CN105296958A - Three-dimensional non-catalytic base load graphene film structure and preparation method thereof in low temperature environment - Google Patents
Three-dimensional non-catalytic base load graphene film structure and preparation method thereof in low temperature environment Download PDFInfo
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Abstract
The invention discloses a three-dimensional non-catalytic base load graphene film structure, which comprises a non-catalytic substrate engine body, a three-dimensional structure and a graphene film, wherein the three-dimensional structure is etched on the surface of the non-catalytic substrate engine body, and the graphene film is covered on the whole surface. The invention also discloses a method for preparing the three-dimensional non-catalytic base load graphene film structure in a low temperature environment, which is simple and convenient to operate, short in production cycle and low in making cost, and can directly form high quality graphene films which are continuous and uniform with non-catalytic substrates with different surface three-dimensional structures on whole surfaces of different materials. The three-dimensional non-catalytic base load graphene film can be used as a transparent electrode on a surface to be applied in devices such as photoelectric devices and micro-electromechanical systems (MEMS) and the like, and also can be used to develop novel nano devices.
Description
Technical field
The invention belongs to field of material technology, relate to a kind of three-dimensional non-catalytic base load graphene film structure and preparation method at low ambient temperatures thereof.
Background technology
Graphene is a kind of two dimensional crystal with hexangle type honeycomb crystalline network by monolayer carbon atomic building.Owing to having the large key of low-dimensional quantum characteristic and the formation of unique sp2 hydridization, its free electron gas shows as two dimension without quality dirac fermion gas, thus Graphene shows and is only the better light transmission of 2.3% and the photoelectric characteristic of the superior electron mobility up to 15,000cm2V-1s-1 etc. in visible region absorption.Meanwhile, grapheme material also has high heat conductance and superpower mechanical property, and the characteristic of these excellences makes grapheme material be expected to become a kind of epoch-making transparent conductive film.
But in the application report of most photoelectric device, Graphene is as transparent conductive film, mostly be that by transfer method, Graphene is transferred to the target substrate such as semi-conductor or isolator and get, this transfer step is often to the cull that graphenic surface brings from catalytic substrate (such as: Copper Foil, nickel foil etc.) surface, fold, tear, impurity, the problems such as defect, thus greatly reduce the performance of Graphene, and then affect the application of photoelectric device.Seeking a kind of graphene preparation method that can directly be deposited to by Graphene on non-catalytic substrate, is the key overcome the above problems.
Plasma enhanced chemical vapor deposition method (PECVD) is a kind of key method of growing graphene.In the process of growing graphene, plasma body can provide high-energy electron, the molecule be stimulated and the various active such as atom, free group material, thus " PECVD " has lot of advantages when depositing nano structured material, such as, substrate growth temperature is low, sample grown speed is fast, and nanostructure sequence is easy to control.These advantages, be doomed " PECVD " be a kind of directly, fast Graphene is prepared into semi-conductor, the appropriate method on the non-catalytic substrates such as isolator.The method is utilized to prepare Graphene, avoid the harm that transfer step is brought Graphene, thus greatly widen the range of application of Graphene at graphene-based MEMS (micro electro mechanical system) (MEMS) device and the field of photoelectric devices such as solar cell, ultracapacitor.
So far, utilize PECVD method, prepared by the substrate of the non-catalytic such as semi-conductor or isolator in the minority report of Graphene, mostly be greater than under the comparatively high temps of 650 DEG C, prepared by the plane non-catalytic substrate of a certain or few several materials, this just causes the material much had compared with low melting point not directly to be used to prepare Graphene.Meanwhile, based in the device application of transparent graphene conductive film, most devices of report are made up of the optical element of various microtexture.So under comparatively high temps, Graphene prepared by the substrate of plane non-catalytic, is difficult to meet its application in various material and various micromechanical devices.Therefore a kind of universality method finding " PECVD " conformal graphene growth is extremely urgent, the method requires the non-catalytic substrate grown that can meet different kind of material, and meets the non-catalytic substrate grown that surface has diverse microcosmic structure simultaneously.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of three-dimensional non-catalytic base load graphene film structure and preparation method at low ambient temperatures thereof, the graphene film continuous uniform of described structure, and its substrate can adopt dissimilar material, and its preparation method is easy and simple to handle, fabrication cycle is short, and cost of manufacture is low, and can complete realization under the condition of lesser temps.
For achieving the above object, the invention provides following technical scheme:
1, a three-dimensional non-catalytic base load graphene film structure, described structure comprises non-catalytic substrate body, the three-dimensional structure that body surface etches, and the graphene film covering whole surface.
Preferably, described three-dimensional structure is periodic arrangement or no periodic array, and described three-dimensional structure is grating, nanoporous, nano wire, nanometer rod, one or more in pyramid, ledge structure.
2, the preparation method of described three-dimensional non-catalytic base load graphene film structure, it is characterized in that, step is as follows:
A. by photoetching, ion etching or wet etching prepare three-dimensional structure in non-catalytic substrate, and clean up and drying;
B. the substrate through steps A is placed in the temperature control cavity of plasma enhanced chemical vapor deposition unit, drains the air in cavity, then in cavity, fill shielding gas;
C. the temperature control cavity after step B being filled shielding gas is evacuated to the vacuum state of growth, then 500-650 DEG C is warming up to, pass into carbon-source gas and the shielding gas playing current-carrying effect, open plasma strengthens source, maintain air pressure at 1-10Pa, make graphene film at the non-catalytic substrate surface direct growth 60-120min of three-dimensional structure;
D. after the growth of step C graphene film terminates; close plasma enhancing source immediately; and stop passing into carbon-source gas in temperature control cavity; temperature control cavity speed under shielding gas and graphene film growth pressure is cooled to 10-30 DEG C; take out the non-catalytic substrate of three-dimensional structure, namely its full surface is coated with the graphene film of continuous uniform.
Preferably, described non-catalytic substrate is that fusing point stablizes unvaporized inorganic materials lower than the growth temperature of graphene film under graphene film growth temperature condition.
Preferably, described non-catalytic substrate is silicon-dioxide, silicon, germanium, gallium arsenide, indium phosphide, silicon nitride, silicon carbide, zinc oxide or aluminum oxide.
Preferred, described shielding gas is one or more mixing in nitrogen, hydrogen, argon gas, helium, neon, Krypton and xenon, and described carbon-source gas is one or more mixing in methane, ethene, acetylene, methyl alcohol, ethanol, Benzene and Toluene gas.
Preferably, described in steps A, cleaning way is as follows: the non-catalytic substrate of three-dimensional structure is put successively each ultrasonic cleaning 10-15min in acetone, 95vol% ethanol, water, then dry up with nitrogen.
Preferably, the method draining air in temperature control cavity in step B is as follows: temperature control cavity is evacuated to 1-5Pa, then fills shielding gas to 1atm, then repeats the above-mentioned operation vacuumizing, fill shielding gas, until the air in temperature control cavity drains; Or the air pressure in temperature control cavity is remained on 1atm, and the shielding gas 10-30min passing into large discharge in temperature control cavity rinses, and makes the air in temperature control cavity drain.
Preferably, described plasma enhancing source is radio frequency plasma body source.
Preferably, RF plasma power is 10-100W.
Beneficial effect of the present invention is: the invention provides a kind of three-dimensional non-catalytic base load graphene film structure, the graphene film continuous uniform of structure, and its substrate can adopt dissimilar material.And under the invention provides a kind of low temperature environment three-dimensional structure non-catalytic substrate on the universality method of conformal growth graphene film, easy and simple to handle, fabrication cycle is short, cost of manufacture is low, can directly at differing materials, with the graphene film of the high-quality continuous uniform of complete surperficial conformal covering on the non-catalytic substrate with different surfaces three-dimensional structure, this Graphene is the film of polycrystalline, its atom number of plies can be controlled by the adjusting process condition such as throughput ratio, RF plasma power of carbon-source gas and shielding gas, forms single or multiple lift; The crystallinity, sheet resistance, light transmission etc. of Graphene are also controlled by the adjusting process condition such as throughput ratio, RF plasma power of carbon-source gas and shielding gas.Can be applied on the devices such as photoelectric device, MEMS (micro electro mechanical system) (MEMS) as the transparency electrode on surface at the suprabasil graphene film of the non-catalytic of three-dimensional structure, also can be used for development of new nano-device.
Accompanying drawing explanation
In order to make object of the present invention, technical scheme and beneficial effect clearly, the invention provides following accompanying drawing and being described:
Fig. 1 is the non-catalytic base load graphene film structure in grating three-dimensional structure;
Fig. 2 is the non-catalytic base load graphene film structure of the three-dimensional structure in different shape;
Fig. 3 prepares the schematic diagram of graphene film for " PECVD ";
Fig. 4 is transmittance and the sheet resistance trend map of the non-catalytic base load graphene film structure that embodiment 1 is prepared under different growth time condition;
Fig. 5 is Raman (Raman) spectrum of embodiment 2 in the non-catalytic substrate of differing materials from different three-dimensional structure after conformal covering graphene film.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.
The experimental technique of unreceipted actual conditions in embodiment, usually conveniently condition, or according to the condition that manufacturer advises.
Embodiment 1
One, the method for complete surperficial conformal covering graphene film on the quartz substrate of optical grating construction, comprises the following steps:
A. by the method for photoetching and ion etching, at the periodic optical grating construction of the surface etch of quartz substrate, the quartz substrate of optical grating construction is prepared;
B. the quartz substrate of optical grating construction is put successively each ultrasonic cleaning 10-15min in acetone, 95vol% ethanol, pure water, dry up with nitrogen;
C. the quartz substrate of dried for step B optical grating construction being put caliber is in the tubular type PECVD system temperature control cavity of 30mm, sealing temperature controlled cavity; Temperature control cavity vacuum pump after sealing is evacuated to 1Pa, in vacuum cavity, fill argon gas to 1atm, then be evacuated to 1Pa with vacuum pump, repeatable operation makes for three times the air in vacuum cavity drain, then in vacuum cavity, filling hydrogen is 10sccm, and air pressure maintains 5Pa;
D. the vacuum cavity after step C being filled hydrogen is warming up to 600 DEG C, methane gas 1.5sccm and hydrogen 1sccm is passed in vacuum cavity, open radio-frequency plasma strengthen source and be set to 50W, air pressure maintains 5Pa, make graphene growth 60-120min (interval 10min, totally 7 samples), (" PECVD " prepares the schematic diagram of Graphene as shown in Figure 3, wherein, 1 is PECVD diamond heating system; 2 is radio-frequency plasma enhancing source; 3 is the temperature control cavity of PECVD tube furnace; 4 is graphene film; 5 is the non-catalytic substrate of three-dimensional structure; 6 is the vacuum pump of PECVD tube furnace system, is furnished with vacuum meter);
E. after step D graphene growth terminates, close radio-frequency plasma immediately and strengthen source, and stop passing into methane gas in temperature control cavity, vacuum cavity speed under 10sccm hydrogen and 5Pa pressure is cooled to room temperature, take out the quartz substrate of optical grating construction, namely its full surface is coated with the graphene film of continuous uniform, and its atom number of plies is 2 ~ 5 layers.
Resulting structures as shown in Figure 1a, wherein 1 represent quartz substrate, 2 periodic grating structure representing the surface etch of quartz substrate, 3 representatives are at the graphene film of the continuous uniform of full surface coverage, and resulting structures SEM (scanning electronic microscope) shape appearance figure is as shown in topic 1b.
Two, the optical performance test of three-dimensional non-catalytic base load graphene film structure is as follows:
1, test transmittance to 7 samples that step e obtains by " UV, visible light scene photometer ", and compare at the transmittance that visible wavelength is 550nm place each sample, result as shown in Figure 4; Transmittance reduces along with the increase of growth time, and this illustrates that time expand is the critical developmental factor thickening Graphene; In the sample of gained, the Graphene transmittance that the growth time of 60min is corresponding is the highest, is 92.5%.
2,7 samples that step e obtains are starched and the method being connected silver-colored line by brushing silver, electrode is prepared at the two ends of each sample, then " four-point probe " is utilized, test the I-V graphic representation of graphene film on each sample, and correspondence calculates sheet resistance corresponding to each sample, as shown in Figure 4, the graphene film thickened can increase the conductive capability of Graphene, reduce the sheet resistance of Graphene, when growth time is 120min, the conductivity of Graphene is best, and corresponding sheet resistance is 1200 Ou Fang; Compare the plane non-catalytic substrate of report, the non-catalytic substrate of three-dimensional structure being prepared the more difficult control of three-dimensional conformal graphene film, the especially side of microscopic three-dimensional structural, there is more uncontrollabilities in the attachment of Graphene.But by contrast, the sheet resistance of the conformal Graphene of the three-dimensional that we prepare but reduces ~ 500 Ou Fang, this just confirms that the PECVD graphene growth method that we report is the conformal high-quality graphene growth method of a kind of low-resistance three-dimensional.
Embodiment 2
One, in different base, comprise the silicon chip of pyramid structure, the silicon chip of nano thread structure, the silicon chip of optical grating construction, the method for complete surperficial conformal covering graphene film on five kinds of substrates such as the quartz plate of optical grating construction and the germanium wafer of optical grating construction, comprises the following steps:
A. by the method for photoetching and ion etching, at the periodic optical grating construction of surface etch of silicon base, quartz substrate and germanium substrate; Periodic pyramid and nano thread structure is not had in silicon substrate surface preparation by the method for wet etching;
B. the substrates of different of different structure is put respectively successively each ultrasonic cleaning 10-15min in acetone, 95vol% ethanol, pure water, dry up with nitrogen;
C. the substrates of different of dried for step B different structure is placed in simultaneously tubular type PECVD system temperature control cavity (as shown in Figure 3) that caliber is 30mm, sealing temperature controlled cavity; Temperature control cavity vacuum pump after sealing is evacuated to 1Pa, in vacuum cavity, fill argon gas to 1atm, then be evacuated to 1Pa with vacuum pump, repeatable operation makes for three times the air in vacuum cavity drain, then in vacuum cavity, filling hydrogen is 10sccm, and air pressure maintains 10Pa;
D. the vacuum cavity after step C being filled hydrogen is warming up to 600 DEG C, passes into ethylene gas 3sccm and hydrogen 2sccm in vacuum cavity, and open radio-frequency plasma and strengthen source and be set to 30W, air pressure maintains 8Pa, makes graphene growth 90min;
E. after step D graphene growth terminates, close radio-frequency plasma immediately and strengthen source, and stop passing into ethylene gas in temperature control cavity, vacuum cavity speed under 10sccm hydrogen and 5Pa pressure is cooled to room temperature, take out the substrates of different of all different structures, its full surface is by the graphene film of conformal covering continuous uniform, and the atom number of plies is 2-5 layer.
Resulting structures as shown in Figure 2 a, wherein the structure shown in Fig. 2 a is the structure various three-dimensional structure concentrated in together, its expression can fall substrate etching in any three-dimensional structure, wherein 1 represent substrate, 2 represent substrate surface etching periodic grating structure, 3 representatives are at the graphene film of the continuous uniform of full surface coverage, and Fig. 2 b represents SEM figure (scanning electronic microscope) of pyramid structure structure.
Two, the optical performance test of three-dimensional non-catalytic base load graphene film structure is as follows:
Each the conformal substrate being coated with graphene film obtained in step e is once put into Raman spectrometer and carries out Raman sign, obtain the Raman spectrogram of each sample, as shown in Figure 5, the Graphene as seen from Figure 5 prepared by different base has similar Raman chromatogram characteristic.It can thus be appreciated that for the non-catalytic substrate of dissimilar three-dimensional structure, with the non-catalytic substrate of differing materials, PECVD method is the universality growth method obtaining conformal Graphene.
Embodiment 3
The method of complete surperficial conformal covering graphene film in the silicon base of club shaped structure, comprises the following steps:
A. by the method for wet etching in basic solution, draw there is no the three-dimensional bar-shaped knot of preiodic type in the surface etch of silicon base, prepare the silicon substrate of club shaped structure;
B. the silicon substrate of club shaped structure is put successively each ultrasonic cleaning 10-15min in acetone, 95vol% ethanol, pure water, dry up with nitrogen;
C. the silicon substrate of dried for step B club shaped structure being put caliber is in the tubular type PECVD system temperature control cavity of 30mm, sealing temperature controlled cavity; Temperature control cavity vacuum pump after sealing is evacuated to 1Pa, in vacuum cavity, fill argon gas to 1atm, then be evacuated to 1Pa with vacuum pump, repeatable operation makes for three times the air in vacuum cavity drain, then in vacuum cavity, filling hydrogen is 20sccm, and air pressure maintains 10Pa;
D. the vacuum cavity after step C being filled hydrogen is warming up to 650 DEG C, passes into acetylene gas 3sccm and hydrogen 2sccm in vacuum cavity, and open radio-frequency plasma and strengthen source and be set to 30W, air pressure maintains 10Pa, makes graphene growth 60min;
E. after step D graphene growth terminates, close radio-frequency plasma immediately and strengthen source, and stop passing into acetylene gas in temperature control cavity, vacuum cavity speed under 20sccm hydrogen and 10Pa pressure is cooled to room temperature, take out the silicon substrate of club shaped structure, its conformal graphene film being coated with continuous uniform in full surface, its atom number of plies is 1-3 layer;
Embodiment 4
The method of complete surperficial conformal covering graphene film in the silicon base of the non-polished of arbitrary structures, comprises the following steps:
A. the non-polished silicon substrate of purchase is put each ultrasonic cleaning 10-15min in acetone, 95vol% ethanol, pure water successively, dry up with nitrogen;
C. the silicon base of dried for step B non-polished being put caliber is in the tubular type PECVD system temperature control cavity of 30mm, sealing temperature controlled cavity; Temperature control cavity vacuum pump after sealing is evacuated to 1Pa, in vacuum cavity, fill argon gas to 1atm, then be evacuated to 1Pa with vacuum pump, repeatable operation makes for three times the air in vacuum cavity drain, then in vacuum cavity, filling hydrogen is 10sccm, and air pressure maintains 5Pa;
D. the vacuum cavity after step C being filled hydrogen is warming up to 650 DEG C, passes into acetylene gas 1.5sccm and hydrogen 1sccm in vacuum cavity, and open radio-frequency plasma and strengthen source and be set to 10W, air pressure maintains 5Pa, makes graphene growth 60min;
E. after step D graphene growth terminates, close radio-frequency plasma immediately and strengthen source, and stop passing into methane gas in temperature control cavity, vacuum cavity speed under 10sccm hydrogen and 5Pa pressure is cooled to room temperature, take out the silicon base of non-polished, its full surface and conformal graphene film being coated with continuous uniform, its atom number of plies is 1-2 layer;
Embodiment 5
The method of complete surperficial conformal covering graphene film at the bottom of the indium phosphide of ledge structure, comprises the following steps:
A. by the method for high temperature annealing substrate, acyclic ledge structure is prepared on the surface at the bottom of indium phosphide, obtains at the bottom of the indium phosphide of ledge structure;
B. by putting each ultrasonic cleaning 10-15min in acetone, 95vol% ethanol, pure water at the bottom of the indium phosphide of ledge structure successively, dry up with nitrogen;
C. be in the tubular type PECVD system temperature control cavity of 30mm (as shown in Figure 2) by putting caliber at the bottom of the indium phosphide of dried for step B ledge structure, sealing temperature controlled cavity; Temperature control cavity vacuum pump after sealing is evacuated to 1Pa, in vacuum cavity, fill argon gas to 1atm, then be evacuated to 1Pa with vacuum pump, repeatable operation makes for three times the air in vacuum cavity drain, then in vacuum cavity, filling hydrogen is 20sccm, and air pressure maintains 10Pa;
D. the vacuum cavity after step C being filled hydrogen is warming up to 650 DEG C, passes into acetylene gas 3sccm and hydrogen 2sccm in vacuum cavity, and open radio-frequency plasma and strengthen source and be set to 50W, air pressure maintains 10Pa, makes graphene growth 30min;
E. after step D graphene growth terminates, close radio-frequency plasma immediately and strengthen source, and stop passing into methane gas in temperature control cavity, vacuum cavity speed under 20sccm hydrogen and 10Pa pressure is cooled to room temperature, at the bottom of the indium phosphide of taking-out platform stage structure, its full surface and conformal graphene film being coated with continuous uniform, its atom number of plies is layer 2-3;
Embodiment 6
The method of complete surperficial conformal covering graphene film in the non-polished germanium substrate on surface with arbitrary structures, comprises the following steps:
A. the germanium substrate of the non-polished of purchase is put each ultrasonic cleaning 10-15min in acetone, 95vol% ethanol, pure water successively, dry up with nitrogen;
B. the substrate of dried for steps A non-polished germanium being put caliber is in the tubular type PECVD system temperature control cavity of 30mm, sealing temperature controlled cavity; Temperature control cavity vacuum pump after sealing is evacuated to 1Pa, in vacuum cavity, fill argon gas to 1atm, then be evacuated to 1Pa with vacuum pump, repeatable operation makes for three times the air in vacuum cavity drain, then in vacuum cavity, filling hydrogen is 10sccm, and air pressure maintains 5Pa;
C. the vacuum cavity after step B being filled hydrogen is warming up to 550 DEG C, passes into methane gas 1.5sccm and hydrogen 1sccm in vacuum cavity, and open radio-frequency plasma and strengthen source and be set to 10W, air pressure maintains 2Pa, makes graphene growth 60min;
D. after step C graphene growth terminates, close radio-frequency plasma immediately and strengthen source, and stop passing into methane gas in temperature control cavity, vacuum cavity speed under 10sccm hydrogen and 5Pa pressure is cooled to room temperature, take out the substrate of non-polished germanium, its full surface and conformal graphene film being coated with continuous uniform, its atom number of plies is individual layer;
What finally illustrate is, above preferred embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by above preferred embodiment to invention has been detailed description, but those skilled in the art are to be understood that, various change can be made to it in the form and details, and not depart from claims of the present invention limited range.
Claims (10)
1. a three-dimensional non-catalytic base load graphene film structure, it is characterized in that, described structure comprises non-catalytic substrate body, the three-dimensional structure that body surface etches, and the graphene film covering whole surface.
2. a kind of three-dimensional non-catalytic base load graphene film structure according to claim 1, it is characterized in that, described three-dimensional structure is periodic arrangement or no periodic array, described three-dimensional structure is grating, nanoporous, nano wire, nanometer rod, one or more in pyramid, ledge structure.
3. the preparation method of three-dimensional non-catalytic base load graphene film structure described in any one of claim 1 ~ 2, it is characterized in that, step is as follows:
A. by photoetching, ion etching or wet etching prepare three-dimensional structure in non-catalytic substrate, and clean up and drying;
B. the substrate through steps A is placed in the temperature control cavity of plasma enhanced chemical vapor deposition unit, drains the air in cavity, then in cavity, fill shielding gas;
C. the temperature control cavity after step B being filled shielding gas is evacuated to the vacuum state of growth, then 500-650 DEG C is warming up to, pass into carbon-source gas and the shielding gas playing current-carrying effect, open plasma strengthens source, maintain air pressure at 1-10Pa, make graphene film at the non-catalytic substrate surface direct growth 60-120min of three-dimensional structure;
D. after the growth of step C graphene film terminates; close plasma enhancing source immediately; and stop passing into carbon-source gas in temperature control cavity; temperature control cavity speed under shielding gas and graphene film growth pressure is cooled to 10-30 DEG C; take out the non-catalytic substrate of three-dimensional structure, namely its full surface is coated with the graphene film of continuous uniform.
4. the preparation method of three-dimensional non-catalytic base load graphene film structure according to claim 3, it is characterized in that, described non-catalytic substrate is that fusing point stablizes unvaporized inorganic materials lower than the growth temperature of graphene film under graphene film growth temperature condition.
5. the preparation method of three-dimensional non-catalytic base load graphene film structure according to claim 4, it is characterized in that, described non-catalytic substrate is silicon-dioxide, silicon, germanium, gallium arsenide, indium phosphide, silicon nitride, silicon carbide, zinc oxide or aluminum oxide.
6. the preparation method of three-dimensional non-catalytic base load graphene film structure according to claim 3; it is characterized in that; described shielding gas is one or more mixing in nitrogen, hydrogen, argon gas, helium, neon, Krypton and xenon, and described carbon-source gas is one or more mixing in methane, ethene, acetylene, methyl alcohol, ethanol, Benzene and Toluene gas.
7. the preparation method of three-dimensional non-catalytic base load graphene film structure according to claim 3, it is characterized in that, described in steps A, cleaning way is as follows: the non-catalytic substrate of three-dimensional structure is put successively each ultrasonic cleaning 10-15min in acetone, 95vol% ethanol, water, then dry up with nitrogen.
8. the preparation method of three-dimensional non-catalytic base load graphene film structure according to claim 3, it is characterized in that, the method draining air in temperature control cavity in step B is as follows: temperature control cavity is evacuated to 1-5Pa, then shielding gas is filled to 1atm, repeat the above-mentioned operation vacuumizing, fill shielding gas again, until the air in temperature control cavity drains; Or the air pressure in temperature control cavity is remained on 1atm, and the shielding gas 10-30min passing into large discharge in temperature control cavity rinses, and makes the air in temperature control cavity drain.
9. the preparation method of three-dimensional non-catalytic base load graphene film structure according to claim 3, it is characterized in that, described plasma enhancing source is radio frequency plasma body source.
10. the preparation method of three-dimensional non-catalytic base load graphene film structure according to claim 9, it is characterized in that, RF plasma power is 10-100W.
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| CN109019573A (en) * | 2018-09-04 | 2018-12-18 | 山西大学 | A kind of preparation method of the three-dimensional grapheme of controlled distribution |
| CN109887768A (en) * | 2019-04-04 | 2019-06-14 | 西安交通大学 | A kind of roll-to-roll manufacturing method of upright graphene |
| CN109850908A (en) * | 2019-04-12 | 2019-06-07 | 中国科学院重庆绿色智能技术研究院 | A kind of preparation method and product of silica/graphene complex |
| CN109850908B (en) * | 2019-04-12 | 2020-01-14 | 中国科学院重庆绿色智能技术研究院 | Preparation method and product of silicon dioxide/graphene compound |
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