claim 1, which is characterized in that the hard coat is at 900 DEG C
When hardness number be 35~45GPa, elasticity modulus be 450~550GPa.
4. multicomponent nitride hard coating according to claim 1-3, which is characterized in that including following specific
Step:
S1. the basis material after cleaning drying is put into PVD vacuum coating chamber, and is evacuated to 1~6 × 10-3Pa；
S2. heating cavity to 300~400 DEG C and keeps constant temperature, is passed through Ar controlled atmosphere section chamber pressure, to matrix carry out high energy beam from
Sub- etch cleaner；
S3. Ar air valve is closed, N is passed through2, chamber pressure is adjusted, corresponding target is lighted using cathodic arc evaporation sedimentation and is arranged
Target current, under nitrogen atmosphere, bias are set as -80~-150V, deposit (TiaAlbCrcTadWe) N coating, multicomponent is made
Nitride hard coating.
5. the preparation method of multicomponent nitride hard coating according to claim 4, which is characterized in that institute in step S1
Stating basis material is hard alloy or high-speed steel.
6. the preparation method of multicomponent nitride hard coating according to claim 5, which is characterized in that the hard closes
Gold is WC-Co-TiC alloy, WC-Co alloy, WC-TiC-TaC (NbC)-Co alloy.
7. the preparation method of multicomponent nitride hard coating according to claim 4, which is characterized in that institute in step S2
Stating chamber pressure is 0.5~1Pa.
8. the preparation method of multicomponent nitride hard coating according to claim 4, which is characterized in that institute in step S3
Stating chamber pressure is 2~4Pa, and the target current is 65~95A.
9. the preparation method of multicomponent nitride hard coating according to claim 4, which is characterized in that institute in step S3
The time for stating deposition is 60~120min.
10. the described in any item multicomponent nitride hard coatings of claim 1-3 are in turning, milling and drilling manufacture field
Application.
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