CN107161987B - The preparation method of powder graphene - Google Patents
The preparation method of powder graphene Download PDFInfo
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- CN107161987B CN107161987B CN201710560855.3A CN201710560855A CN107161987B CN 107161987 B CN107161987 B CN 107161987B CN 201710560855 A CN201710560855 A CN 201710560855A CN 107161987 B CN107161987 B CN 107161987B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
A kind of preparation method of powder graphene, it is characterised in that include the following steps: S1: initiator and substrate, which are placed in, to be generated in the device of microwave, and the substrate is placed on the initiator；S2: inert gas formation protective atmosphere is passed through to described can generate in the device of microwave；And S3: introducing carbon source to described can generate in the device of microwave, the device that can generate microwave generates microwave to generate the powder graphene.The quick preparation of graphene may be implemented in powder graphene preparation method of the invention, and the graphene quality produced is high, is easy to scale.
Description
Technical field
The present invention relates to the preparation technical fields of graphene, and in particular to the preparation method of microwave growth powder graphene.
Background technique
Graphene have excellent property, possess huge specific surface area, high Young's modulus and electron mobility with
And highest thermal conductivity etc..These excellent properties make graphene have broad application prospects.Growth graphene at present
Main stream approach have method from top to bottom and from bottom to top method.Method for growing graphene from bottom to top, such as chemical gaseous phase
Sedimentation (CVD), but CVD method needs harsh growth conditions, such as high temperature and high vacuum, and metallic catalyst is needed to urge
Metaplasia is long, and needs to consume more energy during the growth process, and furthermore the speed of growth is slower, and production cost is caused greatly to mention
Height significantly limits the application field of this kind of graphene.Top-to-bottom method, such as liquid phase stripping method, from natural graphite
It sets out, powder graphene is prepared by the method for removing, but such methods generally require the processing by oxidizing species,
More defect can be introduced to the graphene of preparation.And generally to pass through solution phase, it is more to will cause powder graphene surface
Pollutant retains.
In order to realize the business application of graphene, how inexpensive, extensive, quick preparation high-quality powder graphene is extremely
It closes important.However up to the present, this is still a great challenge.
Summary of the invention
In order to overcome drawbacks described above, the object of the present invention is to provide a kind of preparation methods of powder graphene.
A kind of preparation method of powder graphene, include the following steps: S1: initiator and substrate, which are placed in, to be generated
In the device of microwave；S2: inert gas formation protective atmosphere is passed through to described can generate in the device of microwave；And S3: to
Described can generate introduces carbon source in the device of microwave, the device that can generate microwave generates microwave to generate the powder
Body graphene.
According to an embodiment of the present invention, the device that can generate microwave is micro-wave oven.
Another embodiment according to the present invention, the initiator are conductor or semiconductor.
Another embodiment according to the present invention further includes being placed in substrate described to generate microwave in S1 step
Device in, the substrate is any high-temperature stable, the substance that can be used as substrate.
Another embodiment according to the present invention, the substrate are oxide layer silicon base, metallic substrates, substrate of glass, cloud
Female substrate, sodium chloride substrate or molecular screen base bottom.
Another embodiment according to the present invention, the inert gas are argon gas, Krypton or xenon.
Another embodiment according to the present invention, the carbon source is hydrocarbon, alcohol, ether, ketone, one or more in phenol.
Another embodiment according to the present invention, the carbon source are gaseous carbon source, liquid carbon source or solid-state carbon source.
Another embodiment according to the present invention, after the liquid carbon source is by the bubbling inert gas or its volatilization
It can be generated in the device of microwave described in being introduced into.
Another embodiment according to the present invention, the solid-state carbon source be placed directly within can generate in the device of microwave or
It can be generated in the device of microwave described in being introduced into after volatilizing.
Another embodiment according to the present invention introduces the inert gas with constant flow rate, pulsed introduces the carbon
Source, or the carbon source, the pulsed introducing inert gas are introduced with constant flow rate.
The quick preparation of graphene, and the graphene produced may be implemented in powder graphene preparation method of the invention
Quality is high, is easy to scale.
Further, the device that preparation method of the invention uses is relatively simple and cheap, can be by micro- to household
Wave furnace carry out simple transformation can fast-growth graphene, the cheap large-scale production of graphene may be implemented.
Further, preparation method graphene fast speed of the invention, may be implemented the fast-growth of graphene.
Further, preparation method graphene of the invention can grow graphene in any substrate, and repeatability is higher
And growth is not limited by area, can theoretically grow very big area, and graphene can be carried out in any substrate
Growth.
Detailed description of the invention
Its example embodiment is described in detail by referring to accompanying drawing, above and other feature of the invention and advantage will become
It is more obvious.
Fig. 1 is the schematic diagram for the micro-wave oven that the present invention designs；
Fig. 2A is the TEM of the graphene of embodiment 1；
Fig. 2 B is the SAED figure of the graphene of embodiment 1；
Fig. 3 is the SEM figure of the graphene of embodiment 1；
Fig. 4 is the SEM figure of the graphene of embodiment 2；
Fig. 5 is the SEM figure of the graphene of embodiment 3；
Fig. 6 is the SEM figure of the graphene of embodiment 4；
Fig. 7 is the SEM figure of the graphene of embodiment 5；
Fig. 8 is the Raman figure of the graphene of embodiment 1；
Fig. 9 is the Raman figure of the graphene of embodiment 2；
Figure 10 is the Raman figure of the graphene of embodiment 3；
Figure 11 is the Raman figure of the graphene of embodiment 4；
Figure 12 is the Raman figure of the graphene of embodiment 5；And
Figure 13 is the Raman figure of the graphene of embodiment 6.
Specific embodiment
It elaborates With reference to embodiment to the present invention.
The present invention prepares powder graphene using microwave, includes the following steps: S1: initiator and substrate are placed in can
In the device for generating microwave；S2: inert gas formation protective atmosphere is passed through to that can generate in the device of microwave；And S3: to
It can generate and introduce carbon source in the device of microwave, the device that can generate microwave generates microwave to generate powder graphene.
The device that microwave can be generated is used to generate microwave, and under the action of microwave, charge can be accumulated on initiator, realizes
Point discharge can make its rapid cleavage at carbon fragment, carbon fragment is nucleated and grows in atmosphere later when carbon source passes through
Obtain powder graphene.
The device that microwave can be generated can be any device that can generate microwave, such as can be household microwave oven.
Initiator can be conductor or semiconductor.Such as it can be silicon wafer or copper sheet.
It can also include that substrate is placed in and can be generated in the device of microwave in S1 step, the effect of substrate is for holding
It practices midwifery raw graphene.Substance that substrate can be any high-temperature stable, can be used as substrate.Such as substrate is oxide layer silicon
Substrate, metallic substrates, substrate of glass, mica substrate, sodium chloride substrate or molecular screen base bottom.
Into the device that can generate microwave by inert gas, inertia growing environment is provided with the growth for graphene.
Inert gas is can to generate gas, such as argon gas, Krypton, xenon of plasma etc. under microwave condition.
Carbon source can be hydrocarbon, alcohol, ether, ketone, one or more in phenol.Carbon source can be gaseous carbon source, liquid carbon source or
Solid-state carbon source.Gaseous carbon source can be methane, ethane, propane, butane, pentane, isopentane, neopentane, ethylene, propylene, 1-
Butylene, 2- butylene, acetylene, propine, 1- butine, one of methyl ether or a variety of.Liquid carbon source can be n-hexane, 2- methylpent
Alkane, 3- methylpentane, 2,2- dimethylbutanes, 2,3- dimethylbutanes, normal heptane, 2,2- dimethyl pentanes, 2,3- dimethyl
Pentane, 3- methyl hexane, 2,4- dimethyl pentanes, 3,3- dimethyl pentanes, 2,2,3- triptanes, 2- methyl hexane, 3-
Ethylpentane, normal octane, 2,2,3,3- 4-methyl-butanes, 2- methyl heptane, 2,3,3- trimethylpentanes, 2,3- dimethyl oneself
Alkane, 2,5- dimethylhexanes, 4- methyl heptane, 2,2,3- trimethylpentanes, 3- methyl heptane, 3,4- dimethylhexanes, 2,4-
Dimethylhexane, 2- methyl -3- ethylpentane, 2,2,4- trimethylpentanes, 3,3- dimethylhexanes, 3- ethyl hexane, 2,3,
4- trimethylpentane, 3- methyl -3- ethylpentane, 2,2- dimethylhexanes, nonane, 2- methyloctane, 3- methyloctane, 4- first
Base octane, 2,2- dimethyl heptanes, 2,3- dimethyl heptanes, 2,4- dimethyl heptanes, 2,5- dimethyl heptanes, 2,6- dimethyl
Heptane, 3,3- dimethyl heptanes, 3,4- dimethyl heptanes, 3,5- dimethyl heptanes, 4,4- dimethyl heptanes, 3- second dimethyl-g
Alkane, 4- second dimethyl heptane, 2,2,3- trimethyl cyclohexanes, 2,2,4- trimethyl cyclohexanes, 2,2,5- trimethyl cyclohexanes, 2,3,
3- trimethyl cyclohexane, 2,3,4- trimethyl cyclohexanes, 2,3,5- trimethyl cyclohexanes, 2,4,4- trimethyl cyclohexanes, 3,3,4- tri-
The own heptane of methyl, 2- methyl -3- ethyl hexane, 2- methyl -4- ethyl hexane, 3- methyl -3- ethyl hexane, 3-
Methyl -4- ethyl hexane, 2,2,3,3- tetramethylpentanes, 2,2,3,4- tetramethylpentanes, 2,2,4,4- tetramethyls penta
Alkane, 2,3,3,4- tetramethylpentanes, 2,2- dimethyl -3- ethylpentanes, 2,3- dimethyl -3- ethylpentanes, 2,
4- dimethyl -3- ethylpentane, 3,3- diethylpentanes, ethyl alcohol, propyl alcohol, n-butyl alcohol, 2- butine, benzene, toluene, ethylbenzene,
Propyl benzene, at least one of ether or a variety of.Solid-state carbon source can be benzoic acid, pyrene and its derivative, and at least one in phenol
Kind.
Liquid carbon source can be introduced by the bubbling inert gas, or volatilized gas introducing can generate it is micro-
In the device of wave, it is also possible to directly cross in the device for generating microwave.The gas that solid-state carbon source can be volatilized introduces energy
In the device for enough generating microwave, it is also possible to directly cross in the device for generating microwave.
During the preparation process, inert gas and carbon source ratio are any.Inert gas and the incorporation way of carbon source can be perseverance
Constant current speed introduces, and is also possible to introduce inert gas, pulsed introducing carbon source with constant flow rate, or introduce carbon with constant flow rate
Source, pulsed introduce inert gas.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1
Selecting household microwave oven 1 is the device that can generate microwave, and household microwave oven 1 is the board micro-wave oven (electricity of commercially available beauty
Source frequency is 50Hz, microwave frequency 2450Hz, and voltage rating is AC 220V, input power 1150W, and microwave power is
700W, microwave generator inside ceiling voltage is 4200V).The circle that diameter is 5cm is respectively opened at the both ends that household microwave oven 1 opposes
Hole, the above diameter that welds each later is 5cm, the stainless steel hollow cylinder 2 of a length of 10cm, the quartz ampoule 3 for being 2.54cm by diameter
Across two sections of stainless steel hollow cylinders 2, the interlude of quartz ampoule 3 is in microwave cavity, and specific structure is as shown in Figure 1.
It will be placed on the 300nm oxide layer silicon wafer of a piece of 1.5cm × 4cm as initiator a piece of as substrate
The 300nm oxide layer silicon wafer of 0.8cm × 0.8cm, initiator and substrate are placed to quartz ampoule 3 be located in microwave cavity later
In interlude.Then, argon gas 5min is passed through to quartz ampoule 3 to exclude air in quartz ampoule 3 with the flow velocity of 300sccm, later will
Micro-wave oven is adjusted to top grade, opens micro-wave oven, can promptly appreciate that generate bright electric discharge phenomena in micro-wave oven at this time.At this time with
The flow velocity of 50sccm is passed through 50sccm methane to quartz ampoule 3.It can be received with filter paper, mesh, porous cotton etc. in the tail end of quartz ampoule 3
Collect graphene, or directly tail gas is passed through in liquid and collects graphene.
8min is continued with 30sccm flow velocity in the present embodiment, 2mg graphene powder has finally been prepared, i.e., has often led in system
2mg graphene can be prepared by entering 126mg carbon.
Embodiment 2
In addition to substrate is simple glass, other conditions are same as Example 1.
Embodiment 3
In addition to substrate is mica, other conditions are same as Example 1.
Embodiment 4
In addition to substrate is salt (NaCl), other conditions are same as Example 1.
Embodiment 5
Using the identical micro-wave oven of embodiment 1.By the 300nm oxide layer silicon wafer of a piece of 1.5cm × 4cm as initiator
The upper 300nm oxide layer silicon wafer for placing a piece of 0.8cm × 0.8cm as substrate, later places initiator and substrate to stone
English pipe 3 is located in the interlude in microwave cavity.Then, argon gas 5min is passed through to quartz ampoule 3 to exclude with the flow velocity of 300sccm
Micro-wave oven is adjusted to top grade later by air in quartz ampoule 3, opens micro-wave oven, can be promptly appreciated that generate in micro-wave oven at this time and be become clear
Electric discharge phenomena.It is bubbled at this time with the Ar gas of 100sccm flow velocity into Ethanol tank by Bubbling method and takes ethyl alcohol out of.In quartz ampoule 3
Tail end can collect graphene with filter paper, mesh, porous cotton etc., or directly tail gas is passed through in liquid and collects graphene.
Embodiment 6
Using the identical micro-wave oven of embodiment 1.By the 300nm oxide layer silicon wafer of a piece of 1.5cm × 4cm as initiator
Placement is located in the interlude in microwave cavity to quartz ampoule 3.And will about 10mg pyrene as air-flow upstream distance microwave furnace among
In the quartz ampoule 3 of about 10cm.Then, to be passed through argon gas 5min to quartz ampoule 3 with the flow velocity of 300sccm hollow to exclude quartz ampoule 3
Micro-wave oven is adjusted to top grade later by gas, is opened micro-wave oven, can be promptly appreciated that generate bright electric discharge phenomena in micro-wave oven at this time.
Graphene can be collected with filter paper, mesh, porous cotton etc. in the tail end of quartz ampoule 3, or directly tail gas is passed through in liquid and is received
Collect graphene.
TEM and the SAED figure of the graphene of embodiment 1 is shown respectively in Fig. 2A and Fig. 2 B.By the object of visible preparation in TEM figure
Matter is lamellar structure, and size is in 100nm or so, and the number of plies is 3-15 layers.SAED figure is it can be seen that the substance of preparation is graphite
Alkene.
Fig. 3, which is shown, to be schemed using 300nm oxide layer silicon wafer as substrate, using methane for the SEM of the graphene of carbon source for growth.By this
Figure is it can be seen that dendritic intersection construction is presented in graphene.
Fig. 4, Fig. 5, Fig. 6 be shown respectively using glass, mica and salt be as substrate, using methane carbon source preparation graphite
The SEM of alkene schemes.It can be seen that dendritic intersection construction is presented in graphene.
Fig. 7 show using 300nm oxide layer silicon wafer be as substrate, using ethyl alcohol carbon source preparation graphene SEM figure.By this
Figure is it can be seen that dendritic intersection construction is presented in graphene.
Fig. 8, which is shown, to be schemed using 300nm oxide layer silicon wafer as substrate, using methane for the Raman of the graphene of carbon source for growth.By
The figure can be seen that graphene quality is higher.
Fig. 9, Figure 10, Figure 11 be shown respectively using glass, mica and salt be as substrate, using methane carbon source preparation stone
The Raman of black alkene schemes.Have in figure it can be seen that graphene quality is higher.
Figure 12 show using 300nm oxide layer silicon wafer be as substrate, using ethyl alcohol carbon source preparation graphene Raman figure.
It can be seen that the substance of preparation is graphene and quality is higher by the figure.
Figure 13 is shown to be schemed using the Raman for the graphene that pyrene is carbon source preparation.The sample, which is derived from, has grown 3 wall of rear quartz ampoule
Object is scraped, can be seen that the substance of preparation is graphene and quality is higher by the figure.
Carbon source is placed in except the device that can generate microwave in embodiment 1-6, and can be generated by quartz ampoule introducing
In the device of microwave, it will be appreciated by those skilled in the art that microwave can also be generated for carbon source introducing otherwise
In device.It is also possible to that directly carbon source is placed directly within and can be generated in the device of microwave, the gaseous state in preparation process in device
Carbon source rapid cleavage is at carbon fragment, and carbon fragment is nucleated in atmosphere and grows to obtain powder graphene later
Inert gas and carbon source are introduced with constant flow rate in embodiment 1-6, but invention is not limited thereto.Inert gas
It can also be other any suitable modes, such as inert gas with constant rate of speed introducing, carbon source arteries and veins with the incorporation way of carbon source
Rush formula introducing；Or carbon source is introduced with constant rate of speed, inert purge gas pulses formula introduces.
Certainly, the present invention can also have other various embodiments, without deviating from the spirit and substance of the present invention, ripe
It knows those skilled in the art and makes various corresponding changes and modifications, but these corresponding changes and change in accordance with the present invention
Shape all should fall within the scope of protection of the appended claims of the present invention.
Claims (9)
1. a kind of preparation method of powder graphene, it is characterised in that include the following steps:
S1: initiator and substrate, which are placed in, to be generated in the device of microwave；
S2: inert gas formation protective atmosphere is passed through to described can generate in the device of microwave；And
S3: introducing carbon source to described can generate in the device of microwave, the device that can generate microwave generates microwave, realizes
Point discharge is to generate the powder graphene；
Wherein, the initiator is conductor or semiconductor.
2. preparation method according to claim 1, which is characterized in that the device that can generate microwave is micro-wave oven.
3. preparation method according to claim 1, which is characterized in that in S1 step further include substrate is placed in it is described
It can generate in the device of microwave, the substrate is oxide layer silicon base, metallic substrates, substrate of glass, mica substrate, sodium chloride
Substrate or molecular screen base bottom.
4. preparation method according to claim 1, which is characterized in that the inert gas is argon gas, Krypton or xenon.
5. preparation method according to claim 1, which is characterized in that the carbon source be hydrocarbon, alcohol, ether, ketone, it is a kind of in phenol or
It is a variety of.
6. preparation method according to claim 1, which is characterized in that the carbon source be gaseous carbon source, liquid carbon source or
Solid-state carbon source.
7. preparation method according to claim 6, which is characterized in that the liquid carbon source passes through the bubbling inert gas
Or it can be generated in the device of microwave described in being introduced into after its volatilization.
8. preparation method according to claim 6, which is characterized in that the solid-state carbon source, which is placed directly within, can generate microwave
Device in or its volatilization after be introduced into described in can generate in the device of microwave.
9. preparation method according to claim 1, which is characterized in that introduce the inert gas, pulse with constant flow rate
Formula introduces the carbon source, or introduces the carbon source, the pulsed introducing inert gas with constant flow rate.
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| CN107572508A (en) * | 2017-10-12 | 2018-01-12 | 北京大学 | The equipment for producing graphene powder |
| CN110282617B (en) * | 2019-07-26 | 2021-01-29 | 北京石墨烯研究院 | Graphene powder and preparation method thereof |
| CN110451496B (en) * | 2019-09-17 | 2021-04-20 | 北京石墨烯研究院 | Method for preparing powder graphene through continuous release |
| CN110950386B (en) * | 2019-12-09 | 2021-02-09 | 北京大学 | Preparation method of transition metal sulfide nanosheet powder |
| CN112592667A (en) * | 2020-12-14 | 2021-04-02 | 稻兴科技(深圳)有限公司 | Heat-conductive electric appliance insulation foam adhesive tape for high temperature and manufacturing method thereof |
| CN115196621B (en) * | 2021-09-28 | 2023-09-19 | 云南华谱量子材料有限公司 | Method and device for preparing graphene by catalyst-assisted microwave excitation metal discharge |
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| CN103011136A (en) * | 2011-09-23 | 2013-04-03 | 浙江大学 | Method for synthetizing graphene film |
| CN104919077A (en) * | 2013-01-14 | 2015-09-16 | 加州理工学院 | Method and system for graphene formation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103011136A (en) * | 2011-09-23 | 2013-04-03 | 浙江大学 | Method for synthetizing graphene film |
| CN104919077A (en) * | 2013-01-14 | 2015-09-16 | 加州理工学院 | Method and system for graphene formation |
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