CN108975320A - A kind of graphene film and preparation method thereof - Google Patents
A kind of graphene film and preparation method thereof Download PDFInfo
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- CN108975320A CN108975320A CN201811143776.3A CN201811143776A CN108975320A CN 108975320 A CN108975320 A CN 108975320A CN 201811143776 A CN201811143776 A CN 201811143776A CN 108975320 A CN108975320 A CN 108975320A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/26—Mechanical properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
Abstract
Type of the present invention discloses a kind of graphene, it is shape in curved surface and the high-quality graphene film for being wrapped in foam nickel surface.Also disclose a kind of preparation method of graphene film, it include: that nickel foam is put into tube furnace, graphene is prepared by CVD method in the atmosphere of argon hydrogen mixture, wherein hydrogen accounts for 10% in argon hydrogen mixture, mixed gas flow is 400sccm in entire reaction process, it uses ethyl alcohol as carbon source, is reacted 10 minutes in 1000 DEG C of environment.Present invention ethyl alcohol prepares graphene as carbon source, using CVD method, and raw material is easy to get, and cost is relatively low, and the reaction time is short, and operating process is simple and easy to control, and graphene film obtained has excellent purity, preferable mechanical performance and higher flexible and electric conductivity.
Description
Technical field
The present invention relates to a kind of graphene films and preparation method thereof.
Background technique
Graphene has always been considered as the structure of assuming that property, can not individually be stabilized, until 2004, Britain Man Chesi
Especially big physicist An Deliehaimu and Constantine's Nuo Woxiao love, are successfully isolated from graphite in an experiment
Graphene, and confirm that it can be with individualism, two people also obtain because of " in the initiative experiment of two-dimensional graphene material " jointly
Nobel Prize in physics in 2010.
The scientific circles that appear in of graphene have evoked huge great waves, and correlative study paper is sharply increased, received as formation
The new potentiality material in " the rear silicon epoch " of rice size transistor and circuit, it is intended to using graphene research and development also in the world
It sharply increases, the U.S., South Korea, the research of the country such as China is especially active.Graphene will become achievable high speed transistor, height
The core material of a variety of devices of new generation such as sensor, laser, touch panel, battery and high performance solar batteries
Material.
Up to now, it has been found that graphene have outstanding physics and electrical properties, as high-specific surface area, high conductivity,
High mechanical strength, be easy to modify etc..Graphene is zero gap semiconductor, there is unique carrier properties, is Relativistic Mechanics
The research of phenomenon provides an important channel；The resistance very little that electronics transmits in graphene, when sub-micron distance is mobile
It does not scatter, there is good electronic transport property；Graphene good toughness has experiment to show to hold in their every 100nm distances
The maximum pressure received is best one of the material of the mechanical property that finds so far up to 2.9 N.
The distinctive band structure of graphene is separated from each other hole and electronics, results in the generation of new electronics conduction phenomenon,
Such as quantum Interference, irregular quantum hall effect.Novoselov etc. observes that graphene is imitated with room-temperature quantum Hall
It answers, original temperature range is made to expand 10 times.
Summary of the invention
The technical problems to be solved by the present invention are: providing a kind of new method to prepare graphene, made from this method
Graphene film has excellent purity, preferable mechanical performance and higher flexible and electric conductivity, the preparation method step letter
It is single, it is of less demanding to experiment condition.
In order to solve the above-mentioned technical problem, the technical scheme is that a kind of do carbon source with ethyl alcohol, by CVD method system
The method of standby graphene.
Further, the graphene of method preparation, it is characterised in that: purity is high, good mechanical property are flexible
And good conductivity.
The present invention provides a kind of preparation methods of graphene, comprising the following steps:
Step S1: nickel foam is cleaned up, and is put into the tube furnace for being connected with argon hydrogen mixture；Step S2: adjustment temperature and
The changing rule of time prepares graphene by CVD method.
Further, the preparation method of the graphene, it is characterised in that: in the step S1, nickel foam be cut into 1cm ×
Nickel foam is put into 10% dilute hydrochloric acid ultrasound 5 minutes, is put into length with hair dryer flash baking, then by nickel foam by the rectangle of 2cm
Degree is about to be then fed into the heating region of tube furnace in the quartz boat of 5cm；Hydrogen in the argon hydrogen mixture led in tube furnace
10% is accounted for, gas flow is 400sccm in the whole process.
Further, the preparation method of the graphene, it is characterised in that: in the step S2, in-furnace temperature is from room temperature
Time used in rising to 800 DEG C be 50 minutes, then from 800 DEG C be increased to 1000 DEG C used in the time be 10 minutes, then lead to ethyl alcohol
Steam 10 minutes, the argon hydrogen mixture of 400sccm is connected in whole process in tube furnace quartz ampoule.
Further, the preparation method of the graphene, it is characterised in that: the logical alcohol vapour process in last 10 minutes is
Gas circuit is transformed, then the ethyl alcohol container for allowing argon hydrogen mixture to be passed through heating is reacted by entering tube furnace after pipeline outflow
Room.
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 mainly uses argon hydrogen mixture, nickel foam and ethyl alcohol, these
Material is 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 on the whole, and there are no pollution to the environment.
Detailed description of the invention
Fig. 1 is the electron scanning micrograph of graphene of the present invention；Fig. 2 is the Raman characterization of graphene 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 observes its pattern by scanning electron microscope, the microscopic appearance observed and the stone in working before
The pattern of black alkene fits like a glove.It can be seen from the graphene electron scanning micrograph of Fig. 1, scale bar of the graphene at 50 μm
It is down in apparent sheet microscopic appearance；The peak 2D and the two graphenes of the peak G of graphene are shown from the Raman characterization figure of Fig. 2
Characteristic peak.
Embodiment two:
The present invention also provides a kind of preparation methods of graphene, comprising the following steps: step S1: nickel foam is cleaned up, and is put
Enter to be connected in the tube furnace of argon hydrogen mixture；Step S2: adjusting the changing rule of temperature and time, prepares stone by CVD method
Black alkene.
Preferably, the preparation method of the graphene, it is characterised in that: in the step S1, nickel foam be cut into 1cm ×
Nickel foam is put into 10% dilute hydrochloric acid ultrasound 5 minutes, is put into length with hair dryer flash baking, then by nickel foam by the rectangle of 2cm
Degree is about to be then fed into the heating region of tube furnace in the quartz boat of 5cm；Hydrogen in the argon hydrogen mixture led in tube furnace
10% is accounted for, gas flow is 400sccm in the whole process.
Preferably, the preparation method of the graphene, it is characterised in that: in the step S2, in-furnace temperature is from room temperature
Time used in rising to 800 DEG C be 50 minutes, then from 800 DEG C be increased to 1000 DEG C used in the time be 10 minutes, then lead to ethyl alcohol
Steam 10 minutes, the argon hydrogen mixture of 400sccm is connected in whole process in tube furnace quartz ampoule.
Preferably, the preparation method of the graphene, it is characterised in that: the logical alcohol vapour process in last 10 minutes is
Gas circuit is transformed, then the ethyl alcohol container for allowing argon hydrogen mixture to be passed through heating is reacted by entering tube furnace after pipeline outflow
Room.
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: prepared by CVD method, the graphene of acquisition has excellent purity, preferably
Mechanical performance and higher flexible and electric conductivity, preparation process it is simple.
2. the preparation of graphene according to claim 1, comprising the following steps:
Step S1: nickel foam is cleaned up, and is put into the tube furnace for being connected with argon hydrogen mixture；
Step S2: adjusting the changing rule of temperature and time, prepares graphene by CVD method.
3. the preparation method of graphene according to claim 2, it is characterised in that: in the step S1, nickel foam is cut into
Nickel foam is put into 10% dilute hydrochloric acid ultrasound 5 minutes, is quickly dried up with hair dryer, then foam by the rectangle of 1cm × 2cm
It is about that quartz boat is sent into the heating region of tube furnace, the argon to circulate in tube furnace in the quartz boat of 5cm that nickel, which is put into length,
Wherein hydrogen accounts for 10% to hydrogen mixed gas, and mixed gas flow is 400sccm in the whole process.
4. the preparation method of graphene according to claim 2, it is characterised in that: in the step S2, in-furnace temperature from
Room temperature rise to 800 DEG C used in the time be 50 minutes, then from 800 DEG C be increased to 1000 DEG C used in the time be 10 minutes, furnace medium temperature
Degree leads to alcohol vapour 10 minutes after reaching 1000 DEG C, is connected with the argon hydrogen mixing of 400sccm in whole process in tube furnace quartz ampoule
Gas.
5. the preparation method of graphene according to claim 4, it is characterised in that: the logical alcohol vapour mistake in last 10 minutes
Journey is that gas circuit is transformed, and is flowed out after allowing argon hydrogen mixture to be passed through the ethyl alcohol container of heating by pipeline, finally enters tube furnace
Reaction chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811143776.3A CN108975320A (en) | 2018-09-29 | 2018-09-29 | A kind of graphene film and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110152705A (en) * | 2019-05-06 | 2019-08-23 | 杭州电子科技大学 | A kind of preparation method of TaON@Ni@graphene ternary heterojunction catalysis material |
| CN111564322A (en) * | 2020-06-10 | 2020-08-21 | 青岛粲耀新材料科技有限责任公司 | Graphene super capacitor for battery |
-
2018
- 2018-09-29 CN CN201811143776.3A patent/CN108975320A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110152705A (en) * | 2019-05-06 | 2019-08-23 | 杭州电子科技大学 | A kind of preparation method of TaON@Ni@graphene ternary heterojunction catalysis material |
| CN110152705B (en) * | 2019-05-06 | 2021-11-23 | 杭州电子科技大学 | Preparation method of TaON @ Ni @ graphene ternary heterojunction photocatalytic material |
| CN111564322A (en) * | 2020-06-10 | 2020-08-21 | 青岛粲耀新材料科技有限责任公司 | Graphene super capacitor for battery |
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Application publication date: 20181211 |
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| WD01 | Invention patent application deemed withdrawn after publication |