CN105110794B - Preparation method of graphene film and graphene film - Google Patents
Preparation method of graphene film and graphene film Download PDFInfo
- Publication number
- CN105110794B CN105110794B CN201510481379.7A CN201510481379A CN105110794B CN 105110794 B CN105110794 B CN 105110794B CN 201510481379 A CN201510481379 A CN 201510481379A CN 105110794 B CN105110794 B CN 105110794B
- Authority
- CN
- China
- Prior art keywords
- graphene oxide
- film
- graphene
- graphene film
- preparing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The invention provides a preparation method of a graphene film, which comprises the following steps: the method is simple in process and easy to popularize, and the obtained graphene film has extremely strong shielding efficiency and good heat dissipation performance.
Description
Technical Field
The invention relates to the field of electronic products, in particular to a preparation method of a graphene film, and the invention also relates to the graphene film.
Background
With the expansion and popularization of the application range of electronic and electrical devices, the requirements on the performance and structure of the electronic devices are more and more strict, including higher processing speed, higher processing frequency, smaller volume, lighter weight and higher power. The renewal of electronic equipment brings great convenience and excellent experience for people's life, also brings some problems simultaneously: (1) more heat is generated; (2) the electromagnetic wave pollution is more serious.
Therefore, a product with good heat dissipation performance and capable of reducing electromagnetic pollution needs to be developed.
Disclosure of Invention
The preparation method of the graphene film is simple and easy to operate, and the graphene film prepared by the method has the characteristic of quick heat dissipation.
Another objective of the present invention is to provide a graphene film with good heat dissipation and excellent shielding performance.
The technical scheme of the invention is realized as follows: a preparation method of a graphene film comprises the following steps:
a) soaking and stirring graphene oxide by ultrasonic waves;
b) filtering impurities;
c) coating the graphene oxide solution on a PET film, and continuously drying to form a coiled material;
d) carbonizing, reducing functional groups in the graphite oxide, and forming air holes and cavities in the graphene film by released gas when the functional groups are decomposed to form foams;
e) and graphitizing to obtain the graphene film.
Preferably, step a includes: mixing graphene oxide and water according to the proportion of 1 (10-100), soaking by ultrasonic waves, and stirring and mixing for 2-8 hours at the rotating speed of 500-3000 rps.
More preferably, in step a, the graphene oxide is mixed with water in a ratio of 1: 20.
Preferably, in the step b, impurities in the graphene oxide are filtered by using a vibrating screen.
Preferably, step c includes: and continuously coating the graphene oxide slurry on a PET (polyethylene terephthalate) film in a scraper coating mode, drying the PET film through a continuous drying tunnel, stripping and separating the formed graphene oxide film and the PET substrate, and respectively rolling to obtain the continuous graphene oxide film coiled material.
Preferably, in step d, the carbonization process is carried out at a heating rate of 10 ℃/min under the protection of nitrogen, and the temperature is increased from room temperature to 800 ℃.
Preferably, in step e, the graphitization process is to raise the temperature from room temperature to 2300 ℃ at a temperature raising rate of 20 ℃/min under the protection of argon.
A graphene film prepared by the method.
The preparation method of the graphene film is simple in process, convenient to operate, stable in quality of the obtained product, good in effect and suitable for popularization and application. The graphene film disclosed by the invention has a good heat dissipation effect, especially has strong shielding efficiency, is suitable for being used on electronic products, improves the comfort level of the products, and is more beneficial to human bodies.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a diagram illustrating a shielding test result of a graphene thermal conductive film according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
Example according to the method disclosed herein, the following operations are performed:
a) mixing graphene oxide and water according to a ratio of 1:20, wherein the ratio can be adjusted within a range of 1 (10-100), and specifically, determining according to the requirement of actual operation, and stirring, mixing and mixing for 2-8 hours at a rotating speed of 500-3000rps by using a high-speed dispersion machine with an ultrasonic rod;
b) filtering impurities in the graphene oxide by using a vibrating screen;
c) coating the graphene oxide slurry on a PET film in a scraper coating mode, drying the PET film by using an oven of a coating machine, and peeling and rolling to obtain a graphene oxide film with the thickness of 10-200 um;
d) under the protection of nitrogen, raising the temperature from room temperature to 800 ℃ at the temperature rise rate of 10 ℃/min for carbonization;
e) and (3) under the protection of argon, raising the temperature from room temperature to 2300 ℃ at the heating rate of 20 ℃/min, graphitizing to obtain the graphene heat-conducting film, wherein the protective gases, namely nitrogen and argon, can also adopt other protective gases according to the cost or other requirements.
In order to detect the shielding performance of the obtained graphene heat-conducting film, the inventor performs a shielding performance test according to the following procedures:
(1) test equipment
An Agilent E5061B loss network analyzer, DN1015A material shielding effectiveness test coaxial clamp and coaxial cable.
(2) Test sample
The test specimens prepared according to the method of the invention were circular test specimens with an outer diameter of phi 115mm and a thickness of 0.3 mm.
(3) Basis of test
SJ 20524-1995 measurement method of material shielding effectiveness
(4) Test results
As shown in fig. 1.
It can be seen that in the frequency range of 30-1500 MHz, the shielding effectiveness increases with increasing frequency, the shielding effectiveness at 30MHz is 67.6Db, and the shielding effectiveness at 1500MHz is 93.7 Db.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. The preparation method of the graphene film is characterized by comprising the following steps:
a) soaking and stirring graphene oxide by ultrasonic waves;
b) filtering impurities;
c) coating the graphene oxide solution on a PET (polyethylene terephthalate) film, continuously drying, stripping and separating the formed graphene oxide film from a substrate PET, and respectively rolling to obtain a graphene oxide film coiled material;
d) separating the graphene oxide film cut pieces by using carbon paper, stacking the graphene oxide film cut pieces into a pile, and carbonizing the graphene oxide film cut pieces in a carbonization furnace, wherein the carbonization process is to increase the temperature from room temperature to 800 ℃ at the heating rate of 10 ℃/min under the protection of nitrogen so as to reduce functional groups in the graphene oxide, and when the functional groups are decomposed, gas released forms air holes and cavities in the graphene film to form a foam shape;
e) graphitizing to obtain a graphene film;
in the step e, the graphitization process is that the temperature is increased to 2300 ℃ from room temperature at the heating rate of 20 ℃/min under the protection of argon.
2. The method for preparing a graphene film according to claim 1, wherein: in the step a, the method comprises the following steps: mixing graphene oxide and water according to the proportion of 1 (10-100), soaking by ultrasonic waves, and stirring and mixing for 2-8 hours at the rotating speed of 500-3000 rps.
3. The method for preparing a graphene film according to claim 2, wherein: in the step a, the graphene oxide and water are mixed according to the proportion of 1: 20.
4. The method for preparing a graphene film according to claim 1, wherein: and in the step b, filtering impurities in the graphene oxide by adopting a vibrating screen.
5. The method for preparing a graphene film according to claim 1, wherein: in step c, the method comprises the following steps: and coating the graphene oxide slurry on the PET film in a scraper coating mode, drying, peeling and rolling to obtain the graphene oxide film.
6. A graphene film, characterized in that: prepared by the method of any one of claims 1 to 5.
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810115742.7A CN108178148B (en) | 2015-08-07 | 2015-08-07 | Preparation method of graphene film and graphene film |
CN201510481379.7A CN105110794B (en) | 2015-08-07 | 2015-08-07 | Preparation method of graphene film and graphene film |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510481379.7A CN105110794B (en) | 2015-08-07 | 2015-08-07 | Preparation method of graphene film and graphene film |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810115742.7A Division CN108178148B (en) | 2015-08-07 | 2015-08-07 | Preparation method of graphene film and graphene film |
Publications (2)
Publication Number | Publication Date |
---|---|
CN105110794A CN105110794A (en) | 2015-12-02 |
CN105110794B true CN105110794B (en) | 2020-03-10 |
Family
ID=54658961
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201510481379.7A Active CN105110794B (en) | 2015-08-07 | 2015-08-07 | Preparation method of graphene film and graphene film |
CN201810115742.7A Active CN108178148B (en) | 2015-08-07 | 2015-08-07 | Preparation method of graphene film and graphene film |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810115742.7A Active CN108178148B (en) | 2015-08-07 | 2015-08-07 | Preparation method of graphene film and graphene film |
Country Status (1)
Country | Link |
---|---|
CN (2) | CN105110794B (en) |
Families Citing this family (20)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105502368B (en) * | 2015-12-30 | 2018-09-25 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of graphene film |
CN106634854A (en) * | 2016-07-18 | 2017-05-10 | 常州富烯科技股份有限公司 | Foamed graphene/phase-change composite energy storage material and preparation method therefor |
CN106243379B (en) * | 2016-07-23 | 2019-10-18 | 天津大学 | A kind of electromagnetic shielding foamed composite and preparation method based on graphene oxide and polymer |
CN106495133A (en) * | 2016-11-09 | 2017-03-15 | 嘉兴中易碳素科技有限公司 | High heat conduction Flexible graphene method for manufacturing thin film |
CN108203091B (en) * | 2017-01-23 | 2019-01-18 | 常州富烯科技股份有限公司 | A method of continuously preparing graphene heat conducting film |
CN107601468A (en) * | 2017-10-23 | 2018-01-19 | 南京旭羽睿材料科技有限公司 | A kind of preparation method of graphene film |
CN108328606B (en) * | 2018-02-12 | 2020-07-03 | 浙江大学 | Regular porous graphene film and preparation method thereof |
CN108455580A (en) * | 2018-04-04 | 2018-08-28 | 苏州天煜新材料科技有限公司 | A kind of graphene film weblike material and preparation method thereof |
CN108550903B (en) * | 2018-05-07 | 2020-06-19 | 杭州高烯科技有限公司 | Aluminum ion battery |
CN109694055B (en) * | 2018-12-28 | 2021-12-03 | 常州富烯科技股份有限公司 | High-density graphene foam film and preparation method thereof |
CN110129992B (en) * | 2019-06-04 | 2021-04-27 | 缪梦程 | Carbon fiber paper for fuel cell and preparation method thereof |
CN112063967A (en) * | 2020-09-03 | 2020-12-11 | 中国电子科技集团公司第三十三研究所 | Preparation method of silver-plated graphene film |
CN112340723B (en) * | 2020-09-30 | 2021-07-06 | 杭州乐可适新材料科技有限公司 | Graphene film for treating sewage of decorative material production workshop and processing technology thereof |
CN112366023B (en) * | 2020-12-06 | 2022-08-19 | 武汉汉烯科技有限公司 | High-conductivity and high-stability flexible graphene electrode and preparation method thereof |
CN113354415A (en) * | 2021-07-06 | 2021-09-07 | 中国科学院山西煤炭化学研究所 | Preparation method of ultrahigh-thermal-conductivity graphene film |
CN113771443B (en) * | 2021-08-31 | 2023-09-29 | 常州富烯科技股份有限公司 | Graphene heat conduction gasket reinforced by sintered graphene foam blocks and preparation method thereof |
CN113620283B (en) * | 2021-09-03 | 2023-01-31 | 陕西六元碳晶股份有限公司 | Graphene and processing method and application thereof |
CN114834129A (en) * | 2022-05-24 | 2022-08-02 | 福建永安市永清石墨烯研究院有限公司 | Preparation method of graphene composite heat-conducting film |
CN115972636A (en) * | 2022-12-21 | 2023-04-18 | 常州富烯科技股份有限公司 | Film making equipment, film making method, graphene heat-conducting film and preparation method thereof |
CN117023569B (en) * | 2023-08-17 | 2024-05-07 | 小米汽车科技有限公司 | Graphene electrothermal film and preparation method thereof, negative electrode, lithium metal battery and dendrite removing method thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103449423A (en) * | 2013-08-27 | 2013-12-18 | 常州第六元素材料科技股份有限公司 | Graphene heat conducting membrane and preparation method thereof |
CN103663444A (en) * | 2013-12-17 | 2014-03-26 | 张家港康得新光电材料有限公司 | Graphene composite film for heat dissipation and preparation method thereof |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP5499980B2 (en) * | 2010-08-02 | 2014-05-21 | 富士電機株式会社 | Method for producing graphene thin film |
CN103489649A (en) * | 2012-06-12 | 2014-01-01 | 海洋王照明科技股份有限公司 | Composite current collector and method for manufacturing same |
CN104271500B (en) * | 2012-06-29 | 2016-10-26 | 海洋王照明科技股份有限公司 | A kind of graphene film and its production and use |
CN104129780B (en) * | 2014-07-21 | 2016-08-24 | 中国科学院深圳先进技术研究院 | Graphene film and preparation method thereof |
-
2015
- 2015-08-07 CN CN201510481379.7A patent/CN105110794B/en active Active
- 2015-08-07 CN CN201810115742.7A patent/CN108178148B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103449423A (en) * | 2013-08-27 | 2013-12-18 | 常州第六元素材料科技股份有限公司 | Graphene heat conducting membrane and preparation method thereof |
CN103663444A (en) * | 2013-12-17 | 2014-03-26 | 张家港康得新光电材料有限公司 | Graphene composite film for heat dissipation and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
CN105110794A (en) | 2015-12-02 |
CN108178148B (en) | 2020-04-28 |
CN108178148A (en) | 2018-06-19 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN105110794B (en) | Preparation method of graphene film and graphene film | |
JP6633259B1 (en) | Method for continuously producing graphene thermal conductive film | |
CN105536585B (en) | A kind of carbon nano tube dispersion method | |
CN108455580A (en) | A kind of graphene film weblike material and preparation method thereof | |
CN105694427B (en) | A kind of application of graphene composite material as electromagnetic shielding material | |
CN113122184B (en) | Preparation method of biomass porous carbon wave-absorbing material | |
CN105502368B (en) | A kind of preparation method of graphene film | |
CN104961493B (en) | A kind of preparation method of biomass-based porous silicon carbide absorbing material | |
CN111137879B (en) | Method for preparing graphene heat dissipation film by using self-propagating stripping technology | |
CN103922330A (en) | Method for preparing graphene powder by using dry process | |
CN110670107B (en) | Titanium carbide nanosheet/carbon nanotube electromagnetic shielding film and preparation method thereof | |
CN108584942A (en) | A kind of preparation method of grapheme foam carbon composite | |
CN113753880A (en) | Method for preparing three-dimensional graphene structure through 3D printing | |
CN112225201A (en) | Method for preparing thick graphene heat dissipation film by utilizing silk screen | |
CN110282625A (en) | A kind of preparation method and application of electrode material for super capacitor | |
CN104828808B (en) | A kind of preparation method of graphene film | |
CN114408908A (en) | Graphene heat dissipation film and preparation method thereof | |
CN106744878B (en) | A kind of scale crushes the method for preparing large stretch of footpath graphene | |
CN112280383A (en) | Porous titanium carbide MXene/reduced graphene oxide-based conductive ink and preparation method thereof | |
CN113979428B (en) | Preparation method of heat-conducting wave-absorbing composite film and heat-conducting wave-absorbing composite film | |
CN103694487A (en) | Preparation method of carbon fiber-polyimide composite film | |
CN108101035B (en) | Green preparation method of high-quality graphene | |
CN104558777B (en) | Preparation method of natural graphite/polymer electromagnetic shielding composite | |
KR102256444B1 (en) | Polyethylene porous separator and manufacturing method thereof | |
CN114014310B (en) | Multifunctional graphene foam and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |