CN108220908B - A kind of method that graphene and onion realization superslide is formed in situ in frictional interface - Google Patents
A kind of method that graphene and onion realization superslide is formed in situ in frictional interface Download PDFInfo
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- CN108220908B CN108220908B CN201711360852.1A CN201711360852A CN108220908B CN 108220908 B CN108220908 B CN 108220908B CN 201711360852 A CN201711360852 A CN 201711360852A CN 108220908 B CN108220908 B CN 108220908B
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/513—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using plasma jets
Abstract
The present invention relates to a kind of methods that graphene and onion realization superslide is formed in situ in frictional interface, fullerene carbon and class graphitic carbon nano structural membrane are deposited on the material surfaces such as metal, ceramics and polymer by this method, composition friction is secondary, forms graphene and onion in frictional interface;Its reason is that the secondary contact area of friction can be effectively reduced by sphere-contact or non-commensurability plane-plane contact or reduce frictional interface active force for the graphene and onion formed on frictional interface, to significantly reduce coefficient of friction and wear rate, service life, sensitivity and reliability are improved to reach;The requirement for not being able to satisfy 10-15 its object is to solve service lifes, sensitivity and the reliabilities such as existing high-end equipment, aerospace components.
Description
Technical field
The fields such as lengthen the life the invention belongs to vacuum coating, surface treatment, moving component, is related to a kind of frictional interface original position shape
The method for realizing superslide at graphene and onion.
Background technique
China's manufacturing industry scale has leapt to the first in the world, but greatly without strong, not smart, key components and parts and core technology with
High-end equipment is due to a lack of stability and reliability, so that external dependence degree is high, these, which become, restricts Hi-tech Industry Development
Bottleneck.Reduce mechanical moving element fretting wear be considered as effectively extending its working life and improve its reliability of operation,
Stablize one of sexual approach.For there is the contact interface of relative motion under actual working conditions, superslide will fundamentally solve to rub
Energy dissipation caused by wearing and mechanical damage problem.Developing has the superslide film of engineering application value to extend movement portion
The working life of part simultaneously improves its reliability of operation, has important meaning to the realization of development and the energy-saving and emission-reduction of industrial technology
Justice.
In terms of solid superslide research, focus primarily upon using two-dimensional graphene as the non-commensurability structure superslide of representative and with carbon
Amorphous interface superslide based on film.
Currently, being concentrated mainly on micro/nano-scale by the non-commensurability structure superslide of representative of two-dimensional graphene, macroscopic view is realized
Structure superslide must then construct complicated micro-nano mechanical system, wrap up spool or sphere by forming graphene to effectively reduce
Non- commensurability is presented in contact area under micro/nano-scale, to break through the bottlenecks of moisture sensitivity and scale effect.
Superslide material with engineering application value, it is necessary to realize the characteristics such as large scale, high-mechanic, that is, requiring can be big
Area preparation, high rigidity performance.Hydrogeneous carbon-based solid lubricating film be most be hopeful under actual working conditions (atmospheric environment and
Engineering scale) realize superslide characteristic.
Summary of the invention
The purpose of the present invention is to provide a kind of methods that graphene and onion realization superslide is formed in situ in frictional interface.
A kind of method that graphene and onion realization superslide is formed in situ in frictional interface, it is characterised in that specific steps are as follows:
1) fullerene is carbon nano-structured is obtained by methane or acetylene through plasma chemical vapor deposition technique;It is passed through pure
Degree is greater than 99.99% CH4Or C2H2Gas, adjustment pulsed bias to 800-1200 V, conduction ratio 0.5-0.7, frequency 30-80
KHz, methane gas air pressure are maintained at 14-18 Pa, and methane and hydrogen pressure ratio 1:1-1:3 are adjustable, prepare fullerene C film;
Film hardness 18-32GPa, 1-5 microns of thickness, surface smoothness 0.1-0.5nm;
2) class graphitic carbon nano structure is obtained by methane or acetylene through plasma chemical vapor deposition technique;Using auxiliary
Power supply heating is base reservoir temperature control at 150-350 DEG C, is passed through the CH that purity is greater than 99.99%4Or C2H2Gas, adjustment pulse are inclined
Be depressed into 800-1000 V, conduction ratio 0.5-0.8, frequency 30-50 KHz, methane gas air pressure is maintained at 15-18 Pa, methane with
Hydrogen pressure ratio 1:0-1:1 is adjustable, prepares class graphite C film;Test result film hardness 7-14GPa, 1-5 microns of thickness, surface
Finish 0.05-0.5nm.
Plasma activated chemical vapour deposition includes direct current, DC pulse, high power pulsed source, exchange or radio-frequency power supply.
Two kinds of carbon structure film pairings of the present invention, composition friction is secondary, forms graphene and onion in frictional interface.In atmosphere
Or it is adjusted between coefficient of internal friction 0.005-0.01 under condition of nitrogen gas.Fullerene carbon and class graphite C film can be used for metal,
The wear-resistant and reduction coefficient of friction of ceramics and polymerizable material surface.
Fullerene carbon and class graphitic carbon nano structural membrane are deposited on the materials such as metal, ceramics and polymer by the present invention
Surface, composition friction is secondary, forms graphene and onion in frictional interface.The graphene formed on frictional interface and onion can pass through
Sphere-contact or non-commensurability plane-plane contact are effectively reduced the secondary contact area of friction or reduce frictional interface active force, thus significantly
Coefficient of friction and wear rate are reduced, service life, sensitivity and reliability is improved to reach, solves existing high-end equipment, boat
The service lifes such as empty aerospace components, sensitivity and reliability are not able to satisfy the requirement of 10-15.
Present invention incorporates the advantage of non-commensurability structure superslide and amorphous interface superslide, both guarantee to realize large scale, height
The characteristics such as carrying form graphene package spool or sphere further through friction induction in situ and are connect under micro/nano-scale with effectively reducing
Non- commensurability is presented in contacting surface product.
Detailed description of the invention
Fig. 1 is the Raman spectrogram of amorphous carbon, class graphite C film and fullerene C film.
Fig. 2 is class graphite C film and fullerene C film to the high-resolution-ration transmission electric-lens figure for forming onion after rubbing.
Fig. 3 is class graphite C film and fullerene C film to the high-resolution-ration transmission electric-lens figure for forming graphene after rubbing.
Fig. 4 is the secondary coefficient of friction variation diagram that rubs under the conditions of different loads.
Fig. 5 is that class graphite C film and fullerene C film lead to the signal of superslide to graphene and onion is formed after rubbing
Figure.
Specific embodiment
Embodiment 1 prepares deposition fullerene C film on silicon wafer
(1) conventional cleaning;
(2) when chamber house vacuum reaches 1 × 10-4When start plated film, argon gas is controlled in 5 Pa, 800 V of bias, conduction ratio
0.8,50 KHz of frequency are cleaned 30 minutes;
(3) pulsed bias is set as -1000V, conduction ratio 0.4,70 Hz of frequency;, methane 17Pa;Deposition film 120 minutes
Shutdown cooling afterwards;
(4) it takes out and tests after sample is cooled to room temperature, test result film hardness 30GPa, 1.5 microns of thickness, surface
Finish 0.1nm, film color are in black.
(5) as shown in Figure 1, fullerene C film typical case's Raman spectrogram includes that (peak position is in 1527cm for a steamed bun peak-1)
With an acromion (about in 1200cm-1).
Embodiment 2 prepares nitriding in situ and deposition class graphite C film on GCr15 ball
It is embodied as follows:
(1) conventional cleaning: vacuum chamber is put in oil removing, derusting, drying into;
(2) when chamber house vacuum reaches 1 × 10-4When start plated film, argon gas is controlled in 5 Pa, 900 V of bias, conduction ratio
0.8,50 KHz of frequency are cleaned 30 minutes;
(3) pulsed bias is set as -800V, conduction ratio 0.6,80 Hz of frequency;, nitrogen 8Pa;Nitriding 30 minutes;
(4) pulsed bias is set as -850V, conduction ratio 0.5, frequency 50Hz;, methane 15Pa;And 230 DEG C are heated to, it sinks
Product film shuts down cooling after 120 minutes;
(5) it takes out and tests after sample is cooled to room temperature, test result film hardness 27GPa, 1.3 microns of thickness, surface
Finish 0.07nm, film color is in black-and-blue.
As shown in Figure 1, class graphite C film typical case's Raman spectrogram includes that (peak position is in the above 1550cm for a steamed bun peak-1)
With an acromion (about in 1380cm-1).
Embodiment 3
Two kinds of film composition frictions are secondary, form onion (Fig. 2) and graphene (Fig. 3) in frictional interface.In different loads item
Coefficient of friction is in 0.005 ± 0.002 adjustable (Fig. 4) under part.It reduces what scraping mechanism can be understood as being formed on frictional interface
The secondary contact area of friction can be effectively reduced by sphere-contact or non-commensurability plane-plane contact or reduce friction for graphene and onion
Interface interaction power, as shown in Figure 5.
Claims (2)
1. the method that graphene and onion realize superslide is formed in situ in a kind of frictional interface, it is characterised in that by fullerene carbon and
Class graphitic carbon nano structural membrane is composed of friction pair, forms graphene and onion in frictional interface;
Fullerene is carbon nano-structured to be obtained by methane or acetylene through plasma chemical vapor deposition technique;Purity is passed through to be greater than
99.99% CH4Or C2H2Gas, adjustment pulsed bias to 800-1200 V, conduction ratio 0.5-0.7, frequency 30-80 KHz, first
Alkane gas atmosphere is maintained at 14-18 Pa, and the air pressure ratio of methane and hydrogen is 1:1-1:3, prepares fullerene C film;Film
Hardness 18-32GPa, 1-5 microns of thickness, surface smoothness 0.1-0.5nm;
Class graphitic carbon nano structure is obtained by methane or acetylene through plasma chemical vapor deposition technique;Using accessory power supply plus
Heat makes base reservoir temperature control at 150-350 DEG C, is passed through the CH that purity is greater than 99.99%4Or C2H2Gas, adjustment pulsed bias is extremely
800-1000 V, conduction ratio 0.5-0.8, frequency 30-50 KHz, methane gas air pressure are maintained at 15-18 Pa, methane and hydrogen
Air pressure ratio be 1:0-1:1, prepare class graphite C film;Test result film hardness 7-14GPa, 1-5 microns of thickness, surface light
Cleanliness 0.05-0.5nm.
2. the method as described in claim 1, it is characterised in that the plasma activated chemical vapour deposition includes direct current, direct current arteries and veins
Punching, high power pulsed source, exchange or radio-frequency power supply.
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CN109650380B (en) * | 2019-01-21 | 2022-04-19 | 中国科学院兰州化学物理研究所 | Method for preparing carbon nano onion by dry friction in vacuum environment |
CN109867275B (en) * | 2019-03-11 | 2020-10-30 | 西安石油大学 | Method for preparing carbon nano onion by vacuum ball milling |
CN110387524B (en) * | 2019-07-25 | 2021-07-20 | 中国科学院兰州化学物理研究所 | Solid-liquid ultra-smooth method for silicon-doped carbon film |
CN110894593B (en) * | 2019-11-29 | 2022-03-04 | 岭南师范学院 | Steel collar containing graphite-like carbon coating and preparation method thereof |
CN112375246B (en) * | 2020-11-27 | 2021-07-13 | 中国科学院兰州化学物理研究所 | Method for modifying polymer surface by carbon dioxide plasma discharge under atmospheric pressure |
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