CN105060278A - Preparation method of self-supporting three-dimensional foam porous carbon film - Google Patents
Preparation method of self-supporting three-dimensional foam porous carbon film Download PDFInfo
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Abstract
The invention discloses a method for preparing a self-supporting three-dimensional foam porous carbon film, which comprises the following steps: S1. carrying out ultrasonic cleaning on foam nickel, drying, and putting into a pipe furnace; S2. introducing inert gas into the pipe furnace, and keeping the foam nickel in an atmospheric-pressure inert environment; S3. heating the working region of the pipe furnace to 550-620 DEG C, introducing hydrogen into the pipe furnace, and treating the foam nickel; S4. introducing hydrocarbons into the pipe furnace, cracking the hydrocarbons by using the foam nickel as the catalyst to generate carbon atoms which are molten into the foam nickel to form carbonous foam nickel; S5. cooling the pipe furnace, and taking out the carbonous foam nickel; and S6. immersing the carbonous foam nickel in an etching solution until the nickel atoms in the carbonous foam nickel are etched, thereby obtaining the self-supporting three-dimensional foam porous carbon film. The preparation method has low requirements for working atmosphere temperature. The prepared self-supporting three-dimensional foam porous carbon film has the characteristics of porous structure and self-supporting, and can be conveniently transferred to any substrate.
Description
Technical field
The invention belongs to three-dimensional carbon technical field of membrane, more specifically, relate to a kind of preparation method of the self-supporting class three-dimensional foam shape porous carbon film based on foam nickel base.
Background technology
Carbon film comprises the chemical bond of sp3 hydridization, sp2 hydridization and sp1 hydridization, and wherein the overwhelming majority is the chemical bond of sp2 hydridization and sp3 hydridization.In carbon film, three kinds of chemical bond content its performances different have very different, and therefore carbon film has and range of application widely.Porous carbon film has high-specific surface area, high thermal conductivity, high conductivity, low density, high chemical stability and abundant and vesicular structure widely, make it have a wide range of applications in fields such as electronics, machinery, sensings, particularly in energy storage original paper as electrode materials.But the pore size distribution in porous carbon is little, be unfavorable for electrolytic solution and ion transport.Three-dimensional foam shape porous carbon film, except having the advantage of porous carbon film, also has the vesicular structure of classification, and this structure has quality and transferring charge passage fast.Make it can be widely used in absorption, Chu Qing, in catalysis and energy energy storage device.
At present, the preparation method of porous amorphous carbon-film has a lot, comprises template, activation method, nanometer casting etc.But these technology all exist process complexity, expend time in, inefficiency, be difficult to control, the problem such as the high and contaminate environment of production cost.The more important thing is, these methods can not for the preparation of three-dimensional foam shape porous carbon film.This shows, there are some defects and constrain its fundamental research and application in current amorphous carbon film technology of preparing.
At present, chemical vapour deposition (chemicalvapordeposition-CVD) is a kind of method of vapor-phase growing preparing material, it one or more is contained the compound, the elementary gas that form film element pass into the reaction chamber being placed with base material, by the Technology of space gas-phase chemical reaction depositing solid films on matrix surface.But general chemical gaseous phase depositing process can only form product at matrix surface, this patent, by infiltrating carbon atom to the regulation and control CVD of parameter in the inside of matrix, forms carbon film in the process that matrix corrosion dissolves.
Summary of the invention
For above defect or the Improvement requirement of prior art, the invention provides a kind of preparation method of self-supporting class three-dimensional foam shape porous carbon film, its object is to solve process in the preparation method of prior art complicated, expend time in, inefficiency, be difficult to control, the technical problem that production cost is high.
The invention provides a kind of preparation method of self-supporting class three-dimensional foam shape porous carbon film, comprise the steps:
S1: nickel foam ultrasonic cleaning is clean, and put into tube furnace after drying;
S2: pass into rare gas element and keep nickel foam to be in normal pressure inert environments in described tube furnace;
S3: carry out intensification to the operation interval of described tube furnace and make it reach 550 DEG C-620 DEG C, then pass into the hydrogen of 5sccm-100sccm in described tube furnace, carries out 550 DEG C of-620 DEG C of pyroprocessing 20 minutes ~ 50 minutes to described nickel foam;
S4: pass into 5sccm-100sccm hydrocarbon polymer in described tube furnace, Formed atom after making the cracking of foamed nickel catalyst hydrocarbon polymer also dissolves in nickel foam and forms carbonaceous foam nickel;
S5: obtain carbonaceous foam nickel after cooling process is carried out to described tube furnace;
S6: be immersed in corrosive fluid by carbonaceous foam nickel, obtains self-supporting class three-dimensional foam shape porous carbon film after the nickle atom in carbonaceous foam nickel has been corroded.
Further, in step s 4 which, growth temperature is 550 DEG C-620 DEG C, and growth time is 5 minutes ~ 60 minutes, and growth air pressure is normal pressure.
Further, substrate used is nickel foam, the thickness of described nickel foam 100 μm-1000 μm.
Further, in step s 5, described corrosive fluid is ferric chloride in aqueous solution, dilute hydrochloric acid solution, at least one in dilution heat of sulfuric acid and dilute nitric acid solution.
Further, in step s 2, described rare gas element is at least one or two gas and vapor permeation in argon gas or helium.
Further, described hydrocarbon polymer is any one or combination multiple arbitrarily in methane, ethane, propane, butane, hexane, pentane, heptane, octane, nonane, decane, propylene, ethene, butylene, amylene, acetylene.
Further, the thickness of described self-supporting class three-dimensional foam shape porous carbon film is 70nm-500nm, and bore dia is 1nm-90nm.
The present invention obtains self-supporting class three-dimensional foam shape porous carbon film under lower growth temperature, and this carbon film has unique three-dimensional foam shape and vesicular structure, and can self-supporting, conveniently transfers in any substrate and carries out various correlative study.Compared with the technology prepared with current carbon film, the present invention has the following advantages: (1) self-supporting, can transfer on any substrate; (2) simple to operate quick with preparation process; (3) equipment is simple and cost is low; (4) carbon film has three-dimensional foam shape structure; (5) big area carbon film can be prepared; (6) growth temperature is lower, technique environmental protection; (7) carbon film has vesicular structure, and thickness can conveniently control.
Accompanying drawing explanation
Fig. 1 is the structural representation of the preparation facilities of the self-supporting class three-dimensional foam shape porous carbon film that the embodiment of the present invention provides;
Fig. 2 is the realization flow figure of the preparation method of the self-supporting class three-dimensional foam shape porous carbon film that the embodiment of the present invention provides;
Fig. 3 be self-supporting class three-dimensional foam shape porous carbon film prepared by the embodiment of the present invention 3 Raman spectrogram;
Fig. 4 is the X-ray diffractogram of the self-supporting class three-dimensional foam shape porous carbon film prepared by the embodiment of the present invention 3; Figure a is the X-ray diffractogram of sample before corrosion of preparation at 600 DEG C; Figure b is the X-ray diffractogram of sample after corrosion of preparation at 600 DEG C.
Fig. 5 is the scanning electron microscope shape appearance figure of the self-supporting class three-dimensional foam shape porous carbon film prepared by the embodiment of the present invention 3; A, b, c figure is the scanning electron microscope shape appearance figure of uncorroded carbonaceous foam nickel under scale is 100m, 30m, 5m respectively, and d, e, f figure is the scanning electron microscope pattern under scale is 100m, 30m, 200nm of prepared carbon film respectively.
Fig. 6 is the optical photograph of the self-supporting class three-dimensional foam shape porous carbon film prepared by the embodiment of the present invention 3.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
For achieving the above object, according to one aspect of the present invention, provide a kind of preparation method of self-supporting class three-dimensional foam shape porous carbon film, comprise the steps:
S1: nickel foam ultrasonic cleaning is clean, puts into tube furnace after drying;
S2: pass into rare gas element and keep nickel foam to be in normal pressure inert environments in described tube furnace; Normal pressure comparatively low pressure time, the velocity of diffusion of carbon atom is slower, and carbon atom not easily precipitate into substrate surface, could retain in the substrate thus at the carbon film of process formation afterwards.
S3: raise described tube furnace operation interval temperature and make it reach 550 DEG C-620 DEG C, temperature is lower than 550 DEG C, carbon atom in infiltration nickel foam very little, finally cannot form complete carbon film, temperature is higher than 620 DEG C, in temperature-fall period, can separate out formation Graphene containing the carbon atom in the nickel foam of carbon atom, the final carbon film formed contains Graphene.In tube furnace, pass into 5sccm-100sccm hydrogen again, make it be in atmosphere of hydrogen, and 550 DEG C of-620 DEG C of pyroprocessing are carried out 20 to 50 minutes to described nickel foam;
S4: pass into 5sccm-100sccm hydrocarbon polymer in described tube furnace, make foamed nickel catalyst hydrocarbon polymer cracking (for methane CH4 CH4 → C+H2) Formed atom dissolve in nickel foam and form carbonaceous foam nickel afterwards, this course work air pressure be normal pressure (normal pressure comparatively low pressure time, the velocity of diffusion of carbon atom is slower, carbon atom not easily precipitate into substrate surface, could retain in the substrate thus form carbon film in process afterwards), this process maintains 5 minutes-60 minutes;
S5: subsequently cooling process is carried out to described tube furnace, take out carbonaceous foam nickel after cooling;
S6: be immersed in corrosive fluid by carbonaceous foam nickel, can obtain self-supporting class three-dimensional foam shape porous carbon film after the nickle atom in carbonaceous foam nickel has been corroded.
Further, in step s 4 which, temperature is 550 DEG C-620 DEG C, and the time is 5 minutes-60 minutes, and air pressure is normal atmosphere.
Further, the thickness of described three-dimensional foam shape graphite porous carbon film is 70nm-500nm, and bore dia is 1nm-90nm.
Further, in step s 5, described corrosive fluid is ferric chloride in aqueous solution, dilute hydrochloric acid solution, at least one in dilution heat of sulfuric acid and dilute nitric acid solution.
Further, the thickness of described metal foam nickel substrate is 100 μm-1000 μm.
Further, in step s 2, described rare gas element is at least one in argon gas or helium.
Further, described hydrocarbon polymer is any one or combination multiple arbitrarily in methane, ethane, propane, butane, hexane, pentane, heptane, octane, nonane, decane, propylene, ethene, butylene, amylene, acetylene.
The present invention obtains self-supporting class three-dimensional foam shape porous carbon film under lower growth temperature, and this carbon film has unique three-dimensional foam shape and vesicular structure, and can self-supporting, conveniently transfers in any substrate and carries out various correlative study.Compared with the technology prepared with current carbon film, the present invention has the following advantages: (1) self-supporting, can transfer on any substrate; (2) simple to operate quick with preparation process; (3) equipment is simple and cost is low; (4) carbon film has three-dimensional foam shape structure; (5) big area carbon film can be prepared; (6) growth temperature is lower, technique environmental protection; (7) carbon film has vesicular structure, and thickness can conveniently control.
The present invention for the technical scheme realizing above-mentioned technical purpose and take is: utilize chemical vapour deposition technique, take hydrocarbon polymer as carbon source, nickel foam is substrate, dissolve in base foam nickel by controlling the carbon atom of carbon source cracking under hot conditions, and follow-up cooling and last substrate corrosion obtain self-supporting class three-dimensional foam shape porous carbon film.Wherein, according to porous needs, the thickness of porous carbon film can be controlled at 70nm-500nm, and pore diameter distribution is at 1nm-90nm.
The preparation method that the invention provides a kind of three-dimensional foam shape porous carbon film of novel texture is: utilize chemical vapour deposition technique, take hydrocarbon polymer as carbon source, nickel foam is that substrate controls thermal treatment and the carbon source cracking of base foam nickel by temperature and gas Flow-rate adjustment, then cooling is controlled, obtain three-dimensional foam shape porous carbon film finally by the corrosion of base foam nickel, detailed process is:
First by foam nickel base successively at acetic acid and ethanolic soln, deionized water for ultrasonic is cleaned, and is positioned over tube furnace central authorities after oven dry, and tube furnace is evacuated in backward tube furnace passes into rare gas element argon gas, keeps normal pressure.Then, be warmed up to 550-620 DEG C with 10-50 DEG C of per minute, pass into hydrogen simultaneously, heat-treat nickel foam, heat treatment time 20-50 minute, then passes into hydrocarbon polymer, and this process is hydrocarbon cracking process.This process temperature is growth temperature, 550-620 DEG C of scope, the growth temperature hold-time is 5-60 minute, gas pressure intensity in this process is still normal pressure, then room temperature is cooled to the rate of temperature fall of 5-30 DEG C of per minute, the nickel foam of finally taking out also is immersed in corrosive fluid ferric chloride Solution and erodes foam nickel base, obtains described carbon film.
Before growth, pass into hydrogen heat-treat nickel foam, can cleaning foam nickel foam surface, be more conducive to the cracking of foam nickel base catalytic hydrocarbon.Utilize chemical vapour deposition technique, nickel foam can catalytic hydrocarbon cracking molten carbon at relatively low temperature, control growth temperature range between 550-620 DEG C, both met the temperature requirement of foam nickel base catalytic hydrocarbon cracking, also adapted in the demand compared with grown at low temperature carbon film.Controlling growth air pressure is normal pressure, and growth time, at 5-60 minute, can ensure that being dissolved with enough carbon atoms in nickel foam when growing forms carbon film.
In above-mentioned technology of preparing scheme, substrate is 100 μm-1000 μm thick nickel foam, and the nickel foam of this thickness range is widely used in the catalytic metal substrate of chemical vapour deposition.
When ultrasonic cleaning process is carried out to nickel foam, as preferentially, adopt acetic acid and alcohol, cleaning 10-40 minute.
It is simple that chemical vapour deposition technique has equipment, easy to operate, and the advantage that cost is low and controllability is good, therefore as technology of preparing of the present invention.
In the present invention, the several process of technical scheme comprises: the cleaning of base foam nickel and intensification thermal treatment, the cracking of high temperature carbon source, cooling and last base foam nickel corrosion, these processes are indispensable in the preparation of three-dimensional foam shape carbon film.
In above-mentioned several process: in intensification heat treatment process, heat-up rate controls 20-50 DEG C of per minute scope, and growth temperature is 550-620 DEG C of scope, and when growth temperature, heat treatment time is in 10-50 minute scope or longer.In heat treatment process, hydrogen flowing quantity scope is 5-100sccm.In high temperature carbon source cracking process, temperature is 550-620 DEG C of scope, and the hold-time is 20-50 minute or longer.In high temperature carbon source cracking process, hydrocarbon polymer flow range is 5-100sccm.Room temperature is cooled to 5-30 DEG C of per minute speed in temperature-fall period.Operating air pressure is normal pressure in the above process.In base foam nickel corrosion process, corrosive fluid can be ferric chloride in aqueous solution, because the reaction of ferric chloride in aqueous solution and nickel foam is very fast, and can not produce the structure of gas breaks carbon film in reaction process, so choose ferric chloride in aqueous solution to do corrosive fluid.
Below in conjunction with accompanying drawing and specific examples, preparation method provided by the invention is described in further detail, it is pointed out that the following stated embodiment is intended to be convenient to the understanding of the present invention, and any restriction effect is not play to it.Table 1-4 shows the list of important parameter in the present invention:
The experiment parameter of carbon film prepared by table 1 under 550 DEG C of conditions
The experiment parameter of carbon film prepared by table 2 under 580 DEG C of conditions
The experiment parameter of carbon film prepared by table 3 under 600 DEG C of conditions
The experiment parameter of carbon film prepared by table 4 under 620 DEG C of conditions
A kind of preparation method of self-supporting class three-dimensional foam shape porous carbon film of novel texture is provided in the present embodiment, the present embodiment relate to utilize chemical vapour deposition in the transition metal substrate of foamy structure with hydrocarbon polymer be carbon source preparation there is big area self-supporting class three-dimensional foam shape porous carbon film.Chemical vapor depsotition equipment is as Fig. 1, and implementing procedure figure is as Fig. 2, and existing for embodiment 3, details are as follows:
(1) with 500 microns of nickel foam for substrate, by foam nickel base ultrasonic cleaning 10 minutes in acetic acid and ethanolic soln, dry up and be placed on (Fig. 1) in the middle part of tube furnace silica tube, be evacuated to base vacuum (lower than 10-3Torr).
(2) in silica tube, pass into the argon gas that flow is 100sccm, until stable gas pressure is normal pressure, heat-up rate is 20 DEG C of per minutes.Temperature closes argon gas after reaching 600 DEG C, passes into the hydrogen that flow is 80sccm simultaneously.
(3) temperature be 600 DEG C, flow heat-treats nickel foam under being the hydrogen atmosphere of 80sccm, the treatment time is 10 minutes.
(4) in silica tube, pass into the methane gas that flow is 8sccm, and reduce hydrogen flowing quantity to 80sccm, air pressure remains normal pressure, and start methane cracking process, this process time is 25 minutes.
(5) be cooled to 450 DEG C with 10 DEG C of per minute speed, open tube furnace bell, make temperature be down to room temperature, in temperature-fall period methane and hydrogen flowing quantity and air pressure constant.
(6) take out nickel foam be immersed in deionized water configuration ferric chloride Solution in corrode, formed self-supporting class three-dimensional foam shape porous carbon film (as Fig. 3-6).
Fig. 3 shows the Raman spectrogram of prepared carbon film, can show from D peak and G peak the structure that prepared carbon film is amorphous.
Fig. 4 shows the X-ray diffractogram of sample on monocrystalline silicon piece prepared by embodiment 3, the X-ray diffractogram of sample before corrosion of preparation at a:600 DEG C; The X-ray diffractogram of sample after corrosion of preparation at b:600 DEG C; As can be seen from X-ray diffraction, this carbon film is the carbon film of amorphous.
Fig. 5 shows the scanning electron microscope shape appearance figure in different amplification of embodiment 3 uncorroded carbonaceous foam nickel and prepared carbon film, a, b, c figure is uncorroded carbonaceous foam nickel is being 100m, 30m at scale respectively, scanning electron microscope shape appearance figure under 5m, d, e, f figure be prepared carbon film be 100m at scale respectively, scanning electron microscope pattern under 30m, 200nm.As can be seen from the figure this carbon film has the constructional feature of porous, and pore diameter distribution is at 1nm-90nm.
Fig. 6 shows the optical photograph of the carbon film prepared by embodiment 3, and photo shows this carbon film area and is greater than, and smooth, can self-supporting, conveniently transfers on any substrate.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. a preparation method for self-supporting class three-dimensional foam shape porous carbon film, is characterized in that, comprise the steps:
S1: nickel foam ultrasonic cleaning is clean, and put into tube furnace after drying;
S2: pass into rare gas element and keep nickel foam to be in normal pressure inert environments in described tube furnace;
S3: carry out intensification to the operation interval of described tube furnace and make it reach 550 DEG C-620 DEG C, then pass into the hydrogen of 5sccm-100sccm in described tube furnace, carries out 550 DEG C of-620 DEG C of pyroprocessing 20 minutes ~ 50 minutes to described nickel foam;
S4: pass into 5sccm-100sccm hydrocarbon polymer in described tube furnace, Formed atom after making the cracking of foamed nickel catalyst hydrocarbon polymer also dissolves in nickel foam and forms carbonaceous foam nickel;
S5: obtain carbonaceous foam nickel after cooling process is carried out to described tube furnace;
S6: be immersed in corrosive fluid by carbonaceous foam nickel, obtains self-supporting class three-dimensional foam shape porous carbon film after the nickle atom in carbonaceous foam nickel has been corroded.
2. preparation method as claimed in claim 1, it is characterized in that, in step s 4 which, growth temperature is 550 DEG C-620 DEG C, and growth time is 5 minutes ~ 60 minutes, and growth air pressure is normal pressure.
3. preparation method as claimed in claim 1, it is characterized in that, substrate used is nickel foam, and the thickness of described nickel foam is 100 μm-1000 μm.
4. preparation method as claimed in claim 1, it is characterized in that, in step s 5, described corrosive fluid is ferric chloride in aqueous solution, dilute hydrochloric acid solution, at least one in dilution heat of sulfuric acid and dilute nitric acid solution.
5. preparation method as claimed in claim 1, is characterized in that, in step s 2, described rare gas element is at least one or two gas and vapor permeation in argon gas or helium.
6. preparation method as claimed in claim 1, it is characterized in that, described hydrocarbon polymer is any one or combination multiple arbitrarily in methane, ethane, propane, butane, hexane, pentane, heptane, octane, nonane, decane, propylene, ethene, butylene, amylene, acetylene.
7. preparation method as claimed in claim 1 or 2, it is characterized in that, the thickness of described self-supporting class three-dimensional foam shape porous carbon film is 70nm-500nm, and bore dia is 1nm-90nm.
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Cited By (3)
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| CN107792844A (en) * | 2017-12-12 | 2018-03-13 | 中国科学院过程工程研究所 | A kind of preparation method of three-dimensional foam carbon |
| CN110436436A (en) * | 2019-07-19 | 2019-11-12 | 广东工业大学 | A kind of three-dimensional microstructures self-supporting flexible, porous carbon film and its preparation method and application |
| CN113151801A (en) * | 2021-03-03 | 2021-07-23 | 电子科技大学 | Preparation method of self-supporting suspended carbon film |
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| CN103613094A (en) * | 2013-11-28 | 2014-03-05 | 华中科技大学 | Method for preparing graphene and porous amorphous carbon films simultaneously |
| CN103643217A (en) * | 2013-11-28 | 2014-03-19 | 华中科技大学 | Method for preparing self-supporting graphite porous amorphous carbon thin film |
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| EP2407423A1 (en) * | 2009-03-10 | 2012-01-18 | Toyo Tanso Co., Ltd. | Porous carbon and process for producing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107792844A (en) * | 2017-12-12 | 2018-03-13 | 中国科学院过程工程研究所 | A kind of preparation method of three-dimensional foam carbon |
| CN110436436A (en) * | 2019-07-19 | 2019-11-12 | 广东工业大学 | A kind of three-dimensional microstructures self-supporting flexible, porous carbon film and its preparation method and application |
| CN110436436B (en) * | 2019-07-19 | 2022-10-04 | 广东工业大学 | Three-dimensional microstructure self-supporting flexible porous carbon film and preparation method and application thereof |
| CN113151801A (en) * | 2021-03-03 | 2021-07-23 | 电子科技大学 | Preparation method of self-supporting suspended carbon film |
| CN113151801B (en) * | 2021-03-03 | 2022-12-27 | 电子科技大学 | Preparation method of self-supporting suspended carbon film |
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Application publication date: 20151118 |