CN110734054A - Preparation method of graphene films - Google Patents
Preparation method of graphene films Download PDFInfo
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- CN110734054A CN110734054A CN201911151669.XA CN201911151669A CN110734054A CN 110734054 A CN110734054 A CN 110734054A CN 201911151669 A CN201911151669 A CN 201911151669A CN 110734054 A CN110734054 A CN 110734054A
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- adopting
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- quartz plate
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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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
Abstract
The invention relates to a preparation method of graphene films, which comprises the following operation steps of (1) forming a high-molecular precursor film on the surface of a substrate by adopting a rotary coating method, (2) forming a pre-oxidation thin layer by adopting a pre-oxidation process, and (3) forming the graphene film by adopting a high-temperature carbonization process.
Description
Technical Field
The invention relates to the technical field of graphene films, in particular to a preparation method of graphene films.
Background
The single-layer or multi-layer SP2 atomic-broken structure layer formed by attaching graphene to monocrystalline silicon, all-metal, metal oxide or other substrates has great application prospect in the fields of semiconductors and microelectronics, and the conventional method for preparing the thin-layer graphene controls the gradual and orderly accumulation and generation of carbon atoms on the surface of the substrate, and comprises a surface growth method and a vapor deposition method.
It can be seen that, besides requiring very expensive catalysts, the work-up and purification of the product is rather cumbersome and the defect control of the obtained graphene thin film is not ideal. Meanwhile, the processes and equipment of the methods are very complex, the production cost is high, and the process amplification and mass production are difficult.
Disclosure of Invention
In view of the above problems, the invention provides a brand new way, simplifies the preparation process, reduces the difficulty of amplifying the preparation process, reduces the production cost of the graphene film, and provides a technical basis for the large-scale production of the graphene film.
The preparation method adopts the following technical scheme that the preparation method of graphene films comprises the operation steps of (1) forming a high-molecular precursor film on the surface of a substrate by adopting a rotary coating method, (2) forming a pre-oxidation thin layer by adopting a pre-oxidation process, and (3) forming the graphene film by adopting a high-temperature carbonization process.
Preferably, the specific steps in the step (1) are that a polished quartz plate is used as a substrate, the quartz plate is cleaned by ultrasonic oscillation and dried under the protection of nitrogen atmosphere, a catalyst solution is prepared by ferric nitrate, citric acid, ethanol and water according to a fixed proportion of , a catalyst film is coated on the surface of the quartz plate by using a rotary coating machine, and the thickness and uniformity of the film are controlled by the angular speed of the rotary coating machine and the time length of a high-low rotation speed gear.
Preferably, the pre-oxidation temperature in the step (2) is set to be between 180 ℃ and 400 ℃, the temperature is gradually increased from low to high, and the residence time of the process step is 60-120 min.
Preferably, the high-temperature carbonization temperature in the step (3) is 600-800 ℃.
The invention has the following beneficial effects: the idea of pyrolysis and carbonization of the polymer precursor is adopted, so that the process of continuous accumulation of carbon atoms on the surface of the substrate is avoided, an expensive catalyst is not needed, and the aromatization of the generated graphene film is complete; the preparation method is simple and convenient, has simple process and equipment requirements, is easy to amplify the process, and has low production cost and strong controllability of product quality.
Detailed Description
The following examples may assist those skilled in the art in a more complete understanding of the present invention, but are not intended to limit the invention in any way.
The invention provides technical schemes, in particular to a preparation method of graphene films, which comprises the following operation steps of (1) forming a high-molecular precursor film on the surface of a substrate by adopting a rotary coating method, (2) forming a pre-oxidation thin layer by adopting a pre-oxidation process, (3) forming the graphene film by adopting a high-temperature carbonization process;
the method comprises the specific steps of (1) adopting a polished quartz plate as a substrate, drying the polished quartz plate under the protection of nitrogen atmosphere after ultrasonic oscillation cleaning, preparing a catalyst solution by ferric nitrate, citric acid, ethanol and water according to a fixed proportion of , coating a catalyst film on the surface of the quartz plate by using a rotary coating machine, and controlling the thickness and uniformity of the film by the angular speed of the rotary coating machine and the time length of high and low speed gears;
in the step (2), the pre-oxidation temperature is set to be between 180 ℃ and 400 ℃, the temperature gradually increases from low to high, and the retention time of the process step is 60-120 min;
the high-temperature carbonization temperature in the step (3) is 600-.
The technical solutions provided by the embodiments of the present invention are described in detail above, and the principles and implementations of the embodiments of the present invention are explained in the present disclosure by using specific examples, and the descriptions of the above embodiments are only used to help understand the principles of the embodiments of the present invention, and meanwhile, for those skilled in the art , there may be changes in the specific implementations and implementations of the embodiments of the present invention, and in summary, the content of the present description should not be construed as limiting the present invention.
Claims (4)
- The preparation method of the 1 and graphene films is characterized by comprising the following operation steps:(1) forming a high-molecular precursor film on the surface of the substrate by adopting a rotary coating method;(2) forming a pre-oxidation thin layer by adopting a pre-oxidation process;(3) and forming the graphene film by adopting a high-temperature carbonization process.
- 2. The method for preparing graphene films according to claim 1, wherein the step (1) comprises the steps of polishing a quartz plate as a substrate, cleaning the quartz plate by ultrasonic oscillation, drying the quartz plate under the protection of nitrogen atmosphere, preparing a catalyst solution from ferric nitrate, citric acid, ethanol and water according to a fixed ratio of , coating the surface of the quartz plate with the catalyst film by a spin coating machine, and controlling the thickness and uniformity of the film by the angular speed and the time length of high and low rotational speed gears of the spin coating machine.
- 3. The method as claimed in claim 1, wherein the pre-oxidation temperature in step (2) is set to be between 180 ℃ and 400 ℃, the temperature gradually increases from low to high, and the residence time in the process step is 60-120 min.
- 4. The method for preparing kinds of graphene films as claimed in claim 1, wherein the high temperature carbonization temperature in step (3) is 600-800 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911151669.XA CN110734054A (en) | 2019-11-21 | 2019-11-21 | Preparation method of graphene films |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911151669.XA CN110734054A (en) | 2019-11-21 | 2019-11-21 | Preparation method of graphene films |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110734054A true CN110734054A (en) | 2020-01-31 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911151669.XA Pending CN110734054A (en) | 2019-11-21 | 2019-11-21 | Preparation method of graphene films |
Country Status (1)
| Country | Link |
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| CN (1) | CN110734054A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106082178A (en) * | 2016-06-01 | 2016-11-09 | 华东理工大学 | A kind of method preparing graphene film on insulating body |
| CN107051228A (en) * | 2017-06-02 | 2017-08-18 | 大连理工大学 | A kind of method of the ultra-thin porous graphene seperation film of direct growth |
| CN107285302A (en) * | 2017-08-17 | 2017-10-24 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of graphene |
| CN108358198A (en) * | 2018-03-07 | 2018-08-03 | 中国工程物理研究院化工材料研究所 | Multiple environment response driving graphene oxide film, preparation method and application |
-
2019
- 2019-11-21 CN CN201911151669.XA patent/CN110734054A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106082178A (en) * | 2016-06-01 | 2016-11-09 | 华东理工大学 | A kind of method preparing graphene film on insulating body |
| CN107051228A (en) * | 2017-06-02 | 2017-08-18 | 大连理工大学 | A kind of method of the ultra-thin porous graphene seperation film of direct growth |
| CN107285302A (en) * | 2017-08-17 | 2017-10-24 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of graphene |
| CN108358198A (en) * | 2018-03-07 | 2018-08-03 | 中国工程物理研究院化工材料研究所 | Multiple environment response driving graphene oxide film, preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 王丽民 等: "有机-无机转化法制备石墨烯薄膜带的探索研究", 《材料导报 A：综述篇》 * |
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Application publication date: 20200131 |