CN109850879A - A kind of high-quality graphene film and preparation method thereof - Google Patents
A kind of high-quality graphene film and preparation method thereof Download PDFInfo
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- CN109850879A CN109850879A CN201910283760.0A CN201910283760A CN109850879A CN 109850879 A CN109850879 A CN 109850879A CN 201910283760 A CN201910283760 A CN 201910283760A CN 109850879 A CN109850879 A CN 109850879A
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- graphene
- graphene film
- polystyrene
- copper foil
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Abstract
Type of the present invention discloses a kind of high-quality graphene film and preparation method thereof, and preparation process includes: that (1) using solid granule polystyrene does carbon source；(2) graphene is formed in copper foil substrate surface absorption nucleation in the method system by CVD；(3) copper foil is etched away with corrosive liquid, then transfers graphene to arbitrary SiO again2Single layer large-area graphene is obtained in/Si substrate or substrate of glass.The raw materials used in the present invention is easy to get, and technology maturation, cost is relatively low, and short preparation period, operating process is simple and easy to control, and graphene obtained has excellent purity, preferable mechanical performance, flexibility, electric conductivity.
Description
Technical field
The present invention relates to a kind of high-quality graphene films and preparation method thereof.
Background technique
Two dimensional crystal material generally refers to the material that scale in the two-dimensional direction reaches nano-scale.Early stage scientists
Think, can not find stringent two dimensional crystal material in nature, because it does not have thermodynamic stability.Until 2004,
The method of scientist's first passage mechanical stripping has obtained graphene, just confirms that the graphene of two-dimensional structure can be stablized and deposits
?.Since self-discovery, the excellent properties of the various aspects of graphene just cause the attention of scientists and have started one and grind
Study carefully the upsurge of graphene, Recent study field aspect from material science to electronic device is related to extensively.
Single-layer graphene is by carbon atom sp2Hydridization stacking forms and each carbon atom hydridization forms 3 covalent bonds,
Forming 3 σ keys with closest 3 carbon atoms around respectively, the atom of remaining 1 p electronics and surrounding forms pi bond, this
The film thickness that kind way of stacking is formed is about 0.335 nm.Preparing the common method of graphene in recent years has very much, including machinery
Stripping method, epitaxial growth method, chemical stripping reduction method, chemical vapour deposition technique (CVD) etc..
The principle of chemical vapour deposition technique (CVD) be reactive material under the high temperature conditions, decompose or synthesis gaseous state and solid
It is deposited in body substrate, finally obtains solid material.Graphene is obtained using chemical vapor deposition, the requirement to experimental facilities is compared
Simply, relative low price, the graphene prepared is relatively large sized, and defect is relatively low.And chemistry can be passed through
Method etch away metallic substrates, can transfer graphene on arbitrary target substrate, be conducive to the application of graphene film.
Invention is exactly in this way herein.Carbon source is done with solid granule polystyrene, preparing large area single-layer graphene makes
Preparation cost is cheaper.
Summary of the invention
The technical problems to be solved by the present invention are: being prepared as carbon source by CVD method with solid granule polystyrene
High quality monolayer graphene, the graphene film of acquisition have excellent purity, preferable mechanical performance and it is higher flexible and
Electric conductivity, the preparation method step is simple, of less demanding to experiment condition.
In order to solve the above-mentioned technical problem, the technical scheme is that under normal pressure in tube furnace, existed by CVD method
Graphene film is prepared on substrate copper foil.The graphene film of the method preparation, it is characterised in that: purity is high, mechanicalness
Can be good, flexible and good conductivity.
The present invention provides a kind of preparation methods of graphene film, comprising the following steps: step S1: uses white particles
Presoma of the shape polystyrene as carbon；Step S2: using copper foil as substrate；Step S3: true in single temperature zone open-type by CVD method
It is reacted in empty tube furnace.
Further, the preparation method of the graphene film, it is characterised in that: in the step S1, with tinfoil paper paper bag
Wrap up in the upstream end that the weighing bottle equipped with polystyrene is placed on quartz ampoule, when the temperature of polystyrene reach 330~380 DEG C it
Between when acutely volatilization crack out carbon atom.
Further, the preparation method of the graphene, it is characterised in that: in the step S2, copper foil (it is 25 μm thick, it is pure
The size of degree 99.80%) is the cm of 1 cm × 1, respectively with 50 DEG C of 10% dilute hydrochloric acid, isopropanol, deionized water ultrasounds 15
min。
Further, the preparation method of the graphene, it is characterised in that: in the step S3, tube furnace temperature setting
It is 1000 DEG C, the gas (10% H2/Ar) of 400 sccm, reaction time: 3 min of constant temperature is passed through in reaction process.
After above-mentioned technical proposal, the invention has the following advantages:
1) graphene film prepared by the present invention has excellent purity, preferable mechanical performance and higher flexible and conduction
Property；
2) present invention prepares graphene using CVD method, and raw material are easy to get, and cost is relatively low, and experimentation is simple；
3) preparation method of the invention is simple, does not use harmful chemical agents, there are no pollution to the environment for experiment.
Detailed description of the invention
Fig. 1 is the transmission electron microscope photo of graphene film of the present invention；Fig. 2 is the Raman characterization of graphene film of the invention
Figure.
Specific embodiment
In order that the present invention can be more clearly and readily understood, right below according to specific embodiment and in conjunction with attached drawing
The present invention is described in further detail.
Embodiment one:
A kind of graphene film is the transmission image under damaged graphene film high magnification numbe in Fig. 1, due to diffraction phenomena edge
There is a clearly diffraction fringe in place, it is possible to prove that sample is single-layer graphene film；It is aobvious from the Raman characterization figure of Fig. 2
Show the peak 2D and the peak G of graphene.
Embodiment two:
The present invention provides a kind of preparation methods of graphene film, comprising the following steps: step S1: poly- with white particles shape
Presoma of the styrene as carbon；Step S2: using copper foil as substrate；Step S3: by CVD method in single temperature zone open-type vacuum tube
It is reacted in formula furnace.
Preferably, the preparation method of the graphene film, it is characterised in that: in the step S1, with tinfoil paper paper bag
Wrap up in the upstream end that the weighing bottle equipped with polystyrene is placed on quartz ampoule, when the temperature of polystyrene reach 330~380 DEG C it
Between when acutely volatilization crack out carbon atom.
Preferably, the preparation method of the graphene, it is characterised in that: in the step S2, copper foil (it is 25 μm thick, it is pure
The size of degree 99.80%) is the cm of 1 cm × 1, respectively with 50 DEG C of 10% dilute hydrochloric acid, isopropanol, deionized water ultrasounds 15
min。
Preferably, the preparation method of the graphene, it is characterised in that: in the step S3, tube furnace temperature setting
It is 1000 DEG C, the gas (10% H2/Ar) of 400 sccm, reaction time: 3 min of constant temperature is passed through in reaction process.
The present invention is synthesized using CVD method, graphene film obtained have excellent purity, preferable mechanical performance and
Higher flexible and electric conductivity, the preparation method step is simple, requires experiment condition low.
Particular embodiments described above, pair present invention solves the technical problem that, technical scheme and beneficial effects carry out
It is further described, it should be understood that the above is only a specific embodiment of the present invention, is not limited to this
Invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in this hair
Within bright protection scope.
Claims (5)
1. a kind of graphene film, it is characterised in that: it is prepared by CVD method, the graphene film of acquisition has excellent purity,
Preferable mechanical performance and higher flexible and electric conductivity, preparation process are simple.
2. the preparation of graphene film according to claim 1, comprising the following steps: step S1: using white particles shape
Presoma of the polystyrene as carbon；Step S2: using copper foil as substrate；Step S3: by CVD method in single temperature zone open-type vacuum
It is reacted in tube furnace.
3. the preparation method of graphene film according to claim 2, it is characterised in that: in the step S1, use tinfoil paper
Paper bag wraps up in the upstream end that the weighing bottle equipped with polystyrene is placed on quartz ampoule, when the temperature of polystyrene reaches 330~380
Acutely volatilization cracks out carbon atom when between DEG C.
4. the preparation method of graphene film according to claim 2, it is characterised in that: in the step S2, copper foil is (thick
25 μm, purity 99.80%) size be the cm of 1 cm × 1, respectively with 10% dilute hydrochloric acid, isopropanol, 50 DEG C of deionized water
15 min of ultrasound.
5. the preparation method of graphene fiber according to claim 2, it is characterised in that: in the step S3, tube furnace
Temperature setting is 1000 DEG C, the gas (10% H2/Ar) of 400 sccm is passed through in reaction process, the reaction time: constant temperature 3 divides
Clock.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910283760.0A CN109850879A (en) | 2019-04-10 | 2019-04-10 | A kind of high-quality graphene film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910283760.0A CN109850879A (en) | 2019-04-10 | 2019-04-10 | A kind of high-quality graphene film and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
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| CN109850879A true CN109850879A (en) | 2019-06-07 |
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ID=66903606
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| CN201910283760.0A Pending CN109850879A (en) | 2019-04-10 | 2019-04-10 | A kind of high-quality graphene film and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110282617A (en) * | 2019-07-26 | 2019-09-27 | 北京石墨烯研究院 | A kind of graphene powder and preparation method thereof |
| CN113445030A (en) * | 2020-03-25 | 2021-09-28 | 北京石墨烯研究院 | Method for improving cleanliness of graphene film |
-
2019
- 2019-04-10 CN CN201910283760.0A patent/CN109850879A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110282617A (en) * | 2019-07-26 | 2019-09-27 | 北京石墨烯研究院 | A kind of graphene powder and preparation method thereof |
| CN113445030A (en) * | 2020-03-25 | 2021-09-28 | 北京石墨烯研究院 | Method for improving cleanliness of graphene film |
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| PB01 | Publication | ||
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Application publication date: 20190607 |