CN104372299B - Sandwich construction hard, wear-resisting, lubricant coating and preparation method thereof - Google Patents
Sandwich construction hard, wear-resisting, lubricant coating and preparation method thereof Download PDFInfo
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- CN104372299B CN104372299B CN201310432322.9A CN201310432322A CN104372299B CN 104372299 B CN104372299 B CN 104372299B CN 201310432322 A CN201310432322 A CN 201310432322A CN 104372299 B CN104372299 B CN 104372299B
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- wear
- coating
- resisting
- sandwich construction
- lubricant coating
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Classifications
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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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
Abstract
The invention discloses a kind of sandwich construction hard, wear-resisting, lubricant coating and preparation method thereof, the sandwich construction coating is that alternating deposit Mo Al Si N and Mo Ag N coatings prepare the Mo Al Si N/Mo Ag N coatings of multilayer in the _ substrate by magnetron sputtering.The sandwich construction coating of the present invention has the high-quality superhard thin film being coated with higher hardness and inoxidizability temperature and low coefficient of friction and wear rate, particularly suitable high-speed dry type cutting instrument (milling cutter, drill bit) and other wear-resisting workpieces.The preparation method deposition velocity of the present invention is fast, and efficiency high, production cost is low.
Description
Technical field
The invention belongs to thin-film material and Surface Science technical field, and in particular to a kind of multilayer Mo-Al-Si-N/Mo-
Ag-N hard, wear-resisting, lubricant coating and its production and use.
Background technology
Hard and superhard coating are due to its higher hardness, good wearability, corrosion resistance and chemical stability etc.,
Through being widely used in the fields such as cutting industry, mould industry, geological drilling, weaving, automobile making, machine-building, Aero-Space,
And play more and more important effect.By taking application of the hard coat in cutting industry as an example, cutting tool surface coating hard is applied
After layer, compared with non-coated tool, the working durability improves more than 5~10 times.It is not coated with importantly, coated cutting tool can be processed
The material that the cutter of layer can not be processed, therefore be considered as to cut the revolution in history.
In process, on the one hand the high-speed friction between coated tool and workpiece can cause meaningless energy expenditure,
On the other hand also the temperature of coating surface is drastically raised, causes the mechanical performance of coating to deteriorate under thermal shock repeatedly.
Some data show that direct and indirect economic loss of the China every year caused by friction is up to billions of.If it is possible to drop
The coefficient of friction of low tool coating, will greatly save material and save the energy.In addition, with production efficiency and machining accuracy
Raising, the particularly technology such as DRY CUTTING, high-speed cutting and high-speed milling appearance, it is desirable to the face coat of instrument not only has
There is high hardness, and to have low coefficient of friction.Therefore, there is high hard, the high-quality coating of low-friction coefficient not only to have for research and development
There is realistic meaning and good economic benefit, and meet environmental protection under harmonious society's main body, the theory of energy-conservation, with important society
Can meaning.
As things go, in addition to DLC (DLC) coating, the lubricity of most hard and superhard coating
Can be all very poor.As can be seen from Table 1, industrial circle applies more TiN bases and CrN base coatings, and their coefficient of friction is general
Both greater than 0.4, after addition " C ", their coefficient of friction can be reduced to 0.1-0.2, but under the maximum operating temperature of coating
The amplitude of drop is also very big, even below 400 DEG C.The coefficient of friction of diamond-like coating is although relatively low (< 0.1), but be due to
Lower reason limits its application:1) heat endurance of DLC film is poor, occurs hydrogenolysis from stone when temperature is higher than 200 DEG C
Inkization changes, and during higher than 450 DEG C, starts obvious oxidative phenomena and complete hydrogenolysis occur from DLC film performance will substantially be deteriorated;
2) the most frequently used material of the tool matrix of DLC films deposited is tungsten-cobalt series hard alloy, but the cobalt in hard alloy is in CVD bar
Diamond can be promoted to cause the bond strength of diamond-film-like and substrate very low to graphite conversion under part, while the hardness of coating is anxious
Play declines.
Table 1:Famous Coatings Corporation's production coat type and performance
Therefore how can be in broadness by special prepared into component selections and structure design using magnetron sputtering technique
Have high rigidity in temperature range (0-800 DEG C) concurrently, the wear-resistant coating of low-friction coefficient turns into the focus of research.
The content of the invention
Have hard concurrently in broad temperature interval (0-800 DEG C) it is an object of the invention to provide one kind, it is wear-resisting, lubrication many
Rotating fields coating.
It is a further object of the present invention to provide one kind it is simple to operate, sedimentation rate is fast, it is easy to produce this multilayer knot in batches
The method of structure coating.
To realize the above purpose of the present invention, the present invention is adopted the following technical scheme that:
A kind of sandwich construction hard, wear-resisting, lubricant coating, it is characterised in that the coating includes alternate Mo-Al-Si-N
With Mo-Ag-N film layers, the sandwich construction with least one Mo-Al-Si-N/Mo-Ag-N, i.e., described sandwich construction hard,
Wear-resisting, lubricant coating is made up of the double-layer structure of one layer of Mo-Al-Si-N and one layer of Mo-Ag-N film layer.
Preferably, the coating has the repetitive structure of at least two Mo-Al-Si-N/Mo-Ag-N multilayers, i.e., described many
Rotating fields hard, wear-resisting, lubricant coating are by one layer of Mo-Al-Si-N and one layer of Mo-Ag-N film layer, then add at least one layer Mo-
The sandwich construction of Al-Si-N and one layer of Mo-Ag-N film layer is constituted.
It is highly preferred that the coating has the repetitive structure of at least three Mo-Al-Si-N/Mo-Ag-N multilayers.
It is further preferred that the coating has the repetitive structure of at least four Mo-Al-Si-N/Mo-Ag-N multilayers.
Another aspect of the present invention, described sandwich construction hard, wear-resisting, lubricant coating preparation method, including use
The method of magnetron sputtering the step of alternating deposit Mo-Al-Si-N and Mo-Ag-N film layer, passes through the elder generation on substrate on substrate
One layer of Mo-Ag-N film layer is deposited, redeposited one layer of Mo-Al-Si-N film layer forms a Mo-Al-Si-N/Mo-Ag-N many
Rotating fields.
Preferably, the alternating deposit Mo-Al-Si-N and it is repeated at least once more the step of Mo-Ag-N film layers, that is, is formed
The repetitive structure of two Mo-Al-Si-N/Mo-Ag-N multilayers.
It is highly preferred that the step of alternating deposit Mo-Al-Si-N and Mo-Ag-N film layers is repeated at least twice, i.e. shape
Into the repetitive structure of three Mo-Al-Si-N/Mo-Ag-N multilayers.
It is further preferred that the step of alternating deposit Mo-Al-Si-N and Mo-Ag-N film layers is repeated at least three times,
Form the repetitive structure of four Mo-Al-Si-N/Mo-Ag-N multilayers.
In a preferred embodiment, the alternating deposit Mo-Al-Si-N and wrap the step of Mo-Ag-N film layers
Include:
1) by stainless steel substrates it is polished, cleaning, drying after obtain film substrate;
2) Mo-Ag and Mo-Al-Si composition targets are separately mounted on DC cathode, stainless steel substrate loads sample stage, adjusted
The distance of whole target and substrate is 55mm;
3) start shooting, be evacuated to 1x10-3Then pa, heating substrate leads to people's argon nitrogen mixed gas to 400 DEG C, adjusts Ar/N2Stream
Amount is than to 3: 1, adjusting operating air pressure to 1.0Pa;
4) magnetron sputtering power supply is opened, adjustment sputtering power is respectively 90W and 120W, and dual-target sputtering is started simultaneously at, and is adjusted
The rotating speed of whole substrate, it is 90min to control total sputtering time;
5) sputtering is completed, and closes sputtering, heating power supply, stops ventilation, and sample cools under conditions of molecular pump is vacuumized
To less than 90 DEG C, molecular pump, powered-down source are closed;Room temperature is cooled under natural vacuum, sample is then taken out.
Another aspect of the invention, described sandwich construction hard, wear-resisting, lubricant coating, it is adaptable to high-speed dry type cutting
The high-quality superhard thin film being coated with instrument (milling cutter, drill bit) and wear-resisting workpiece.
Higher hardness and inoxidizability temperature and low coefficient of friction are had according to the sandwich construction coating of the present invention
And wear rate, the high-quality being coated with particularly suitable high-speed dry type cutting instrument (milling cutter, drill bit) and other wear-resisting workpieces is superhard thin
Film.
The sandwich construction coating production deposition velocity of the present invention is fast, and efficiency high, production cost is low.
Brief description of the drawings
Fig. 1 is the surface topography photo after 500 DEG C of the Mo-Ag-N coatings annealing 1 hour of the present invention.
Fig. 2 is the surface microstructure electron microscopic picture and diffraction pattern of the sandwich construction coating of the present invention.
Fig. 3 characterizes schematic diagram for the chemical key state of x-ray photoelectron spectrometer of the sandwich construction coating of the present invention.
Fig. 4 is sandwich construction coating X-ray diffraction spectrogram of the invention.
Fig. 5 is sandwich construction coating stereoscan photograph of the invention.
Fig. 6 is sandwich construction coating hardness test schematic diagram of the invention.
Fig. 7 is sandwich construction coating PVvalue testing schematic diagram of the invention.
Fig. 8 is sandwich construction coating cut test schematic diagram of the invention.
Embodiment
Explanation is further spread out to the present invention with reference to more specifically embodiment, it is to be noted that this hair
Bright Rotating fields hard, wear-resisting, lubricant coating are not limited to this specific structure and preparation method.For people in the art
Member it will be readily appreciated that, even if the following description content does not make any adjustments or corrected, can also be directly applied for herein
Other unspecified similar repetitive structures and preparation technology.
A kind of sandwich construction hard, wear-resisting, lubricant coating, it is characterised in that the coating includes alternate Mo-Al-Si-N
With Mo-Ag-N film layers, the sandwich construction with least one Mo-Al-Si-N/Mo-Ag-N, preferably with multiple Mo-Al-
Si-N/Mo-Ag-N multilayer repetitive structure, as shown in figure 5, the repetition for example with least 2 layers Mo-Al-Si-N/Mo-Ag-N
Structure, at least 3 layers Mo-Al-Si-N/Mo-Ag-N repetitive structure, at least 4 layers Mo-Al-Si-N/Mo-Ag-N repetitive structure,
At least 5 layers Mo-Al-Si-N/Mo-Ag-N repetitive structure, but not limited to this.Each layer of Mo-Al-Si-N/Mo-Ag-N film layer
Thickness there is no an any limitation, such as 10nm~800nm, 100~500nm, 150~350nm etc., but not limited to this all should
Within protection scope of the present invention.The thickness of each layer of Mo-Al-Si-N/Mo-Ag-N film layer can also be identical or different,
This is that magnetically controlled sputter method is relatively easy to realization by adjusting sputtering parameter, also should be within protection scope of the present invention.
It is former that sandwich construction hard, the wear-resisting, lubricant coating of the present invention has hard, wear-resisting, three big characteristics of lubrication technologies concurrently
Reason is as follows:
1) Ag modulus of shearing is smaller, therefore Ag films have excellent greasy property;The hardness of Mo-N coatings is high, wear-resisting
Property is good.
2) the high annealing experiment of Mo-Ag-N coatings shows:During annealing, the Ag in coating can be diffused into coating
Surface, form Ag particles or aggregate (as shown in figure 1, the surface topography after the annealing 1 hour of 500 DEG C of Mo-Ag-N coatings:Table
The white particle in face is silver).Follow-up friction and wear test shows, the shape between coating and friction pair is understood during friction
Into one layer of continuous Ag film so as to play a part of effectively lubricating.And the speed that Ag spreads out of Mo-N coatings to coating surface
Directly determine the service life of coating.
3) Mo-Al-Si-N coatings have high consistency, hardness and oxidation resistance temperature, it are deposited on Mo-Ag-N coatings
Surface can effectively slow down the speed that Ag diffuses to the surface and can protect Mo-Ag-N coatings not by high-temperature oxydation.
4) laminated coating structure, i.e., multiple Mo-Al-Si-N/Mo-Ag-N repetition can not only utilize super model graded effect
The overall performance of coating is improved, and can further extend the lubrication time of coating.
Therefore, sandwich construction coating of the invention has higher hardness and inoxidizability temperature and low coefficient of friction
And wear rate, so that the high-quality being coated with particularly suitable high-speed dry type cutting instrument (milling cutter, drill bit) and other wear-resisting workpieces is super
Hard film.
Another aspect of the present invention, alternating deposit Mo-Al-Si-N and Mo-Ag-N film layer prepares multilayer Mo-Al-Si-N/
The step of Mo-Ag-N coatings, includes:
1) by stainless steel substrates it is polished, cleaning, drying after obtain film substrate;
2) Mo-Ag and Mo-Al-Si composition targets are separately mounted on DC cathode, stainless steel substrate loads sample stage, adjusted
The distance of whole target and substrate is 55mm;
3) start shooting, be evacuated to 1x10-3Then pa, heating substrate leads to people's argon nitrogen mixed gas to 400 DEG C, adjusts Ar/N2Stream
Amount is than to 3: 1, adjusting operating air pressure to 1.0Pa;
4) magnetron sputtering power supply is opened, adjustment sputtering power is respectively 90W and 120W, and dual-target sputtering is started simultaneously at, and is adjusted
The rotating speed of whole substrate, it is 90min to control total sputtering time;
5) sputtering is completed, and closes sputtering, heating power supply, stops ventilation, and sample cools under conditions of molecular pump is vacuumized
To less than 90 DEG C, molecular pump, powered-down source are closed;Room temperature is cooled under natural vacuum, sample is then taken out.
The magnetic control sputtering device and technique refer to prior art, and this is well-known to those skilled in the art and normal
Plating membrane meanses.Specifically, for example according to above-mentioned preparation method, the surface that the Mo pieces of X-type are attached to Ag targets is used as Mo-Ag
Target, the Al and silicon chip of strip are attached to the surface of Mo targets as Mo-Al-Si composition targets respectively.By adjusting their area
Than the content that can control a component in coating.Cleaned stainless steel lining bottom is put on substrate pallet, 1X10 is evacuated down to- 3Pa, then heats substrate to 400 DEG C, is passed through nitrogen argon mixture gas (Ar: N2=3: 1), total operating air pressure is 1Pa, sputters work(
Rate is respectively 90W and 120W.After plated film 90 minutes, stop arc, stop the supple of gas or steam, break heating power supply, under conditions of molecular pump is vacuumized,
Gradually cool.When temperature is dropped to below 90 DEG C, molecular pump, powered-down source are closed.After being cooled to room temperature under natural vacuum, bleed off true
Sky, takes out sample, and pattern Microstructure characterization and performance test are carried out to coating, as a result as follows.
As shown in Fig. 2 the sandwich construction coating prepared using transmission electron microscope (JEOL, JEM-2000FX) to preceding method
High resolution electron microscopy picture and corresponding selection diffraction pattern that surface microstructure is obtained after being observed, as a result show coating by face
The crystal phase of heart cubic structure and amorphous phase composition.
As shown in figure 3, being prepared using x-ray photoelectron spectrometer (XPS, Japan, Axis ultradld) to preceding method
The chemical key state of sandwich construction coating characterized, as a result show to be primarily present Si-N in coating, Mo-N, Al-N keys.
As shown in figure 4, testing sandwich construction prepared by preceding method using Phillips X ' Pert types x-ray diffractometer
Abscissa in the x-ray diffraction pattern (XRD) obtained after coating, figure is 2 θ angles, and ordinate is diffracted intensity.As a result show
Coating is face-centred cubic structure.
As shown in figure 5, observing many of preceding method preparation using the field emission scanning electron microscope of JEOL companies of Japan
Obtained photo is shot after Rotating fields film surface appearance, it can be seen that coating is sandwich construction, each basic repeat unit Mo-
Al-Si-N/Mo-Ag-N thickness is 340nm.
As shown in fig. 6, the multilayer knot prepared using the nano-hardness tester (G200) of Aglient companies of the U.S. to preceding method
Structure coating carries out hardness test, as a result shows the hardness up to 43GPa of coating.
As shown in fig. 7, the multilayer knot prepared using U.S. CE TR UMT-2 type friction and wear tests instrument test preceding method
Coefficient of friction of the structure coating at 600 DEG C, as a result shows that the coefficient of friction of coating is low to 0.16.
As shown in figure 8, being observed using three-dimensional optical surface profiler (Wyko NT1100) the cut after testing friction
The result arrived, is 4 × 10-6mm with reference to the rate of depreciation that specific test parameter can calculate coating3/N·m。
Although the embodiment to the present invention gives detailed description and illustrated above, it should be noted that
We can carry out various equivalent changes and modification according to the conception of the present invention to above-mentioned embodiment, and the function produced by it is made
, all should be within protection scope of the present invention during with the spirit still covered without departing from specification and accompanying drawing.
Claims (7)
1. a kind of sandwich construction hard, wear-resisting, lubricant coating, it is characterised in that the coating include alternate Mo-Al-Si-N and
Mo-Ag-N film layers, the coating has the repetitive structure of at least two Mo-Al-Si-N/Mo-Ag-N multilayers, and the Mo-
The thickness of Al-Si-N/Mo-Ag-N monofilms is nanoscale.
2. sandwich construction hard according to claim 1, wear-resisting, lubricant coating, it is characterised in that the coating has extremely
The repetitive structure of few three Mo-Al-Si-N/Mo-Ag-N multilayers.
3. sandwich construction hard according to claim 2, wear-resisting, lubricant coating, it is characterised in that the coating has extremely
The repetitive structure of few four Mo-Al-Si-N/Mo-Ag-N multilayers.
4. sandwich construction hard, wear-resisting, lubricant coating preparation method described in claim any one of 1-3, including use magnetic
The method of control sputtering is on substrate the step of alternating deposit Mo-Al-Si-N and Mo-Ag-N film layer.
5. sandwich construction hard according to claim 4, wear-resisting, lubricant coating preparation method, it is characterised in that described
The step of alternating deposit Mo-Al-Si-N and Mo-Ag-N film layer, includes:
1) by stainless steel substrates it is polished, cleaning, drying after obtain film substrate;
2) Mo-Ag and Mo-Al-Si composition targets are separately mounted on DC cathode, stainless steel substrate loads sample stage, adjust target
The distance of material and substrate is 55mm;
3) start shooting, be evacuated to 1x10-3Pa, heating substrate then passes to argon nitrogen mixed gas to 400 DEG C, adjusts Ar/N2Flow-rate ratio
To 3: 1, adjustment operating air pressure to 1.0Pa;
4) magnetron sputtering power supply is opened, adjustment sputtering power is respectively 90W and 120W, and dual-target sputtering is started simultaneously at, adjustment lining
The rotating speed at bottom, it is 90min to control total sputtering time;
5) sputtering is completed, and closes sputtering, heating power supply, stops ventilation, and sample is cooled to 90 under conditions of molecular pump is vacuumized
Below DEG C, molecular pump, powered-down source are closed;Room temperature is cooled under natural vacuum, sample is then taken out.
6. sandwich construction hard according to claim 5, wear-resisting, lubricant coating preparation method, it is characterised in that described
The step of alternating deposit Mo-Al-Si-N and Mo-Ag-N film layer, repeats at least twice.
7. sandwich construction hard, wear-resisting, lubricant coating described in claim any one of 1-3, it is adaptable to high-speed dry type cutting work
The high-quality superhard thin film being coated with tool and wear-resisting workpiece.
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CN106811725B (en) * | 2015-11-27 | 2019-02-15 | 中国科学院宁波材料技术与工程研究所 | Wide adaptive lubricant coating of temperature range and the preparation method and application thereof |
CN107267940B (en) * | 2017-06-09 | 2019-06-18 | 中国科学院合肥物质科学研究院 | A kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate and its application |
CN112628381B (en) * | 2020-12-02 | 2022-05-10 | 东南大学 | Temperature self-adaptive lubricating gear and preparation method thereof |
WO2023019549A1 (en) * | 2021-08-20 | 2023-02-23 | 湖南泰嘉新材料科技股份有限公司 | Self-lubricating coated hob cutter for band saw blade milling teeth, preparation method therefor, and application thereof |
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WO2007141174A1 (en) * | 2006-06-02 | 2007-12-13 | Bekaert Advanced Coatings | A rotatable sputter target |
KR20110055399A (en) * | 2009-11-19 | 2011-05-25 | 한국생산기술연구원 | Sputtering target mother material of multi-component alloy system and method for manufacturing complex-coating thin film of multi-function |
DE102010053751A1 (en) * | 2010-10-28 | 2012-05-03 | Oerlikon Trading Ag, Trübbach | Molybdenum monoxide layers and their production by PVD |
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