CN109750259A - Preparation method suitable for ultra-low friction magnetic control boron nitride composite lubricating film under water environment - Google Patents
Preparation method suitable for ultra-low friction magnetic control boron nitride composite lubricating film under water environment Download PDFInfo
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- CN109750259A CN109750259A CN201910144575.3A CN201910144575A CN109750259A CN 109750259 A CN109750259 A CN 109750259A CN 201910144575 A CN201910144575 A CN 201910144575A CN 109750259 A CN109750259 A CN 109750259A
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Abstract
The present invention relates to a kind of preparation methods suitable for ultra-low friction magnetic control boron nitride composite lubricating film under water environment, this method refers to: the monocrystalline silicon piece for being cut into 5cm × 5cm is placed on ventilation naturally dry through ultrasonic cleaning, it is embedded in the rotating stand rod in magnetic-controlled sputtering coating equipment vacuum warehouse again and carries out magnetron sputtering to get the boron nitride pellicle monocrystalline silicon piece of deposition different quality.The present invention is simple, easy, and the boron nitride composite lubricating film deposited is pollution-free and has extremely low coefficient of friction under water environment, and about 0.002, there are very good lubrication and abrasion resistance, it is expected to apply the fields such as Yu Haiyang's mechanical equipment and ultraprecise machinery.
Description
Technical field
The present invention relates to composite lubricating film technical fields, more particularly to are suitable for ultra-low friction magnetic control boron nitride under water environment and moisten
The preparation method of sliding film.
Background technique
From ancient times to the present, for contacting with each other and for friction member relative to movement, in high precision then with the friction service life
It is the critical issue that it is operated normally, due to overcoming frictional force meeting off-energy to cause to wear so that the efficiency of machine reduces,
The precision of machine is reduced, so as to shorten life and reliability, at the same time, friction causes temperature to rise again, dissipates if friction is secondary
Heat is bad to will lead to parts expanded by heating, destroys the normal operation of machine, so that phenomenon is killed, and machine overheat can make
It is ineffective to obtain general lubricating oil or composite lubricating film etc., thus accelerates the abrasion of machine, so that the available energy largely loses.
In recent years, solid lubrication rapidly develops, such as with LB film, self-assembled film, polymer ultra-thin film etc., also
MoS2, graphite, polytetrafluoroethylene (PTFE) (PTFE), polymer, oxide be representative solid lubricant obtain extensive use.
No matter but these composite lubricating films universal coefficient of friction under water environment or under air is higher (0.2 ~ 0.6), therefore high-precision
Degree lubrication aspect is still limited.
It is well known that China possesses marine resources abundant, whether the machinery such as offshore equipment, ship, offshore wind farm are set
It is standby, or under water environment it is high-precision machinery for, develop have outstanding resistance to corrosion solid lubricating film all have very
Important meaning.Since 20th century, since China is developed rapidly in modern industry, communications industry, space flight and aviation, science and techniques of defence
And machine operation and micromotor apparatus in the fields such as biomedicine, the rapid development of Nanoelectromechanical device etc., for
The anti-wear and wear-resistant performance of each series lubricant agent under harsh environment made higher requirement.
Since graphene has very outstanding tribological property, and the heat-resisting quantity of boron nitride and chemical stability compare stone
Black alkene is more excellent, and the lattice match of boron nitride and graphene is up to 97.8%, therefore, develops boron nitride composite lubricating film tool
There is prior meaning.
Summary of the invention
Simple and easy it is suitable for ultra-low friction magnetic under water environment technical problem to be solved by the invention is to provide a kind of
Control the preparation method of boron nitride composite lubricating film.
To solve the above problems, of the present invention suitable for ultra-low friction magnetic control boron nitride composite lubricating film under water environment
Preparation method, it is characterised in that: the monocrystalline silicon piece for being cut into 5cm × 5cm is placed on ventilation naturally dry through ultrasonic cleaning,
It is embedded in the rotating stand rod in magnetic-controlled sputtering coating equipment vacuum warehouse again and carries out magnetron sputtering to get the nitridation of deposition different quality
Boron membrane monocrystalline silicon piece.
The condition of the ultrasonic cleaning refers to that ultrasonic power is 35KHz ~ 40KHz, time 30min.
The target of the magnetron sputtering is lanthanum hexaboride, and target-substrate distance is from for 70mm.
The condition of the magnetron sputtering refers to that substrate bias is 100V ~ 800V, target current is 1A ~ 3.5A, substrate duty ratio
For 20% ~ 80%, target current duty ratio be 20% ~ 80%, substrate supply frequency be 40KHz ~ 80KHz, nitrogen flow be 50sccm ~
150sccm and argon flow are the sccm of 45sccm ~ 100.
Compared with the prior art, the present invention has the following advantages:
1, the present invention is directly prepared in monocrystalline silicon sheet surface ultralow suitable for boron nitride under water environment using the method for magnetron sputtering
Friction, lubrication film, overcome existing composite lubricating film cannot work in high temperature and oxidizable environment and poor mobile performance lack
Point, and have lower coefficient of friction.
[friction and wear test method]
The frictional testing machine of u s company is selected to evaluate the coefficient of friction of boron nitride composite lubricating film and friction durability.Back and forth
Movement travel is 5mm, normal load 2N, sliding speed 6Hz, and test environment is dry air environment and water environment.It rubs
It wipes coefficient voluntarily to be recorded by computer, is considered to reach ultra-low friction when coefficient of friction is reduced to 0.01 or less and keeps stablizing,
Namely super lubricating status.Antithesis, the Al for selecting 62O3Stable state coefficient of friction is 0.002 when ball test result is under water environment,
Namely it is in super lubricating status.
2, the present invention, which need not introduce other functional groups, to form continuous, uniform nanoscale in monocrystalline silicon sheet surface
Composite lubricating film, and there is preferable friction and wear behavior.
3, the boron nitride composite lubricating film that the present invention obtains is completely insulated and coefficient of friction is extremely low under water environment, for underwater
High-precision device work application aspect solves lubrication and Problem of Failure provides new approach.
4, the boron nitride composite lubricating film that the present invention obtains has the characteristics that efficient, low temperature, does not influence the performance of substrate and institute
Obtain film thickness uniformly (2.518 μm, referring to Fig. 1), consistency is good.
5, the present invention is simple, easy, and the boron nitride composite lubricating film deposited is pollution-free and has extremely low rub under water environment
Coefficient is wiped, has very good lubrication and abrasion resistance, it is expected to apply the fields such as Yu Haiyang's mechanical equipment and ultraprecise machinery.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 is the SEM picture of boron nitride pellicle thickness of the present invention.
Fig. 2 is friction coefficient curve figure of the boron nitride pellicle of the present invention under the conditions of differentiated friction.
Fig. 3 is the polishing scratch three-D profile sectional view of boron nitride pellicle tribological property of the present invention.
Specific embodiment
Embodiment 1 is suitable for the preparation method of ultra-low friction magnetic control boron nitride composite lubricating film under water environment, and this method is
Refer to: the monocrystalline silicon piece for being cut into 5cm × 5cm is successively ultrasonic under conditions of power is 35KHz with deionized water, dehydrated alcohol
Cleaning 30min is placed on ventilation naturally dry, obtains the monocrystalline silicon piece of clean surface；The monocrystalline silicon piece is embedded in magnetic control again and splashes
It penetrates in the rotating stand rod in filming equipment vacuum warehouse, rotating stand rod is rotated with pivoted frame platform, while autobiography, is guaranteed uniform in coating process
Property.Select target for lanthanum hexaboride, and target-substrate distance is from for 70mm.
Vacuum warehouse is closed, sputtering chamber is vacuumized, its vacuum degree 5 × 10 is made-5Pa, then adjusting substrate bias is
200V, target current 2A, substrate duty ratio are 20%, target current duty ratio is 20%, substrate supply frequency is 40KHz, nitrogen stream
Amount is 100sccm and argon flow is that 45sccm carries out magnetron sputtering to get the boron nitride pellicle monocrystalline silicon piece of deposition.
Prepared boron nitride composite lubricating film is to Al2O3Ball frictional wear experiment the result shows that: reciprocatingly slide distance be 5mm,
Load is 2N, sliding speed 6Hz；Compared by the fretting wear respectively under dry friction and water environment, by tester for friction between
Record learns that boron nitride pellicle stable state coefficient of friction under dry friction environment is 0.1；Stable state coefficient of friction is under water environment
0.002。
It is indicated with the polishing scratch that contourgraph detection leaves on a silicon substrate, after friction carries out 20min, boron nitride pellicle
Wear track depth is 4.1 μm under dry friction environment, and under same experiment condition, the Wear track depth under water environment is only 1.38 μ
M, as shown in Figure 3.In sliding process, by the way that the frictional wear experiment Comparative result under dry friction and water environment to be learnt to (ginseng
See Fig. 2), it is more applicable under water environment by boron nitride composite lubricating film prepared by magnetron sputtering, there is extremely low friction
Coefficient can utmostly protect sample surfaces.Relative to other composite lubricating films, boron nitride composite lubricating film prepared by the present invention
With extremely low coefficient of friction, excellent lubricity and abrasion resistance.
Embodiment 2 is suitable for the preparation method of ultra-low friction magnetic control boron nitride composite lubricating film under water environment, and this method is
Refer to: the monocrystalline silicon piece for being cut into 5cm × 5cm is successively ultrasonic under conditions of power is 35KHz with deionized water, dehydrated alcohol
Cleaning 30min is placed on ventilation naturally dry, obtains the monocrystalline silicon piece of clean surface；The monocrystalline silicon piece is embedded in magnetic control again and splashes
It penetrates in the rotating stand rod in filming equipment vacuum warehouse, rotating stand rod is rotated with pivoted frame platform, while autobiography, is guaranteed uniform in coating process
Property.Select target for lanthanum hexaboride, and target-substrate distance is from for 70mm.
Vacuum warehouse is closed, sputtering chamber is vacuumized, its vacuum degree 5 × 10 is made-5Pa, then adjusting substrate bias is
100V, target current 1A, substrate duty ratio are 20%, target current duty ratio is 20%, substrate supply frequency is 60KHz, nitrogen stream
Amount is 50sccm and argon flow is that 45sccm carries out magnetron sputtering to get the boron nitride pellicle monocrystalline silicon piece of deposition.
Prepared boron nitride composite lubricating film is to Al2O3Ball frictional wear experiment the result shows that: reciprocatingly slide distance be 5mm,
Load is 2N, sliding speed 6Hz；Compared by the fretting wear respectively under dry friction and water environment, by frictional testing machine
Record learns that boron nitride pellicle stable state coefficient of friction under dry friction environment is 0.16；Stable state coefficient of friction is under water environment
0.035。
Embodiment 3 is suitable for the preparation method of ultra-low friction magnetic control boron nitride composite lubricating film under water environment, and this method is
Refer to: the monocrystalline silicon piece for being cut into 5cm × 5cm is successively ultrasonic under conditions of power is 35KHz with deionized water, dehydrated alcohol
Cleaning 30min is placed on ventilation naturally dry, obtains the monocrystalline silicon piece of clean surface；The monocrystalline silicon piece is embedded in magnetic control again and splashes
It penetrates in the rotating stand rod in filming equipment vacuum warehouse, rotating stand rod is rotated with pivoted frame platform, while autobiography, is guaranteed uniform in coating process
Property.Select target for lanthanum hexaboride, and target-substrate distance is from for 70mm.
Vacuum warehouse is closed, sputtering chamber is vacuumized, its vacuum degree 5 × 10 is made-5Pa, then adjusting substrate bias is
200V, target current 1A, substrate duty ratio are 20%, target current duty ratio is 20%, substrate supply frequency is 80KHz, nitrogen stream
Amount is 50sccm and argon flow is that 45sccm carries out magnetron sputtering to get the boron nitride pellicle monocrystalline silicon piece of deposition.
Prepared boron nitride composite lubricating film is to Al2O3Ball frictional wear experiment the result shows that: reciprocatingly slide distance be 5mm,
Load is 2N, sliding speed 6Hz；Compared by the fretting wear respectively under dry friction and water environment, by frictional testing machine
Record learns that boron nitride pellicle stable state coefficient of friction under dry friction environment is 0.12；Stable state coefficient of friction is under water environment
0.04。
Embodiment 4 is suitable for the preparation method of ultra-low friction magnetic control boron nitride composite lubricating film under water environment, and this method is
Refer to: the monocrystalline silicon piece for being cut into 5cm × 5cm is successively ultrasonic under conditions of power is 40KHz with deionized water, dehydrated alcohol
Cleaning 30min is placed on ventilation naturally dry, obtains the monocrystalline silicon piece of clean surface；The monocrystalline silicon piece is embedded in magnetic control again and splashes
It penetrates in the rotating stand rod in filming equipment vacuum warehouse, rotating stand rod is rotated with pivoted frame platform, while autobiography, is guaranteed uniform in coating process
Property.Select target for lanthanum hexaboride, and target-substrate distance is from for 70mm.
Vacuum warehouse is closed, sputtering chamber is vacuumized, its vacuum degree 5 × 10 is made-5Pa, then adjusting substrate bias is
200V, target current 2A, substrate duty ratio are 60%, target current duty ratio is 60%, substrate supply frequency is 40KHz, nitrogen stream
Amount is 50sccm and argon flow is that 45sccm carries out magnetron sputtering to get the boron nitride pellicle monocrystalline silicon piece of deposition.
Prepared boron nitride composite lubricating film is to Al2O3Ball frictional wear experiment the result shows that: reciprocatingly slide distance be 5mm,
Load is 2N, sliding speed 6Hz；Compared by the fretting wear respectively under dry friction and water environment, by frictional testing machine
Record learns that boron nitride pellicle stable state coefficient of friction under dry friction environment is 0.26；Stable state coefficient of friction is under water environment
0.008。
Embodiment 5 is suitable for the preparation method of ultra-low friction magnetic control boron nitride composite lubricating film under water environment, and this method is
Refer to: the monocrystalline silicon piece for being cut into 5cm × 5cm is successively ultrasonic under conditions of power is 40KHz with deionized water, dehydrated alcohol
Cleaning 30min is placed on ventilation naturally dry, obtains the monocrystalline silicon piece of clean surface；The monocrystalline silicon piece is embedded in magnetic control again and splashes
It penetrates in the rotating stand rod in filming equipment vacuum warehouse, rotating stand rod is rotated with pivoted frame platform, while autobiography, is guaranteed uniform in coating process
Property.Select target for lanthanum hexaboride, and target-substrate distance is from for 70mm.
Vacuum warehouse is closed, sputtering chamber is vacuumized, its vacuum degree 5 × 10 is made-5Pa, then adjusting substrate bias is
400V, target current 2A, substrate duty ratio are 20%, target current duty ratio is 20%, substrate supply frequency is 60KHz, nitrogen stream
Amount is 100sccm and argon flow is that 100 sccm carry out magnetron sputtering to get the boron nitride pellicle monocrystalline silicon piece of deposition.
Prepared boron nitride composite lubricating film is to Al2O3Ball frictional wear experiment the result shows that: reciprocatingly slide distance be 5mm,
Load is 2N, sliding speed 6Hz；Compared by the fretting wear respectively under dry friction and water environment, by frictional testing machine
Record learns that boron nitride pellicle stable state coefficient of friction under dry friction environment is 0.24；Stable state coefficient of friction is under water environment
0.1。
Embodiment 6 is suitable for the preparation method of ultra-low friction magnetic control boron nitride composite lubricating film under water environment, and this method is
Refer to: the monocrystalline silicon piece for being cut into 5cm × 5cm is successively ultrasonic under conditions of power is 40KHz with deionized water, dehydrated alcohol
Cleaning 30min is placed on ventilation naturally dry, obtains the monocrystalline silicon piece of clean surface；The monocrystalline silicon piece is embedded in magnetic control again and splashes
It penetrates in the rotating stand rod in filming equipment vacuum warehouse, rotating stand rod is rotated with pivoted frame platform, while autobiography, is guaranteed uniform in coating process
Property.Select target for lanthanum hexaboride, and target-substrate distance is from for 70mm.
Vacuum warehouse is closed, sputtering chamber is vacuumized, its vacuum degree 5 × 10 is made-5Pa, then adjusting substrate bias is
200V, target current 3.5A, substrate duty ratio are 20%, target current duty ratio is 80%, substrate supply frequency is 80KHz, nitrogen
Flow is 50sccm and argon flow is that 100 sccm carry out magnetron sputtering to get the boron nitride pellicle monocrystalline silicon piece of deposition.
Prepared boron nitride composite lubricating film is to Al2O3Ball frictional wear experiment the result shows that: reciprocatingly slide distance be 5mm,
Load is 2N, sliding speed 6Hz；Compared by the fretting wear respectively under dry friction and water environment, by frictional testing machine
Record learns that boron nitride pellicle stable state coefficient of friction under dry friction environment is 0.26；Stable state coefficient of friction is under water environment
0.068。
Embodiment 7 is suitable for the preparation method of ultra-low friction magnetic control boron nitride composite lubricating film under water environment, and this method is
Refer to: the monocrystalline silicon piece for being cut into 5cm × 5cm is successively ultrasonic under conditions of power is 38KHz with deionized water, dehydrated alcohol
Cleaning 30min is placed on ventilation naturally dry, obtains the monocrystalline silicon piece of clean surface；The monocrystalline silicon piece is embedded in magnetic control again and splashes
It penetrates in the rotating stand rod in filming equipment vacuum warehouse, rotating stand rod is rotated with pivoted frame platform, while autobiography, is guaranteed uniform in coating process
Property.Select target for lanthanum hexaboride, and target-substrate distance is from for 70mm.
Vacuum warehouse is closed, sputtering chamber is vacuumized, its vacuum degree 5 × 10 is made-5Pa, then adjusting substrate bias is
800V, target current 3.5A, substrate duty ratio are 80%, target current duty ratio is 80%, substrate supply frequency is 60KHz, nitrogen
Flow is 150sccm and argon flow is that 80 sccm carry out magnetron sputtering to get the boron nitride pellicle monocrystalline silicon piece of deposition.
Prepared boron nitride composite lubricating film is to Al2O3Ball frictional wear experiment the result shows that: reciprocatingly slide distance be 5mm,
Load is 2N, sliding speed 6Hz；Compared by the fretting wear respectively under dry friction and water environment, by frictional testing machine
Record learns that boron nitride pellicle stable state coefficient of friction under dry friction environment is 0.24；Stable state coefficient of friction is under water environment
0.032。
Claims (4)
1. being suitable for the preparation method of ultra-low friction magnetic control boron nitride composite lubricating film under water environment, it is characterised in that: will be cut into
The monocrystalline silicon piece of 5cm × 5cm is placed on ventilation naturally dry through ultrasonic cleaning, then is embedded in magnetic-controlled sputtering coating equipment vacuum
Magnetron sputtering is carried out in rotating stand rod in storehouse to get the boron nitride pellicle monocrystalline silicon piece of deposition different quality.
2. the preparation method suitable for ultra-low friction magnetic control boron nitride composite lubricating film under water environment as described in claim 1,
Be characterized in that: the condition of the ultrasonic cleaning refers to that ultrasonic power is 35KHz ~ 40KHz, time 30min.
3. the preparation method suitable for ultra-low friction magnetic control boron nitride composite lubricating film under water environment as described in claim 1,
Be characterized in that: the target of the magnetron sputtering is lanthanum hexaboride, and target-substrate distance is from for 70mm.
4. the preparation method suitable for ultra-low friction magnetic control boron nitride composite lubricating film under water environment as described in claim 1,
Be characterized in that: the condition of the magnetron sputtering refers to that substrate bias is 100V ~ 800V, target current is 1A ~ 3.5A, substrate duty ratio
For 20% ~ 80%, target current duty ratio be 20% ~ 80%, substrate supply frequency be 40KHz ~ 80KHz, nitrogen flow be 50sccm ~
150sccm and argon flow are the sccm of 45sccm ~ 100.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115128055A (en) * | 2021-03-25 | 2022-09-30 | 华侨大学 | Detection method for tribochemical reaction of active metal abrasive particles and diamond wafer substrate interface |
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| EP0504959A2 (en) * | 1991-03-18 | 1992-09-23 | General Motors Corporation | Carbon-alloyed cubic boron nitride films |
| JPH05320879A (en) * | 1992-05-20 | 1993-12-07 | Nissin Electric Co Ltd | Formation of boron nitride containing film |
| CN101798678A (en) * | 2010-03-29 | 2010-08-11 | 天津师范大学 | Novel super-hard TiB2/c-BN nano multi-layer film prepared by magnetron sputtering technique |
| CN106399938A (en) * | 2016-10-20 | 2017-02-15 | 富耐克超硬材料股份有限公司 | Preparation method for cubic boron nitride film |
| CN108203810A (en) * | 2017-12-20 | 2018-06-26 | 中国科学院兰州化学物理研究所 | A kind of fullerene carbon-coating/class graphene boron nitride MULTILAYER COMPOSITE surpasses the preparation method of composite lubricating film |
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2019
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0504959A2 (en) * | 1991-03-18 | 1992-09-23 | General Motors Corporation | Carbon-alloyed cubic boron nitride films |
| JPH05320879A (en) * | 1992-05-20 | 1993-12-07 | Nissin Electric Co Ltd | Formation of boron nitride containing film |
| CN101798678A (en) * | 2010-03-29 | 2010-08-11 | 天津师范大学 | Novel super-hard TiB2/c-BN nano multi-layer film prepared by magnetron sputtering technique |
| CN106399938A (en) * | 2016-10-20 | 2017-02-15 | 富耐克超硬材料股份有限公司 | Preparation method for cubic boron nitride film |
| CN108203810A (en) * | 2017-12-20 | 2018-06-26 | 中国科学院兰州化学物理研究所 | A kind of fullerene carbon-coating/class graphene boron nitride MULTILAYER COMPOSITE surpasses the preparation method of composite lubricating film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115128055A (en) * | 2021-03-25 | 2022-09-30 | 华侨大学 | Detection method for tribochemical reaction of active metal abrasive particles and diamond wafer substrate interface |
| CN115128055B (en) * | 2021-03-25 | 2024-06-07 | 华侨大学 | Method for detecting interface tribochemical reaction between active metal abrasive particles and diamond wafer substrate |
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