CN107619042A - A kind of extensive method for preparing graphene nano wall - Google Patents
A kind of extensive method for preparing graphene nano wall Download PDFInfo
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- CN107619042A CN107619042A CN201710927169.5A CN201710927169A CN107619042A CN 107619042 A CN107619042 A CN 107619042A CN 201710927169 A CN201710927169 A CN 201710927169A CN 107619042 A CN107619042 A CN 107619042A
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Abstract
A kind of extensive preparation method for preparing graphene nano wall, according to the following steps：（1）Flowed into reacting gas in the quartz ampoule heating zone of end and put the quartz boat equipped with nickel foam and ferrocene, and the stainless steel substrates or the quartz boat of steel wire that are placed with cleaning and dry are placed in reacting gas outflow end quartz ampoule heating zone；（2）Under normal pressure, 1000 ~ 1200 DEG C are warming up under inert gas shielding, maintains inert gas atmosphere, then is passed through volume ratio as 1:6~2:3 hydrogen and carbon-source gas, react 1 minute ~ 3 hours；（3）Turn off carbon-source gas and hydrogen, reacting furnace is down to room temperature under inert gas atmosphere；The present invention has larger surface-to-volume ratio, sharp outer rim, thin layer of transparent and abundant surface defect；Preparation technology is simple, and cost is low, and control process is controllable, has the advantages of easier compared to synthetic methods such as PECVD, can mass produce graphene nano wall.
Description
Technical field
The invention belongs to field of functional materials, is related to graphene nano wall and preparation method thereof.
Background technology
1997, pass through direct current in the presence of thin hydrogen（DC）Sent out in arc discharge evaporation graphite manufacture CNT
The graphene nano wall that existing surface combines.Graphene nano wall is as a kind of new two-dimentional carbon nanomaterial, with conventional levels
Oriented graphite is compared, and people are shown to unique orientation, exposed sharp edge, non-stacking form and huge surface
The graphene nano wall of product and the vertical arrangement of volume ratio feature（English full name Vertical Aligned
Graphenenanowalls, hereinafter referred to as VG）The great interest applied.Up to the present, VG and its derivative is emerging
Application mainly include field emission device, the nano level corona discharge of air, gas sensor and biology sensor, super capacitor
Device, lithium ion battery, fuel cell（Catalyst is supported）, and electrochemical sensor.The method of synthesizing graphite alkene nm wall at present
Mainly there is microwave plasma enhanced chemical vapour deposition technique（English full name Plasma Enhanced Chemical Vapor
Deposition, hereinafter referred to as PECVD）Method, heat wire method.PECVD synthesis can obtain the graphene of non-agglomerated Formregelung growth
Nm wall;.Held high however, it has including the difficult control of the factors such as low-yield, relatively low growth rate, electric field and magnetic field, instrument
Expensive, the shortcomings of preparation condition is complicated.And it is rarely reported and is received using traditional chemical vapour deposition technique directly to synthesize graphene
Rice wall.Because chemical vapour deposition technique simple process, raw material are cheap, and the advantages that growth conditions is easily-controllable, it is following extensive
Metaplasia production graphene nano wall will be very potential.
The content of the invention
It is an object of the invention to provide a kind of extensive method for preparing graphene nano wall, this method is easy to operate, energy
Consume that low, cost is low, efficiency high, graphene nano wall can be grown directly in the substrate such as stainless steel substrates and silk screen.
The present invention is achieved by the following technical solutions.
The extensive preparation method for preparing graphene nano wall of the present invention, according to the following steps.
（1）Flowed into reacting gas in the quartz ampoule heating zone of end and put the quartz boat equipped with nickel foam and ferrocene, and incite somebody to action
The stainless steel substrates or the quartz boat of steel wire for being placed with cleaning and drying are placed on close to reacting gas outflow end quartz ampoule heating zone
In.
（2）Under normal pressure, 1000 ~ 1200 DEG C are warming up under inert gas shielding, maintains inert gas atmosphere, then be passed through body
Product ratio is 1:6~2:3 hydrogen and carbon-source gas, react 1 minute ~ 3 hours.
（3）Turn off carbon-source gas and hydrogen, reacting furnace is down to room temperature under inert gas atmosphere.
Described inert gas is argon gas or nitrogen, and prioritizing selection argon gas, gas flow is 10 ~ 40sccm.Carbon source gas
Body is hydrocarbon, and such as methane, acetylene, gas flow is 80 ~ 180sccm.
Step of the present invention（1）Described in stainless steel substrates or silk screen surface clean, be respectively placed in acetone, 95% ethanol,
Each ultrasonic 3 ~ 60min of deionized water, is then dried up with nitrogen.Purpose is organic matter of stainless steel wire net surface for removing purchase etc.
Impurity.
The present invention has following beneficial effect.
（1）Graphene nano wall prepared by the present invention be it is a kind of perpendicular to the two-dimentional carbon nano-structured of substrate, it have compared with
Big surface-to-volume ratio, sharp outer rim, thin layer of transparent and abundant surface defect.
（2）Preparation technology of the present invention is simple, and cost is low, can large-scale production.
（3）The present invention can control various growth parameter(s)s such as growth time, carbon-source gas flow etc. to realize various length
With the growth of the graphene nano wall of various density.
（4）Present invention firstly discloses chemical vapour deposition technique next life long graphene nm wall is used, it can be people
The growth mechanism for being better understood from graphene nano wall provides window.There is the advantages of easier compared to synthetic methods such as PECVD,
Graphene nano wall can be mass produced.
Brief description of the drawings
Fig. 1 is the experimental provision structural representation for preparing graphene nano wall.
Fig. 2 is that embodiment 1 prepares the scanning electron microscope (SEM) photograph that graphene nano wall multiplication factor is 5000 times.
Fig. 3 is that embodiment 2 prepares the scanning electron microscope (SEM) photograph that graphene nano wall multiplication factor is 24000 times.
Fig. 4, it is that embodiment 3 prepares the scanning electron microscope (SEM) photograph that graphene nano wall multiplication factor is 12000 times.
Fig. 5 is that embodiment 3 prepares the scanning electron microscope (SEM) photograph that graphene nano wall multiplication factor is 3000 times.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiment of the present invention is described in detail.
Method described in example below, it is conventional method unless otherwise specified；The material agents, such as without special
Illustrate, commercially obtain.
Embodiment 1.
With comprising the following steps that for thermal chemical vapor deposition method growth graphene nano wall：
A, the substrate for growing graphene nano wall is respectively placed in acetone, 95% ethanol, deionized water each ultrasonic 3min, Ran Houyong
Nitrogen dries up；
B, the stainless steel cloth in step a is respectively placed in 3 quartz boats.Wherein close to the stone at gas outflow heating furnace end
Ying Zhou is put into nickel foam 0.02g, and latter two quartz boat is respectively put into carbon paper.Be placed with addition catalyst 0.05g ferrocene and
The quartz boat of 0.025g nickel foam is placed in reacting gas and most begun to flow into quartz ampoule heating zone.
C, at ambient pressure, it is passed through 30sccm argon gas and furnace temperature is risen to 1100 DEG C with 27 DEG C/min heating rate, by argon
Controlled atmosphere introduces methane 90sccm hydrogen 30sccm to 15sccm.The quartz boat equipped with catalyst is moved to make it into stove,
5min is reacted under the conditions of this.After completion of the reaction, move the quartz boat equipped with catalyst and add so that flowing into stove exposed to reacting gas
Outside hot part, turn off methane and hydrogen and argon gas is adjusted to 30sccm and be down to room temperature.The SEM figures of the graphene nano wall of gained
As shown in Figure 2.
Embodiment 2.
Different from embodiment 1, quartz ampoule is wiped to drying regime with the cotton for speckling with ethanol.Then according to embodiment
Related condition is reacted in 1, can also obtain graphene nano wall, but only local distribution has.The graphene nano of gained
Wall SEM figures are as shown in Figure 3.
Embodiment 3.
Different from embodiment 1, separately the same terms with embodiment 1 are reacted, and can also obtain graphene nano wall,
But grow simultaneously containing the impurity such as carbon fiber, gained SEM figures such as Fig. 4, shown in Fig. 5.
Claims (3)
- A kind of 1. extensive preparation method for preparing graphene nano wall, it is characterized in that according to the following steps：（1）Flowed into reacting gas in the quartz ampoule heating zone of end and put the quartz boat equipped with nickel foam and ferrocene, and will be placed with Cleaning and the stainless steel substrates or the quartz boat of steel wire dried are placed in reacting gas outflow end quartz ampoule heating zone；（2）Under normal pressure, 1000 ~ 1200 DEG C are warming up under inert gas shielding, maintains inert gas atmosphere, then be passed through volume ratio Example is 1:6~2:3 hydrogen and carbon-source gas, react 1 minute ~ 3 hours；（3）Turn off carbon-source gas and hydrogen, reacting furnace is down to room temperature under inert gas atmosphere；Described inert gas is argon gas or nitrogen, and gas flow is 10 ~ 40sccm；Carbon-source gas are hydrocarbon, and gas flow is 80~180sccm。
- A kind of 2. extensive preparation method for preparing graphene nano wall according to claim 1, it is characterized in that described Carbon-source gas are methane, acetylene.
- A kind of 3. extensive preparation method for preparing graphene nano wall according to claim 1, it is characterized in that step（1） Described in stainless steel substrates or the surface clean of silk screen be：Be respectively placed in acetone, 95% ethanol, deionized water each ultrasonic 3 ~ 60min, then dried up with nitrogen.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113173578A (en) * | 2021-04-14 | 2021-07-27 | 南昌大学 | Nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial and preparation method thereof |
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| JP2015118348A (en) * | 2013-12-20 | 2015-06-25 | 株式会社Ihi | Saturable absorbing element, saturable absorbing element producing method, and laser apparatus |
| KR20150116570A (en) * | 2014-04-08 | 2015-10-16 | 경남대학교 산학협력단 | Method for growing graphene nanowall by using an electric field control techniques of a plasma chemical vapor deposition process |
| CN105129786A (en) * | 2015-08-31 | 2015-12-09 | 南昌大学 | Preparing method for massive single-layer graphene |
| CN105590703A (en) * | 2016-03-10 | 2016-05-18 | 中国科学院重庆绿色智能技术研究院 | Preparation method of graphical three-dimensional graphene/polyurethane flexible conductive film |
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| CN106495136A (en) * | 2016-09-27 | 2017-03-15 | 南昌大学 | A kind of preparation method of circular graphitic alkene |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103718347A (en) * | 2012-06-13 | 2014-04-09 | 株式会社三五 | Negative electrode for lithium secondary batteries and method for producing same |
| JP2015118348A (en) * | 2013-12-20 | 2015-06-25 | 株式会社Ihi | Saturable absorbing element, saturable absorbing element producing method, and laser apparatus |
| KR20150116570A (en) * | 2014-04-08 | 2015-10-16 | 경남대학교 산학협력단 | Method for growing graphene nanowall by using an electric field control techniques of a plasma chemical vapor deposition process |
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| CN106206268A (en) * | 2016-07-22 | 2016-12-07 | 中国科学院重庆绿色智能技术研究院 | Utilize the method that laser ablation three-dimensional grapheme nm wall is patterned |
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| CN113173578A (en) * | 2021-04-14 | 2021-07-27 | 南昌大学 | Nitrogen-doped three-dimensional carbon nanotube/graphene carbon nanomaterial and preparation method thereof |
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Application publication date: 20180123 |