CN108455580A - A kind of graphene film weblike material and preparation method thereof - Google Patents
A kind of graphene film weblike material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of graphene film weblike material preparation methods, and steps are as follows：Graphene oxide solution makes, by solution coating to PI films, dry, obtain graphene film base material；After graphene film base material high temperature cabonization, graphitization, graphene film is rolled with calender, obtains web-like graphene heat dissipation film.The operating type of innovation：Web-like graphene film base material is cut into required specification, obtains the graphene film base material of various specifications, state is web-like；Then it web-like graphene film base material, is placed in general dual layer jig, jig is placed in sintering furnace, according to different-thickness product and the temperature curves of needs is set；Product is subjected to high temperature cabonization, graphitization, cooling；Graphited graphene film substrate product is taken out, product is rolled with calender, obtains web-like graphite radiating film.This method is simple for process, easy to spread, the graphene film, has outstanding shield effectiveness and extremely strong heat dissipation performance.
Description
Technical field
The present invention relates to a kind of graphene film weblike materials and preparation method thereof, and the product produced belongs to a nanometer material
Expect graphene high molecular material carbonated product technical field, be mainly used in done in electronics industry radiate, shielding material use.
A kind of graphene film weblike material preparation method is particularly related to, the invention further relates to a kind of graphene films.
Technical background
It is more next to the performance and structural requirement of electronic equipment with electronics, the expansion of electrical equipment application range and universal
It is stringenter, including higher processing speed, higher processing frequency, smaller volume, lighter weight, higher power.Electricity
The update of sub- equipment brings great convenience and fabulous experience to people's life, while also bringing some problems：(1) it generates heat
More；(2) Contamination of Electromagnetic Wave is more serious.Product radiate both at home and abroad at present mainly with electrographite and natural graphite and metal
Based on material heat dissipation, for this product in order to replace based on highly heat-conductive material electrographite, electrographite coiled material is that existing market is main
One of product, but the limitation of the production capacity because of PI film raw materials manufacturer cause home products supply chain short, often lack
Few raw material, and there is bottleneck in many companies of time integral for many years in production and market application in graphene product.
For this purpose, the present invention is to develop a kind of perfect heat-dissipating, while the product of electromagnetic pollution can be reduced, solve stone
The market of black alkene powder product applies problem, expands out application space of the Chinese graphene product in consumer electronics product.
Invention content
A kind of graphene film of present invention proposition and preparation method thereof, method is simply easily operated, also, according to the party
The graphene film prepared by method, has the characteristics that rapid heat dissipation.
The technical proposal of the invention is realized in this way：A kind of preparation method of graphene film, includes the following steps：
A) ultrasonic wave soaking and stirring graphene oxide
B) graphene oxide solution is applied on PI films, it is continuous drying, form coiled material
C) web-like graphene film base material is placed in general dual layer jig, jig is placed in sintering furnace, and temperature is arranged
Product is carried out high temperature cabonization by line of writing music, and the functional group in high temperature cabonization inside graphene oxide is restored, decomposed, shape
At foam-like coiled material
D) by graphene film foam-like coiled material, be placed in high temperature furnace and be graphitized, after the completion of graphitization cooling obtains graphene
Film substrate.
E) and by graphited graphene film substrate product take out, with calender by graphene film substrate product into
After row calendering, final production goes out the graphene heat dissipation film of web-like.
Further, in the above-mentioned technical solutions, in step a, using reciprocating sieve by the impurity mistake in graphene oxide
Filter, graphene oxide is mixed with water, curing agent is added, ultrasonic wave impregnates, and the rotating speed of 5000-7500rps is taken to be stirred
Mix mixing 8-12h.
Further, in the above-mentioned technical solutions, in step a, in step a, the curing agent is DDM pulvis, described solid
Agent addition is the 4% of graphene oxide and water total weight.
Further, in the above-mentioned technical solutions, in step b, graphene oxide slurries are applied using wire type coating apparatus
Onto PI films, using the drying removal PI stripping windings of 100-150 DEG C of continuity, then by the graphene oxide film of formation
It cuts separation with base material PI, winds respectively, obtain graphene oxide film base material.
Further, in the above-mentioned technical solutions, in step c, graphene oxide film base material is cut into required
Specification (i.e. width, length) obtains the original material (i.e. graphene film base material) of various specifications, and state is web-like.Then volume
Shape graphene film base material, is placed in general dual layer jig.Jig is placed in sintering furnace, and temperature curve is set.It will production
Product carry out high temperature cabonization, and carbonisation is to be increased to 1200 DEG C from room temperature under nitrogen protection with the heating rate of 10 DEG C/min,
Constant temperature cools down, and the product of carbonization is taken out to 12h after the completion of carbonization.
Further, in the above-mentioned technical solutions, in step d, cool down after the completion of carbonization, jig is placed on sintering furnace
In, and temperature curve is set.Product is subjected to high temperature graphitization, high temperature graphitization process be under protection of argon gas with 20 DEG C/
The heating rate of min is increased to 2600~2800 DEG C from room temperature, constant temperature to 13h, cools down after the completion of graphitization, and by stone
The product of inkization takes out.
Further, in the above-mentioned technical solutions, in step e, and graphited graphene film substrate product is taken
Go out, after being rolled graphene film substrate product with calender, final production goes out the graphene heat dissipation film of web-like.
The present invention provides a kind of graphene film weblike material that above-mentioned preparation method obtains, and has extremely strong thermal diffusivity
It can be with outstanding shield effectiveness.
Invention advantageous effect
The preparation method of the graphene film of the present invention, simple for process, product quality easy to operation, and obtaining
Stablize, effect is good, is suitable for promoting and apply.The graphene film of the present invention has high heat dissipation effect, is suitble to all kinds of
It is used in the high heat dissipation of electronic product, improves the speed of service of electronic product and the comfort level of user, increase the use of product
Service life.
Specific implementation mode
The embodiments described below are only a part of the embodiment of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, the every other reality that those of ordinary skill in the art obtain without creative efforts
Example is applied, shall fall within the protection scope of the present invention.
The preparation of 1 TYGO-015JC type products of embodiment
A kind of graphene film weblike material preparation method, includes the following steps：
A) ultrasonic wave soaking and stirring graphene oxide in water；
B) graphene oxide solution is applied on PI films, it is continuous drying, obtain the web-like graphene of removal PI films
Film substrate；
C) by web-like graphene film base material in sintering furnace, high temperature cabonization is carried out using temperature programming, forms graphene film
Steep foam-like coiled material；
D) by graphene film foam-like coiled material, be placed in high temperature furnace and be graphitized, after the completion of graphitization cooling obtains graphene
Film substrate；
E) and the obtained graphene film substrate products of step d) are taken out, with calender by graphene film substrate product
After being rolled, final production goes out the graphene film of web-like.
In step a, graphene oxide is mixed in proportion with water, curing agent EP/DDM pulvis, curing agent addition is added
For graphene oxide and the 4% of water total weight, ultrasonic wave impregnates, and the rotating speed of 5000rps is taken to be stirred mixing 8-12h.
In step b, including：Graphene oxide slurries are coated onto on PI films using wire type coating apparatus, using 100-
150 DEG C of continuity drying removal PI films stripping windings, obtain graphene oxide film base material.
In step c, graphene oxide film base material is cut into wide 60~450mm* long, 110~210m standard specification materials
Material, state is web-like；Then it web-like graphene film base material, is placed in double-layer tool, jig is placed in sintering furnace,
Product is subjected to high temperature cabonization, carbonisation is to be increased under nitrogen protection from room temperature with the heating rate of 10 DEG C/min
1200 DEG C, constant temperature to 12h cools down after the completion of carbonization, and the product of carbonization is taken out.
In step d, cool down after the completion of carbonization, jig is placed in sintering furnace, product is subjected to high temperature graphitization, it is high
Warm graphitizing process is to be increased to 2600~2800 DEG C from room temperature under protection of argon gas with the heating rate of 20 DEG C/min, temperature
Continue to 13h, cools down after the completion of graphitization, and graphited product is taken out.
In step e, by graphited graphene film substrate product, with calender by graphene film substrate product into
After row calendering, final production goes out the graphene heat dissipation film of web-like.
The preparation of 2 TYGO-025J type products of embodiment
A kind of graphene film weblike material preparation method, includes the following steps：
A) ultrasonic wave soaking and stirring graphene oxide in water；
B) graphene oxide solution is applied on PI films, it is continuous drying, obtain the web-like graphene of removal PI films
Film substrate；
C) by web-like graphene film base material in sintering furnace, high temperature cabonization is carried out using temperature programming, forms graphene film
Steep foam-like coiled material；
D) by graphene film foam-like coiled material, be placed in high temperature furnace and be graphitized, after the completion of graphitization cooling obtains graphene
Film substrate；
E) and the obtained graphene film substrate products of step d) are taken out, with calender by graphene film substrate product
After being rolled, final production goes out the graphene film of web-like.
In step a, graphene oxide is mixed in proportion with water, curing agent EP/DDM pulvis, curing agent addition is added
For graphene oxide and the 4% of water total weight, ultrasonic wave impregnates, and the rotating speed of 5500rps is taken to be stirred mixing 8-12h.
In step b, including：Graphene oxide slurries are coated onto on PI films using wire type coating apparatus, using 100-
150 DEG C of continuity drying removal PI films stripping windings, obtain graphene oxide film base material.
In step c, graphene oxide film base material is cut into wide 60~450mm* long, 110~210m standard specification materials
Material, state is web-like；Then it web-like graphene film base material, is placed in double-layer tool, jig is placed in sintering furnace,
Product is subjected to high temperature cabonization, carbonisation is to be increased under nitrogen protection from room temperature with the heating rate of 10 DEG C/min
1200 DEG C, constant temperature to 12h cools down after the completion of carbonization, and the product of carbonization is taken out.
In step d, cool down after the completion of carbonization, jig is placed in sintering furnace, product is subjected to high temperature graphitization, it is high
Warm graphitizing process is to be increased to 2600~2800 DEG C from room temperature under protection of argon gas with the heating rate of 20 DEG C/min, temperature
Continue to 13h, cools down after the completion of graphitization, and graphited product is taken out.
In step e, and graphited graphene film substrate product is taken out, with calender by graphene film base material
After product is rolled, final production goes out the graphene heat dissipation film of web-like.
The preparation of 3 TYGO-040J type products of embodiment
A kind of graphene film weblike material preparation method, includes the following steps：
A) ultrasonic wave soaking and stirring graphene oxide in water；
B) graphene oxide solution is applied on PI films, it is continuous drying, obtain the web-like graphene of removal PI films
Film substrate；
C) by web-like graphene film base material in sintering furnace, high temperature cabonization is carried out using temperature programming, forms graphene film
Steep foam-like coiled material；
D) by graphene film foam-like coiled material, be placed in high temperature furnace and be graphitized, after the completion of graphitization cooling obtains graphene
Film substrate；
E) and the obtained graphene film substrate products of step d) are taken out, with calender by graphene film substrate product
After being rolled, final production goes out the graphene film of web-like.
In step a, graphene oxide is mixed in proportion with water, curing agent EP/DDM pulvis, curing agent addition is added
For graphene oxide and the 4% of water total weight, ultrasonic wave impregnates, and the rotating speed of 6000rps is taken to be stirred mixing 8-12h.
In step b, including：Graphene oxide slurries are coated onto on PI films using wire type coating apparatus, using 150
DEG C or so continuity drying removal PI films stripping winding, obtain graphene oxide film base material.
In step c, graphene oxide film base material is cut into wide 60~450mm* long, 110~210m standard specification materials
Material, state is web-like；Then it web-like graphene film base material, is placed in double-layer tool, jig is placed in sintering furnace,
Product is subjected to high temperature cabonization, carbonisation is to be increased under nitrogen protection from room temperature with the heating rate of 10 DEG C/min
1200 DEG C, constant temperature to 12h cools down after the completion of carbonization, and the product of carbonization is taken out.
In step d, cool down after the completion of carbonization, jig is placed in sintering furnace, product is subjected to high temperature graphitization, it is high
Warm graphitizing process is to be increased to 2600~2800 DEG C from room temperature under protection of argon gas with the heating rate of 20 DEG C/min, temperature
Continue to 13h, cools down after the completion of graphitization, and graphited product is taken out.
In step e, and graphited graphene film substrate product is taken out, with calender by graphene film base material
After product is rolled, final production goes out the graphene heat dissipation film of web-like.
The preparation of 4 TYGO-060J type products of embodiment
A kind of graphene film weblike material preparation method, includes the following steps：
A) ultrasonic wave soaking and stirring graphene oxide in water；
B) graphene oxide solution is applied on PI films, it is continuous drying, obtain the web-like graphene of removal PI films
Film substrate；
C) by web-like graphene film base material in sintering furnace, high temperature cabonization is carried out using temperature programming, forms graphene film
Steep foam-like coiled material；
D) by graphene film foam-like coiled material, be placed in high temperature furnace and be graphitized, after the completion of graphitization cooling obtains graphene
Film substrate；
E) and the obtained graphene film substrate products of step d) are taken out, with calender by graphene film substrate product
After being rolled, final production goes out the graphene film of web-like.
In step a, graphene oxide is mixed with water, curing agent EP/DDM pulvis is added, curing agent addition is oxidation
Graphene and the 4% of water total weight, ultrasonic wave impregnates, and the rotating speed of 6500rps is taken to be stirred mixing 8-12h.
In step b, including：Graphene oxide slurries are coated onto on PI films using wire type coating apparatus, using 150
DEG C or so continuity drying removal PI films stripping winding, obtain graphene oxide film base material.
In step c, graphene oxide film base material is cut into wide 60~450mm* long, 110~210m standard specification materials
Material, state is web-like；Then it web-like graphene film base material, is placed in double-layer tool, jig is placed in sintering furnace,
Product is subjected to high temperature cabonization, carbonisation is to be increased under nitrogen protection from room temperature with the heating rate of 10 DEG C/min
1200 DEG C, constant temperature to 12h cools down after the completion of carbonization, and the product of carbonization is taken out.
In step d, cool down after the completion of carbonization, jig is placed in sintering furnace, product is subjected to high temperature graphitization, it is high
Warm graphitizing process is to be increased to 2600~2800 DEG C from room temperature under protection of argon gas with the heating rate of 20 DEG C/min, temperature
Continue to 13h, cools down after the completion of graphitization, and graphited product is taken out.
In step e, and graphited graphene film substrate product is taken out, with calender by graphene film base material
After product is rolled, final production goes out the graphene heat dissipation film of web-like.
The preparation of 5 TYGO-080J type products of embodiment
A kind of graphene film weblike material preparation method, includes the following steps：
A) ultrasonic wave soaking and stirring graphene oxide in water；
B) graphene oxide solution is applied on PI films, it is continuous drying, obtain the web-like graphene of removal PI films
Film substrate；
C) by web-like graphene film base material in sintering furnace, high temperature cabonization is carried out using temperature programming, forms graphene film
Steep foam-like coiled material；
D) by graphene film foam-like coiled material, be placed in high temperature furnace and be graphitized, after the completion of graphitization cooling obtains graphene
Film substrate；
E) and the obtained graphene film substrate products of step d) are taken out, with calender by graphene film substrate product
After being rolled, final production goes out the graphene film of web-like.
In step a, graphene oxide is mixed with water, curing agent EP/DDM pulvis is added, curing agent addition is oxidation
Graphene and the 4% of water total weight, ultrasonic wave impregnates, and the rotating speed of 7000rps is taken to be stirred mixing 8-12h.
In step b, including：Graphene oxide slurries are coated onto on PI films using wire type coating apparatus, using 100-
150 DEG C or so continuity drying removal PI films stripping windings, obtain graphene oxide film base material.
In step c, graphene oxide film base material is cut into wide 60~450mm* long, 110~210m standard specification materials
Material, state is web-like；Then it web-like graphene film base material, is placed in double-layer tool, jig is placed in sintering furnace,
Product is subjected to high temperature cabonization, carbonisation is to be increased under nitrogen protection from room temperature with the heating rate of 10 DEG C/min
1200 DEG C, constant temperature to 12h cools down after the completion of carbonization, and the product of carbonization is taken out.
In step d, cool down after the completion of carbonization, jig is placed in sintering furnace, product is subjected to high temperature graphitization, it is high
Warm graphitizing process is to be increased to 2600~2800 DEG C from room temperature under protection of argon gas with the heating rate of 20 DEG C/min, temperature
Continue to 13h, cools down after the completion of graphitization, and graphited product is taken out.
In step e, and graphited graphene film substrate product is taken out, with calender by graphene film base material
After product is rolled, final production goes out the graphene heat dissipation film of web-like.
For the heat conductivility of the graphene heat conducting film detected, inventor has carried out heat conductivility test, and process is such as
Under：
(1) test equipment
AT330 analyzers, Germany is resistance to speed 467
(2) test sample
TYGO015、TYGO025、TYGO040、TYGO060、TYGO080
(3) foundation is tested
ASTM E1461-13、ASTM E1269-11、GB/T 1033.1-2008《The test method of material conducts heat efficiency》
(4) test result
Graphene heat dissipation film TYGO-015J thermal coefficients：
Thermal diffusion coefficient-NETZSCH LFA analyses
Graphene heat dissipation film TYGO-025J thermal coefficients：
Thermal diffusion coefficient-NETZSCH LFA analyses
Graphene heat dissipation film TYGO-040J thermal coefficients：
Thermal diffusion coefficient-NETzscH LFA analyses
Graphene heat dissipation film TYGO-060J thermal coefficients are detected using AT330 analyzers：
K value result of calculations (sample B)
B-1：Specific heat 0.794J/ (g*k) * thermal diffusions 785mm^2/s*
Density 2.0210g/cm^3
=thermal coefficient 1259.669W/ (m*k)
B-2：Specific heat 0.794J/ (g*k) * thermal diffusions 812mm^2/s*
Density 2.1095g/cm^3
=thermal coefficient 1360.054W/ (m*k)
Graphene heat dissipation film TYGO-080J thermal coefficients are detected using AT330 analyzers：
K value result of calculations (sample A)
A-1：This hot 0.784J/ (g*k) * thermal diffusions 801mm^2/s*
Density 2.0536g/cm^3
=thermal coefficient 1290.130W/ (m*k)
A-2：Specific heat 0.784J/ (g*k) * thermal diffusions 771mm^2/s*
Density 2.1260g/cm^3
=thermal coefficient 1285.574W/ (m*k)
The foregoing is merely illustrative of the preferred embodiments of the present invention, all in spirit of the invention not to limit invention
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of graphene film weblike material preparation method, which is characterized in that include the following steps：
A) ultrasonic wave soaking and stirring graphene oxide in water；
B) graphene oxide solution is applied on PI films, it is continuous drying, obtain the web-like graphene film of removal PI films
Base material；
C) by web-like graphene film base material in sintering furnace, high temperature cabonization is carried out using temperature programming, forms graphene film bubble
Foam shape coiled material；
D) by graphene film foam-like coiled material, be placed in high temperature furnace and be graphitized, after the completion of graphitization cooling obtains graphene film
Base material；
E) and the obtained graphene film substrate products of step d) are taken out, and are pressed graphene film substrate product with calender
It delays, final production goes out the graphene film of web-like.
2. graphene film weblike material preparation method as described in the appended claim 1, it is characterised in that：In step a, stone will be aoxidized
Black alkene is mixed with water, and curing agent is added, and ultrasonic wave impregnates, and the rotating speed of 5000-7500rps is taken to be stirred mixing 8-12h.
3. graphene film weblike material preparation method as stated in claim 2, it is characterised in that：In step a, the solidification
Agent is EP/DDM pulvis, and the curing agent addition is the 4% of graphene oxide and water total weight.
4. graphene film weblike material preparation method as described in the appended claim 1, it is characterised in that：In step b, including：Make
Graphene oxide slurries are coated onto on PI films with wire type coating apparatus, it is thin using 100-150 DEG C of continuity drying removal PI
Film stripping is wound, and obtains graphene oxide film base material.
5. graphene film weblike material preparation method as described in the appended claim 1, it is characterised in that：In step c, stone will be aoxidized
Black alkene film substrate cuts into required specification, and state is web-like；Then it web-like graphene film base material, is placed on bilayer and controls
In tool, jig is placed in sintering furnace, product is subjected to high temperature cabonization, carbonisation is under nitrogen protection with 10 DEG C/min
Heating rate be increased to 1200 DEG C from room temperature, constant temperature to 12h cools down after the completion of carbonization, and the product of carbonization is taken out.
6. graphene film weblike material preparation method as described in the appended claim 1, it is characterised in that：In step d, carbonization is completed
Cool down afterwards, jig is placed in sintering furnace, product is subjected to high temperature graphitization, high temperature graphitization process is under protection of argon gas
2600~2800 DEG C are increased to from room temperature with the heating rate of 20 DEG C/min, constant temperature to 13h, graphitization cools down after the completion,
And graphited product is taken out.
7. graphene film weblike material preparation method as described in the appended claim 1, it is characterised in that：In step e, and by graphite
The graphene film substrate product of change is taken out, and after being rolled graphene film substrate product with calender, final production goes out
The graphene heat dissipation film of web-like.
8. a kind of graphene film weblike material, it is characterised in that：Any the method in claim 1-7 is used to prepare.
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| CN112322258B (en) * | 2020-12-08 | 2022-01-28 | 福建永安市永清石墨烯研究院有限公司 | Graphene heat-conducting silica gel sheet and preparation method thereof |
| CN112322258A (en) * | 2020-12-08 | 2021-02-05 | 福建永安市永清石墨烯研究院有限公司 | Graphene heat-conducting silica gel sheet and preparation method thereof |
| CN112969355A (en) * | 2021-04-22 | 2021-06-15 | 世星科技股份有限公司 | Graphene heat dissipation film and preparation method thereof |
| CN113582166A (en) * | 2021-08-23 | 2021-11-02 | 德州宇航派蒙石墨烯科技有限责任公司 | Heat conduction membrane manufacture equipment |
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| CN115709992A (en) * | 2022-11-23 | 2023-02-24 | 深圳市贝特瑞新能源技术研究院有限公司 | Graphene oxide, preparation method thereof and composite film comprising graphene oxide |
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