CN107973290A - Elastic graphite alkene Heat Conduction Material and preparation method thereof - Google Patents
Elastic graphite alkene Heat Conduction Material and preparation method thereof Download PDFInfo
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- CN107973290A CN107973290A CN201711200131.4A CN201711200131A CN107973290A CN 107973290 A CN107973290 A CN 107973290A CN 201711200131 A CN201711200131 A CN 201711200131A CN 107973290 A CN107973290 A CN 107973290A
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- graphene oxide
- heat conduction
- graphite alkene
- conduction material
- elastic graphite
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- 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
- C01B2204/20—Graphene characterized by its properties
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- 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
- C01B2204/20—Graphene characterized by its properties
- C01B2204/24—Thermal properties
Abstract
The invention discloses a kind of elastic graphite alkene Heat Conduction Material and preparation method thereof.The preparation method includes：The graphene oxide slurry that solid content is 1~5wt% is provided, and by the graphene oxide slurry coating film forming, removes wherein 80~90% solvent afterwards, forms half-dried graphene oxide film；By the half-dried graphene oxide film in 50~10 DEG C of freeze-dryings, absolutely dry graphene oxide film is obtained；By the absolutely dry graphene oxide film in 90~180 DEG C of preliminary reduction treatments, keep the temperature 1~4h, handled after 800~2500 DEG C of high temperature reductions, keep the temperature 0.5~2h, obtain the elastic graphite alkene Heat Conduction Material.Method provided by the invention is easy to operate, and wherein naturally dry enables to the graphene oxide on surface to form orientation；Using lyophilized so that fitted closely between the graphene oxide layer of material internal, form orientation, and loose structure is presented in material internal.So that material shows good compression resilience.
Description
Technical field
The present invention is more particularly directed to a kind of elastic graphite alkene Heat Conduction Material and preparation method thereof, belongs to grapheme material and prepares skill
Art field.
Background technology
Graphene has excellent heat conductivility, its theoretical thermal conductivity is 5000W/mK.Prepared by existing various graphenes leads
The relevant report of hotting mask.Prepared graphene heat conducting film is two dimensional surface film at present, such heat conducting film thermal conductivity is high, but
Without compression resilience, if applying to non-smooth device surface heat dissipation, then have and contact phenomenon that is bad or cannot contacting, therefore
Application in some fields is restricted.
The content of the invention
It is existing to overcome it is a primary object of the present invention to provide a kind of elastic graphite alkene Heat Conduction Material and preparation method thereof
Technical deficiency.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：
An embodiment of the present invention provides a kind of preparation method of elastic graphite alkene Heat Conduction Material, including：
The graphene oxide slurry that solid content is 1~5wt% is provided, and by the graphene oxide slurry coating film forming,
Wherein 80~90% solvent is removed afterwards, forms half-dried graphene oxide film；
By the half-dried graphene oxide film in -50~-10 DEG C of freeze-dryings, it is thin to obtain absolutely dry graphene oxide
Film；
By the absolutely dry graphene oxide film in 90~180 DEG C of preliminary reduction treatments, keep the temperature 1~4h, after 800
~2500 DEG C of high temperature reduction processing, keep the temperature 0.5~2h, obtain the elastic graphite alkene Heat Conduction Material.
The embodiment of the present invention is additionally provided by the elastic graphite alkene Heat Conduction Material for stating method preparation, is distributed in the bullet
Property graphene Heat Conduction Material surface, the orientation of internal graphene it is different, and the elastic graphite alkene Heat Conduction Material include by
It is orientated the loose structure that different graphenes is enclosed.
Compared with prior art, advantages of the present invention includes：Method provided by the invention is easy to operate, wherein naturally dry
The graphene oxide on surface is enabled to form orientation；Using lyophilized so that tight between the graphene oxide layer of material internal
Closely connected conjunction, forms orientation, and loose structure is presented in material internal.So that material shows good compression resilience.
The elastic graphite alkene Heat Conduction Material under less than 60N pressure can Repeated Compression rebound it is tens of time, rebound degree is more than
80%, thermal conductivity factor reaches as high as 500W/mK, 10~20W/mK of vertical direction thermal conductivity factor on in-plane.
Brief description of the drawings
Fig. 1 is a kind of structure diagram of elastic graphite alkene heat conduction film in an exemplary embodiments of the invention.
Embodiment
In view of deficiency of the prior art, inventor is able to propose the present invention's through studying for a long period of time and largely putting into practice
Technical solution.The technical solution, its implementation process and principle etc. will be further explained as follows.
An embodiment of the present invention provides a kind of preparation method of elastic graphite alkene Heat Conduction Material, including：
The graphene oxide slurry that solid content is 1~5wt% is provided, and by the graphene oxide slurry coating film forming,
Wherein 80~90% solvent is removed afterwards, forms half-dried graphene oxide film；
By the half-dried graphene oxide film in -50~-10 DEG C of freeze-dryings, it is thin to obtain absolutely dry graphene oxide
Film；
By the absolutely dry graphene oxide film in 90~180 DEG C of preliminary reduction treatments, keep the temperature 1~4h, after 800
~2500 DEG C of high temperature reduction processing, keep the temperature 0.5~2h, obtain the elastic graphite alkene Heat Conduction Material.
Further, the preparation method includes：Graphene oxide is prepared using Hummers methods are improved, and by the oxygen
Graphite alkene prepares to form the graphene oxide slurry.
Further, the piece number of plies of the graphene oxide is 1~10 layer, and piece footpath is 5~50 μm.
Further, the preparation method includes：After by the graphene oxide slurry coating film forming, with naturally dry
Mode remove wherein 80~90% solvent.
The embodiment of the present invention is additionally provided by the elastic graphite alkene Heat Conduction Material for stating method preparation, is distributed in the bullet
Property graphene Heat Conduction Material surface, the orientation of internal graphene it is different, and the elastic graphite alkene Heat Conduction Material include by
It is orientated the loose structure that different graphenes is enclosed.
Further, combine closely between graphene sheet layer therein, loose structure is based on closed pore.
Further, the porosity of the graphene film is 50~99%, and the aperture of the loose structure is 1~200 μ
m。
Further, the elastic graphite alkene Heat Conduction Material for flexibility and is capable of the graphene film of compression rebound.
Further, the rebound degree of the graphene film is more than 80%.
Preferably, the thickness of the graphene film is 100~3000 μm.
Further, thermal conductivity factor of the graphene film on membrane plane direction is 100~500W/mK, vertical
In 10~20W/mK of thermal conductivity factor on membrane plane direction.
Wherein, the improvement Hummers methods prepare the method for graphene oxide and see D.C.Marcano,
D.V.Kosynkin, ACS Nano, 2010,4,4806.
The technical solution, its implementation process and principle etc. will be further explained in conjunction with specific embodiments as follows
It is bright.
Embodiment 1
(1) the graphene oxide slurry coating film forming that solid content is 3wt%, naturally dry to 80~90% solvents are waved
Hair；
(2) graphene oxide membrane after drying carries out -28 DEG C of freeze-dryings, obtains absolutely dry graphene oxide membrane；
(3) obtained absolutely dry graphene oxide membrane is subjected to 120 DEG C of preliminary reduction, when insulation 3 is small after, carry out 800 DEG C of height
Temperature reduction, continue insulation 1 it is small when, obtain elastic graphite alkene Heat Conduction Material.
Embodiment 2
(1) the graphene oxide slurry coating film forming that solid content is 5wt%, naturally dry to 80~90% solvents are waved
Hair；
(2) graphene oxide membrane after drying carries out -28 DEG C of freeze-dryings, obtains absolutely dry graphene oxide membrane；
(3) obtained absolutely dry graphene oxide membrane is subjected to 120 DEG C of preliminary reduction, when insulation 3 is small after, carry out 800 DEG C of height
Temperature reduction, continue insulation 1 it is small when, obtain elastic graphite alkene Heat Conduction Material.
Embodiment 3
(1) the graphene oxide slurry coating film forming that solid content is 3wt%, naturally dry to 80~90% solvents are waved
Hair；
(2) graphene oxide membrane after drying carries out -50 DEG C of freeze-dryings, obtains absolutely dry graphene oxide membrane；
(3) obtained absolutely dry graphene oxide membrane is subjected to 120 DEG C of preliminary reduction, when insulation 3 is small after, carry out 800 DEG C of height
Temperature reduction, continue insulation 1 it is small when, obtain elastic graphite alkene Heat Conduction Material.
Embodiment 4
(1) the graphene oxide slurry coating film forming that solid content is 3wt%, naturally dry to 80~90% solvents are waved
Hair；
(2) graphene oxide membrane after drying carries out -10 DEG C of freeze-dryings, obtains absolutely dry graphene oxide membrane；
(3) obtained absolutely dry graphene oxide membrane is subjected to 120 DEG C of preliminary reduction, when insulation 3 is small after, carry out 800 DEG C of height
Temperature reduction, continue insulation 1 it is small when, obtain elastic graphite alkene Heat Conduction Material.
Embodiment 5
(1) the graphene oxide slurry coating film forming that solid content is 3wt%, naturally dry to 80~90% solvents are waved
Hair；
(2) graphene oxide membrane after drying carries out -28 DEG C of freeze-dryings, obtains absolutely dry graphene oxide membrane；
(3) obtained absolutely dry graphene oxide membrane is subjected to 120 DEG C of preliminary reduction, when insulation 3 is small after, carry out 2500 DEG C of height
Temperature reduction, continue insulation 1 it is small when, obtain elastic graphite alkene Heat Conduction Material.
Comparative example 1
(1) the graphene oxide slurry coating film forming that solid content is 3wt%, naturally dry to 80~90% solvents are waved
Hair；
(2) graphene oxide membrane after drying carries out -28 DEG C of freeze-dryings, obtains absolutely dry graphene oxide membrane；
(3) by obtained absolutely dry graphene oxide membrane carry out 120 DEG C reduction, insulation 3 it is small when after, obtain elastic graphite alkene and lead
Hot material.
Comparative example 2
(1) the graphene oxide slurry coating film forming by solid content for 3wt%；
(2) -28 DEG C of freeze-dryings are carried out to coated graphene oxide membrane, obtain absolutely dry graphene oxide membrane；
(3) obtained absolutely dry graphene oxide membrane is subjected to 120 DEG C of preliminary reduction, when insulation 3 is small after, carry out 800 DEG C of height
Temperature reduction, continue insulation 1 it is small when, obtain elastic graphite alkene Heat Conduction Material.
The compression rebound rate for measuring the grapheme material that different embodiments and comparative example obtain respectively (refers to GB/T 6669-
2008, measure permanent deformation P, compression rebound rate：) and thermal conductivity factor R=1-P.
1. embodiment 1~5 of table, the thermal conductivity factor and rebound degree measurement result of the grapheme material that comparative example 1,2 is obtained
Method provided by the invention is easy to operate, and wherein naturally dry enables to the graphene oxide formation on surface to take
To；Using lyophilized so that fitted closely between the graphene oxide layer of material internal, form orientation, and material internal is presented
Loose structure.So that material shows good compression resilience；
The elastic graphite alkene Heat Conduction Material under less than 60N pressure can Repeated Compression rebound it is tens of time, rebound degree is more than
80%, graphene film thermal conductivity factor on membrane plane direction reaches as high as 500W/mK, film vertical direction thermal conductivity factor 10~
20W/mK。
It should be appreciated that the technical concepts and features of above-described embodiment only to illustrate the invention, its object is to allow be familiar with this
The personage of item technology can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all
The equivalent change or modification that Spirit Essence is made according to the present invention, should be covered by the protection scope of the present invention.
Claims (10)
- A kind of 1. preparation method of elastic graphite alkene Heat Conduction Material, it is characterised in that including：The graphene oxide slurry that solid content is 1~5wt% is provided, and by the graphene oxide slurry coating film forming, afterwards Wherein 80~90% solvent is removed, forms half-dried graphene oxide film；By the half-dried graphene oxide film in -50~-10 DEG C of freeze-dryings, absolutely dry graphene oxide film is obtained；By the absolutely dry graphene oxide film in 90~180 DEG C of preliminary reduction treatments, keep the temperature 1~4h, after 800~ 2500 DEG C of high temperature reduction processing, keep the temperature 0.5~2h, obtain the elastic graphite alkene Heat Conduction Material.
- 2. preparation method according to claim 1, it is characterised in that including：Oxidation stone is prepared using Hummers methods are improved Black alkene, and the graphene oxide is prepared to form the graphene oxide slurry.
- 3. preparation method according to claim 2, it is characterised in that：The piece number of plies of the graphene oxide is 1~10 layer, Piece footpath is 5~50 μm.
- 4. preparation method according to claim 1, it is characterised in that including：It is coated into by the graphene oxide slurry After film, wherein 80~90% solvent is removed in a manner of naturally dry.
- 5. elastic graphite alkene Heat Conduction Material prepared by the method as any one of claim 1-4, it is characterised in that：It is distributed in The elastic graphite alkene Heat Conduction Material surface, the orientation of internal graphene are different, and the elastic graphite alkene Heat Conduction Material Include the loose structure being enclosed by being orientated different graphenes.
- 6. elastic graphite alkene Heat Conduction Material according to claim 5, it is characterised in that：The porosity of the graphene film For 50~99%, the aperture of the loose structure is 1~200 μm.
- 7. elastic graphite alkene Heat Conduction Material according to claim 5, it is characterised in that：The elastic graphite alkene Heat Conduction Material For flexibility and it is capable of the graphene film of compression rebound.
- 8. elastic graphite alkene Heat Conduction Material according to claim 7, it is characterised in that：The rebound degree of the graphene film More than 80%.
- 9. elastic graphite alkene Heat Conduction Material according to claim 5, it is characterised in that：The thickness of the graphene film is 100~3000 μm.
- 10. elastic graphite alkene Heat Conduction Material according to claim 5, it is characterised in that：The graphene film is put down in film Thermal conductivity factor on the direction of face is 100~500W/mK, in 10~20W/mK of thermal conductivity factor on membrane plane direction.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110318380A (en) * | 2019-07-08 | 2019-10-11 | 杭州高烯科技有限公司 | A kind of spilled-oil recovery unit |
| CN110342498A (en) * | 2019-07-08 | 2019-10-18 | 浙江大学 | A kind of graphene-based elastic structure and preparation method thereof |
| CN111574968A (en) * | 2020-05-22 | 2020-08-25 | 南京邮电大学 | Interface material with convertible heat conduction and heat insulation performance |
| CN111977639A (en) * | 2019-05-22 | 2020-11-24 | 常州第六元素材料科技股份有限公司 | Pre-reduced graphene oxide film and preparation method thereof, graphene heat conduction film and preparation method thereof |
| CN113265230A (en) * | 2021-06-07 | 2021-08-17 | 山东国烯新材料创新中心有限公司 | Graphene-based composite phase change material with graded heat conduction structure and preparation method thereof |
| CN114180558A (en) * | 2021-12-27 | 2022-03-15 | 广东墨睿科技有限公司 | Preparation method of graphene micro-nano cavity superconducting film, related product and application |
| CN115073793A (en) * | 2022-08-05 | 2022-09-20 | 常州富烯科技股份有限公司 | Graphene heat-conducting film, preparation method thereof and heat-conducting gasket |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111977639A (en) * | 2019-05-22 | 2020-11-24 | 常州第六元素材料科技股份有限公司 | Pre-reduced graphene oxide film and preparation method thereof, graphene heat conduction film and preparation method thereof |
| CN110318380A (en) * | 2019-07-08 | 2019-10-11 | 杭州高烯科技有限公司 | A kind of spilled-oil recovery unit |
| CN110342498A (en) * | 2019-07-08 | 2019-10-18 | 浙江大学 | A kind of graphene-based elastic structure and preparation method thereof |
| CN111574968A (en) * | 2020-05-22 | 2020-08-25 | 南京邮电大学 | Interface material with convertible heat conduction and heat insulation performance |
| CN113265230A (en) * | 2021-06-07 | 2021-08-17 | 山东国烯新材料创新中心有限公司 | Graphene-based composite phase change material with graded heat conduction structure and preparation method thereof |
| CN113265230B (en) * | 2021-06-07 | 2022-05-17 | 山东国烯新材料创新中心有限公司 | Graphene-based composite phase change material with graded heat conduction structure and preparation method thereof |
| CN114180558A (en) * | 2021-12-27 | 2022-03-15 | 广东墨睿科技有限公司 | Preparation method of graphene micro-nano cavity superconducting film, related product and application |
| CN114180558B (en) * | 2021-12-27 | 2023-09-08 | 广东墨睿科技有限公司 | Preparation method of graphene micro-nano cavity superconducting film, related product and application |
| CN115073793A (en) * | 2022-08-05 | 2022-09-20 | 常州富烯科技股份有限公司 | Graphene heat-conducting film, preparation method thereof and heat-conducting gasket |
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Application publication date: 20180501 |