CN112723344A - Preparation method of graphene film - Google Patents
Preparation method of graphene film Download PDFInfo
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- CN112723344A CN112723344A CN202011617881.3A CN202011617881A CN112723344A CN 112723344 A CN112723344 A CN 112723344A CN 202011617881 A CN202011617881 A CN 202011617881A CN 112723344 A CN112723344 A CN 112723344A
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- substrate
- graphene film
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- graphite
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 69
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 29
- 239000010439 graphite Substances 0.000 claims abstract description 29
- 238000004140 cleaning Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000011521 glass Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000010923 batch production Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- 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
- C01B2204/04—Specific amount of layers or specific thickness
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of a graphene film, which comprises the following steps: the method comprises the following steps: processing a substrate, namely taking the substrate, dividing the substrate into small substrates with the same size, and laying the small substrates on filter paper; cleaning the small substrate, and drying for later use; step two: preparing a graphite solution, namely crushing graphite into powder, putting the powder into an N-dimethylformamide solution, preparing the graphite solution under the action of ultrasonic waves, and sealing and storing the graphite solution for later use. Step three: preparing, namely taking out the small substrate prepared in the first step, dripping the graphite oxide solution prepared in the second step on the small substrate, and shaking the small substrate in a left-right rotating mode until the small substrate is spread evenly to prepare a sample; putting the sample into a glass vessel for drying, and forming a layer of solid graphene film on the small substrate by using the graphite solution; and separating the graphene film from the small substrate to obtain the graphene film. Compared with the prior art, the invention has the advantages that: the preparation method is simple, the cost is low, and the requirement of mass production can be met.
Description
Technical Field
The invention relates to the technical field of graphene film preparation, in particular to a preparation method of a graphene film.
Background
Graphene is a polymer made of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future. The physicists andrelim and consanguin norworth schloff, manchester university, uk, successfully separated graphene from graphite by micromechanical exfoliation, thus collectively awarding the 2010 nobel prize for physics. The common powder production method of graphene is a mechanical stripping method, an oxidation-reduction method and a SiC epitaxial growth method, and the film production method is chemical gasPhase deposition (CVD).
The graphene is divided into two categories of graphene powder and graphene film, most of researches on the graphene film are preparation technologies, and although the researched preparation technologies achieve some achievements, the existing preparation method of the graphene film is complex in steps and inconvenient to operate, so that the preparation cost is high, and the large-batch production requirements cannot be met.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the technical defects and provide a preparation method of a graphene film, which is simple and low in cost and can meet the requirement of mass production.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a preparation method of a graphene film comprises the following steps:
the method comprises the following steps: treatment of substrates
(1) Taking a substrate, dividing the substrate into small substrates with the same size, and laying the small substrates on filter paper;
(2) the small substrate is cleaned in the following specific cleaning mode: cleaning the surface of a small substrate with cleaning solution, then washing with deionized water, putting the small substrate into prepared ethanol solution after the cleaning is finished, cleaning again by ultrasonic waves, transferring the small substrate into the prepared acetone solution after the cleaning is finished, cleaning with the ultrasonic waves, washing with the deionized water after the cleaning is finished, and drying for later use;
step two: preparation of graphite solution
Pulverizing graphite into powder, adding into N-dimethylformamide solution, preparing into graphite solution under the action of ultrasonic wave, sealing, and storing.
Step three: preparation of
(1) Taking out the small substrate prepared in the first step, dripping the graphite oxide solution prepared in the second step on the small substrate, and shaking the small substrate in a left-right rotating mode until the small substrate is spread evenly to prepare a sample;
(2) putting the sample into a glass vessel for drying, and forming a layer of solid graphene film on the small substrate by using the graphite solution;
(3) and separating the graphene film from the small substrate to obtain the graphene film.
Preferably, in the first step, the substrate is single-sided conductive glass, and is cut into small substrates with the size of 4X4cm by a glass cutter.
Preferably, in the step one, the content of the ethanol solution and the content of the acetone solution are both 20-25ml, and the ultrasonic cleaning time is 10-15 min.
Preferably, the weight ratio of the graphite to the N-dimethylformamide solution in the second step is 1: 3.
preferably, the thickness of the graphene film prepared in the third step is 100-200 nm.
Compared with the prior art, the invention has the advantages that: in the specific preparation process, the substrate is firstly sliced and cleaned, then the existing graphite and solvent are mixed to prepare graphite solution, and finally the graphene film is formed on the substrate.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention discloses a preparation method of a graphene film, which comprises the following steps:
the method comprises the following steps: treatment of substrates
(3) Taking a substrate, dividing the substrate into small substrates with the same size, and laying the small substrates on filter paper;
(4) the small substrate is cleaned in the following specific cleaning mode: cleaning the surface of a small substrate with cleaning solution, then washing with deionized water, putting the small substrate into prepared ethanol solution after the cleaning is finished, cleaning again by ultrasonic waves, transferring the small substrate into the prepared acetone solution after the cleaning is finished, cleaning with the ultrasonic waves, washing with the deionized water after the cleaning is finished, and drying for later use;
step two: preparation of graphite solution
Pulverizing graphite into powder, adding into N-dimethylformamide solution, preparing into graphite solution under the action of ultrasonic wave, sealing, and storing.
Step three: preparation of
(4) Taking out the small substrate prepared in the first step, dripping the graphite oxide solution prepared in the second step on the small substrate, and shaking the small substrate in a left-right rotating mode until the small substrate is spread evenly to prepare a sample;
(5) putting the sample into a glass vessel for drying, and forming a layer of solid graphene film on the small substrate by using the graphite solution;
(6) and separating the graphene film from the small substrate to obtain the graphene film.
In the first step, the substrate is single-sided conductive glass and is cut into small substrates with the size of 4X4cm by a glass cutter.
In the step one, the content of the ethanol solution and the content of the acetone solution are both 20-25ml, and the ultrasonic cleaning time is 10-15 min.
In the second step, the weight ratio of the graphite to the N-dimethylformamide solution is 1: 3.
the thickness of the graphene film prepared in the step three is 100-200 nm.
In the specific preparation process, the substrate is firstly sliced, and different cleaning agents are utilized for carrying out multiple times of cleaning treatment, so that the cleanliness of the substrate is ensured, the graphene film formed on the substrate can be ensured not to contain magazines to be made into high quality, then the existing graphite and solvent are mixed to be made into graphite solution, and finally the graphene film is formed on the substrate.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (5)
1. A preparation method of a graphene film is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: treatment of substrates
(1) Taking a substrate, dividing the substrate into small substrates with the same size, and laying the small substrates on filter paper;
(2) the small substrate is cleaned in the following specific cleaning mode: cleaning the surface of a small substrate with cleaning solution, then washing with deionized water, putting the small substrate into prepared ethanol solution after the cleaning is finished, cleaning again by ultrasonic waves, transferring the small substrate into the prepared acetone solution after the cleaning is finished, cleaning with the ultrasonic waves, washing with the deionized water after the cleaning is finished, and drying for later use;
step two: preparation of graphite solution
Pulverizing graphite into powder, adding into N-dimethylformamide solution, preparing into graphite solution under the action of ultrasonic wave, sealing, and storing.
Step three: preparation of
(1) Taking out the small substrate prepared in the first step, dripping the graphite oxide solution prepared in the second step on the small substrate, and shaking the small substrate in a left-right rotating mode until the small substrate is spread evenly to prepare a sample;
(2) putting the sample into a glass vessel for drying, and forming a layer of solid graphene film on the small substrate by using the graphite solution;
(3) and separating the graphene film from the small substrate to obtain the graphene film.
2. The method for preparing a graphene film according to claim 1, wherein the method comprises the following steps: in the first step, the substrate is single-sided conductive glass and is cut into small substrates with the size of 4X4cm by a glass cutter.
3. The method for preparing a graphene film according to claim 1, wherein the method comprises the following steps: in the step one, the content of the ethanol solution and the content of the acetone solution are both 20-25ml, and the ultrasonic cleaning time is 10-15 min.
4. The method for preparing a graphene film according to claim 1, wherein the method comprises the following steps: in the second step, the weight ratio of the graphite to the N-dimethylformamide solution is 1: 3.
5. the method for preparing a graphene film according to claim 1, wherein the method comprises the following steps: the thickness of the graphene film prepared in the step three is 100-200 nm.
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CN202011617881.3A CN112723344A (en) | 2020-12-31 | 2020-12-31 | Preparation method of graphene film |
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CN202011617881.3A CN112723344A (en) | 2020-12-31 | 2020-12-31 | Preparation method of graphene film |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103172062A (en) * | 2013-04-17 | 2013-06-26 | 东南大学 | Preparation method of graphene film for dye-sensitized solar cell counter electrodes |
CN103449420A (en) * | 2013-08-22 | 2013-12-18 | 中国科学院金属研究所 | High-quality graphene dispersion method and film preparation method |
CN103864062A (en) * | 2014-01-27 | 2014-06-18 | 沈阳大学 | Preparation method of graphene transparent conductive film |
CN104118869A (en) * | 2014-07-07 | 2014-10-29 | 苏州世优佳电子科技有限公司 | Preparation method of graphene thin films |
-
2020
- 2020-12-31 CN CN202011617881.3A patent/CN112723344A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103172062A (en) * | 2013-04-17 | 2013-06-26 | 东南大学 | Preparation method of graphene film for dye-sensitized solar cell counter electrodes |
CN103449420A (en) * | 2013-08-22 | 2013-12-18 | 中国科学院金属研究所 | High-quality graphene dispersion method and film preparation method |
CN103864062A (en) * | 2014-01-27 | 2014-06-18 | 沈阳大学 | Preparation method of graphene transparent conductive film |
CN104118869A (en) * | 2014-07-07 | 2014-10-29 | 苏州世优佳电子科技有限公司 | Preparation method of graphene thin films |
Non-Patent Citations (1)
Title |
---|
陈彬: "石墨烯制备方法研究进展", 《当代化工研究》 * |
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Application publication date: 20210430 |