CN105110794A - Graphene film and preparation method therefor - Google Patents
Graphene film and preparation method therefor Download PDFInfo
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- CN105110794A CN105110794A CN201510481379.7A CN201510481379A CN105110794A CN 105110794 A CN105110794 A CN 105110794A CN 201510481379 A CN201510481379 A CN 201510481379A CN 105110794 A CN105110794 A CN 105110794A
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Abstract
The invention provides a preparation method for a graphene film. The method comprises the following steps of carrying out ultrasonic soaking and stirring on graphene oxide, carrying out impurity filtration, coating a PET (Polyethyleneglycol Terephthalate) film with a graphene oxide solution, and carrying out carbonization and graphitization, thereby obtaining the graphene film. The method is simple in process and easy to popularize, and the obtained graphene film has extremely high shielding effectiveness and good heat dissipating performance.
Description
Technical field
The present invention relates to electronics field, refer to the preparation method of a kind of preparation method of graphene film especially, the invention still further relates to a kind of graphene film.
Background technology
Along with the expansion of electronics, electric installation range of application and universal, to the performance of electronics and structural requirement more and more stricter, comprise the speed of higher process, higher process frequency, less volume, lighter weight, higher power.The update of electronics brings great convenience and fabulous experience to people's life, and also problem served by band simultaneously: (1) heating is more; (2) Contamination of Electromagnetic Wave is more serious.
For this reason, need to develop a kind of perfect heat-dissipating, the product of electromagnetic pollution can be reduced simultaneously.
Summary of the invention
The present invention proposes the preparation method of a kind of preparation method of graphene film, the simple easy handling of method, and, according to described graphene film prepared by the method, there is the feature of rapid heat dissipation.
It is good that another object of the present invention is to propose a kind of heat radiation, the graphene film of effectiveness of shielding excellence.
Technical scheme of the present invention is achieved in that a kind of preparation method of graphene film, comprises the following steps:
A) ultrasonic wave soaking and stirring graphene oxide; .
B) impurity screening;
C) graphene oxide solution is applied in PET film, successive drying, forms coiled material;
d)carbonization, reduces the functional group inside graphite oxide, and when functional group decomposes, the gas of release, forms pore and cavity in graphene film inside, form spumescence;
E) greying, obtains graphene film.
Preferably, in step a, comprising: by graphene oxide with water in 1:(10 ~ 100) ratio mix, ultrasonic wave is soaked, and adopts the rotating speed of 500-3000rps to carry out being uniformly mixed 2-8 hour.
Be more preferably, in step a, graphene oxide mixes with the ratio of water in 1:20.
Preferably, in step b, adopt reciprocating sieve by the contaminant filter in graphene oxide.
Preferably, in step c, comprising: use scraper for coating mode to be coated onto in PET film by graphene oxide slurries continuous print, dry through continuous print drying tunnel again, the graphene oxide film of formation and base material PET are cut separation, rolling respectively, obtains continuous oxidation graphene film coiled material again.
Preferably, in steps d, carbonization process is be elevated to 800 DEG C with the temperature rise rate of 10 DEG C/min from room temperature under nitrogen protection.
Preferably, in step e, graphitizing process is be elevated to 2300 DEG C with the temperature rise rate of 20 DEG C/min from room temperature under argon shield.
A kind of graphene film adopting aforesaid method to prepare.
The preparation method of described graphene film of the present invention, technique is simple, convenient operation, and the constant product quality obtained, effective, be suitable for propagation and employment.It is good that described graphene film of the present invention has radiating effect, and especially effectiveness of shielding is strong, is adapted at electronic product uses, and improves the comfort level of product, and more useful to human body.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the shielding test result figure of a kind of Graphene heat conducting film of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment, according to method disclosed by the invention, carries out following operation:
A) graphene oxide is mixed with the ratio of water in 1:20, aforementioned proportion can at 1:(10-100) scope in adjustment, specifically determine according to the demand of actually operating, use the high speed dispersor of the ultrasonic rod of band to be uniformly mixed mixing 2 ~ 8 hours with the rotating speed of 500 ~ 3000rps;
B) reciprocating sieve is used to be fallen by the contaminant filter in graphene oxide;
C) scraper for coating mode is used to be coated onto in PET film by graphene oxide slurries, then through the oven for drying of coating machine, then peel off rolling, obtain graphene oxide film, its thickness is 10um ~ 200um;
D) be elevated to 800 DEG C with the temperature rise rate of 10 DEG C/min from room temperature under nitrogen protection and carry out carbonization;
E) under argon shield, be elevated to 2300 DEG C with the temperature rise rate of 20 DEG C/min from room temperature carry out greying and obtain Graphene heat conducting film, above-mentioned shielding gas, i.e. nitrogen and argon gas, also can adopt other shielding gas according to cost or other demands.
In order to detect the shielding properties of the Graphene heat conducting film obtained, inventors performed shielding properties test, process is as follows:
(1) testing apparatus
AgilentE5061B vector network analyzer, DN1015A Materials ' Shielding Effectiveness test coaxial holder, coaxial electrical is pulled.
(2) sample is tested
Prepared according to the methods of the invention, sample is external diameter Φ 115mm circular specimen, thickness 0.3mm.
(3) foundation is tested
SJ20524-1995 " measuring method of Materials ' Shielding Effectiveness "
(4) test result
As shown in Figure 1.
Known in 30-1500MHz range of frequency, effectiveness of shielding raises along with the increase of frequency, and the effectiveness of shielding of 30MHz is the effectiveness of shielding of 67.6Db, 1500MHz is 93.7Db.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. a preparation method for graphene film, is characterized in that, comprises the following steps:
A) ultrasonic wave soaking and stirring graphene oxide;
B) impurity screening;
C) graphene oxide solution is applied in PET film, successive drying, forms coiled material;
D) functional group inside graphite oxide reduced, when functional group decomposes, the gas of release, forms pore and cavity in graphene film inside, forms spumescence;
E) greying, obtains graphene film.
2. the preparation method of graphene film as described in the appended claim 1, it is characterized in that: in step a, comprise: by graphene oxide with water in 1:(10 ~ 100) ratio mix, ultrasonic wave is soaked, and adopts the rotating speed of 500-3000rps to carry out being uniformly mixed 2-8 hour.
3. the preparation method of graphene film as stated in claim 2, it is characterized in that: in step a, graphene oxide mixes with the ratio of water in 1:20.
4. the preparation method of graphene film as described in the appended claim 1, is characterized in that: in step b, adopts reciprocating sieve by the contaminant filter in graphene oxide.
5. the preparation method of graphene film as described in the appended claim 1, is characterized in that: in step c, comprising: use scraper for coating mode to be coated onto in PET film by graphene oxide slurries, then through drying, peeling off rolling, obtaining graphene oxide film.
6. the preparation method of graphene film as described in the appended claim 1; it is characterized in that: in steps d; by graphene oxide film cut-parts; centre carbon paper is kept apart; build up a pile; put into charring furnace and carry out carbonization, carbonization process is be elevated to 800 DEG C with the temperature rise rate of 10 DEG C/min from room temperature under nitrogen protection.
7. the preparation method of graphene film as described in the appended claim 1, it is characterized in that: in step e, graphitizing process is be elevated to 2300 DEG C with the temperature rise rate of 20 DEG C/min from room temperature under argon shield.
8. a graphene film, is characterized in that: have employed arbitrary described method preparation in claim 1-7.
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| CN201510481379.7A CN105110794B (en) | 2015-08-07 | 2015-08-07 | Preparation method of graphene film and graphene film |
| CN201810115742.7A CN108178148B (en) | 2015-08-07 | 2015-08-07 | Preparation method of graphene film and graphene film |
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|---|---|---|---|---|
| CN105502368A (en) * | 2015-12-30 | 2016-04-20 | 中国科学院宁波材料技术与工程研究所 | Graphene film and preparation method thereof |
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Citations (5)
| 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 |
| 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 |
| 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 |
| CN104129780A (en) * | 2014-07-21 | 2014-11-05 | 中国科学院深圳先进技术研究院 | Graphene film and making method thereof |
| EP2868627A1 (en) * | 2012-06-29 | 2015-05-06 | Ocean's King Lighting Science & Technology Co., Ltd | Graphene film, preparation method and application thereof |
Family Cites Families (1)
| 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 |
-
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 (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| EP2868627A1 (en) * | 2012-06-29 | 2015-05-06 | Ocean's King Lighting Science & Technology Co., Ltd | Graphene film, preparation method and application thereof |
| 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 |
| CN104129780A (en) * | 2014-07-21 | 2014-11-05 | 中国科学院深圳先进技术研究院 | Graphene film and making method thereof |
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| CN108178148A (en) | 2018-06-19 |
| CN108178148B (en) | 2020-04-28 |
| CN105110794B (en) | 2020-03-10 |
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