CN108220908A - A kind of method that frictional interface is formed in situ graphene and onion realizes superslide - Google Patents

A kind of method that frictional interface is formed in situ graphene and onion realizes superslide Download PDF

Info

Publication number
CN108220908A
CN108220908A CN201711360852.1A CN201711360852A CN108220908A CN 108220908 A CN108220908 A CN 108220908A CN 201711360852 A CN201711360852 A CN 201711360852A CN 108220908 A CN108220908 A CN 108220908A
Authority
CN
China
Prior art keywords
onion
frictional interface
graphene
film
methane
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201711360852.1A
Other languages
Chinese (zh)
Other versions
CN108220908B (en
Inventor
张俊彦
王永富
高凯雄
张斌
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lanzhou Institute of Chemical Physics LICP of CAS
Original Assignee
Lanzhou Institute of Chemical Physics LICP of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Lanzhou Institute of Chemical Physics LICP of CAS filed Critical Lanzhou Institute of Chemical Physics LICP of CAS
Priority to CN201711360852.1A priority Critical patent/CN108220908B/en
Publication of CN108220908A publication Critical patent/CN108220908A/en
Application granted granted Critical
Publication of CN108220908B publication Critical patent/CN108220908B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical 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
    • C23C16/26Deposition of carbon only
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical 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
    • C23C16/50Chemical 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
    • C23C16/513Chemical 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 frictional interface is formed in situ graphene and onion realization superslide, 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, and graphene and onion are formed in frictional interface;Its reason is that the graphene and onion formed on frictional interface can effectively be dropped low friction pair contact area by sphere-contact or non-commensurability plane-plane contact or reduce frictional interface active force, so as to significantly reduce friction coefficient and wear rate, service life, sensitivity and reliability are improved to reach;Its object is to solve service lifes, sensitivity and the reliabilities such as existing high-end equipment, aerospace components to meet the requirement of 10 15 years.

Description

A kind of method that frictional interface is formed in situ graphene and onion realizes superslide
Technical field
The fields such as lengthen the life the invention belongs to vacuum coating, surface treatment, moving component, be related to a kind of frictional interface original position shape The method for realizing superslide into graphene and onion.
Background technology
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, and so as to which 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 improved 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 abrasion and mechanical damage problem.Superslide film of the development with engineering application value is so as 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.
At present, the non-commensurability structure superslide using two-dimensional graphene as representative is concentrated mainly on micro/nano-scale, to realize macroscopic view Structure superslide must then construct complicated micro-nano mechanical system, and spool or sphere are wrapped up to effectively reduce by forming graphene Non- commensurability is presented in contact area under micro/nano-scale, so as 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 Prepared by area, high rigidity performance.Hydrogeneous carbon-based solid lubricating film is most hopeful under actual working conditions(Atmospheric environment and Engineering scale)Realize superslide characteristic.
Invention content
The purpose of the present invention is to provide a kind of methods that frictional interface is formed in situ graphene and onion realization superslide.
A kind of method that frictional interface is formed in situ graphene and onion realizes superslide, it is characterised in that the specific steps are:
1)Fullerene is carbon nano-structured to be obtained by methane or acetylene through plasma chemical vapor deposition technique;It is big to be passed through purity In 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 is maintained at 14-18 Pa, methane and hydrogen pressure ratio 1:1-1:3 is adjustable, prepares 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 accessory power supply Heating is that base reservoir temperature is controlled at 150-350 DEG C, is passed through the CH that purity is more 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 Pressure ratio 1:0-1:1 is adjustable, prepares class graphite C film;Test result film hardness 7-14GPa, 1-5 microns of thickness, any surface finish Spend 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, and graphene and onion are formed in frictional interface.In air 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, Ceramics and the wear-resistant and reduction friction coefficient on 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, and graphene and onion are formed in frictional interface.The graphene formed on frictional interface and onion can pass through Sphere-contact or non-commensurability plane-plane contact effectively drop low friction pair contact area or reduce frictional interface active force, so as to significantly Friction coefficient 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 cannot meet the requirement of 10-15.
Present invention incorporates the advantages of non-commensurability structure superslide and amorphous interface superslide, both ensure to realize large scale, height The characteristics such as carrying form graphene package spool further through friction induction in situ or sphere are connect with effectively reducing under micro/nano-scale Non- commensurability is presented in contacting surface product.
Description of the drawings
Fig. 1 is the Raman spectrogram of amorphous carbon, class graphite C film and fullerene C film.
Fig. 2 is high-resolution-ration transmission electric-lens figure of the class graphite C film with fullerene C film to formation onion after rubbing.
Fig. 3 is high-resolution-ration transmission electric-lens figure of the class graphite C film with fullerene C film to formation graphene after rubbing.
Fig. 4 is the secondary friction coefficient variation diagram that rubs under the conditions of different loads.
Fig. 5 is that class graphite C film leads to the signal of superslide with fullerene C film to forming graphene and onion after rubbing Figure.
Specific embodiment
Embodiment 1 prepares deposition fullerene C film on silicon chip
(1)Conventional cleaning;
(2)When chamber house vacuum reaches 1 × 10-4When start plated film, argon gas control biases 800 V in 5 Pa, conduction ratio 0.8, 50 KHz of frequency is cleaned 30 minutes;
(3)Pulsed bias is set as -1000V, conduction ratio 0.4,70 Hz of frequency;, methane 17Pa;Deposition film is closed after 120 minutes Machine cools down;
(4)Test, test result film hardness 30GPa, 1.5 microns of thickness, any surface finish are taken out after sample is cooled to room temperature 0.1nm is spent, film color is in black.
(5)As shown in Figure 1, fullerene C film typical case Raman spectrograms include a steamed bun peak(Peak position is in 1527cm-1) With an acromion(About in 1200cm-1).
Embodiment 2 prepares nitriding in situ and deposition class graphite C film on GCr15 balls
Specific implementation is 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 control biases 900 V in 5 Pa, conduction ratio 0.8, 50 KHz of frequency is 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, deposition is thin Film shuts down cooling after 120 minutes;
(5)Test, test result film hardness 27GPa, 1.3 microns of thickness, any surface finish are taken out after sample is cooled to room temperature 0.07nm is spent, film color is in black-and-blue.
As shown in Figure 1, class graphite C film typical case Raman spectrograms include a steamed bun peak(Peak position is in more than 1550cm-1) With an acromion(About in 1380cm-1).
Embodiment 3
Two kinds of film composition frictions are secondary, and onion is formed in frictional interface(Fig. 2)And graphene(Fig. 3).Under the conditions of different loads Friction coefficient is adjustable 0.005 ± 0.002(Fig. 4).It reduces scraping mechanism and can be understood as the graphite formed on frictional interface Alkene and onion can effectively be dropped low friction pair contact area by sphere-contact or non-commensurability plane-plane contact or reduce frictional interface Active force, as shown in Figure 5.

Claims (2)

1. a kind of frictional interface is formed in situ the method that graphene and onion realize superslide, it is characterised in that by fullerene carbon and Class graphitic carbon nano structural membrane is composed of friction pair, and graphene and onion are formed 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 more 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, methane and hydrogen pressure ratio 1:1-1:3 is adjustable, prepares fullerene C film;Film is hard Spend 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 is that base reservoir temperature is controlled at 150-350 DEG C, is passed through the CH that purity is more 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 Pressure ratio 1:0-1:1 is adjustable, prepares class graphite C film;Test result film hardness 7-14GPa, 1-5 microns of thickness, any surface finish Spend 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.
CN201711360852.1A 2017-12-18 2017-12-18 A kind of method that graphene and onion realization superslide is formed in situ in frictional interface Active CN108220908B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711360852.1A CN108220908B (en) 2017-12-18 2017-12-18 A kind of method that graphene and onion realization superslide is formed in situ in frictional interface

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711360852.1A CN108220908B (en) 2017-12-18 2017-12-18 A kind of method that graphene and onion realization superslide is formed in situ in frictional interface

Publications (2)

Publication Number Publication Date
CN108220908A true CN108220908A (en) 2018-06-29
CN108220908B CN108220908B (en) 2019-11-05

Family

ID=62649687

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711360852.1A Active CN108220908B (en) 2017-12-18 2017-12-18 A kind of method that graphene and onion realization superslide is formed in situ in frictional interface

Country Status (1)

Country Link
CN (1) CN108220908B (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109650380A (en) * 2019-01-21 2019-04-19 中国科学院兰州化学物理研究所 A kind of method that dry friction prepares carbon nano-onions under vacuum environment
CN109867275A (en) * 2019-03-11 2019-06-11 西安石油大学 A kind of method that vacuum sphere mill prepares carbon nano-onions
CN110387524A (en) * 2019-07-25 2019-10-29 中国科学院兰州化学物理研究所 A kind of solid-liquid superslide method for mixing silicon carbon film
CN110894593A (en) * 2019-11-29 2020-03-20 岭南师范学院 Steel collar containing graphite-like carbon coating and preparation method thereof
CN112375246A (en) * 2020-11-27 2021-02-19 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
CN113880080A (en) * 2021-11-15 2022-01-04 中国科学院兰州化学物理研究所 Preparation method of ultra-smooth graphene molar structure coating

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030129119A1 (en) * 2002-01-07 2003-07-10 Hsin-Tien Chiu Nanocarbon materials and process for producing the same
JP5649186B2 (en) * 2009-03-11 2015-01-07 国立大学法人 熊本大学 Onion-like carbon and method for producing the same
CN105695953A (en) * 2016-01-19 2016-06-22 中国科学院化学研究所 Manufacturing method and application of three-dimensional carbon negative electrode material
CN106191805A (en) * 2016-06-06 2016-12-07 重庆大学 A kind of preparation method of magnetic graphene laminated film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030129119A1 (en) * 2002-01-07 2003-07-10 Hsin-Tien Chiu Nanocarbon materials and process for producing the same
JP5649186B2 (en) * 2009-03-11 2015-01-07 国立大学法人 熊本大学 Onion-like carbon and method for producing the same
CN105695953A (en) * 2016-01-19 2016-06-22 中国科学院化学研究所 Manufacturing method and application of three-dimensional carbon negative electrode material
CN106191805A (en) * 2016-06-06 2016-12-07 重庆大学 A kind of preparation method of magnetic graphene laminated film

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109650380A (en) * 2019-01-21 2019-04-19 中国科学院兰州化学物理研究所 A kind of method that dry friction prepares carbon nano-onions under vacuum environment
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
CN109867275A (en) * 2019-03-11 2019-06-11 西安石油大学 A kind of method that vacuum sphere mill prepares carbon nano-onions
CN110387524A (en) * 2019-07-25 2019-10-29 中国科学院兰州化学物理研究所 A kind of solid-liquid superslide method for mixing silicon carbon film
CN110894593A (en) * 2019-11-29 2020-03-20 岭南师范学院 Steel collar containing graphite-like carbon coating and preparation method thereof
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
CN112375246A (en) * 2020-11-27 2021-02-19 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
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
CN113880080A (en) * 2021-11-15 2022-01-04 中国科学院兰州化学物理研究所 Preparation method of ultra-smooth graphene molar structure coating
CN113880080B (en) * 2021-11-15 2022-12-02 中国科学院兰州化学物理研究所 Preparation method of ultra-smooth graphene molar structure coating

Also Published As

Publication number Publication date
CN108220908B (en) 2019-11-05

Similar Documents

Publication Publication Date Title
CN108220908B (en) A kind of method that graphene and onion realization superslide is formed in situ in frictional interface
Shang et al. Self-assembled growth, microstructure, and field-emission high-performance of ultrathin diamond nanorods
KR20100033858A (en) Apparatus and method for surface treatment of carbon fiber using resistive heating
CN105668555B (en) A kind of method for preparing three-dimensional grapheme
CN105506579A (en) Preparation method of graphene coated silicon carbide nanowire
CN103374697B (en) The surface treatment method and product of diamond-like carbon film layer
CN111647861A (en) Tetrahedral amorphous carbon film and preparation method and application thereof
Wang et al. Low friction of graphene nanocrystallite embedded carbon nitride coatings prepared with MCECR plasma sputtering
Lee et al. Well-ordered Co nanowire arrays for aligned carbon nanotube arrays
CN106011794B (en) The preparation method of superslide nanocrystalline and amorphous C film under atmospheric environment
Wang et al. Low frictions of self-mated CNx coatings in dry and humid inert gas environments
CN104073834B (en) Preparation method of nanometer diamond-like powder
Bu et al. Industrial compatible re-growth of vertically aligned multiwall carbon nanotubes by ultrafast pure oxygen purification process
Cole et al. In-situ deposition of sparse vertically aligned carbon nanofibres on catalytically activated stainless steel mesh for field emission applications
CN103311104A (en) Method for manufacturing graphene
Park et al. Tribological behavior of nano-undulated surface of diamond-like carbon films
KR101337027B1 (en) Method of manufacturing a graphene structure
CN108275665A (en) A kind of application of threadiness titanium nitride/silicon nitride/nitridation carbon composite nano-material
JPH07256820A (en) Slide member
CN109305672A (en) A kind of preparation method of the single-layer graphene with periodic dimple pattern
Wang et al. Multi-phase carbonaceous coating with super wear resistance
JP2001152316A (en) Plasma carburizing method
Tu et al. Tribological properties of aligned film of amorphous carbon nanorods on AAO membrane in different environments
JPWO2014192916A1 (en) Carbon-coated member and method for producing the same
Chen et al. Tribological thermostability of carbon film with vertically aligned graphene sheets

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant