CN106756821A - A kind of Ti Ag N nano-composite coatings and preparation method thereof - Google Patents
A kind of Ti Ag N nano-composite coatings and preparation method thereof Download PDFInfo
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- CN106756821A CN106756821A CN201611164439.3A CN201611164439A CN106756821A CN 106756821 A CN106756821 A CN 106756821A CN 201611164439 A CN201611164439 A CN 201611164439A CN 106756821 A CN106756821 A CN 106756821A
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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
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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- Physical Vapour Deposition (AREA)
Abstract
The invention belongs to metal material surface deposition super hard nano composite coating technology field, specially a kind of Ti Ag N nano-composite coatings and preparation method thereof, technical problem to be solved is:nc‑TiN/a‑Si3N4The great friction coefficient of nano-composite coating causes to produce amount of heat, coated cutting tool rake face still to produce built-up edge in working angles.Nano-composite coating of the invention:Distinguished by the distance from matrix, included successively from inside to outside:N layers of transition zone, the intermediate layer of TiN film formation and Ti Ag that matrix surface Ti films are formed.Its preparation method is completed using arc ion plating (aip), and it is small that nano-composite coating prepared by the method has the advantages that coating toughness is high, film base junction closes strong, coefficient of friction in addition to hardness higher, also.
Description
Technical field:
The invention belongs to metal material surface deposition nano-composite coating technical field, and in particular to a kind of titanium nitride silver
(hereinafter referred to as Ti-Ag-N) nano-composite coating and preparation method thereof.
Background technology:
At present, with the development of national advanced manufacturing technology, traditional hard alloy or high-speed steel tool are proposed
Higher and higher requirement.Machining technique with Digit Control Machine Tool as representative is just sent out towards directions such as high speed, high accuracy, high reliability
Exhibition.NC cutting tool surface-coating technology, is especially improving various with the coated cutting tool with TiN as representative prepared by CVD and PVD
Obtained a wide range of applications during the processing efficiency of alloy, and be subsequently developed that were TiC, TiCN, TiAlN, AlTiN, CrAlN
Be developed and obtain practical application Deng coating, but because high temperature in working angles to oxidation, the chip of coating to applying
The adhesive wear and coating of layer brittleness problems in itself, the processing problem of above-mentioned alloy are not solved.For example,
TiAlN coatings have high rigidity and good high temperature oxidation resistance, hence it is evident that improve processing efficiency and cutter life, but
Its fragility and coefficient of friction higher, limits the coatings such as TiAlN answering in materials such as high speed, dry cutting and difficult cutting alloys
With also limit its practical application in terms of high-precision mold and other wear resistant friction reducing workpiece coatings.
The fragility of the coatings such as TiAlN how is further reduced, is broken through and is asked when Front-coating mirror internal stress is big, film-substrate cohesion is poor
Topic, place coating before the abrasion because toughness is poor come off on above-mentioned coating need the perfect target of continuation.
Be to solve problem above, the concept of nano-composite coating proposed in 20 end of the centurys, i.e., by nanocrystalline-nanocrystalline or
The composite construction more than two-phase or two-phase of nanocrystalline and amorphous formation, the composite coating has obtained certain exploitation and application, such as
The world such as Blazers, Platit coating major company develops the nc-TiN/a-Si of arc ion plating preparation3N4Nano combined painting
Layer, its high temperature oxidation resistance and toughness have obtained certain raising, but in actual applications, nc-TiN/a-Si3N4It is nano combined
The great friction coefficient of coating causes to produce amount of heat, coated cutting tool rake face still to produce built-up edge, and its in working angles
Toughness is remained to be further improved.
Therefore, preparing a kind of energy has higher hardness with high tenacity and with the NEW TYPE OF COMPOSITE coating compared with low-friction coefficient,
It is very necessary to further raising knife mold performance and service life.
The content of the invention
Technical purpose of the invention is directed to the deficiency of existing coating material system, there is provided one kind has higher hardness with height
Toughness and with Ti-Ag-N nano-composite coatings compared with low-friction coefficient and preparation method thereof.
The present invention realize technical scheme that above-mentioned purpose uses for:
A kind of Ti-Ag-N nano-composite coatings, are distinguished by the distance from matrix, are included successively from inside to outside:In matrix table
Intermediate layer that transition zone that Ti film in face is formed, TiN film are formed and Ti-Ag-N layers.Described matrix refers to stainless steel, hard conjunction
Gold, high-speed steel, the instrument of refractory steel or mould etc..
The preparation method of described Ti-Ag-N nano-composite coatings, it is characterised in that:
(1) transition zone is plated:Using pure titanium target, when vacuum reaches 2 × 10 in vacuum chamber-3Pa~4 × 10-2During Pa, to true
Empty room is heated to 300~500 DEG C;Argon gas is passed through to vacuum chamber, the gas flow needed for setting is 30~300sccm, air pressure control
System is between 0.5~2Pa;Matrix adds pulsed negative bias in -500~-1000V scopes, makes gas that glow discharge to occur, to sample
Carry out aura and clean 10~60min;Adjustment argon flow amount, makes gas pressure in vacuum for 0.1~1.0Pa, while titanium target arc source is opened,
Arc current is 60~150A, and 1~20min of Ti Ions Bombardments is proceeded to sample workpiece;Tune pulsed negative bias extremely -100V~-
600V, depositing Ti film is 1~10min of transition zone;
(2) TiN layer is plated:Using pure titanium target, stop argon gas, lead to nitrogen, set air pressure as 0.2~2Pa scopes;Matrix is applied
Pulsed negative bias -100V~-500V;Regulation target current is 50~150A, and sedimentation time is 1~20min;
(3) Ti-Ag-N layers is plated:Stop argon gas, lead to nitrogen, nitrogen flow is controlled in 10~200sccm, sets air pressure as 0.2
~2Pa scopes;Pulsed negative bias -100V~-600V is applied to matrix;Modulation target current is 60~200A, and sedimentation time is 20
~300min;
(4) after deposition terminates, arc is stopped rapidly, is stopped matrix pulsed negative bias, is stopped being passed through gas, continue to vacuumize, workpiece
Cool to less than 100 DEG C with the furnace, open vacuum chamber, take out workpiece, whole coating process terminate.
Preferably, in the target of the titanium silver alloy target for being used, the content of silver is 5-40% (percentage by weight).Ti-
The thickness of Ag-N nano-composite coatings is 1-10 micron, the nano-indentation hardness value of Ti-Ag-N nano-composite coatings be 30GPa with
On, Ti-Ag-N nano-composite coatings and steel ball are to the coefficient of friction ground below 0.3.
Compared with prior art, the beneficial effects of the invention are as follows:
1st, the present invention be matrix surface be successively Ti films formed transition zone, TiN film formed intermediate layer and Ti-Ag-N
Layer, film-substrate cohesion reaches more than 60N, and Fig. 2 is the film-substrate cohesion of the Ti-Ag-N nano-composite coating samples of present invention deposition
Test curve figure, from curve as can be seen that the film-substrate cohesion of coating is 64N, shows adhesion higher.
2nd, during the Ag of present invention selection and TiN not solid solutions completely adds TiAlN thin film, the Ag of not solid solution is segregated in TiN crystal boundaries
Position, has refined the crystallite dimension of TiN, and Ag is also separated out with nanocrystalline or non crystalline structure, is susceptible to the metal of plastic deformation
The addition of Ag not only greatly reduces coating internal stress, improves coating hardness and fracture toughness, and abrasion to TiN is played
Lubrication and antifriction function, greatly reduce the coefficient of friction of coating.
Brief description of the drawings:
Fig. 1 is the cross-sectional scans electron microscope of the Ti-Ag-N nano-composite coatings of present invention deposition;
Fig. 2 is the film-substrate cohesion test curve figure of the Ti-Ag-N nano-composite coating samples of present invention deposition.
Specific embodiment:
A kind of Ti-Ag-N nano-composite coatings, are distinguished by the distance from matrix, are included successively from inside to outside:Ti films are formed
Transition zone, TiN film formed intermediate layer and Ti-Ag-N layers.Described matrix refers to stainless steel, hard alloy, high-speed steel, resistance to
Instrument or mould of hot die steel etc..
The preparation method of specific Ti-Ag-N nano-composite coatings, embodiment is as follows:
Embodiment 1
Plating transition zone:Base material uses high-speed steel (trade mark is W18Cr4V), and specimen size is 25mm × 10mm × 2mm, plated film
Face size is 25mm × 10mm.After the preceding surface of plated film first passes through grinding, polishing, ultrasonic cleaning, drying, vacuum chamber sample stage is put into
On, treat that vacuum reaches 6 × 10 in vacuum chamber-3During Pa, 400 DEG C are heated to vacuum chamber, argon gas is passed through to vacuum chamber, set gas
Body flow is 100sccm, and air pressure is controlled in 2.0Pa, and matrix adds pulsed negative bias -800V, and aura cleaning is carried out to sample
20min;Then, argon stream amount is adjusted, gas pressure in vacuum is adjusted to 0.2Pa, while opening titanium target arc source, arc stream stabilization exists
70A, Ti Ions Bombardments 5min is carried out to sample;Adjust pulsed negative bias to -300V, depositing Ti film 3min;Then, using pure titanium
Target, stops argon gas and is passed through nitrogen, and adjustment air pressure is 1.5Pa;Adjustment matrix pulsed negative bias are -300V, and adjustment target current is 90A,
Depositing TiN film 3min;Hereafter, into nano-composite coating deposition process, stop pure titanium target, open titanium silver target, nitrogen pressure adjustment
It is 0.9Pa;Pulsed negative bias -400V is adjusted, adjustment target current is 110A, and sedimentation time is 60min;After deposition terminates, stop rapidly
Arc, stop matrix pulsed negative bias, stopping and be passed through gas, continue to vacuumize, workpiece cools to less than 100 DEG C with the furnace, opening vacuum
Room, takes out workpiece, and coating process terminates.
Gained Ti-Ag-N nano-composite coatings outward appearance is golden yellow, and the gross thickness of sem test coating is 3.1 micro-
Rice;Nano-indenter test coating hardness is 28.6GPa, and sound emission scratching instrument testing coating adhesion is 72N.
Embodiment 2
Base material uses hard alloy (trade mark is YG6), and specimen size is 20mm × 20mm × 4mm, and coated surface size is
20mm×20mm.After the preceding surface of plated film first passes through grinding, polishing, ultrasonic cleaning, drying, it is put on vacuum chamber sample stage, treats true
Vacuum reaches 4 × 10 in empty room-3During Pa, gas mass flow controller is opened, lead to argon gas to 1.0Pa, matrix adds pulse to bear
- 600V is biased into, aura cleaning 15min is carried out to sample;Then, argon stream amount is adjusted, gas pressure in vacuum is adjusted to
0.6Pa, while opening titanium target arc source, arc stream stabilization carries out Ti Ions Bombardments 5min to sample in 80A;Adjust pulsed negative bias to-
300V, depositing Ti metal level 3min;Then, using pure titanium target, stop argon gas and be passed through nitrogen, adjustment air pressure is 1.0Pa;Adjustment matrix
Pulsed negative bias are -300V, and adjustment target current is 90A, depositing TiN film 6min;Hereafter, deposited into nano-composite coating
Journey, stops pure titanium target, opens titanium silver target, and nitrogen pressure is adjusted to 0.8Pa;Pulsed negative bias -400V is adjusted, adjusting target current is
110A, depositing Ti-Ag-N films 30min;After deposition terminates, arc is stopped rapidly, stopped matrix pulsed negative bias, stopped being passed through gas, after
Continuous to vacuumize, workpiece cools to less than 100 DEG C with the furnace, opens vacuum chamber, takes out workpiece, and coating process terminates.
Gained Ti-Ag-N nano-composite coatings outward appearance is golden yellow, and the gross thickness of sem test coating is 1.6 micro-
Rice;Nano-indenter test coating hardness is 31.6GPa, and sound emission scratching instrument testing coating adhesion is 64N.
Embodiment 3
Base material uses high-speed steel (trade mark is W6Mo5Cr4V2), and specimen size is 20mm × 10mm × 2mm, coated surface size
It is 20mm × 10mm.After the preceding surface of plated film first passes through grinding, polishing, ultrasonic cleaning, drying, it is put on vacuum chamber sample stage, treats
Vacuum reaches 4 × 10 in vacuum chamber-3During Pa, lead to argon gas to 2.0Pa, matrix adds pulsed negative bias to -700V, sample is carried out
Aura cleans 30min;Then, Ar throughputs are adjusted, gas pressure in vacuum is adjusted to 0.3Pa, while opening titanium target arc source, arc stream
Stabilization carries out Ti Ions Bombardments 8min to sample in 80A;Using pure titanium target, stop argon gas and be passed through nitrogen, adjustment air pressure is 1.0Pa;
Adjustment matrix pulsed negative bias are -300V, and adjustment target current is 90A, depositing TiN film 6min;Hereafter, into nano-composite coating
Deposition process, stops pure titanium target, opens titanium silver target, and adjustment nitrogen pressure is 1.2Pa;Adjustment matrix pulsed negative bias are adjusted to -200V
Whole target current is 95A, depositing Ti-Ag-N films 60min;After deposition terminates, arc is stopped rapidly, is stopped substrate bias, is stopped being passed through gas,
Continue to vacuumize, workpiece cools to less than 100 DEG C with the furnace, open vacuum chamber, take out workpiece, coating process terminates.
Gained Ti-Ag-N nano-composite coatings outward appearance is golden yellow, and the gross thickness of sem test coating is 4.5 micro-
Rice;Nano-indenter test coating hardness is 30.1GPa, and sound emission scratching instrument testing coating adhesion is 79N.
Embodiment 4
Base material uses hard alloy (trade mark is YT5), and specimen size is 20mm × 20mm × 4mm, and coated surface size is
20mm×20mm.After the preceding surface of plated film first passes through grinding, polishing, ultrasonic cleaning, drying, it is put on vacuum chamber sample stage, treats true
Vacuum reaches 4 × 10 in empty room-3During Pa, gas quality flow rate controller is opened, lead to argon gas to air pressure 1.0Pa, matrix adds arteries and veins
Rush negative bias and be depressed into -1000V, aura cleaning 10min is carried out to sample;Then, Ar throughputs are adjusted, gas pressure in vacuum is adjusted to
0.4Pa, while opening titanium target arc source, arc stream stabilization carries out Ti Ions Bombardments 4min to sample in 80A;Then, using pure titanium
Target, stops argon gas and is passed through nitrogen, and adjustment air pressure is 0.9Pa;Adjustment matrix pulsed negative bias are -100V, and adjustment target current is 90A,
Depositing TiN film 6min;Hereafter, into nano-composite coating deposition process, stop pure titanium target, open titanium silver target, adjust nitrogen pressure
It is 0.4Pa;To -400V, adjustment target current is 95A, depositing Ti-Ag-N films 60min to adjustment matrix pulsed negative bias;Deposition terminates
Afterwards, arc is stopped rapidly, is stopped substrate bias, is stopped being passed through gas, continue to vacuumize, workpiece cools to less than 100 DEG C with the furnace, opens true
Empty room, takes out workpiece, and this coating process terminates.
Gained Ti-Ag-N nano-composite coatings outward appearance is golden yellow, and the gross thickness of sem test coating is 3.6 micro-
Rice;Nano-indenter test coating hardness is 32.1GPa, and sound emission scratching instrument testing coating adhesion is 73N.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.
Claims (3)
1. a kind of Ti-Ag-N nano-composite coatings, it is characterised in that:Distinguished by the distance from matrix, included successively from inside to outside:
Matrix surface Ti films formed transition zone, TiN film formed intermediate layer and Ti-Ag-N layers.
2. the preparation method of Ti-Ag-N nano-composite coatings according to claim 1, it is characterised in that including following step
Suddenly:
(1) transition zone is plated:Using pure titanium target, when vacuum reaches 2 × 10 in vacuum chamber-3Pa~4 × 10-2During Pa, to vacuum chamber
It is heated to 300~500 DEG C;Argon gas is passed through to vacuum chamber, the gas flow needed for setting is 30~300sccm, air pressure control exists
Between 0.5~2Pa;Matrix adds pulsed negative bias in -500~-1000V scopes, makes gas that glow discharge to occur, and sample is carried out
Aura cleans 10~60min;Adjustment argon flow amount, makes gas pressure in vacuum for 0.1~1.0Pa, while titanium target arc source is opened, arc electricity
It is 60~150A to flow, and 1~20min of Ti Ions Bombardments is proceeded to sample workpiece;Pulsed negative bias to -100V~-600V are adjusted, is sunk
Product Ti films are 1~10min of transition zone;
(2) TiN layer is plated:Using pure titanium target, stop argon gas, lead to nitrogen, set air pressure as 0.2~2Pa scopes;Pulse is applied to matrix
Back bias voltage -100V~-600V;Regulation target current is 50~150A, and sedimentation time is 1~20min;
(3) Ti-Ag-N layers is plated:Stop argon gas, lead to nitrogen, nitrogen flow is controlled in 10~200sccm, sets air pressure as 0.2~3Pa
Scope;Pulsed negative bias -100V~-600V is applied to matrix;Modulation target current be 60~200A, sedimentation time be 20~
300min;
(4) after deposition terminates, arc is stopped rapidly, is stopped matrix pulsed negative bias, is stopped being passed through gas, continue to vacuumize, workpiece is with stove
It is cooled to less than 100 DEG C.
3. the preparation method of Ti-Ag-N nano-composite coatings according to claim 2, in the titanium silver alloy target for being used
In target, the content of silver is 5-40%.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108018529A (en) * | 2017-11-09 | 2018-05-11 | 南京工业大学 | A kind of aluminum-based fuel cell bipolar plate surface composite coating and preparation method thereof |
CN116174546A (en) * | 2023-04-28 | 2023-05-30 | 佛山高谱机械科技有限公司 | Pipe thermal bending method based on composite action of electric conduction and self lubrication |
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CN103101244A (en) * | 2011-11-15 | 2013-05-15 | 现代自动车株式会社 | Coating layer with low-friction for vehicle component and method for producing the same |
CN103160783A (en) * | 2013-03-26 | 2013-06-19 | 沈阳金锋特种刀具有限公司 | TiCuN nano composite coating and preparation method thereof |
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CN1570196A (en) * | 2004-04-30 | 2005-01-26 | 麦桥 | Surface antibiotic, wearable stainless steel products and its production method |
CN101698363A (en) * | 2009-10-30 | 2010-04-28 | 华南理工大学 | TiN/(TiN+CrN)/CrAlN nano composite coating and preparation method thereof |
CN103101244A (en) * | 2011-11-15 | 2013-05-15 | 现代自动车株式会社 | Coating layer with low-friction for vehicle component and method for producing the same |
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