CN104264146A - Functionalized graphene-based transparent conductive heat-conducting film and preparation method thereof - Google Patents
Functionalized graphene-based transparent conductive heat-conducting film and preparation method thereof Download PDFInfo
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- CN104264146A CN104264146A CN201410511439.0A CN201410511439A CN104264146A CN 104264146 A CN104264146 A CN 104264146A CN 201410511439 A CN201410511439 A CN 201410511439A CN 104264146 A CN104264146 A CN 104264146A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000002834 transmittance Methods 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000007306 functionalization reaction Methods 0.000 claims description 25
- 239000006185 dispersion Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 239000011159 matrix material Substances 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 125000003396 thiol group Chemical class [H]S* 0.000 claims description 4
- 238000004176 ammonification Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims 2
- 238000000576 coating method Methods 0.000 abstract description 5
- 238000005507 spraying Methods 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000010422 painting Methods 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 238000009987 spinning Methods 0.000 abstract 2
- 239000003431 cross linking reagent Substances 0.000 abstract 1
- 239000011261 inert gas Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 6
- 230000009467 reduction Effects 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003303 reheating Methods 0.000 description 2
- 238000007761 roller coating Methods 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000001652 electrophoretic deposition Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000009718 spray deposition Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Manufacturing Of Electric Cables (AREA)
Abstract
The invention discloses a functionalized graphene-based transparent conductive heat-conducting film and a preparation method thereof. The method comprises the following steps: with functionalized graphene as a raw material, dissolving the functionalized graphene or a mixture of the functionalized graphene and a crosslinking agent into a selected solvent; adopting the methods such as spraying, roll painting, spinning and hanging, coating a transparent film of 200nm to 20 mu m on a substrate, wherein the size of the film can be controlled according to the spinning method; after the film is dried, the sheet resistance of the film is 10<9> omega/square to 10<5> omega/square; and the light transmittance of the film is 80-95%; under the condition of introducing an inert gas to protect, carrying out high-temperature treatment on the dried film at 1,000-2800 DEG C; and cooling to obtain the transparent film of which the sheet resistance is 10<3> ohm/square 10<-2> ohm/square and the thermal conductivity is 1-2,000W/m. DEG C. The functionalized graphene-based transparent conductive heat-conducting film is simple in process, easy to regulate and control, and low in cost; continuous operation can be achieved; the width of the transparent conductive heat-conducting film produced by once can reach 2m; and the obtained product has excellent conductivity, heat-conducting property and light transmittance performance, and can be widely applied to the fields such as touch screens, and solar energy and electronic products.
Description
Technical field
The present invention be more particularly directed to a kind of electrically conducting transparent heat conducting film based on functionalization graphene and preparation method thereof, belong to material sciemtifec and technical sphere.
Background technology
Graphene is the 5th kind of allotropic substance of carbon after diamond, graphite, soccerballene, carbon nanotube, and it has excellent mechanical property, electric property, and such as, its Young's modulus about 1000 GP, electronic conduction speed is up to 8 × 10
5m/s, thus has wide practical use in field of photoelectric technology.
The important potential application direction of of current Graphene prepares transparent conductive film.The preparation of existing transparent graphene conductive film has graphite oxide preparation method, graphite method, matrix material method, CVD with starting material classification, has spray deposition, filter deposition method, CVD, spin coating method, electrophoretic deposition, self-assembly method etc. with preparation method classification.
Wherein, graphite oxide method can be realized by the following two kinds mode: (1) hydrazine steam reduction graphene oxide membrane, reheating annealing reduction; (2) there iing dispersion agent to deposit chemical reduction graphene oxide solution in case, obtaining graphene film by the graphene oxide solution of reduction, reheating annealing reduction.In first kind of way, because the vapour permeability of grapheme material is poor, steam reduction can only be worked in uppermost surface, causes sheet resistance to reach capacity along with the thickness increase of film.And second way complicated operation, the covalency of graphene oxide sheet or non-covalent change are needed, to enable obtained redox graphene sheet disperse in the solution, but mixing of dispersion agent can cause unmodifiable photoelectric properties to affect on Graphene transparent conductive material.
Thus, the preparation method of existing transparent graphene conductive film and the transparent graphene conductive film of preparation thereof are still difficult to use in commercial purpose.
Summary of the invention
The object of the present invention is to provide a kind of electrically conducting transparent heat conducting film based on functionalization graphene and preparation method thereof, to overcome deficiency of the prior art.
For realizing aforementioned invention object, the technical solution used in the present invention is as follows:
Based on a preparation method for the electrically conducting transparent heat conducting film of functionalization graphene, comprise the steps:
(1) functionalization graphene be dispersed in selected solvent form dispersion liquid, and by described dispersion on selected matrix, form transparent or semitransparent film,
(2) by after described transparent or semitransparent film drying, insert in protective atmosphere and carry out pyroprocessing, after cooling, obtain electrically conducting transparent heat conducting film.
As one of feasible embodiment, step (1) can comprise: be dissolved in selected solvent by the mixture of functionalization graphene and linking agent and form dispersion liquid.
As one of comparatively preferred embodiment, described dispersion liquid comprises 0.1 ~ 20 wt % functionalization graphene.
Further, described functionalization graphene can be selected from ammonification, thiol-based or sulfonated graphene.
Further, described selected solvent can be selected from but be not limited to water, ethanol, DMF or acetone.
Further, described selected matrix can be selected from but be not limited to Copper Foil, silicon chip, glass or polymeric membrane.
As one of comparatively preferred embodiment, step (1) comprising: be coated on by dispersion liquid on selected matrix, forms the transparent or semitransparent film that thickness is 200nm ~ 20 μm.
As one of comparatively preferred embodiment, the resistance of transparent or semitransparent film is after drying 10
9~ 10
5Ω/, transmittance is 80 ~ 95%.
Further, the coating method adopted in step (1) can be selected from but is not limited to spraying, roller coating, spin coating or hangs painting method.
As one of comparatively preferred embodiment; step (2) comprising: dried transparent or semitransparent film is inserted protective atmosphere; higher than 1000 DEG C, but carry out pyroprocessing less than or equal under the condition of 2800 DEG C, after cooling, obtain electrically conducting transparent heat conducting film.
Further, described protective atmosphere can be formed by argon gas, helium, nitrogen, hydrogen etc.
Adopt the electrically conducting transparent heat conducting film based on functionalization graphene prepared by any one method aforementioned.
Further, the resistance of the described electrically conducting transparent heat conducting film based on functionalization graphene is 10
3~ 10
-2Ω/, transmittance is 80 ~ 95%, and thermal conductivity is 80 ~ 2000W/m. DEG C.
Compared with prior art, advantage of the present invention comprises: prepare electrically conducting transparent heat conducting film by adopting functionalization graphene as raw material, technique is simple, be easy to regulation and control, with low cost, can realize continuous operations, the electrically conducting transparent heat conducting film width that single is produced can reach 2 meters, and the electrically conducting transparent heat conducting film that obtains has excellent conductive, heat conduction and light transmission, the fields such as touch-screen, sun power and electronic product can be widely used in.
Embodiment
Be described in detail to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not making creative work, all belongs to the scope of protection of the invention.
Below in conjunction with some embodiments, technical scheme of the present invention is further described.Various raw materials involved in following embodiment, such as graphene oxide, sulfonated graphene, thiol-based Graphene etc. are all produced by the approach known to industry or are bought.
embodiment 1:ammonification Graphene is made into 2%(wt) aqueous solution of concentration, adopt the method for spraying on Copper Foil, apply the thick nesa coating of one deck 2 μm, after drying, recording sheet resistance is 8.7*10
10Ω/, film transmittance 87%; Dried film is when logical nitrogen protection through 1200 DEG C of pyroprocessing, and obtaining sheet resistance is 350 Ω/, and heat conduction is the transparent film of 108 W/m. DEG C.
embodiment 2:sulfonated graphene is made into 10%(wt) aqueous solution of concentration, adopt the method for roller coating to apply the thick nesa coating of one deck 1 μm on the glass substrate, after drying, recording sheet resistance is 5.3*10
7Ω/, film transmittance 89%; Dried film is when logical nitrogen protection through 1200 DEG C of pyroprocessing, and obtaining sheet resistance is 78 Ω/, and heat conduction is the transparent film of 310 W/m. DEG C, and this film can replace ito film to be used for electronic touch screen and electronics compliant conductive product.
embodiment 3:thiol-based Graphene is made into 1%(wt) ethanolic soln of concentration, adopt the method for spraying on PET, apply the thick nesa coating of one deck 600nm, after drying, recording sheet resistance is 12*10
10Ω/; Dried film is when logical nitrogen protection through 1600 DEG C of pyroprocessing, and obtaining sheet resistance is 0.25 Ω/, and heat conduction is the transparent film of 946 W/m. DEG C, film transmittance 92%.
reference examples 1:graphene oxide is made into 2%(wt) aqueous solution of concentration, adopt suction filtration mode to form the film of thick about 20 μm, after drying when logical nitrogen protection through 1000 DEG C of pyroprocessing, obtaining sheet resistance is 8760 Ω/, and heat conduction is 8 W/m. DEG C.
reference examples 2:graphene oxide is made into 1%(wt) ethanolic soln of concentration; adopt the method for spraying on PET, apply the transparent film forming thick about 600nm; after drying when logical nitrogen protection through 600 DEG C of pyroprocessing; obtaining sheet resistance is 2568 Ω/; heat conduction is the transparent film of 13 W/m. DEG C, and film transmittance is 90%.
Should be appreciated that the above is only the specific embodiment of the present invention, should be understood that; for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1., based on a preparation method for the electrically conducting transparent heat conducting film of functionalization graphene, it is characterized in that comprising the steps:
(1) functionalization graphene be dispersed in selected solvent form dispersion liquid, and by described dispersion on selected matrix, form transparent or semitransparent film,
(2) by after described transparent or semitransparent film drying, insert in protective atmosphere and carry out pyroprocessing, after cooling, obtain electrically conducting transparent heat conducting film.
2. according to claim 1 based on the preparation method of the electrically conducting transparent heat conducting film of functionalization graphene, it is characterized in that step (1) comprising: be dissolved in selected solvent by the mixture of functionalization graphene and linking agent and form dispersion liquid.
3. according to claim 1 or 2 based on the preparation method of the electrically conducting transparent heat conducting film of functionalization graphene, it is characterized in that described dispersion liquid comprises 0.1 ~ 20 wt % functionalization graphene.
4. according to claim 1 or 2 based on the preparation method of the electrically conducting transparent heat conducting film of functionalization graphene, it is characterized in that described functionalization graphene comprises ammonification, thiol-based or sulfonated graphene.
5. according to claim 1 or 2 based on the preparation method of the electrically conducting transparent heat conducting film of functionalization graphene, it is characterized in that described selected solvent comprises water, ethanol, DMF, NMP or acetone.
6. according to claim 1 or 2 based on the preparation method of the electrically conducting transparent heat conducting film of functionalization graphene, it is characterized in that step (1) comprising: be coated on by dispersion liquid on selected matrix, form the transparent film that thickness is 200nm ~ 20 μm.
7. according to claim 1 or 2 based on the preparation method of the electrically conducting transparent heat conducting film of functionalization graphene, it is characterized in that, the resistance of transparent film is after drying 10
9~ 10
5Ω/, transmittance is 80 ~ 95%.
8. according to claim 1 based on the preparation method of the electrically conducting transparent heat conducting film of functionalization graphene; it is characterized in that step (2) comprising: dried transparent or semitransparent film is inserted protective atmosphere; higher than 1000 DEG C; but carry out pyroprocessing less than or equal under the conditions of 2800 DEG C, after cooling, obtain electrically conducting transparent heat conducting film.
9. adopt the electrically conducting transparent heat conducting film based on functionalization graphene that according to any one of claim 1-8 prepared by method.
10. the electrically conducting transparent heat conducting film based on functionalization graphene according to claim 9, is characterized in that its resistance is 10
3~ 10
-2Ω/, transmittance is 80 ~ 95%, and thermal conductivity is 80 ~ 2000W/m. DEG C.
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| CN201410511439.0A CN104264146A (en) | 2014-09-29 | 2014-09-29 | Functionalized graphene-based transparent conductive heat-conducting film and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106191855A (en) * | 2016-08-19 | 2016-12-07 | 上海华友金裕微电子有限公司 | A kind of surface treatment method of Graphene bistrique |
| CN107850871A (en) * | 2015-07-13 | 2018-03-27 | 高通股份有限公司 | For wearable device by using thermal solution of the wrist strap as fin |
| EP3656894A1 (en) * | 2018-11-25 | 2020-05-27 | Nanjing Graphene Research Institute Corporation | Method for electroplating copper on non-metallic surfaces using graphene-based ink |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913592A (en) * | 2010-08-10 | 2010-12-15 | 浙江大学 | Covalent functionalized graphene and preparation method 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 |
-
2014
- 2014-09-29 CN CN201410511439.0A patent/CN104264146A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913592A (en) * | 2010-08-10 | 2010-12-15 | 浙江大学 | Covalent functionalized graphene and preparation method 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 |
Non-Patent Citations (1)
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|---|
| 黄毅等: "石墨烯的功能化及其相关应用", 《中国科学 B辑：化学》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107850871A (en) * | 2015-07-13 | 2018-03-27 | 高通股份有限公司 | For wearable device by using thermal solution of the wrist strap as fin |
| CN107850871B (en) * | 2015-07-13 | 2020-08-14 | 高通股份有限公司 | Method and apparatus for using a wristband as a wearable device heat sink |
| CN106191855A (en) * | 2016-08-19 | 2016-12-07 | 上海华友金裕微电子有限公司 | A kind of surface treatment method of Graphene bistrique |
| EP3656894A1 (en) * | 2018-11-25 | 2020-05-27 | Nanjing Graphene Research Institute Corporation | Method for electroplating copper on non-metallic surfaces using graphene-based ink |
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