CN103613094B - A kind of method simultaneously preparing Graphene and porous amorphous carbon film - Google Patents
A kind of method simultaneously preparing Graphene and porous amorphous carbon film Download PDFInfo
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- CN103613094B CN103613094B CN201310624078.6A CN201310624078A CN103613094B CN 103613094 B CN103613094 B CN 103613094B CN 201310624078 A CN201310624078 A CN 201310624078A CN 103613094 B CN103613094 B CN 103613094B
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Abstract
The invention discloses a kind of method simultaneously preparing Graphene and porous amorphous carbon film, be positioned in tube furnace after metal nickel sheet substrate being carried out ultrasonic cleaning, and drying including S1；S2 is passed through noble gas in tube furnace；S3 carries out hyperthermic treatment and reaches 750 DEG C～1000 DEG C and keep 10 minutes～50 minutes tube furnace, is passed through hydrogen, and metal nickel sheet substrate is carried out heat treatment in tube furnace；S4 is passed through the Hydrocarbon that flow is 20sccm～100sccm in tube furnace so that the metal nickel sheet substrate catalytic hydrocarbon after Overheating Treatment cracks and grows Graphene and amorphous carbon film after the molten carbon of nickel sheet simultaneously；S5 carries out cooling process to tube furnace, and obtains Graphene and porous amorphous carbon film after growth having the nickel sheet of Graphene and amorphous carbon film be immersed in corrosive liquid erode substrate nickel sheet.The present invention, with Hydrocarbon as carbon source, is dissolved in carbon atom by carbon source under control hot conditions in the absorption cracking and nickel sheet on substrate nickel sheet surface and can be obtained Graphene and amorphous carbon film simultaneously.
Description
Technical field
The invention belongs to chemical gaseous phase sedimentation preparation of film technical field, same more particularly, to one
Time prepare Graphene and the method for porous amorphous carbon film.
Background technology
Carbon is one of element of enriching the most of nature content, and the carbon materials being made up of carbon has
A variety of isomers.The Geim etc. of Univ Manchester UK in 2004 utilizes mechanical separation side
Method is prepared first on one block of graphite and observes a kind of special carbon film---mono-layer graphite (Graphene),
Thus open the research boom of grapheme material.Graphene is made up of monolayer atom, has two dimension
Honeycomb texture, this special structure impart the unique optics of grapheme material, electricity, calorifics and
Mechanical performance.These superior performances make its nano electron device, lithium ion battery electrode material,
Ultracapacitor, electrode of solar battery material, hydrogen storage material, sensor, optical material, medicine
The aspects such as carrier show huge application potential.The fundamental and applied research of Graphene comes into fast
Violent developmental stage, Graphene has become as " super " material in current new material.
At present, the preparation method of grapheme material mainly has: mechanical stripping method, chemical oxidization method, crystalline substance
External epitaxial growth, chemical vapour deposition technique, organic synthesis method and CNT stripping method etc..Chemistry
Vapour deposition is as a kind of quick and easy, low cost and can to prepare the technological means of large-area graphene standby
Paid close attention to by scientist.Chemical vapour deposition technique generally utilize Hydrocarbon for carbon source, at high temperature bar
Under part, carbon source cracking formation of deposits Graphene on transition metal.Can only under the conditions of conventional technique
Obtain monolayer and multi-layer graphene thin film.
Amorphous carbon-film is the one in numerous carbon materials, and this material just starts in eighties of last century the forties
Research, eighties of last century starts application the sixties.Amorphous carbon-film can be described as diamond, and (carbon atom is only
Sp3 hydridization) and the intermediate state of graphite (carbon atom only has sp2 hydridization) structure.According to contained hydridization carbon
Atom sp2 and sp3 content is different, and amorphous carbon-film is generally divided into diamond like carbon amorphous carbon-film, and (sp3 contains
Amount > sp2 content) and class graphite amorphous carbon-film (sp2 content > sp3 content).Amorphous carbon-film demonstrates
The mechanics of excellence, Optical and frictional properties etc., such as high rigidity, good chemical stability and biology
The compatibility, especially ultra-low friction factor and high-wearing feature can etc. make its machinery, electronics, communication and
Aerospace field has a wide range of applications.Porous amorphous carbon-film is in addition to having above advantage, also
Have the advantages that specific surface area is big and pore-size distribution is abundant, can be widely applied to the energy and biomedicine
Field.
At present, the method preparing amorphous carbon-film has: particle beam (ion, electronics, photon etc.) assists
Deposition technique, Vacuum Arc deposition technique, magnetron sputtering technique, plasma enhanced chemical vapor deposition
Technology and thermal chemical vapor deposition technology etc..But all there is Railway Project, one in all these technology
It is exactly that C film preparation process ambient temperature is high, so, general amorphous carbon-film is all prepared in rigid substrate
On (such as quartz glass, Muscovitum, silicon chip or directly at surface of the work) so that amorphous carbon-film
Application is by certain restriction；Its two be the amorphous carbon-film prepared by these technology be all dense film,
Loose structure carbon film cannot be obtained；It three is prepared by these technology to be mostly diamond like carbon amorphous carbon
Film；It four is the self-supporting amorphous carbon-film that these technology cannot obtain special construction, self-supporting amorphous carbon
Film can easily be transferred to any substrate.It can thus be seen that current amorphous carbon film technology of preparing
There are some defects and constrain its basic research and application.
Summary of the invention
For disadvantages described above or the Improvement requirement of prior art, object of the present invention is to provide one
Prepare Graphene and the method for porous amorphous carbon film simultaneously.
For achieving the above object, according to one aspect of the present invention, it is provided that one prepares graphite simultaneously
Alkene and the method for porous amorphous carbon film, comprise the steps:
S1: be positioned in tube furnace after metal nickel sheet substrate is carried out ultrasonic cleaning, and drying；
S2: be passed through noble gas in described tube furnace；
S3: described tube furnace is carried out hyperthermic treatment and reaches 750 DEG C～1000 DEG C and keep 10 minutes
～50 minutes, in described tube furnace, it is passed through hydrogen, and described metal nickel sheet substrate is carried out heat treatment；
S4: be passed through the Hydrocarbon that flow is 20sccm～100sccm in described tube furnace so that
Metal nickel sheet substrate catalytic hydrocarbon after Overheating Treatment cracks and gives birth to after the molten carbon of nickel sheet simultaneously
Long Graphene and amorphous carbon film；Gas pressure intensity during Gai is normal pressure；
S5: described tube furnace is carried out cooling process, and growth is had Graphene and amorphous carbon film
Nickel sheet is immersed in corrosive liquid after eroding substrate nickel sheet and obtains Graphene and porous amorphous carbon film.
Further, in step s3, the flow being passed through hydrogen is 50sccm～200sccm.
Further, in step s 5, described corrosive liquid is ferric chloride in aqueous solution.
Further, in step s 2, during described noble gas is argon or helium at least one.
Further, in step s 2, the flow being passed through noble gas is 50sccm～500sccm.
Further, described Hydrocarbon be methane, ethane, propane, butane, hexane, penta
In alkane, heptane, octane, propylene, ethylene, butylene, amylene, acetylene any one or the most multiple
Combination.
The present invention utilizes chemical vapour deposition technique, with Hydrocarbon as carbon source, by controlling high temperature
Under the conditions of carbon source in the absorption cracking and nickel sheet on substrate nickel sheet surface, dissolve in carbon atom, and follow-up fall
Gentle last substrate etching obtains Graphene and amorphous carbon film.The invention have the advantages that (1)
Equipment is simple and low cost；(2) simple to operate quick with preparation process；(3) one secondary growths can be same
Time obtain high-quality graphene and two kinds of products of amorphous carbon film；(4) Graphene and amorphous carbon film are all
There is self-supporting, can transfer to respectively on any substrate；(5) can prepare large-area graphene/
Amorphous carbon film/Graphene sandwich structure or the double-deck composite carbon of Graphene/amorphous carbon film
Thin film.Therefore there is important potential research using value.
Accompanying drawing explanation
Fig. 1 is to prepare Graphene and the device of porous amorphous carbon film while the embodiment of the present invention provides
Structural representation；
Fig. 2 is to prepare Graphene and the method for porous amorphous carbon film while the embodiment of the present invention provides
Flowchart；
Fig. 3 is the Graphene simultaneously prepared by a secondary growth and the porous of the embodiment of the present invention 2 offer
The fluorescence Raman spectrogram of amorphous carbon film；
Fig. 4 is Graphene and the porous amorphous carbon that the embodiment of the present invention 2 passes through that a secondary growth is prepared simultaneously
The picture of the scanning electron microscope of thin film；
Fig. 5 is Graphene and the porous amorphous carbon that the embodiment of the present invention 2 passes through that a secondary growth is prepared simultaneously
The picture of the transmission electron microscope of thin film.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing
And embodiment, the present invention is further elaborated.Should be appreciated that described herein specifically
Embodiment only in order to explain the present invention, is not intended to limit the present invention.Additionally, it is disclosed below
Just may be used as long as technical characteristic involved in each embodiment of the present invention does not constitutes conflict each other
To be mutually combined.
The present invention relates to chemical gaseous phase sedimentation preparation of film technical field.More particularly, it relates to
Utilizing chemical gaseous phase to be deposited in nickel metal substrate by a secondary growth, to prepare large-area graphene thin simultaneously
Film and porous amorphous carbon film.Simple and the easily operated control of chemical vapour deposition technique equipment, this skill
Art not only can prepare large-area graphene but also can prepare amorphous carbon film, and its advantage is self-evident.This
Invention utilize chemical vapour deposition technique pass through a secondary growth prepare simultaneously Graphene and amorphous carbon film and
Its compound carbon film material will be greatly facilitated basic research and the wider application of carbon film material.
The present invention prepares in the method for Graphene and porous amorphous carbon film while providing, by once
Growth obtains large-area graphene simultaneously and porous amorphous carbon film, Graphene and amorphous carbon film can
With the most flawless intact separation, and Graphene and the amorphous carbon film after separating can turn respectively
Move on on any substrate, it is also possible to Graphene and amorphous carbon film are stacked together, prepare large area
Graphene/amorphous carbon film/Graphene sandwich structure or Graphene/amorphous carbon film are double-deck
Composite carbon thin film.Therefore, this technology is quick and easy and low cost prepares large-area graphene with many
Hole amorphous carbon film and composite carbon thin film thereof provide a kind of brand-new thinking, can greatly promote C film material
The basic research of material and wider application.
The technical scheme that the present invention is taked by realizing above-mentioned technical purpose is: utilize chemical gaseous phase to deposit
Technology, with Hydrocarbon as carbon source, by carbon source under control hot conditions on substrate nickel sheet surface
Dissolve in carbon atom in absorption cracking and nickel sheet, and follow-up cooling and last substrate etching obtain Graphene
And amorphous carbon film.
According to preparing the technology needs of Graphene and porous amorphous carbon film simultaneously, Graphene thickness is several
Layer is to ten between which floor, and amorphous carbon film has the construction features of porous, and pore diameter distribution exists
Between 10nm～50nm, and there is certain light transmission.Graphene and carbon film all have self-supporting.
The present invention provide a kind of prepare Graphene and porous amorphous carbon film simultaneously method be: utilize
Chemical vapour deposition technique, with Hydrocarbon as carbon source, is serving as a contrast by controlling carbon source under hot conditions
Absorption cracking and the carbon atom on nickel sheet surface, the end dissolve in nickel sheet, and follow-up cooling and last substrate are rotten
Erosion obtains Graphene and amorphous carbon film, and detailed process is:
First by metal nickel sheet substrate ultrasonic cleaning in acetic acid and ethanol solution, pipe after drying, it is positioned over
Formula stove central authorities, are passed through noble gas argon in tube furnace.Then, with 10～40 DEG C of intensifications per minute
Ramp to 750～1000 DEG C, is passed through hydrogen simultaneously, and nickel sheet is carried out heat treatment, heat treatment time
10～50 minutes.Then being passed through Hydrocarbon, this process is that Hydrocarbon is inhaled on substrate nickel sheet surface
Attached cracking and carbon atom dissolve in the process of nickel sheet, and this process temperature is growth temperature, at 750～1000 DEG C
Scope, the growth temperature retention time is 10～50 minutes, and the gas pressure intensity during being somebody's turn to do is normal pressure.So
After be cooled to room temperature with 5～20 DEG C of rate of temperature fall per minute, finally growth after nickel sheet be immersed in corruption
Lose and chlorination processes ferrous solution erode substrate nickel sheet, obtain Graphene and porous amorphous carbon film simultaneously,
Graphene and amorphous carbon film can the most flawless intact be separated, and clean several through deionized water
Can be transferred to respectively in any substrate after secondary, it is also possible to Graphene and amorphous carbon film are stacked together,
Preparation large-area graphene/amorphous carbon film/Graphene sandwich structure or Graphene/amorphous carbon film
Double-deck composite carbon thin film.
The process utilizing chemical vapour deposition technique to grow Graphene and amorphous carbon-film in nickel sheet is at height
The process of molten carbon in nickel sheet catalytic cracking of hydrocarbon and nickel sheet under the conditions of temperature.Due in higher temperature
High-quality Graphene could be obtained under the conditions of degree, by optimizing temperature range, determine at 750～1000 DEG C
In the range of can grow high-quality Graphene.In order to obtain high-quality amorphous carbon film simultaneously, adopt
With being passed through the hydrocarbon gas that range of flow is 20～100sccm scopes in atmospheric conditions, both protected
Card is in 750～1000 DEG C of temperature ranges, dissolved with substantial amounts of carbon atom in nickel sheet, promotes Graphene with many
Grow while the amorphous carbon-film of hole, disordered carbon can be suppressed again in the deposition on nickel sheet surface, thus ensure
The quality of Graphene.Finally by controlling cooling, nickel sheet superficial growth has high-quality Graphene, nickel
Amorphous carbon film is formed dissolved with substantial amounts of carbon atom in sheet, after corroding nickel sheet in ferric chloride solution,
High-quality graphene and amorphous carbon film can be obtained simultaneously.
Wherein, substrate is the metallic nickel plate sheet of 1 μm～500 μ m-thick.Substrate nickel sheet is carried out ultrasonic
During cleaning treatment, as preferentially, acetic acid and ethanol can be used, clean 10～40 minutes.Chemistry gas
It is simple that phase deposition technique has equipment, easy to operate, low cost and the good advantage of controllability, therefore makees
For technology of preparing of the present invention.
In the embodiment of the present invention, substrate nickel sheet is cleaned and intensification heat treatment, carbon source exist under the high temperature conditions
Adsorbing cracking and the molten carbon of nickel sheet, cooling and last substrate nickel sheet corrosion in nickel sheet, these processes are same
Time prepare in Graphene and porous amorphous carbon film technology indispensable.In intensification heat treatment process, rise
Temperature speed controlling is 10～40 DEG C of scopes per minute, and maximum temperature is 750～1000 DEG C of scopes, the highest
During temperature, heat treatment time is in 10～50 minutes scopes or longer.Hydrogen flowing quantity model in heat treatment process
Enclose is 50～200sccm.During carbon source adsorbs cracking and the molten carbon of nickel sheet under the high temperature conditions in nickel sheet
Temperature is 750～1000 DEG C of scopes, and the retention time is 10～50 minutes or longer.
In the cracking of nickel sheet surface adsorption and nickel sheet, carbon during carbon atom is dissolved under hot conditions carbon source
Hydrogen compound range of flow is 20～100sccm.Temperature-fall period is cooled to 5～20 DEG C of speed per minute
Room temperature.Operating air pressure is normal pressure in the above process, is easier realization, cost-effective and operation letter
Single.In substrate nickel sheet corrosion process, corrosive liquid is ferric chloride in aqueous solution, due to ferric chloride in aqueous solution with
The reaction of nickel sheet is very fast, and will not produce the structure of gas breaks amorphous carbon film in course of reaction,
So ferric chloride in aqueous solution can be chosen do corrosive liquid.
Use preparation method of the present invention less demanding to ambient temperature, simple and quick, by once
Growth can prepare the smooth Graphene of large area and large area even porous amorphous carbon film simultaneously,
The area of Graphene and amorphous carbon film is controlled, can easily be transferred to any substrate.Use this
Bright preparation method can prepare large-area graphene/amorphous carbon film/Graphene sandwich structure or stone
Ink alkene/amorphous carbon film double-deck composite carbon thin film.Therefore there is important potential research and application
It is worth.
The embodiment of the present invention obtains Graphene and amorphous carbon film, Graphene by a secondary growth simultaneously
Thickness can be at which floor to ten which floor controls, and amorphous carbon film has transparent and porous construction features.
What is more important, Graphene and amorphous carbon film can the most flawless intact separation, and separate
After Graphene and amorphous carbon film can transfer to respectively on any substrate.The embodiment of the present invention is system
Standby Graphene and amorphous carbon film and composite construction thereof provide a kind of new way；Particularly as follows: substrate metal
The cleaning of nickel sheet, tube furnace are passed through hydrogen to the high-temperature heat treatment of nickel sheet, be passed through under the high temperature conditions
Hydrocarbon gas carries out growing, lowering the temperature and ferric chloride solution etching nickel sheet acquisition graphite in nickel sheet
Alkene and amorphous carbon film.This method of Graphene and amorphous carbon film of simultaneously preparing is currently without being reported
Road, (1) equipment that the invention have the advantages that is simple and low cost；(2) simple to operate and preparation
Polyvinyl chloride；(3) one secondary growths can obtain high-quality graphene and amorphous carbon film two kinds product simultaneously
Thing；(4) Graphene and amorphous carbon film all have self-supporting, can transfer to any substrate respectively
On；(5) large-area graphene/amorphous carbon film/Graphene sandwich structure or Graphene can be prepared
/ amorphous carbon film double-deck composite carbon thin film.Therefore there is important potential research using value.
The method provided the present invention below in conjunction with accompanying drawing and instantiation describes in further detail, and needs
It is noted that embodiment described below is intended to be easy to the understanding of the present invention, and it is not risen any
Restriction effect.Table one shows the list of important parameter in the present invention:
Table one
The present embodiment provides a kind of method simultaneously preparing Graphene and porous amorphous carbon film, this reality
Execute example relate to the use of chemical gaseous phase deposition with Hydrocarbon for carbon source in nickel metal substrate by once
Large-area graphene film and porous amorphous carbon film are prepared in growth simultaneously.Chemical vapor depsotition equipment is such as
Shown in Fig. 1, embodiment flow process is as in figure 2 it is shown, now as a example by embodiment 2, details are as follows:
(1) with 200 microns of polycrystalline nickel sheet as substrate, by metal nickel sheet substrate at acetic acid and ethanol solution
Middle ultrasonic cleaning 10 minutes, dries up and is placed on (Fig. 1) in tube furnace quartz ampoule, be evacuated to background true
Empty (less than 10-3Torr)。
(2) in quartz ampoule, the argon that flow is 100sccm it is passed through, until stable gas pressure is normal pressure,
Programming rate be 20 DEG C per minute.Temperature closes argon after reaching 900 DEG C, and be passed through flow is simultaneously
The hydrogen of 80sccm.
(3) temperature be 900 DEG C, flow be 80sccm hydrogen atmosphere under nickel foil is carried out heat treatment,
The process time is 10 minutes.
(4) in quartz ampoule, it is passed through the methane gas that flow is 50sccm, and reduces hydrogen flowing quantity extremely
5sccm, air pressure remains normal pressure, and methane starts to dissolve in carbon atom in absorption cracking and nickel sheet in nickel sheet,
This process time is 25 minutes.
(5) it is cooled to 450 DEG C with 10 DEG C of speed per minute, opens tube furnace bell, make temperature be down to
Room temperature, in temperature-fall period, methane and hydrogen flowing quantity and air pressure are constant.
(6) take out substrate nickel sheet, configure ferric chloride solution with deionized water, the substrate nickel sheet taken out
It is immersed in ferric chloride solution, after eroding nickel sheet, obtains Graphene and porous amorphous carbon film simultaneously,
Graphene and amorphous carbon film can the most flawless intact be separated, and can transfer to any
Applied research (such as Fig. 3～5) is carried out on substrate.
(7) Graphene and amorphous carbon film can be transferred to any after deionized water cleans several times respectively
In substrate, it is also possible to Graphene and amorphous carbon film are stacked together, preparation large-area graphene/non-
Brilliant C film/Graphene sandwich structure or the double-deck composite carbon of Graphene/amorphous carbon film are thin
Film.
Fig. 3 shows glimmering by the Graphene prepared by a secondary growth and amorphous carbon film of embodiment 2
Light Raman spectrogram.Wherein (a) is the fluorescence Raman spectrum picture of Graphene, and Raman spectrum picture shows
Show D peak (1350cm-1) substantially do not have, show that gained graphene-structured is orderly, G peak (1580cm-1)
Sharply, broadening is little, and display graphene-structured is intact, by 2D (2700cm-1) peak and the ratio at G peak
Understanding gained Graphene is multi-layer graphene；B () is the fluorescence Raman spectrum picture of amorphous carbon film,
Raman spectrum picture display G peak (1580cm-1) higher than D peak (1400cm-1), 2D does not occur
Peak (2700cm-1), but occur in that D+G peak (2970cm-1), show that amorphous carbon film structure is bright
Show and be different from Graphene.
Fig. 4 shows embodiment 2 sweeping by the Graphene prepared by a secondary growth and amorphous carbon film
Retouch the picture of ultramicroscope.Wherein (a) be Graphene the picture of scanning electron microscope, stone
Continuously and free from admixture granule adheres on ink alkene surface；B () is the scanning electron microscope of amorphous carbon film
Picture, amorphous carbon film has the construction features of porous, and pore diameter distribution is at 10nm-50nm, table
Face does not has impurity.Fig. 4 shows Graphene and the intact separation of amorphous carbon film, and noresidue
Thing, does not the most influence each other.
Fig. 5 shows that embodiment 2 is by the Graphene prepared by a secondary growth and the height of amorphous carbon film
The microscopical picture of Resolution Transmission Electron and choose electronic diffraction picture (upper right corner) accordingly.Wherein
A () is picture and the corresponding SEAD (right side of the high resolution transmission electron microscopy of Graphene
Upper angle), free from admixture between number layer graphene, structural integrity is orderly；B () is the height of amorphous carbon film
The microscopical picture of Resolution Transmission Electron and corresponding SEAD (upper right corner), C film without
Impurity adheres to, and SEAD display C film is amorphous carbon film.
As it will be easily appreciated by one skilled in the art that and the foregoing is only presently preferred embodiments of the present invention,
Not in order to limit the present invention, all made within the spirit and principles in the present invention any amendment, etc.
With replacement and improvement etc., should be included within the scope of the present invention.
Claims (5)
1. the method simultaneously preparing Graphene and porous amorphous carbon film, it is characterised in that include
Following step:
S1: be positioned in tube furnace after metal nickel sheet substrate is carried out ultrasonic cleaning, and drying；
S2: be passed through noble gas in described tube furnace；
S3: described tube furnace is carried out hyperthermic treatment and reaches 750 DEG C～1000 DEG C and keep 10 minutes
～50 minutes, in described tube furnace, it is passed through hydrogen, and described metal nickel sheet substrate is carried out heat treatment；
The flow being passed through hydrogen is 50sccm～200sccm.
S4: be passed through the Hydrocarbon that flow is 20sccm～100sccm in described tube furnace so that
Metal nickel sheet substrate catalytic hydrocarbon after Overheating Treatment cracks and gives birth to after the molten carbon of nickel sheet simultaneously
Long Graphene and amorphous carbon film；Gas pressure intensity during Gai is normal pressure；
S5: described tube furnace is carried out cooling process, and growth is had Graphene and amorphous carbon film
Nickel sheet is immersed in corrosive liquid after eroding substrate nickel sheet and obtains Graphene and porous amorphous carbon film.
2. the method for claim 1, it is characterised in that in step s 5, described corrosion
Liquid is ferric chloride in aqueous solution.
3. preparation method as claimed in claim 1, it is characterised in that in step s 2, described
Noble gas is at least one in argon or helium.
4. the preparation method as described in any one of claim 1-3, it is characterised in that in step S2
In, the flow being passed through noble gas is 50sccm～500sccm.
5. preparation method as claimed in claim 1, it is characterised in that described Hydrocarbon is first
Alkane, ethane, propane, butane, hexane, pentane, heptane, octane, propylene, ethylene, butylene,
Any one or the most multiple combination in amylene, acetylene.
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| CN104538196A (en) * | 2014-12-08 | 2015-04-22 | 华中科技大学 | Preparation method of sandwich structure composite carbon material film |
| CN105060278A (en) * | 2015-09-02 | 2015-11-18 | 华中科技大学 | Preparation method of self-supporting three-dimensional foam porous carbon film |
| CN105355465A (en) * | 2015-11-13 | 2016-02-24 | 哈尔滨工业大学 | Preparation method of amorphous carbon/vertical graphene composite electrode material |
| CN105779965B (en) * | 2016-01-21 | 2019-08-20 | 北京师范大学 | A method of porous doped diamond film is prepared using particle beams control technique |
| CN106345319B (en) * | 2016-08-25 | 2019-05-17 | 浙江大学 | It is a kind of without support full carbon film of active carbon and its preparation method and application |
| CN107445147A (en) * | 2017-09-11 | 2017-12-08 | 张洪 | The preparation method and equipment of a kind of graphene |
| CN107761071B (en) * | 2017-10-27 | 2020-05-29 | 南昌航空大学 | Preparation method of graphene film without defect peak |
| CN109136827A (en) * | 2018-08-20 | 2019-01-04 | 北京科技大学 | The method for improving deepsea mining system components anticorrosion antiwear from growth carbonaceous membrane |
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| CN101831633A (en) * | 2010-04-21 | 2010-09-15 | 清华大学 | Method for preparing composite film of graphene and amorphous carbon |
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| Low-temperature synthesis of multilayer graphene/amorphous carbon hybrid films and their potential application in solar cells;Tongxiang Cui et al.;《Nanoscale Research Letters》;20121231;第7卷(第453期);第2页左栏倒数第5行-右栏第13行，第4页右栏第3-5行，第5页右栏倒数第1-2行 * |
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