CN107686976A - A kind of preparation method of star molybdenum-disulfide radical the compound lubricating film - Google Patents
A kind of preparation method of star molybdenum-disulfide radical the compound lubricating film Download PDFInfo
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- CN107686976A CN107686976A CN201710695375.8A CN201710695375A CN107686976A CN 107686976 A CN107686976 A CN 107686976A CN 201710695375 A CN201710695375 A CN 201710695375A CN 107686976 A CN107686976 A CN 107686976A
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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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
-
- 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
- C23C14/0623—Sulfides, selenides or tellurides
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Lubricants (AREA)
Abstract
The present invention provides a kind of preparation method of star molybdenum-disulfide radical the compound lubricating film, using closed field unbalanced magnetron sputtering MoS2Target, Ti targets and rare earth fluoride target, in the presence of working gas Ar, by controlling MoS2The power of the electric current and rare earth fluoride target of target and Ti targets, to prepare molybdenum disulfide based coextruded film.The film not only compact structure, antifriction performance is excellent, and significantly improves traditional MoS2The wearability of base film, life-span improve several times.
Description
Technical field
The present invention relates to greasing substance preparation field, the preparation of more particularly to a kind of star molybdenum-disulfide radical the compound lubricating film
Method.
Background technology
After Spacecraft Launch is entered the orbit, there is very big difference, main performance in the space environment where it with surface air environment
:Condition of high vacuum degree, high/low temperature alternation, microgravity, intense radiation and elemental oxygen.Under these special space environment effects, tradition
Space lubricant grease it is volatile, easily climb shifting, degradable failure, can not meet the needs of in engineering.Particularly, grease volatilizees
Caused pollutant is that the big of optics load is avoided.
MoS2Solid lubricant coating has zero volatilization pollution, high-low temperature resistant alternation, resistance to space compared with the lubricant grease of space
Irradiation, the features such as spatial stability is good, therefore be used widely in the optical remote sensing load with anti-pollution requirement.But
It is traditional space MoS2Solid lubricating film moisture resistant ability, easily it is corroded under atmospheric environment.In Spacecraft Launch
Before, after solid lubricating film is after the installation under ground environment, debugging, storage, the friction life-span decays in advance, leverages it
In-orbit service life, the requirement of 8~15 years extra long lifes of Optical remote satellite of new generation can not be met.Therefore, it is long-lived to star
Life solid lubricant coating proposes urgent development demand.
Molybdenum-disulfide radical composite lubricating film prepared by the present invention, on the one hand because addition and the gradient mistake of Ti prime coats
The design for crossing layer enhances the adhesion of functional layer and substrate, and the addition of another aspect rare earth fluoride causes membrane structure more
Fine and close, hardness lifting, blocks the intrusion of air reclaimed water and oxygen, thus film possesses higher friction durability and moisture resistance
Can, and can still keep low coefficient of friction and good greasy property because additive is all micro.
The content of the invention
Preparation method it is an object of the invention to provide a kind of star with molybdenum-disulfide radical the compound lubricating film, to solve MoS2
Film the problem of humidity resistance is poor under atmospheric environment, friction durability is short.
In order to solve the above-mentioned technical problem, the technical scheme is that:A kind of compound profit of star molybdenum-disulfide radical is provided
The preparation method of synovial membrane, comprises the following steps:
It is prepared by S1, target:
Load Ti targets and MoS on two direct current target position of filming equipment respectively2Target, load on a radio frequency target position dilute
Native fluoride target, to Ti targets, MoS2Target and rare earth fluoride target carry out surface polishing respectively, and scale removal is to exposing fresh table
Skin;
S2, preparation of samples:
Sample is polished, polished, demagnetization, is dried up after cleaning, loads filming equipment;
S3, substrate pretreated:
Coating chamber is evacuated to 3.0 × 10-4~3.0 × 10-5Pa, importing working gas Ar, control flow 20~
50sccm, substrate bias are arranged to 100~200V, maintain 15~20min, allow Ar plasma bombardment targets, realize matrix table
The cleaning and activation in face;
S4, plating prime coat:
Ti target currents are linearly enhanced to 3~5A, and other targets are closed, 50~60min of sputtering time;
S5, plating transition zone:
Ti target currents linear decline is to 0.25~0.5A, MoS2Target current is linearly enhanced to 1~2A, and sputtering time 50~
60min;
S6, plating functional layer:
Maintain Ti target currents and MoS in step S52The electric current of target, opens rare earth fluoride target, Power Control 50~
200w, 350~400min of sputtering time.
Further, in the step S2, polished successively using 600#, 1200# sand paper.
Further, in the step S2, sample is thrown with the diamond paste of 2.5 μm of label on polishing machine
Light processing.
Further, in the step S2, the method for sample clean is:It is cleaned by ultrasonic respectively in acetone and absolute ethyl alcohol
10~15min.
Further, in the step S3, coating chamber air pressure is 3.0 × 10-4Pa, flow 30sccm, substrate bias
For 200V, time 20min.
Further, in the step S4, Ti target currents are linearly enhanced to 3A, sputtering time 60min by 0.2A.
Further, in the step S5, Ti target currents are by 3A linear declines to 0.25A, MoS2Target current is by 0.3A lines
Property is enhanced to 1A, sputtering time 60min.
Further, in the step S6, Ti target currents are 0.25A, MoS2Target current is 1A, rare earth fluoride target power output
For 100w, sputtering time 350min.
The beneficial effect that star provided by the invention is obtained with the preparation method of molybdenum-disulfide radical the compound lubricating film is:
(1) adhesion of functional layer and substrate is enhanced, film layer is effectively prevent and peels off lubrication failure caused by possibility, it is right
There is larger help in the raising of friction durability;
(2) on the premise of greasy property is not reduced, the friction durability of film has been obviously improved, for the longevity continuously to work
The lubrication of life space precise movable part provides a kind of effective measures;
(3) the gold doping MoS best compared to current report effect2Film cost significantly reduces;
(4) non-balance magnetically controlled sputter equipment is used, with reference to the independent control of each composition target, technological parameter is handling good, weight
Renaturation is good;
(5) humidity resistance is good, and storage request reduces, the performance degradation unobvious within the manufacturing cycle of space operation part;
(6) it is applied to the lubrication of following long-life space precise motion.
Brief description of the drawings
Invention is described further below in conjunction with the accompanying drawings:
Fig. 1 is molybdenum-disulfide radical the compound lubricating film film layer structure schematic diagram;
Fig. 2 is that molybdenum-disulfide radical the compound lubricating film SEM made from the embodiment of the present invention schemes;
Fig. 3 is that the SEM of molybdenum-disulfide radical the compound lubricating film cross section made from the embodiment of the present invention schemes;
Fig. 4 is molybdenum-disulfide radical the compound lubricating film friction test curve made from the embodiment of the present invention.
1 is matrix in figure, and 2 be Ti prime coats, and 3 be MoS2/ Ti transition zones, 4 be MoS2/ Ti/ rare earth fluoride functional layers.
Embodiment
Preparation below in conjunction with the drawings and specific embodiments to star proposed by the present invention with molybdenum-disulfide radical the compound lubricating film
Method is described in further detail.Wherein Fig. 1 is molybdenum-disulfide radical the compound lubricating film film layer structure schematic diagram, and Fig. 2 is the present invention
Molybdenum-disulfide radical the compound lubricating film SEM made from embodiment schemes, and Fig. 3 is the compound profit of molybdenum-disulfide radical made from the embodiment of the present invention
The SEM figures of synovial membrane cross section, Fig. 4 is molybdenum-disulfide radical the compound lubricating film friction test curve made from the embodiment of the present invention.Root
According to following explanation and claims, advantages and features of the invention will become apparent from.It should be noted that accompanying drawing is using very simple
The form of change and non-accurately ratio is used, only for the purpose of facilitating and clarifying the purpose of the embodiments of the invention.
The core concept of the present invention is, using closed field unbalanced magnetron sputtering MoS2Target, Ti targets and rare earth fluoride
Target, in the presence of working gas Ar, by controlling MoS2The electric current of target and Ti targets, the power of rare earth fluoride target are prepared into
Molybdenum disulfide based coextruded film.The film not only compact structure, antifriction performance is excellent, and significantly improves traditional MoS2Base is thin
The wearability of film, life-span improve several times.
It is as follows to implement step:
Step 1) target prepares:Load Ti targets and MoS on two direct current target position of filming equipment respectively2Target, at one
Load rare earth fluoride target on radio frequency target position, scale removal is polished to exposing fresh surface in surface;
Step 2) preparation of samples:Polished successively using 600#, 1200# sand paper, the Buddha's warrior attendant of 2.5 μm of label is used on polishing machine
Stone abrasive pastes are processed by shot blasting to sample, and demagnetization is carried out to sample on degausser, ultrasonic in acetone, absolute ethyl alcohol respectively
10~15min is cleaned, quick drying, loads filming equipment;
Step 3) substrate pretreated:Coating chamber is evacuated to 3.0 × 10-4~3.0 × 10-5Pa, working gas Ar is imported,
20~50sccm of flow is controlled, substrate bias is arranged to 100~200V, maintains 15~20min, allows Ar plasma bombardment targets
Material, realize the cleaning and activation of matrix surface;
Step 4) plates prime coat:Ti target currents are gradually increased to 3~5A, and other targets are closed, 50~60min of sputtering time;
Step 5) plates transition zone:Ti target currents progressively drop to 0.25~0.5A, MoS2Target current progressively rises to 1~2A,
50~60min of sputtering time;
Step 6) plates functional layer:Ti target currents and MoS2Target current maintains the terminal level of step 5), while opens dilute
Native fluoride target, Power Control is in 50~200w, 350~400min of sputtering time.
Now illustrate the preparation method of the present invention with a specific embodiment, comprise the following steps:
Step 1) target prepares:Load Ti targets and MoS on two direct current target position of filming equipment respectively2Target, at one
Load rare earth fluoride target on radio frequency target position, scale removal is polished to exposing fresh surface in surface;
Step 2) preparation of samples:Polished successively using 600#, 1200# sand paper, the Buddha's warrior attendant of 2.5 μm of label is used on polishing machine
Stone abrasive pastes are processed by shot blasting to sample, and demagnetization is carried out to sample on degausser, ultrasonic in acetone, absolute ethyl alcohol respectively
15min is cleaned, quick drying, loads filming equipment;
Step 3) substrate pretreated:Coating chamber is evacuated to 3.0 × 10-4Pa, working gas Ar is imported, control flow
30sccm, substrate bias are arranged to 200V, maintain 20min, allow Ar plasma bombardment targets, realize the cleaning of matrix surface with
Activation;
Step 4) plates prime coat:Ti target currents are gradually increased to 3A by 0.2A, and other targets are closed, sputtering time 60min;
Step 5) plates transition zone:Ti target currents 3A progressively drops to 0.25A, MoS2Target current progressively rises to 1A by 0.3A,
Sputtering time 60min;
Step 6) plates functional layer:Ti target currents 0.25A, MoS2Target current 1A, rare earth fluoride target power output 100w, during sputtering
Between 350min.
Obviously, those skilled in the art can carry out the essence of various changes and deformation without departing from the present invention to the present invention
God and scope.So, if these modifications and variations of the present invention belong to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprising including these changes and modification.
Claims (8)
1. a kind of star preparation method of molybdenum-disulfide radical the compound lubricating film, it is characterised in that comprise the following steps:
It is prepared by S1, target:
Load Ti targets and MoS on two direct current target position of filming equipment respectively2Target, rare earth fluorine is loaded on a radio frequency target position
Compound target, to Ti targets, MoS2Target and rare earth fluoride target carry out surface polishing respectively, and scale removal is to exposing fresh epidermis;
S2, preparation of samples:
Sample is polished, polished, demagnetization, is dried up after cleaning, loads filming equipment;
S3, substrate pretreated:
Coating chamber is evacuated to 3.0 × 10-4~3.0 × 10-5Pa, working gas Ar is imported, control 20~50sccm of flow, matrix
Bias is arranged to 100~200V, maintains 15~20min, allows Ar plasma bombardment targets, realizes the cleaning and work of matrix surface
Change;
S4, plating prime coat:
Ti target currents are linearly enhanced to 3~5A, and other targets are closed, 50~60min of sputtering time;
S5, plating transition zone:
Ti target currents linear decline is to 0.25~0.5A, MoS2Target current is linearly enhanced to 1~2A, 50~60min of sputtering time;
S6, plating functional layer:
Maintain Ti target currents and MoS in step S52The electric current of target, rare earth fluoride target is opened, Power Control is splashed in 50~200w
Penetrate 350~400min of time.
2. the star as claimed in claim 1 preparation method of molybdenum-disulfide radical the compound lubricating film, it is characterised in that the step
In S2, polished successively using 600#, 1200# sand paper.
3. the star as claimed in claim 1 preparation method of molybdenum-disulfide radical the compound lubricating film, it is characterised in that the step
In S2, sample is processed by shot blasting with the diamond paste of 2.5 μm of label on polishing machine.
4. the star as claimed in claim 1 preparation method of molybdenum-disulfide radical the compound lubricating film, it is characterised in that the step
In S2, the method for sample clean is:It is cleaned by ultrasonic 10~15min respectively in acetone and absolute ethyl alcohol.
5. the star as claimed in claim 1 preparation method of molybdenum-disulfide radical the compound lubricating film, it is characterised in that the step
In S3, coating chamber air pressure is 3.0 × 10-4Pa, flow 30sccm, substrate bias 200V, time 20min.
6. the star as claimed in claim 1 preparation method of molybdenum-disulfide radical the compound lubricating film, it is characterised in that the step
In S4, Ti target currents are linearly enhanced to 3A, sputtering time 60min by 0.2A.
7. the star as claimed in claim 1 preparation method of molybdenum-disulfide radical the compound lubricating film, it is characterised in that the step
In S5, Ti target currents are by 3A linear declines to 0.25A, MoS2Target current is linearly enhanced to 1A by 0.3A, and sputtering time is
60min。
8. the star as claimed in claim 1 preparation method of molybdenum-disulfide radical the compound lubricating film, it is characterised in that the step
In S6, Ti target currents are 0.25A, MoS2Target current is 1A, and rare earth fluoride target power output is 100w, sputtering time 350min.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110331370A (en) * | 2019-07-25 | 2019-10-15 | 清华大学 | A kind of molybdenum-disulfide radical complex multi layer films and preparation method thereof |
CN110527951A (en) * | 2019-10-15 | 2019-12-03 | 河南科技大学 | A kind of the compound lubricating film and preparation method thereof, workpiece |
CN110578115A (en) * | 2019-10-15 | 2019-12-17 | 河南科技大学 | Doped sulfide composite film, preparation method thereof and workpiece containing doped sulfide composite film |
CN115323326A (en) * | 2022-08-17 | 2022-11-11 | 中国科学院兰州化学物理研究所 | Preparation method and application of space atomic oxygen irradiation resistant long-life molybdenum disulfide-based composite film |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110331370A (en) * | 2019-07-25 | 2019-10-15 | 清华大学 | A kind of molybdenum-disulfide radical complex multi layer films and preparation method thereof |
CN110527951A (en) * | 2019-10-15 | 2019-12-03 | 河南科技大学 | A kind of the compound lubricating film and preparation method thereof, workpiece |
CN110578115A (en) * | 2019-10-15 | 2019-12-17 | 河南科技大学 | Doped sulfide composite film, preparation method thereof and workpiece containing doped sulfide composite film |
CN110578115B (en) * | 2019-10-15 | 2021-08-20 | 河南科技大学 | Doped sulfide composite film, preparation method thereof and workpiece containing doped sulfide composite film |
CN110527951B (en) * | 2019-10-15 | 2021-10-15 | 河南科技大学 | Composite lubricating film, preparation method thereof and workpiece |
CN115323326A (en) * | 2022-08-17 | 2022-11-11 | 中国科学院兰州化学物理研究所 | Preparation method and application of space atomic oxygen irradiation resistant long-life molybdenum disulfide-based composite film |
CN115323326B (en) * | 2022-08-17 | 2023-11-24 | 中国科学院兰州化学物理研究所 | Preparation method and application of long-life molybdenum disulfide-based composite film resistant to space atomic oxygen irradiation |
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