CN107841717B - A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method - Google Patents
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method Download PDFInfo
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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
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
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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
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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Abstract
The invention discloses a kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method, include the steps that preparing composite solid lubrication film, can also have before preparing composite solid lubrication film the step of pre-sputtering preparation combines layer film in advance in substrate, can also have after preparation combines layer film in advance, prepare the step of preparing transition layer film before composite solid lubrication film.The present invention solves MoS2The problem that base solid lubricant film wearability in use is poor and use environment is harsh provides a kind of low-friction coefficient MoS2The preparation method of base composite solid lubrication film, provides MoS2A possibility that more occasions of base film use, and extend the service life of film.
Description
Technical field
The present invention relates to the coating fields to metal, and in particular to a kind of low-friction coefficient MoS2Base Metal-oxide is multiple
Close the preparation method of solid lubricating film.
Background technique
Solid lubricant film can be used for lubricant grease and use limited, bad environments and Maintenance free occasions, common to be applied to
The fields such as space technology, electrical engineering and automobile engineering.
Physical gas phase deposition technology, which refers to, is gasificated into gaseous state original for material source surface using physical method under vacuum conditions
Son, molecule or partial ionization have the technology of certain specific function film at ion, and in matrix surface deposition.Physical vapor is heavy
Product technology is broadly divided into vacuum vapor deposition techniques, sputter-deposition technology and ion-plating technique.Magnetron sputtering plating has been at present
It is widely used in: large-area glass plated film field, semiconductor, electronics plated film field, disk, hard disk plated film field, decoration film coating
Field.Since magnetron sputtering plating is compared to vapor deposition, target without phase-change, be convenient for automatic by chemical composition stability, good process repeatability
The defects of changing, and film is easy to uniform deposition, being not in molten drop phenomenon, therefore it is suitable for the series functions such as solid lubricating film
Based on film layer preparation.
Common solid lubricating film has: ferrous sulfide, molybdenum disulfide and tungsten disulfide sulfides film, diamond-like
With class graphite solid composite lubricating film, the soft metals such as gold, silver, tin, lead, magnesium, indium solid lubricant, lead oxide, boron oxide, oxidation
The metal oxide solids lubricant such as zinc, molybdenum trioxide, silica, the metal fluorides high temperature lubricating such as calcirm-fluoride, barium fluoride
Material.Wherein, molybdenum disulfide has good anisotropy and lower friction factor, and S has to the very strong adherency of metal
Power enables molybdenum disulfide to be perfectly adhered to metal surface, plays lubricating function always, especially in items such as high temperature, high vacuum
Still there is lower friction factor under part, be a kind of solid lubricating film of better performances.
Currently, molybdenum disulfide solid lubricating film begins to gradually aoxidize under atmospheric environment at 400 DEG C or so, friction system
Number increases, and with the increase of humidity in atmosphere, its coefficient of friction also increases, and limits the use of molybdenum disulfide solid lubricating film
Range.And when relative humidity is lower than 15% under atmospheric environment, the lubricant effect of molybdenum disulfide is best.Therefore in order to improve two sulphur
The oxidative resistance and moisture-proof for changing molybdenum, expand its use scope, often through metal, nonmetallic, the oxide of addition elemental
Or metal sulfide, fluoride etc. form two components or multiple groups part solid lubricant system to improve the lubrication of film, wear-resisting
Damage and moisture-resistant antioxygenic property.
On the other hand, when the adhesive force between solid lubricant and metal base is greater than shear strength in solid lubricating film
When, sliding can just occur inside the solid lubricating film, without between substrate metal and substrate metal or substrate gold
Belong between lubricant.Therefore, adhesive force differs bigger with shear strength, and better, friction is the greasy property of the material
Number and abrasion are also smaller.
For the film-base junction resultant force for improving solid lubricating film, on the one hand can be adjusted by technical parameter, into
Row operating air pressure, substrate heating, substrate bias adjusting and optimizing；On the other hand film-base can be reduced by film-base Performance Match
Internal stress is to carry out the optimization that solid lubricating film performance is realized in the methods of thin film material system selection, substrate surface treatment.
The shear strength for reducing solid lubricating film is that solid lubrication ingredient (such as stone of low shear strength is added in film
Ink, molybdenum disulfide etc.) Lai Shixian, and the wearability of solid lubricating film can significantly be mentioned by addition soft metal oxide
Height, while can also promote greasy property, playing the role of collaboration reduces coefficient of friction.
Since oxidation film inherently has boundary lubrication effect, research finds the lubricity and metal bottom of metal oxide
The free energy of formation Δ G of material reaction product is the oxide of positive value except zinc oxide makes an exception, and coefficient of friction is high and unstable.Usually
Solid lubricating film selects Pb3O4As adding ingredient, increasingly cause today concerned by people, Pb in environmental issue3O4Just by
Walk market of fading out.
Chinese patent CN201310549941.6 discloses a kind of preparation process of dry lubrication film, is with molybdenum disulfide, phosphorus
Acid, zinc oxide etc. are prepared through slurry, and dry lubrication film is prepared in the processes such as oil removing, derusting, sandblasting, spraying, solidification.But this is specially
The process repeatability of the obtained dry lubrication film of benefit is bad, is not easy to automate, and film is not easy to uniform deposition, it may appear that molten drop etc.
Defect phenomenon, and the film of dry lubrication film-base junction resultant force is low, and the shear strength of film is higher.
Therefore, in order to improve the oxidative resistance and moisture-proof of molybdenum disulfide, improve the lubrication of film, wear-resistant and moisture-resistant
Antioxygenic property improves film-base junction resultant force of solid lubricating film, reduces the shear strength of solid lubricating film, solve two sulphur
Change the problem that molybdenum base solid lubricant film wearability in use is poor and use environment is harsh, it is desirable to provide a kind of low-friction coefficient
MoS2The preparation method of Quito member composite solid lubrication film, to provide a possibility that more occasions of molybdenum disulfide base film use,
And extend the service life of film.
Summary of the invention
The present invention is in view of the above-mentioned problems, provide a kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubricant is thin
The preparation method of film.
Technical solution used by the present invention solves the above problems is: a kind of low-friction coefficient MoS2Base Metal-oxide
The preparation method of composite solid lubrication film, comprising the following steps: prepare composite solid lubrication film: by Ti or Al metallic target
Material, ZnO target material and MoS2Target cosputtering prepares composite solid lubrication film.
Wherein, molybdenum disulfide, which is co-deposited Ti, Al metal, can reduce MoS2The content of oxygen impurities in solid lubricating film, from
And the hardness and abrasion resistance properties of film are improved, wherein MoS2Gold is embedded in will form superhard hexagon after Ti metal co-deposition
Belong to substrate surface, performance is best；
The hardness of zinc oxide is about 4.5, is a kind of relatively soft material, can be used in grease making as lubricating additive
With, the elastic constant of zinc oxide is smaller, and thermal stability and heat conductivity are preferable, and boiling point is high, and thermal expansion coefficient is low, and
Since zinc oxide has boundary lubrication effect, the free energy of formation Δ G with metal base reaction product is positive value, and the system that rubs
Number is low and stablizes, and being suitable as adding ingredient is used to prepare the good solid lubricating film of low-friction coefficient, wearability, while also can
Promote greasy property, playing the role of collaboration reduces coefficient of friction.
Further, low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film with a thickness of 0.8 μm~
3.2μm。
Further, preparing composite solid lubrication film further includes before being splashed in advance in substrate using Ti or Al metal targets
Penetrate the step of preparation combines layer film in advance.Wherein pre-deposition binder course before magnetron sputtering plating, can reduce film and matrix it
Between stress, improve the binding force between film and matrix, while forming oxide film under the high temperature conditions, prevent matrix
Further oxidation.
Further, preparation combines the step of layer film in advance, specifically: it is pre- in substrate using Ti or Al metal targets
Sputtering combines layer film 8min~15min, and pre-sputtering power is d.c. sputtering target power supply 100W, the pre- thickness for combining layer film
For 25nm~35nm.
Further, substrate are as follows: monocrystalline silicon or stainless steel.
Further, prepare composite solid lubrication film, specifically: background vacuum be 5 × 10-4Pa, operating air pressure
Are as follows: Ar protective gas, 0.5Pa air pressure, base reservoir temperature are room temperature, and substrate rotation speed is 0.05r/s, target-substrate distance 15cm~
Pass through Ti or Al metal targets and ZnO target, MoS under the conditions of the technological parameter of 17cm2Three target co-sputtering of target prepares composite solid
Body composite lubricating film, wherein Ti or Al metal targets use power for the d.c. sputtering target power supply of 10W~50W, and ZnO target material uses
50W radio-frequency sputtering target power supply, MoS2Target uses 100W radio-frequency sputtering target power supply, and the cosputtering time is 3h.
Further, after preparation combines layer film in advance, to prepare before composite solid lubrication film further include that prepare transition zone thin
The step of film.
Further, transition layer film is prepared, specifically: in 0.5h, use Ti or Al metal targets, ZnO target material
And MoS2Three target co-sputtering of target prepares transition layer film, wherein the d.c. sputtering target power supply power of Ti or Al metal targets by
10W~50W drops to 5W~25W, and the radio-frequency sputtering target power supply power of ZnO target material drops to 25W, MoS by 50W2The radio frequency of target splashes
Power of shooting at the target by 40W is raised to 100W.
Further, composite solid lubrication film is prepared are as follows: in the d.c. sputtering target power supply function of Ti or Al metal targets
Rate is 5W~25W, and the radio-frequency sputtering target power supply power of ZnO target material is 25W, MoS2The radio-frequency sputtering target power supply power of target is
Continue to be coated with 2.5h on the basis of transition layer film under conditions of 100W.
The invention has the advantages that
1. it is that common metal target assists soft is Zinc oxide doped to arrive molybdenum disulfide material that the present invention, which selects adding ingredient,
In system, collaboration antifriction effect is formed, while guaranteeing film strength and certain wear-resisting property, processing film is at low cost, uses
Magnetron sputtering prepares film, and is aided with transition zone design, and process flow is simple, and prepared film comprehensive performance reaches requirement,
Feasibility with industrialized production；
2. the present invention after membranous layer ingredient system optimization, preparation technology parameter debugging, prepares, internal structure is fine and close, has
The low-friction coefficient solid lubricating film excellent down to 0.072, abrasion resistance properties, solid lubricant and friction surface, which are formed, to be shifted
Film has good friction reducing effect, extends the service life of matrix；
3. solid lubricant coating formation process of the present invention is simple, preparation cost is low.
Detailed description of the invention
It forms part of this specification, show embodiment party of the invention for further understanding attached drawing of the invention
Case, and be used to illustrate preparation flow of the invention together with specification.In the accompanying drawings:
Fig. 1 is low-friction coefficient MoS made from the embodiment of the present invention 22Base Metal-oxide composite solid lubrication film warp
Wear morphology after abrasion；
Fig. 2 is low-friction coefficient MoS made from the embodiment of the present invention 22Base Metal-oxide composite solid lubrication film warp
Polishing scratch cross section profile after abrasion；
Fig. 3 is low-friction coefficient MoS made from the embodiment of the present invention 22Base Metal-oxide composite solid lubrication film
SEM figure；
Fig. 4 is low-friction coefficient MoS made from the embodiment of the present invention 22Base Metal-oxide composite solid lubrication film is cut
The SEM in face schemes；
Fig. 5 is low-friction coefficient MoS made from the embodiment of the present invention 62Base Metal-oxide composite solid lubrication film warp
Wear morphology after abrasion；
Fig. 6 is low-friction coefficient MoS made from the embodiment of the present invention 62Base Metal-oxide composite solid lubrication film warp
Polishing scratch cross section profile after abrasion；
Fig. 7 is low-friction coefficient MoS made from the embodiment of the present invention 62Base Metal-oxide composite solid lubrication film
SEM figure；
Fig. 8 is low-friction coefficient MoS made from the embodiment of the present invention 62Base Metal-oxide composite solid lubrication film is cut
The SEM in face schemes；
Fig. 9 is low-friction coefficient MoS made from the embodiment of the present invention 102Base Metal-oxide composite solid lubrication film
Wear morphology after experience wear；
Figure 10 is low-friction coefficient MoS made from the embodiment of the present invention 102Base Metal-oxide composite solid lubrication film
Polishing scratch cross section profile after experience wear；
Figure 11 is low-friction coefficient MoS made from the embodiment of the present invention 102Base Metal-oxide composite solid lubrication film
SEM figure；
Figure 12 is low-friction coefficient MoS made from the embodiment of the present invention 102Base Metal-oxide composite solid lubrication film
The SEM in section schemes；
Figure 13 is low-friction coefficient MoS made from the embodiment of the present invention 122Base Metal-oxide composite solid lubrication film
Wear morphology after experience wear；
Figure 14 is low-friction coefficient MoS made from the embodiment of the present invention 122Base Metal-oxide composite solid lubrication film
Polishing scratch cross section profile after experience wear；
Figure 15 is low-friction coefficient MoS made from the embodiment of the present invention 122Base Metal-oxide composite solid lubrication film
SEM figure；
Figure 16 is low-friction coefficient MoS made from the embodiment of the present invention 122Base Metal-oxide composite solid lubrication film
The SEM in section schemes；
Figure 17 is comparative example 1 of the present invention, embodiment 2, MoS made from embodiment 62Quito member composite solid lubrication film
PVvalue testing figure；
Figure 18 is comparative example 1 of the present invention, embodiment 10, MoS made from embodiment 122Quito member composite solid lubrication film
PVvalue testing figure；
Figure 19 is the embodiment of the present invention 2, embodiment 3, MoS made from embodiment 4 and comparative example 12Quito member complex solid
The XRD diagram of composite lubricating film；
Figure 20 is the embodiment of the present invention 6, embodiment 7, MoS made from embodiment 8 and comparative example 12Quito member complex solid
The XRD diagram of composite lubricating film；
Figure 21 is embodiment 10, MoS made from embodiment 12 and comparative example 12The XRD of Quito member composite solid lubrication film
Figure.
Specific embodiment
The embodiment of the present invention is described in detail below in conjunction with attached drawing, but the present invention can be defined by the claims
Implement with the multitude of different ways of covering.
Embodiment 1
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method
(1) surface polishing, acetone and alcohol is carried out to monocrystal silicon substrate to be cleaned by ultrasonic, it is spare after drying；
(2) splash-proofing sputtering process parameter is arranged: background vacuum is 5 × 10-4Pa, operating air pressure are as follows: Ar protective gas, 0.5Pa
Air pressure, base reservoir temperature are room temperature, and substrate rotation speed is 0.05r/s, target-substrate distance 17cm；
(3) composite solid lubrication film is prepared: by Ti metal targets and ZnO target material, MoS2Work of the target in step (2)
Cosputtering prepares composite solid lubrication film under skill Parameter Conditions, and wherein Ti metal targets use power for the d.c. sputtering of 10W
Target power supply, ZnO target material use 50W radio-frequency sputtering target power supply, MoS2Target uses 100W radio-frequency sputtering target power supply, when cosputtering
Between be 3h, obtaining a kind of membrane structure is Ti-ZnO-MoS2Low-friction coefficient MoS2Base Metal-oxide composite solid lubricant
Film, the film with a thickness of 3 μm.
Embodiment 2
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method
(1) surface polishing, acetone and alcohol is carried out to monocrystal silicon substrate to be cleaned by ultrasonic, it is spare after drying；
(2) splash-proofing sputtering process parameter is arranged: background vacuum is 5 × 10-4Pa, operating air pressure are as follows: Ar protective gas, 0.5Pa
Air pressure, base reservoir temperature are room temperature, and substrate rotation speed is 0.05r/s, target-substrate distance 15cm；
(3) preparation combines layer film in advance: using Ti metal targets, pre-sputtering prepares and combines layer film in advance in substrate
10min, pre-sputtering power is d.c. sputtering target power supply 100W, in advance in conjunction with layer film with a thickness of 30nm；
(4) composite solid lubrication film is prepared: by Ti metal targets and ZnO target material, MoS2Target is thin in pre- binder course
Cosputtering prepares composite solid lubrication film on the basis of film, and wherein Ti metal targets use power for the d.c. sputtering target of 13W
Power supply, ZnO target material use 50W radio-frequency sputtering target power supply, MoS2Target uses 100W radio-frequency sputtering target power supply, and the cosputtering time is
3h, obtaining a kind of membrane structure is Ti/Ti-ZnO-MoS2Low-friction coefficient MoS2Base Metal-oxide composite solid lubricant
Film, the film with a thickness of 2.05 μm.
Using Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences MFT-R4000 high speed reciprocating friction Wear Tester to above
The film of technique preparation has carried out performance detection.Test condition are as follows: room temperature, RH50%.Friction pair material is Φ 4mm steel ball, is drawn
Using 120 ° of cone angle, the diamond penetrator of tip radius 0.2mm, reciprocating friction speed is 240mm/min for trace experiment.Test result
Are as follows: film fails critical load (LC2) for 26N, and coefficient of friction is 0.079 (240mm/min reciprocating friction speed, 10N load),
Line tear strength is 1.67 × 10-7。
Composite solid lubricant film polishing scratch in process of friction and wear is shallower, and wear scar width is relatively narrow, in the portion that ink trace is deeper
Position will appear part slight crack, illustrate in process of friction and wear, and the wearability of film is preferable, while film layer is in certain hardness,
It will appear fracture phenomena under fatigue stress effect, film shows the wear mechanism that adhesive wear and fatigue wear combine.It should
Film wear morphology and polishing scratch cross section profile are as shown in Figure 1 and Figure 2.
The microscopic appearance of composite solid lubrication film made from the embodiment is tested, test results are shown in figure 3, and test should
The microscopic appearance in composite solid lubrication film section made from embodiment, test result is as shown in Fig. 4.The results show that this implementation
Composite solid lubrication film surface compact made from example visually observes film in mirror surface, and scanning electron microscope lower surface is in 20nm or so
Graininess, occasionally there is under 100,000 times of visuals field particle agglomeration to form the bulky grain protrusion of 250nm or so together；Film sections are in cause
Close shape.
Embodiment 3
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method
Except when preparing composite solid lubrication film Ti metal targets use power for the d.c. sputtering target power supply of 25W in addition to, system
For the composite solid lubrication film obtained with a thickness of 2.5 μm, remaining is identical as the preparation method of embodiment 2.
Embodiment 4
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method
Except when preparing composite solid lubrication film Ti metal targets use power for the d.c. sputtering target power supply of 50W in addition to, system
For the composite solid lubrication film obtained with a thickness of 2.3 μm, remaining is identical as the preparation method of embodiment 2.
Embodiment 5
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method
(1) surface polishing, acetone and alcohol is carried out to stainless steel base to be cleaned by ultrasonic, it is spare after drying；
(2) splash-proofing sputtering process parameter is arranged: background vacuum is 5 × 10-4Pa, operating air pressure are as follows: Ar protective gas, 0.5Pa
Air pressure, base reservoir temperature are room temperature, and substrate rotation speed is 0.05r/s, target-substrate distance 16cm；
(3) it prepares transition layer film: in 0.5h, using Ti metal targets, ZnO target material and MoS2Three target of target is being tied in advance
Cosputtering prepares transition layer film on the basis of closing layer film, wherein the d.c. sputtering target power supply power of Ti metal targets is by 13W
8W is dropped to, the radio-frequency sputtering target power supply power of ZnO target material drops to 25W, MoS by 50W2The radio-frequency sputtering target power supply power of target
100W is raised to by 40W；
(4) it prepares composite solid lubrication film: being 8W, ZnO target material in the d.c. sputtering target power supply power of Ti metal targets
Radio-frequency sputtering target power supply power be 25W, MoS2The radio-frequency sputtering target power supply power of target be 100W under conditions of in transition zone
Continue to be coated with 2.5h on the basis of film, obtaining a kind of membrane structure is Ti/Ti-ZnO-MoS2Low-friction coefficient MoS2Fund
Category-oxide composite solid lubrication film, the film with a thickness of 2.0 μm.
Embodiment 6
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method
(1) surface polishing, acetone and alcohol is carried out to monocrystal silicon substrate to be cleaned by ultrasonic, it is spare after drying；
(2) splash-proofing sputtering process parameter is arranged: background vacuum is 5 × 10-4Pa, operating air pressure are as follows: Ar protective gas, 0.5Pa
Air pressure, base reservoir temperature are room temperature, and substrate rotation speed is 0.05r/s, target-substrate distance 15cm；
(3) preparation combines layer film in advance: using Ti metal targets, pre-sputtering prepares and combines layer film in advance in substrate
10min, pre-sputtering power is d.c. sputtering target power supply 100W, in advance in conjunction with layer film with a thickness of 28nm；
(4) it prepares transition layer film: in 0.5h, using Ti metal targets, ZnO target material and MoS2Three target of target is being tied in advance
Cosputtering prepares transition layer film on the basis of closing layer film, wherein the d.c. sputtering target power supply power of Ti metal targets is by 10W
5W is dropped to, the radio-frequency sputtering target power supply power of ZnO target material drops to 25W, MoS by 50W2The radio-frequency sputtering target power supply power of target
100W is raised to by 40W；
(5) it prepares composite solid lubrication film: being 5W, ZnO target material in the d.c. sputtering target power supply power of Ti metal targets
Radio-frequency sputtering target power supply power be 25W, MoS2The radio-frequency sputtering target power supply power of target be 100W under conditions of in transition zone
Continue to be coated with 2.5h on the basis of film, obtaining a kind of membrane structure is Ti/Ti-ZnO-MoS2Low-friction coefficient MoS2Fund
Category-oxide composite solid lubrication film, the film with a thickness of 3.18 μm.
Using Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences MFT-R4000 high speed reciprocating friction Wear Tester to above
The film of technique preparation has carried out performance detection.Test condition are as follows: room temperature, RH50%.Friction pair material is Φ 4mm steel ball, is drawn
Using 120 ° of cone angle, the diamond penetrator of tip radius 0.2mm, reciprocating friction speed is 240mm/min for trace experiment.Test result
Are as follows: diaphragm failure critical load (LC2) is 20N, and coefficient of friction is 0.072 (240mm/min reciprocating friction speed, 10N load
Lotus), 0.08 (240mm/min reciprocating friction speed, 5N load), line tear strength is 1.0 × 10-7。
Composite solid lubricant film polishing scratch in process of friction and wear is shallower, and wear scar width is relatively narrow, in the portion that ink trace is deeper
Position will appear part slight crack, illustrate in process of friction and wear, and the wearability of film is preferable, while film layer is in certain hardness,
It will appear fracture phenomena under fatigue stress effect, film shows the wear mechanism that adhesive wear and fatigue wear combine.It should
Film wear morphology and polishing scratch cross section profile are as shown in Figure 5, Figure 6.
The microscopic appearance of composite solid lubrication film made from the embodiment is tested, test results are shown in figure 7；Test should
The microscopic appearance in composite solid lubrication film section made from embodiment, test result is as shown in Fig. 8.As the result is shown: the implementation
Composite solid lubrication film compact structure made from example visually observes film in mirror surface, and surface sweeping Electronic Speculum lower surface is left in 10-20nm
Right graininess；Section is in piece column, there is the obvious direction of growth.
Embodiment 7
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method
(1) surface polishing, acetone and alcohol is carried out to monocrystal silicon substrate to be cleaned by ultrasonic, it is spare after drying；
(2) splash-proofing sputtering process parameter is arranged: background vacuum is 5 × 10-4Pa, operating air pressure are as follows: Ar protective gas, 0.5Pa
Air pressure, base reservoir temperature are room temperature, and substrate rotation speed is 0.05r/s, target-substrate distance 16cm；
(3) preparation combines layer film in advance: using Ti metal targets, pre-sputtering prepares and combines layer film in advance in substrate
15min, pre-sputtering power is d.c. sputtering target power supply 100W, in advance in conjunction with layer film with a thickness of 35nm；
(4) it prepares transition layer film: in 0.5h, using Ti metal targets, ZnO target material and MoS2Three target of target is being tied in advance
Cosputtering prepares transition layer film on the basis of closing layer film, wherein the d.c. sputtering target power supply power of Ti metal targets is by 18W
12W is dropped to, the radio-frequency sputtering target power supply power of ZnO target material drops to 25W, MoS by 50W2The radio-frequency sputtering target power supply power of target
100W is raised to by 40W；
(5) it prepares composite solid lubrication film: being 12W, ZnO target in the d.c. sputtering target power supply power of Ti metal targets
The radio-frequency sputtering target power supply power of material is 25W, MoS2The radio-frequency sputtering target power supply power of target be 100W under conditions of in transition
Continue to be coated with 2.5h on the basis of layer film, obtaining a kind of membrane structure is Ti/Ti-ZnO-MoS2Low-friction coefficient MoS2Base
Metal-oxide composite solid lubrication film, the film with a thickness of 3.2 μm.
Embodiment 8
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method
(1) surface polishing, acetone and alcohol is carried out to monocrystal silicon substrate to be cleaned by ultrasonic, it is spare after drying；
(2) splash-proofing sputtering process parameter is arranged: background vacuum is 5 × 10-4Pa, operating air pressure are as follows: Ar protective gas, 0.5Pa
Air pressure, base reservoir temperature are room temperature, and substrate rotation speed is 0.05r/s, target-substrate distance 16cm；
(3) preparation combines layer film in advance: using Ti metal targets, pre-sputtering prepares and combines layer film in advance in substrate
14min, pre-sputtering power is d.c. sputtering target power supply 100W, in advance in conjunction with layer film with a thickness of 35nm；
(4) it prepares transition layer film: in 0.5h, using Ti metal targets, ZnO target material and MoS2Three target of target is being tied in advance
Cosputtering prepares transition layer film on the basis of closing layer film, wherein the d.c. sputtering target power supply power of Ti metal targets is by 25W
20W is dropped to, the radio-frequency sputtering target power supply power of ZnO target material drops to 25W, MoS by 50W2The radio-frequency sputtering target power supply power of target
100W is raised to by 40W；
(5) it prepares composite solid lubrication film: being 20W, ZnO target in the d.c. sputtering target power supply power of Ti metal targets
The radio-frequency sputtering target power supply power of material is 25W, MoS2The radio-frequency sputtering target power supply power of target be 100W under conditions of in transition
Continue to be coated with 2.5h on the basis of layer film, obtaining a kind of membrane structure is Ti/Ti-ZnO-MoS2Low-friction coefficient MoS2Base
Metal-oxide composite solid lubrication film, the film with a thickness of 1.8 μm.
Embodiment 9
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method
(1) surface polishing, acetone and alcohol is carried out to stainless steel base to be cleaned by ultrasonic, it is spare after drying；
(2) splash-proofing sputtering process parameter is arranged: background vacuum is 5 × 10-4Pa, operating air pressure are as follows: Ar protective gas, 0.5Pa
Air pressure, base reservoir temperature are room temperature, and substrate rotation speed is 0.05r/s, target-substrate distance 16cm；
(3) composite solid lubrication film is prepared: by Al metal targets and ZnO target material, MoS2Work of the target in step (2)
Cosputtering prepares composite solid lubrication film under skill Parameter Conditions, and wherein Al metal targets use power for the d.c. sputtering of 10W
Target power supply, ZnO target material use 50W radio-frequency sputtering target power supply, MoS2Target uses 100W radio-frequency sputtering target power supply, when cosputtering
Between be 3h, obtaining a kind of membrane structure is Al-ZnO-MoS2Low-friction coefficient MoS2Base Metal-oxide composite solid lubricant
Film, the film with a thickness of 0.8 μm.
Embodiment 10
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method
(1) surface polishing, acetone and alcohol is carried out to monocrystal silicon substrate to be cleaned by ultrasonic, it is spare after drying；
(2) splash-proofing sputtering process parameter is arranged: background vacuum is 5 × 10-4Pa, operating air pressure are as follows: Ar protective gas, 0.5Pa
Air pressure, base reservoir temperature are room temperature, and substrate rotation speed is 0.05r/s, target-substrate distance 17cm；
(3) preparation combines layer film in advance: using Al metal targets, pre-sputtering prepares and combines layer film 8min in advance in substrate,
Pre-sputtering power is d.c. sputtering target power supply 100W, in advance in conjunction with layer film with a thickness of 25nm；
(4) composite solid lubrication film is prepared: by Al metal targets and ZnO target material, MoS2Target is thin in pre- binder course
Cosputtering prepares composite solid lubrication film on the basis of film, and wherein Al metal targets use power for the d.c. sputtering target of 10W
Power supply, ZnO target material use 50W radio-frequency sputtering target power supply, MoS2Target uses 100W radio-frequency sputtering target power supply, and the cosputtering time is
3h, obtaining a kind of membrane structure is Al/Al-ZnO-MoS2Low-friction coefficient MoS2Base Metal-oxide composite solid lubricant
Film, the film with a thickness of 2.82 μm.
Using Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences MFT-R4000 high speed reciprocating friction Wear Tester to above
The film of technique preparation has carried out performance detection.Test condition are as follows: room temperature, RH50%.Friction pair material is Φ 4mm steel ball, is drawn
Using 120 ° of cone angle, the diamond penetrator of tip radius 0.2mm, reciprocating friction speed is 240mm/min for trace experiment.Test result
Are as follows: diaphragm failure critical load (LC2) is 12N, and coefficient of friction is 0.13 (240mm/min reciprocating friction speed, 10N load),
Line tear strength is 6.3 × 10-8。
Composite solid lubricant film polishing scratch in process of friction and wear is shallower, and wear scar width is relatively narrow, in the portion that ink trace is deeper
Position will appear part slight crack, illustrate in process of friction and wear, and the wearability of film is preferable, while film layer is in certain hardness,
It will appear fracture phenomena under fatigue stress effect, film shows the wear mechanism that adhesive wear and fatigue wear combine.It should
Film wear morphology and polishing scratch cross section profile are as shown in Fig. 9, Figure 10.
The microscopic appearance of composite solid lubrication film made from the embodiment is tested, test result is as shown in figure 11；Test
The microscopic appearance in composite solid lubrication film section, test result made from the embodiment are as shown in figure 12.As the result is shown: should
Composite solid lubrication film surface compact made from embodiment visually observes film in mirror surface, and scanning electron microscope lower surface is in 10-
The graininess of 20nm or so；Film sections are in close column.
Embodiment 11
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method
(1) surface polishing, acetone and alcohol is carried out to stainless steel base to be cleaned by ultrasonic, it is spare after drying；
(2) splash-proofing sputtering process parameter is arranged: background vacuum is 5 × 10-4Pa, operating air pressure are as follows: Ar protective gas, 0.5Pa
Air pressure, base reservoir temperature are room temperature, and substrate rotation speed is 0.05r/s, target-substrate distance 17cm；
(3) it prepares transition layer film: in 0.5h, using Al metal targets, ZnO target material and MoS2Three target of target is being tied in advance
Cosputtering prepares transition layer film on the basis of closing layer film, wherein the d.c. sputtering target power supply power of Al metal targets is by 10W
5W is dropped to, the radio-frequency sputtering target power supply power of ZnO target material drops to 25W, MoS by 50W2The radio-frequency sputtering target power supply power of target by
40W is raised to 100W；
(4) it prepares composite solid lubrication film: being 5W, ZnO target material in the d.c. sputtering target power supply power of Al metal targets
Radio-frequency sputtering target power supply power be 25W, MoS2The radio-frequency sputtering target power supply power of target be 100W under conditions of in transition zone
Continue to be coated with 2.5h on the basis of film, obtaining a kind of membrane structure is Al-ZnO-MoS2Low-friction coefficient MoS2Base Metal-
Oxide composite solid lubrication film, the film with a thickness of 2.4 μm.
Embodiment 12
A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method
(1) surface polishing, acetone and alcohol is carried out to monocrystal silicon substrate to be cleaned by ultrasonic, it is spare after drying；
(2) splash-proofing sputtering process parameter is arranged: background vacuum is 5 × 10-4Pa, operating air pressure are as follows: Ar protective gas, 0.5Pa
Air pressure, base reservoir temperature are room temperature, and substrate rotation speed is 0.05r/s, target-substrate distance 17cm；
(3) preparation combines layer film in advance: using Al metal targets, pre-sputtering prepares and combines layer film in advance in substrate
11min, pre-sputtering power is d.c. sputtering target power supply 100W, in advance in conjunction with layer film with a thickness of 31nm；
(4) it prepares transition layer film: in 0.5h, using Al metal targets, ZnO target material and MoS2Three target of target is being tied in advance
Cosputtering prepares transition layer film on the basis of closing layer film, wherein the d.c. sputtering target power supply power of Al metal targets is by 10W
5W is dropped to, the radio-frequency sputtering target power supply power of ZnO target material drops to 25W, MoS by 50W2The radio-frequency sputtering target power supply power of target by
40W is raised to 100W；
(5) it prepares composite solid lubrication film: being 5W, ZnO target material in the d.c. sputtering target power supply power of Al metal targets
Radio-frequency sputtering target power supply power be 25W, MoS2The radio-frequency sputtering target power supply power of target be 100W under conditions of in transition zone
Continue to be coated with 2.5h on the basis of film, obtaining a kind of membrane structure is Al/Al-ZnO-MoS2Low-friction coefficient MoS2Fund
Category-oxide composite solid lubrication film, the film with a thickness of 0.874 μm.
Using Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences MFT-R4000 high speed reciprocating friction Wear Tester to above
The film of technique preparation has carried out performance detection.Test condition are as follows: room temperature, RH50%.Friction pair material is Φ 4mm steel ball, is drawn
Using 120 ° of cone angle, the diamond penetrator of tip radius 0.2mm, reciprocating friction speed is 240mm/min for trace experiment.Test result
Are as follows: diaphragm failure critical load (LC2) is 31.8N, and coefficient of friction is 0.101 (240mm/min reciprocating friction speed, 10N load
Lotus), line tear strength is 2.1 × 10-8。
Composite solid lubricant film polishing scratch in process of friction and wear is shallower, and wear scar width is relatively narrow, in the portion that ink trace is deeper
Position will appear part slight crack, illustrate in process of friction and wear, and the wearability of film is preferable, while film layer is in certain hardness,
It will appear fracture phenomena under fatigue stress effect, film shows the wear mechanism that adhesive wear and fatigue wear combine.It should
Film wear morphology and polishing scratch cross section profile are as shown in Figure 13, Figure 14.
The microscopic appearance of composite solid lubrication film made from the embodiment is tested, test result is as shown in figure 15；Test
The microscopic appearance in composite solid lubrication film section, test result made from the embodiment are as shown in figure 16.As the result is shown: should
Composite solid lubrication film compact structure made from embodiment visually observes film in mirror surface, and surface sweeping Electronic Speculum lower surface is in 10-
The graininess of 20nm or so, partial particulate accumulate in the bulky grain for being formed together 60-80nm or so, there is apparent boundary between bulky grain
Line；Section is in piece column, there is the more apparent direction of growth.
Comparative example 1
A kind of low-friction coefficient MoS2The preparation method of base oxide composite solid lubrication film
(1) surface polishing, acetone and alcohol is carried out to monocrystal silicon substrate to be cleaned by ultrasonic, it is spare after drying；
(2) splash-proofing sputtering process parameter is arranged: background vacuum is 5 × 10-4Pa, operating air pressure are as follows: Ar protective gas, 0.5Pa
Air pressure, base reservoir temperature are room temperature, and substrate rotation speed is 0.05r/s, target-substrate distance 15cm；
(3) composite solid lubrication film is prepared: by ZnO target material, MoS2Target is under the conditions of the technological parameter of step (2)
Cosputtering prepares composite solid lubrication film, and wherein ZnO target material uses 50W radio-frequency sputtering target power supply, MoS2Target uses 100W
Radio-frequency sputtering target power supply, cosputtering time are 3h, and obtaining a kind of membrane structure is ZnO-MoS2MoS2Base oxide complex solid
Composite lubricating film, the film with a thickness of 3 μm.
Experimental example 1
Using Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences MFT-R4000 high speed reciprocating friction Wear Tester to comparison
The coefficient of friction of film prepared by example 1, embodiment 2, embodiment 6 is detected.Test condition are as follows: room temperature, RH50%.Friction is secondary
Material is Φ 4mm steel ball, and scratch experiment is using 120 ° of cone angle, the diamond penetrator of tip radius 0.2mm, reciprocating friction speed
240mm/min.Test result is as shown in figure 17.
As shown in Figure 17, comparative example 1, embodiment 2, MoS made from embodiment 62Quito member composite solid lubrication film at
The film friction coefficient divided is low, and abrasion resistance properties are good, good bonding strength.
Experimental example 2
Using Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences MFT-R4000 high speed reciprocating friction Wear Tester to comparison
The coefficient of friction of film prepared by example 1, embodiment 10, embodiment 12 is detected.Test condition are as follows: room temperature, RH50%.Friction
Auxiliary material is Φ 4mm steel ball, and scratch experiment is using 120 ° of cone angle, the diamond penetrator of tip radius 0.2mm, reciprocating friction speed
For 240mm/min.Test result is as shown in figure 18.
As shown in Figure 18, embodiment 10, MoS made from embodiment 122Quito member composite solid lubrication film ingredient it is thin
Film coefficient of friction is low, and abrasion resistance properties are good, good bonding strength.
Experimental example 3
To MoS made from embodiment 2, embodiment 3, embodiment 4 and comparative example 12Quito member composite solid lubrication film
Object mutually does X-ray diffraction analysis, and analysis result is as shown in figure 19.
It appears from figure 19 that MoS made from embodiment 2, embodiment 3, embodiment 42Quito member composite solid lubrication film
MoS made from object phase and comparative example 12The object of Quito member composite solid lubrication film is compared, and characteristic peak is reduced, and under peak value
Drop, crystallization degree decline, this improves the uniformity of film surface, reduces the coefficient of friction for preparing film.
Experimental example 4
To MoS made from embodiment 6, embodiment 7, embodiment 8 and comparative example 12Quito member composite solid lubrication film
Object mutually does X-ray diffraction analysis, and analysis result is as shown in figure 20.
As shown in Figure 20, embodiment 6, embodiment 7, MoS made from embodiment 52Quito member composite solid lubrication film
MoS made from object phase and comparative example 12The object of Quito member composite solid lubrication film is compared, and characteristic peak is reduced, and under peak value
Drop, crystallization degree decline, this improves the uniformity of film surface, reduces the coefficient of friction for preparing film.
Experimental example 5
To MoS made from embodiment 10, embodiment 12 and comparative example 12The object of Quito member composite solid lubrication film is mutually X
X ray diffraction analysis x, analysis result are as shown in figure 21.
As shown in Figure 21, embodiment 10, MoS made from embodiment 122The object phase of Quito member composite solid lubrication film with
MoS made from comparative example 12The object of Quito member composite solid lubrication film is compared, and characteristic peak is reduced, and peak-fall, crystallization
Degree decline, this improves the uniformity of film surface, reduces the coefficient of friction for preparing film.
These are only the preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method, which is characterized in that packet
It includes following steps: preparing composite solid lubrication film: by Ti or Al metal targets, ZnO target material and MoS2Target magnetic control co-sputtering
Prepare composite solid lubrication film；Ti or Al metal targets use d.c. sputtering, ZnO target material and MoS2Target is splashed using radio frequency
It penetrates；The low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film is with a thickness of 0.8 μm~3.2 μm；The system
It further include that pre-sputtering preparation combines layer film in advance in substrate using Ti or Al metal targets before standby composite solid lubrication film
The step of.
2. preparation method according to claim 1, which is characterized in that the preparation combines the step of layer film in advance, specifically
Are as follows: Ti or Al metal targets pre-sputtering combination layer film 8min~15min in substrate is used, pre-sputtering power is d.c. sputtering
Target power supply 100W, in advance in conjunction with layer film with a thickness of 25nm~35nm.
3. preparation method according to claim 2, which is characterized in that the substrate are as follows: monocrystalline silicon or stainless steel.
4. preparation method according to claim 1, which is characterized in that it is described to prepare composite solid lubrication film, specifically:
It is 5 × 10 in background vacuum-4Pa, operating air pressure are as follows: Ar protective gas, 0.5Pa air pressure, base reservoir temperature are room temperature, substrate rotation
Rotary speed is 0.05r/s, under the conditions of the technological parameter of target-substrate distance 15cm~17cm by Ti or Al metal targets and ZnO target material,
MoS2Three target co-sputtering of target prepares composite solid lubrication film, and wherein metal targets use power to splash for the direct current of 10W~50W
It shoots at the target power supply, ZnO target material uses 50W radio-frequency sputtering target power supply, MoS2Target uses 100W radio-frequency sputtering target power supply, when cosputtering
Between be 3h.
5. preparation method according to claim 1, which is characterized in that it is described preparation in advance combine layer film after, prepare it is compound
Further include the steps that preparing transition layer film before solid lubricating film.
6. preparation method according to claim 5, which is characterized in that it is described to prepare transition layer film, specifically: in 0.5h
It is interior, use Ti or Al metal targets, ZnO target material and MoS2Three target co-sputtering of target prepares transition layer film, wherein Ti or Al gold
The d.c. sputtering target power supply power for belonging to target drops to 5W~25W by 10W~50W, the radio-frequency sputtering target power supply power of ZnO target material by
50W drops to 25W, MoS2The radio-frequency sputtering target power supply power of target is raised to 100W by 40W.
7. preparation method according to claim 5 or 6, which is characterized in that described to prepare composite solid lubrication film are as follows:
The d.c. sputtering target power supply power of Ti or Al metal targets is 5W~25W, and the radio-frequency sputtering target power supply power of ZnO target material is 25W,
MoS2The radio-frequency sputtering target power supply power of target continues to be coated with 2.5h on the basis of transition layer film under conditions of being 100W.
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| CN111139478B (en) * | 2019-12-06 | 2021-02-26 | 清华大学 | MoS2Use of ZnO heterostructure as reversible light-controlled wetting material and method of use |
| CN113061858A (en) * | 2021-03-15 | 2021-07-02 | 陕西科技大学 | CrMoN/MoS2Wide-temperature-range lubricating wear-resistant composite film and preparation method thereof |
| CN114000106A (en) * | 2021-10-15 | 2022-02-01 | 九江学院 | Low-friction-coefficient MoS2Base composite solid lubricating coating and preparation method thereof |
| CN114086137B (en) * | 2021-11-18 | 2022-07-15 | 中国地质大学（北京） | Rotating joint pin applied to spacecraft mechanism and preparation method thereof |
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