CN106191790A - The preparation method of wear-resistant coating - Google Patents
The preparation method of wear-resistant coating Download PDFInfo
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- CN106191790A CN106191790A CN201610522067.0A CN201610522067A CN106191790A CN 106191790 A CN106191790 A CN 106191790A CN 201610522067 A CN201610522067 A CN 201610522067A CN 106191790 A CN106191790 A CN 106191790A
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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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Abstract
The present invention relates to the preparation method of a kind of wear-resistant coating, for preparing hard coat at substrate surface, said method comprising the steps of: select the substrate of predetermined size and performance；It is carried out being dried to the surface to be deposited of substrate；In the vacuum chamber of arc ion plating film device, the surface to be deposited of substrate is carried out sputter clean；Noble gas and N is fed in vacuum chamber2, use arc ion plating (aip) cvd nitride thing hard coat on the surface of the substrate, in deposition process, gradient increases or circulation gradient increases N2Flow, in order to adjust the residual stress in hard coat；Hard coat on substrate is carried out vacuum annealing, the final wear-resistant coating obtaining big thickness.Increased by gradient or circulate increase N2Flow, effectively reduces the residual stress of big thickness coatings；Coating has more preferable anti-scratch ability and fracture toughness.
Description
Technical field
The present invention relates to arc ion plating (aip), more particularly, it relates to the preparation method of a kind of wear-resistant coating.
Background technology
Hard coat is as a kind of important protective coating, and tribological property and corrosion resistance with its excellence are by extensively
Be applied to the protection on surface of the parts such as cutting tool and gear.Industrial, arc ion plating (aip) is typical as one
Physical gas phase deposition technology, because of its high ionization level, high deposition rate, simple operation and other advantages, is widely used in hard coat
Preparation.This technology forms ganoine thin film on substrate, but the residual stress of the ganoine thin film obtained is usually compressive stress, and
And numerical value is the biggest, even as high as-17GPa, excessive residual compressive stress can make ganoine thin film come off from substrate, or make it
Warpage, bulge.
Multiple method proposed to suppress too high residual compressive stress, including improving depositing operation, preparation multilamellar
Make annealing treatment after film, employing component gradient, introducing transition zone and deposition, etc..Such as, at application publication number it is
In the Chinese patent application of CN104131250A, disclose nano combined cutter coat and the system thereof of a kind of gradient components design
Preparation Method.
Although these methods effectively improve the residual stress of hard coat, improve film-substrate cohesion, but when hard is coated with
When layer thickness increases, even if the mean stress of hard coat does not increase, (coating cross sections amasss x coating and puts down film base interfacial shear force
All stress) also can significantly rise so that big thickness hard coat is difficult to prepare.On the other hand, hard coat in use,
After the high rigidity region of surface layer and near surface layer is worn consumption, the hardness of coating is substantially reduced, and abrasive resistance will be notable
Decline, even cause the protection of hard coat to lose efficacy.
Summary of the invention
The technical problem to be solved in the present invention is, when increasing for hard coat thickness of the prior art, wearability
The defect that can decline, it is provided that the preparation method of a kind of wear-resistant coating, it is possible to improve the anti-wear performance of hard coat.
The technical solution adopted for the present invention to solve the technical problems is: construct the preparation method of a kind of wear-resistant coating, uses
In preparing hard coat at substrate surface, said method comprising the steps of:
S101, select the substrate of predetermined size and performance；
S102, surface to be deposited to substrate are carried out being dried；
S103, in the vacuum chamber of arc ion plating film device, the surface to be deposited of substrate is carried out sputter clean；
S104, in vacuum chamber, feed noble gas and N2, use arc ion plating (aip) to deposit on the surface of the substrate
Nitride hard coating, in deposition process, gradient increases or circulation gradient increases N2Flow, in order to adjust hard coat
Interior residual stress；
S105, the hard coat on substrate is carried out vacuum annealing, the final wear-resistant coating obtaining big thickness.
According to method of the present invention, according to the vacuum chamber size of arc ion beam coating equipment determine gradient increase or
Circulation gradient increases N2The numerical value of flow and at the N of each gradient2The sedimentation time that flow is kept.
According to method of the present invention, increase N in gradient2In the case of flow, increase N with N number of gradient2Flow, often
Individual gradient keeps the predetermined time, and the temporal summation that N number of gradient is kept is total sedimentation time, and wherein N is integer.
According to method of the present invention, increase N in circulation gradient2In the case of flow, total sedimentation time is divided
For increasing N with L gradient in M cycle, each cycle2Flow, each gradient keeps predetermined time, and L gradient is protected
The temporal summation held is the time span in single cycle, and wherein M, L are integer.
According to method of the present invention, the inert gas flow in vacuum chamber keeps constant, and increases N2Flow, described
Stagnation pressure in vacuum chamber changes in the range of from 0.5Pa to 1.6Pa.
According to method of the present invention, before deposition, the stagnation pressure regulation in vacuum chamber is to predetermined fixed value, in gradient
Increase or circulation gradient increases N2During flow, reduce inert gas flow accordingly so that stagnation pressure keeps constant, should
Predetermined fixed value is in the range of 0.5Pa to 1.6Pa.
According to method of the present invention, using arc ion plating (aip) cvd nitride thing hard on the surface of the substrate
During coating, the target of selection is Ti, TiAl or TiCrAl.
According to method of the present invention, described N2Flow increases with 5～10sccm for gradient.
According to method of the present invention, depositing temperature is 100～400 DEG C, and total sedimentation time is 300～500 minutes.
The method implementing the present invention, is had the advantages that and is increased or circulate increase N by gradient2Flow, effectively drops
The low residual stress of big thickness coatings；Coating has more preferable anti-scratch ability and fracture toughness；The polishing scratch of big thickness coatings
Surface ratio is more smooth, and the bur of worn-out surface and abrasive dust the most less, coating has good tribological property.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
Fig. 1 is the flow chart of the preparation method of the wear-resistant coating of the present invention；
The N that Fig. 2 is passed through when being according to embodiments of the invention, deposition coating2The time dependent schematic diagram of flow；
Fig. 3 A and Fig. 3 B is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2Institute during flow
The Cross Section Morphology schematic diagram of the big thickness coatings obtained；
Fig. 4 A and 4B is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2Gained during flow
The various compositions of the big thickness coatings arrived are along the distribution schematic diagram of layer depth；
Fig. 5 is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2During flow obtained big
The residual stress of thickness coatings is along the distribution schematic diagram of layer depth；
Fig. 6 A and 6B is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2Gained during flow
The section hardness of the big thickness coatings arrived is along the distribution schematic diagram of layer depth；
Fig. 7 A and 7B is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2Gained during flow
The Rockwell vickers indentation schematic diagram of the big thickness coatings arrived；
Fig. 8 A and 8B is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2Gained during flow
The schematic diagram of the cut intensity of the big thickness coatings arrived；
Fig. 9 is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2During flow obtained big
The coefficient of friction of thickness coatings is along with the change curve schematic diagram of time；
Figure 10 A and Figure 10 B is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2During flow
Obtained by big thickness coatings grinding defect morphology after 120 minutes frictional experiments and component analysis schematic diagram；
Figure 11 is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2During flow obtained
Big thickness coatings polishing scratch profile schematic diagram after 120 minutes frictional experiments.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right
The present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, and
It is not used in the restriction present invention.
Fig. 1 is the flow chart of the preparation method 100 of the wear-resistant coating of the present invention.As it is shown in figure 1, in the present invention, wear-resisting
The preparation method 100 of coating mainly comprises the steps that
Step 101, selects the substrate of predetermined appropriate size and performance.This substrate be wear-resistant coating to be deposited cutter,
Mould and parts etc., generally select steel；
Step 102: be carried out being dried to the surface to be deposited of substrate.Specifically, ethanol, metal are used the most successively
Detergent and deionized water carry out ultrasonic cleaning, and the time is 3-8 minute, then be dried N2Surface is dried up so that substrate
Surface cleaning to be deposited, be beneficial to be combined with coating.Afterwards, substrate is loaded in the vacuum chamber of arc ion plating film device；
Step 103: in vacuum chamber, the surface to be deposited of substrate is carried out sputter clean.Target is loaded in vacuum chamber,
Make substrate and target just to suspension.Close door for vacuum chamber, to vacuum chamber forvacuum, make the pressure in vacuum chamber less than 6.0 ×
10-3Pa.Afterwards, open heating power supply and vacuum chamber is toasted, substrate is preheated to 100-300 DEG C.It is passed through in vacuum chamber
Noble gas, boosts to predetermined initial pressure in making vacuum chamber.Matrix is added pulsed bias, the surface to be deposited to substrate
Carry out sputter clean.
Wherein, the material of this target can select as required, and such as Ti, TiAl, TiCrAl etc. can be formed by nitridation
The material of hard coat.Noble gas preferred Ar gas, Kr gas etc., and the stream of noble gas is regulated according to the size of vacuum chamber
Amount.This initial pressure can be such as 0.5Pa.Pulsed bias is negative 700-1000V, and dutycycle is 20%～50%, during bombardment
Between be 1～5 minute.
Step 104: after sputter clean terminates, uses arc ion plating to deposit hard coat on the surface of the substrate.Regulation
The pulsed bias of matrix is negative 50～150V, and dutycycle is 20%～50%, and arc current is 50～70A, depositing temperature be 100～
400 DEG C, total sedimentation time is 300～500 minutes.N is fed in vacuum chamber2, the hard that the surface of substrate is deposited is coated with
Layer is the nitride of target material, such as, when target selects Ti, TiAl, TiCrAl material respectively, formed respectively TiN,
TiAlN, TiCrAlN hard coat.
In deposition process, gradient increases or circulation gradient increases N2Flow, in order to effectively adjust hard coat
Interior residual stress, it is thus achieved that the hard coat of big thickness.
Gradient increases or circulation gradient increases N2The numerical value of flow and at the N of each gradient2It is heavy that flow is kept
The long-pending time, can change according to the vacuum chamber size of arc ion plating film device.N is increased in gradient2In the case of flow, with N
Individual gradient increases N2Flow.Each gradient keeps the predetermined time, when the temporal summation that N number of gradient is kept is total deposition
Between (can refer to Fig. 2).Wherein N is integer, and its numerical value can change according to the vacuum chamber size of arc ion plating film device.Logical
Often, N2Flow can increase with 5～10sccm for gradient, preferably 5sccm, 10sccm.The numerical value of N can be 10～20.Corresponding
Ground, the scheduled time that each gradient keeps is 15-30 minute.These are only citing, the invention is not restricted to this.
N is increased in circulation gradient2In the case of flow, total sedimentation time is divided into M cycle, in each cycle with
L gradient increases N2Flow.Each gradient keeps predetermined time, and the temporal summation that L gradient is kept is the single cycle
Time span (can refer to Fig. 2).Wherein M, L are integer, and its numerical value can be according to the vacuum chamber size of arc ion plating film device
And change.Generally, N2Flow can increase with 5～10sccm for gradient, preferably 5sccm, 10sccm.The numerical value of M can be 3～
The numerical value of 6, L can be 10～20.The scheduled time that each gradient keeps is 2-10 minute.These are only citing, the present invention is not
It is limited to this.
It should be noted that either gradient increases or circulation gradient increases N2Flow, can enter in two ways
OK.One of which is, the inert gas flow in vacuum chamber keeps constant, and increases N2Flow, so, total in vacuum chamber
Pressure can be along with N2Change, from initial pressure start change.But in the range of stagnation pressure is maintained at predetermined maximum pressure.Such as, always
Pressure can from 0.5Pa to 1.6Pa in the range of change.Another kind is, before deposition, the stagnation pressure regulation in vacuum chamber is to predetermined
Fixed value.Increase or circulation gradient increase N in gradient2During flow, reduce inert gas flow accordingly so that total
Pressure keeps constant.This predetermined fixed value is in the range of 0.5Pa to 1.6Pa.
Step 105: after the process of deposition hard coat terminates, the hard coat on substrate is carried out vacuum annealing, finally
Obtain the wear-resistant coating of big thickness.The temperature of annealing is 200～500 DEG C.
With specific embodiment, the present invention is illustrated below.
In an embodiment of the present invention, selecting 316L rustless steel as substrate material, its elastic modulus E and Poisson's ratio υ are divided
Not Wei 195GPa and 0.3, substrate surface be 12K polish minute surface.Sizes of substrate is 50 × 10 × 0.8mm, 30 × 30 × 0.8mm two
Plant specification.
Successively by the ultrasonic surface clean to be deposited to substrate of metal detergent, deionized water 5 minutes, then with dry N2
After skin drying, load in the vacuum chamber of arc ion plating film device.In this embodiment, Tyke promise TSU-400 type is used
Multi-function ion plating machine.
It follows that the surface to be deposited of substrate is carried out sputter clean.In this embodiment, prepare at substrate surface
TiAlN coating, the TiAl target therefore selecting atomic ratio to be 1:1.Target is just hung by substrate, and target-substrate distance is 200mm.Close true
Empty room door, to vacuum chamber forvacuum, base vacuum is 5.0 × 10-3Pa；It is preheated to 200 DEG C, then to be passed through flow be 50sccm
Ar gas, boost to 0.5Pa, add negative 900V and the pulsed bias of dutycycle 30%, substrate surface is carried out sputter clean, bombardment
1 minute time.
After sputter clean terminates, deposit hard coat on the surface of the substrate.In coating deposition process, pulsed bias is negative
100V, dutycycle 30%, arc current 55～60A, depositing temperature is 350 DEG C, and sedimentation time is 400 minutes.Fixing Ar throughput
50sccm is constant, takes gradient to increase N2Flow and circulation increase N2Flow makes the side that stagnation pressure changes between 0.5～1.2Pa
Method, prepares the big thickness TiAlN coating of two kinds of techniques respectively.
The concrete Flow-rate adjustment parameter of both approaches is shown in Fig. 2.When Fig. 2 is according to embodiments of the invention, deposition coating
The N being passed through2The time dependent schematic diagram of flow.Illustrated therein is gradient and increase N2Flow and circulation increase N2The two of flow
The scheme of kind.
N is increased in gradient2In the case of flow, increase N with 5sccm for gradient2Flow, totally 20 gradients, each gradient
Keep 20 minutes.Stagnation pressure in vacuum chamber can be along with N2Change, from initial pressure 0.5Pa start increase.During total deposition
Between be 400 minutes.
N is increased in circulation gradient2In the case of flow, total sedimentation time is divided into 4 cycles, in each cycle with
5sccm is that gradient increases N2Flow, totally 20 gradients, each gradient keep 5 minutes.Within each cycle, in vacuum chamber
Stagnation pressure can be along with N2Change, from initial pressure 0.5Pa start increase.Total sedimentation time is 400 minutes.
It follows that the characteristic of hard coat is analyzed.
SUPRA55 type scanning electron microscope (SEM) utilizing ZEISS to produce observes the Cross Section Morphology of coating and measures the thickness of coating
Degree；And utilize the subsidiary energy dispersion X-ray spectrogrph (EDX) of scanning electron microscope, analyze coating composition along layer depth point
Cloth.Use the membrane stress instrument that Supro Instruments produces, testing coating thin film full thickness mean stress；Use delamination
Radius-of-curvature method is measured the residual stress of big thickness coatings and is distributed along layer depth, is corroded by evening chemical, successively peels off painting
Layer, measures change and the peel ply thickness of test piece curvature, calculates stress and is distributed along layer depth.Hardness test uses MH-6 type micro-
Durometer, tests load 25g, and the load time keeps 10s；The film-substrate cohesion of coating is respectively adopted qualitatively and quantitatively two ways
Measure, use HT-3002 complexity scratching instrument to carry out quantitative test, test load 0～100N, coasting distance 3mm, use
VDI3198 Rockwell impression grading method carries out qualitative test, uses the Rockwell apparatus with 120 ° of Diamond Cone indenter, selects
150Kgf load, loads 12s at strip, and utilizes SEM to observe the situation of indentation edge coating breaks down；Friction-wear test
Selecting UMT-3 frictional testing machine, using radius is the Si of 4mm3N4Friction ball, at load 10N, friction radius 9mm and rotating speed
Under the conditions of the friction testing of 800r/min, after the friction and wear test of 120min, obtain the coefficient of friction of big thickness coatings,
And utilize the contourograph of the Dektak XT model of Brooker, measure polishing scratch Cross Section Morphology and calculate wear rate.
Fig. 3 A and Fig. 3 B is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2Institute during flow
The Cross Section Morphology schematic diagram of the big thickness coatings obtained.As shown in figs.3 a and 3b, flat smooth is compared in the cross section of big thickness coatings,
And matrix is well combined in interface with coating, thickness respectively reaches 68.79 μm and 64.48 μm.Scanning electron in Fig. 3 A shows
Micro mirror result shows, gradient increases N2In the big thickness coatings that flow obtains, there is more bulky grain near film base interface,
N2Under the technique that flow is relatively low, coating compactness is the most on the low side, and the existence in bulky grain and part cavity effectively alleviates stress
Accumulation, droplet size is substantially in 0.95 μm～10.33 μ m.Scanning electron microscope result in Fig. 3 B shows, follows
Ring gradient increases N2Big thickness coatings obtained during flow shows the structure of similar multilayer film, increases N in circulation gradient2Stream
The thickness of the coating that each cycle period of amount obtains is roughly the same, relatively uniform, greatly along the distribution of coating layer thickness direction bulky grain
The existence in granule and part cavity effectively alleviates the accumulation of stress.
Fig. 4 A and 4B is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2Gained during flow
The various compositions of the big thickness coatings arrived are along the distribution schematic diagram of layer depth.As illustrated in figures 4 a and 4b, the content of Ti element is along coating
Depth direction has faint change, and the distribution of Al element and N element there occurs significantly change because of the regulation of technique.Increase in gradient
Add N2In the big thickness coatings that flow obtains, the content of N element is gradually increased to surface from film base interface, corresponding Al element
Content gradually decreases, and this is owing to interface TiAl content is high, along with N2Flow increases, and TiAlN gets more and more, and Al element is by N
Element portions substitutes.N is increased in circulation gradient2In big thickness coatings obtained during flow, also present same regularity.
Additionally, the change of work stagnation pressure, necessarily cause the change that Ti, Al element is collided during arriving coating surface, N2
When flow increases, stagnation pressure raises, and in coating, the content of metallic element declines the most therewith.
Fig. 5 is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2During flow obtained big
The residual stress of thickness coatings is along the distribution schematic diagram of layer depth.As it is shown in figure 5, gradient increases and circulation increases N2Prepared by flow
Two kinds of big thickness coatings, during coatings growth, along with the change of N element content, its residual stress along layer depth direction by
Gradually accumulate and increase.Along with the increase of thicknesses of layers, the stress that general trend shows along layer depth direction is gradually increased, and gradient increases
Add N content and circulation gradient increases N content, although do not change stress and build up the trend of increase along layer depth, but effectively
Slow down the speed that stress increases along layer depth accumulation.It will be seen that at two kinds of N2Under the technique of Flow-rate adjustment, two kinds of coatings
Residual stress be in reduced levels all the time, particularly we test its full thickness mean stress and are respectively as follows: gradient and increase N2
The big thickness coatings that flow obtains is-0.74GPa, and circulation gradient increases N2Big thickness coatings obtained during flow is-
0.92GPa, converts as film base interfacial shear force, gradient increase N2The big thickness coatings that flow obtains is 509N, and circulation gradient increases
Add N2Big thickness coatings obtained during flow is 593N, and this level and thickness are 5 μm, the film sample of residual stress-10GPa
Quite.
Gained when Fig. 6 A and 6B is to increase N2 flow and circulation gradient increase N2 flow according to embodiments of the invention, gradient
The section hardness of the big thickness coatings arrived is along the distribution schematic diagram of layer depth.As shown in Figure 6 A and 6B, by coating/basal body interface to being coated with
The direction on layer surface, the section hardness of Fig. 6 A floating coat is gradually increased, and the closer to coating surface, its hardness number is the biggest, this and N unit
Cellulose content increases, and it is consistent that nitride increases trend.This it appears that light and dark multiple structure, hardness number from Fig. 6 B
Distribution consistent with the circulation of N element content.The case hardness of two kinds of big thickness coatings of test is respectively (1825.9 ± 62)
HV and (1979.5 ± 88) HV, it is found that coating surface hardness is higher than section hardness, this is because coating is column crystal growth
Structure, section hardness test is pressed into from the side of column crystal, and case hardness test is pressed into from the top of column crystal.Section hardness
Can represent its firmness change trend, case hardness is only its true hardness.
Fig. 7 A and 7B is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2Gained during flow
The Rockwell vickers indentation schematic diagram of the big thickness coatings arrived.It can be seen that have no obvious coating shedding or radial cracking,
Illustrating that the fracture toughness of big thickness coatings is relatively good, film-substrate cohesion is preferable.
Fig. 8 A and 8B is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2Gained during flow
The schematic diagram of the cut intensity of the big thickness coatings arrived.As shown in figs. 8 a and 8b, can significantly find from figure, initial
Running in stage, the coefficient of friction of coating increases sharply, and is primarily due in initial process of friction and wear, and contact conditions is from two
Between object, abrasive wear is gradually converted into interface sliding.After the running-in period of 1000s, gradient coating progressivelyes reach steady shape
State, friction factor is stable between 0.7～0.8, and circulates the friction factor change fluctuation of coating the most greatly, and shows certain
Periodically, this is owing in process of friction and wear, film layer is worn, relevant with the periodic distribution of circulation coating composition.Work as friction
Abrasion about 5000s, the coefficient of friction of the big thickness coatings of gradient is reduced to about 0.65, and this is owing to increasing along with wearing-in period
Adding, harder near surface layer wears off, and simultaneously with the oxidative wear of part, causes the interface between friction pair to become flat
Sliding, make coefficient of friction be reduced.
Fig. 9 is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2During flow obtained big
Thickness coatings grinding defect morphology after 120 minutes frictional experiments and component analysis schematic diagram.Observe it is found that big through SEM
The worn-out surface smoother of thickness coatings is smooth, and the bur of worn-out surface and abrasive dust the most less, the big thickness of TiAlN is described
Coating has good tribological property.
Figure 10 A and Figure 10 B is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2During flow
Obtained by big thickness coatings grinding defect morphology after 120 minutes frictional experiments and component analysis schematic diagram.Such as Figure 10 A and figure
Shown in 10B, observe it is found that the worn-out surface smoother of big thickness coatings is smooth through SEM, and the bur of worn-out surface
The most less with abrasive dust, illustrate that the big thickness coatings of TiAlN has good tribological property, and big thickness when gradient increases N2 flow
Coating has more preferable wearability.
Figure 11 is to increase N according to embodiments of the invention, gradient2Flow and circulation gradient increase N2During flow obtained
Big thickness coatings polishing scratch profile schematic diagram after 120 minutes frictional experiments.It can be seen that the maximum Wear track depth of coating is little
In the thickness of coating, fretting wear distance about 5426m after 120 minutes is described, and big thickness coatings is the most worn out, represents
Go out good wearability.
Above example by way of example only, according to the teachings of the present invention, for different conditions, can make adaptability
Adjustment.
Implement the preparation method of the wear-resistant coating of the present invention, increased by gradient and circulate increase N2Flow, on matrix
It is prepared for the hard coat of two kinds of big thickness, and its mechanical property has been carried out systematic research, find N2Flow is to big thickness
The regulating effect of coating composition is obvious, and the content of Ti element is little along layer depth changes in distribution, and the content of Al and N element is with N2Stream
Amount is changed significantly；The residual stress of the hard coat of big thickness along the distribution of layer depth, general trend from film base interface to surface by
Cumulative greatly, gradient increase N2The big thickness coatings that flow obtains and circulation gradient increase N2The big thickness coatings that flow obtains complete
Thickness mean stress is respectively-0.74GPa and-0.92GPa, changes N2Flow technique effectively reduces the remnants of big thickness coatings
Stress；Additionally, the section hardness distribution of big thickness coatings is consistent with N element content distribution, gradient increases N2Flow obtains
Big thickness coatings and circulation gradient increase N2The case hardness of the big thickness coatings that flow obtains respectively reaches (1825.9 ± 62)
HV and (1979.5 ± 88) HV；Adhesion test result shows, circulates big thickness coatings and has more preferable anti-scratch ability and break
Split toughness；The worn-out surface smoother of big thickness coatings is smooth, and the bur of worn-out surface and abrasive dust the most less, coating has
There is good tribological property, and gradient coating is compared circulation coating and had lower coefficient of friction and wear rate, shows more
Good anti-wear performance.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (9)
1. a preparation method for wear-resistant coating, for preparing hard coat at substrate surface, it is characterised in that described method bag
Include following steps:
S101, select the substrate of predetermined size and performance；
S102, surface to be deposited to substrate are carried out being dried；
S103, in the vacuum chamber of arc ion plating film device, the surface to be deposited of substrate is carried out sputter clean；
S104, in vacuum chamber, feed noble gas and N2, use arc ion plating (aip) cvd nitride thing on the surface of the substrate
Hard coat, in deposition process, gradient increases or circulation gradient increases N2Flow, in order to adjust in hard coat is residual
Residue stress；
S105, the hard coat on substrate is carried out vacuum annealing, the final wear-resistant coating obtaining big thickness.
Method the most according to claim 1, it is characterised in that determine according to the vacuum chamber size of arc ion beam coating equipment
Gradient increases or circulation gradient increases N2The numerical value of flow and at the N of each gradient2The sedimentation time that flow is kept.
Method the most according to claim 2, it is characterised in that increase N in gradient2In the case of flow, increase with N number of gradient
Add N2Flow, each gradient keeps predetermined time, and the temporal summation that N number of gradient is kept is total sedimentation time, wherein N
For integer.
Method the most according to claim 2, it is characterised in that increase N in circulation gradient2In the case of flow, total deposition
Time is divided into M cycle, increases N with L gradient in each cycle2Flow, each gradient keeps predetermined time, L
The temporal summation that individual gradient is kept is the time span in single cycle, and wherein M, L are integer.
5. according to the method described in claim 3 or 4, it is characterised in that the inert gas flow in vacuum chamber keeps constant, and
Increase N2Flow, the stagnation pressure in described vacuum chamber changes in the range of from 0.5Pa to 1.6Pa.
6., according to the method described in claim 3 or 4, it is characterised in that before deposition, the stagnation pressure regulation in vacuum chamber is to predetermined
Fixed value, gradient increase or circulation gradient increase N2During flow, reduce inert gas flow accordingly so that
Stagnation pressure keeps constant, and this predetermined fixed value is in the range of 0.5Pa to 1.6Pa.
Method the most according to claim 1, it is characterised in that sink on the surface of the substrate using arc ion plating (aip)
During long-pending nitride hard coating, the target of selection is Ti, TiAl or TiCrAl.
8. according to the method described in claim 3 or 4, it is characterised in that described N2Flow increases with 5～10sccm for gradient.
Method the most according to claim 1, it is characterised in that depositing temperature is 100～400 DEG C, total sedimentation time is
300～500 minutes.
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