CN108912803A - A kind of preparation method of graphene heat dissipation slurry - Google Patents
A kind of preparation method of graphene heat dissipation slurry Download PDFInfo
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- CN108912803A CN108912803A CN201810543032.4A CN201810543032A CN108912803A CN 108912803 A CN108912803 A CN 108912803A CN 201810543032 A CN201810543032 A CN 201810543032A CN 108912803 A CN108912803 A CN 108912803A
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- graphene
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- dissipation slurry
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
Abstract
A kind of preparation method of graphene heat dissipation slurry, belongs to field of novel carbon material, it is mainly concerned with the preparation of the preparation of graphene, graphene heat dissipation slurry.This method reacts mill method as raw material using graphite powder, carbon dioxide first and prepares functionalization graphene, then functionalization graphene is reduced to graphene, then mixes graphene under certain condition with certain proportion with binder, dispersing agent, diluent, auxiliary agent.The present invention prepares graphene using mechanical stripping method, is a kind of simple, environmental-friendly, efficient, inexpensive, new technology that can be grapheme modified with macroscopic preparation of graphene and edge.Preparation process of the present invention is simple, and perfect heat-dissipating, graphene is evenly distributed, low in cost, can volume production, this slurry can realize cooling application in various bases, have a extensive future.
Description
Technical field
The invention belongs to the preparation technical field of carbon material, be related to a kind of bigger serface, high-termal conductivity graphene and
The preparation method of perfect heat-dissipating, widely used graphene heat dissipation slurry, belongs to field of novel carbon material.
Background technique
It is well known that graphene is one of 21 century most promising material, graphene has highly stable structure, height
Carrier mobility, highly conductive and thermal conductivity, the specific surface area that superpower mechanicalness is easy, high and good optical transmittance etc.
Excellent physicochemical properties show in numerous tradition such as electronics, space flight, optics, Yi Yuan, environment, new material and emerging field
Wide application prospect out.
All there is fever serious situation in electronic product currently on the market, if heat distributes not in time, it will
Seriously affect the job stability and security reliability of electronic product.In addition, since electronic product has sternly weight and volume
The requirement of lattice, thermally conductive high, heat-transfer matcrial that density is small is by the particularly important of change.Graphene has high thermal conductivity (thermally conductive system
Number is up to 5300W/mK) and heat emissivity coefficient, much higher than the highest gold, silver of thermal coefficient, copper, aluminium in metal etc., and have
There is good flexibility, therefore graphene is applied to field of radiating, there is huge application prospect.However, existing graphite
Alkene preparation method is at high cost, low yield, pollution is big, risk is high, defect is big, prepared graphene heat dissipation slurry processing fiber crops
Tired, costly, heat dissipation effect is also undesirable.
Summary of the invention
The purpose of the present invention is to provide a kind of graphene heat dissipation slurries and preparation method thereof, electric in the prior art to solve
There is heat conduction and heat radiation hardly possible in sub- product.
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme that：
The present invention relates to a kind of preparation fields of carbon material, are related to a kind of using reaction mill method preparation high quality, big ratio
Surface area, fault of construction are small, can volume production graphene preparation method.
A kind of graphene heat dissipation slurry, which is characterized in that the component including following parts by weight：
Graphene is 1-40 parts, and dispersing agent is 0.5-5 parts, and solvent is 50-150 parts, and binder is 40-100 parts, and auxiliary agent is
1-10 parts.
A kind of preparation method of above-mentioned graphene heat dissipation slurry, includes the following steps：
First graphite powder, carbon dioxide are placed in reaction mill equipment, reaction mill equipment is sealed, starting reaction mill equipment,
After reacting a period of time, functionalization graphene is obtained；Functionalization graphene is reduced to graphene again, then by graphene and is dispersed
0.1-6h is mixed in agent, solvent, and graphene dispersing solution is made in ultrasonic disperse 0.5-10h, then by graphene dispersing solution and viscous
Knot agent, auxiliary agent are mixed, then grinding distribution 0-12h, and graphene heat dissipation slurry is made.
Reaction mill equipment selects tube mill, from planetary ball mill, horizontal ball mill, sand mill and bar type ball mill
One kind.
Graphite powder is one or more of natural flake graphite, amorphous graphite, blocky graphite or aquadag.
Total amount of fill of graphite powder is the 1/8-2/3 for reacting grinding jar body total volume.
Carbon dioxide gas is filled in reaction mill equipment, charged pressure 0.1MPa-25MPa.
Reaction mill equipment is reacted with the revolving speed continuously grinding of 100-5000rpm；Reaction is consumed time：3-72 hours.
Functionalization graphene be reduced to method that graphene uses be direct reducer reduction method, Microwave-assisted Reduction method,
One or more of ultraviolet irradiation reduction method, chemical reduction method, electrochemical reducing or thermal reduction.
The dispersing agent be cyclodextrin, N-Methyl pyrrolidone, n-methyl-2-pyrrolidone, fatty alcohol polyoxyethylene ether,
One or more of mono alkenyl butyryl imines, oleic acid, neopelex or cetyl trimethylammonium bromide.
The solvent is water, alcohols solvent, esters solvent, ketones solvent, ether solvent, benzene, dimethyl sulfoxide, ethylenediamine
Or one or more of dimethylbenzene.
The binder be rosin, epoxy resin, phenolic resin, acrylic resin, synthetic cellulose, organic siliconresin,
One or more of polyester resin.
The auxiliary agent is in diluent, defoaming agent, stabilizer, levelling agent, preservative, crosslinking agent, film forming agent or tackifier
One or more.
In above-mentioned graphene heat dissipation slurry, graphene thermal conductivity is high, and thermal coefficient is up to 5300W/mK.The present invention with
Macromolecule resin makees binder, and graphene is Heat Conduction Material, is coated in heat source surface with slurry obtained by above-mentioned material prescription,
Since graphene can distribute rapid thermal in the form of convection current, infra-red radiation, heat source temperature can be greatly lowered
Degree, can solve that electronic product heat conduction and heat radiation currently on the market is difficult, common heat dissipation product heat dissipation effect is undesirable, not can solve electricity
The problems such as sub- product heat dissipation hardly possible.
Above-mentioned preparation method simple process, easy for construction flexibly cost is relatively low, easily solid, has excellent heat conduction and heat radiation
Function.Graphene used in the present invention is prepared with mechanical stripping method, and fault of construction is small, at low cost, can volume production.The present invention produces work
Skill is safe and simple, low in cost, environmentally protective, has significant market application value.
Detailed description of the invention：
Fig. 1 is the Raman figure of functionalization graphene made from present example；
Fig. 2 is the XRD diagram of functionalization graphene made from present example；
Fig. 3 is the infrared figure of functionalization graphene made from present example；
Fig. 4 is the SEM figure of functionalization graphene made from present example.
Fig. 5 is the heat dissipation effect test result figure of each made slurry of example of the present invention.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be understood that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
Embodiment 1
(1) planetary ball mill ball grinder is taken out, adds zirconium oxide bead into reaction mill equipment, continues to add natural squama
Piece graphite powder seals ball grinder, until zirconium oxide bead and reactant total volume reach the 1/3 of tank body volume into ball grinder
Carbon dioxide gas is poured, then releases gas, so in triplicate.Carbon dioxide gas is filled with into ball grinder again, until
Pressure reaches between 0.1MPa-25MPa, fastens air valve, and ball grinder is mounted on ball mill.
(2) setting drum's speed of rotation be 800rpm, start ball mill, continuous operation 36 hours.Air valve is opened, sample is screened out
Product are to get functionalization graphene.Gained limbic function graphite alkene specific surface area is up to 639m2/g。
(3) functionalization graphene is reduced to graphene with hydro-thermal method.Take 5 parts of graphenes, 1 part of dispersing agent, 50 parts of solvents
Blender is added after mixing and stirs 4h, graphene dispersing solution is made in re-ultrasonic dispersion 7h.
(4) 60 parts of binders, 2 parts of auxiliary agents and (3) middle gained graphene dispersing solution mixing are taken, nano-level grinder grinding is added
Disperse 3h, as graphene heat dissipation slurry.
Embodiment 2
(1) graphene preparation method such as embodiment 1.
(2) blender stirring 4h, re-ultrasonic dispersion is added after taking 7 parts of graphenes, 1.3 parts of dispersing agents, 62 parts of solvent mixing
Graphene dispersing solution is made in 7h.
(4) 67 parts of binders, 2.3 parts of auxiliary agents and (3) middle gained graphene dispersing solution mixing are taken, nano-level grinder is added and grinds
Mill dispersion 3h, as graphene heat dissipation slurry.
Fig. 1-Fig. 4 is various phenograms of the embodiment 1 using the carboxylated graphene of reaction mill method preparation.
The heat dissipation slurry of graphene obtained by the various embodiments described above 1 and 2 is scratched respectively in Kapton (5cm*
On 5cm), it is 30 μm or so that it is identical, which to starch thickness, for control graphene heat dissipation, and the polyimides without graphene coated heat dissipation slurry is thin
Film, the Kapton of coating 1 graphene of embodiment heat dissipation slurry, the polyimides of coating 2 graphene of embodiment heat dissipation slurry are thin
Film is placed on same warm table simultaneously and is heated simultaneously, each with infrared thermometer (Xi Ma -852B) real-time detection
The temperature of a Kapton, and note down (since 25 DEG C of room temperature), temperature-time curve is made, referring to Fig. 5.
Claims (10)
1. a kind of preparation method of graphene heat dissipation slurry, which is characterized in that including graphene, dispersing agent, solvent, binder,
Auxiliary agent；Preparation method includes the following steps：First graphite powder, carbon dioxide are placed in reaction mill equipment, reaction mill equipment is close
Envelope, starting reaction mill equipment obtain functionalization graphene after reacting a period of time；Functionalization graphene is reduced to graphite again
Alkene, then 0.1-6h is mixed in graphene and dispersing agent, solvent, graphene dispersing solution is made, so in ultrasonic disperse 0.5-10h
Graphene dispersing solution is mixed afterwards, then grinding distribution 0-12h with binder, auxiliary agent, graphene heat dissipation slurry is made.
2. a kind of preparation method of graphene heat dissipation slurry described in accordance with the claim 1, which is characterized in that graphene 1-40
Part, dispersing agent is 0.5-5 parts, and solvent is 50-150 parts, and binder is 40-100 parts, and auxiliary agent is 1-10 parts.
3. a kind of preparation method of graphene heat dissipation slurry described in accordance with the claim 1, which is characterized in that reaction mill equipment choosing
Tube mill, from one of planetary ball mill, horizontal ball mill, sand mill and bar type ball mill；Graphite powder is always filled out
Loading amount is the 1/8-2/3 for reacting grinding jar body total volume；Carbon dioxide gas is filled in reaction mill equipment, charged pressure is
0.1MPa-25MPa；Reaction mill equipment is reacted with the revolving speed continuously grinding of 100-5000rpm；Reaction is consumed time：3-72 hours.
4. a kind of preparation method of graphene heat dissipation slurry described in accordance with the claim 1, which is characterized in that graphite powder is natural
One or more of crystalline flake graphite, amorphous graphite, blocky graphite or aquadag.
5. a kind of preparation method of graphene heat dissipation slurry described in accordance with the claim 1, which is characterized in that functionalization graphene
The method that graphene uses is reduced to go back for direct reducer reduction method, Microwave-assisted Reduction method, ultraviolet irradiation reduction method, chemistry
One or more of former method, electrochemical reducing or thermal reduction.
6. a kind of preparation method of graphene heat dissipation slurry described in accordance with the claim 1, which is characterized in that the dispersing agent is
Cyclodextrin, N-Methyl pyrrolidone, n-methyl-2-pyrrolidone, fatty alcohol polyoxyethylene ether, mono alkenyl butyryl imines, oleic acid,
One or more of neopelex or cetyl trimethylammonium bromide.
7. a kind of preparation method of graphene heat dissipation slurry described in accordance with the claim 1, which is characterized in that the solvent is
One of water, alcohols solvent, esters solvent, ketones solvent, ether solvent, benzene, dimethyl sulfoxide, ethylenediamine or dimethylbenzene or
It is several.
8. a kind of preparation method of graphene heat dissipation slurry described in accordance with the claim 1, which is characterized in that the binder is
One of rosin, epoxy resin, phenolic resin, acrylic resin, synthetic cellulose, organic siliconresin, polyester resin are several
Kind.
9. a kind of preparation method of graphene heat dissipation slurry described in accordance with the claim 1, which is characterized in that the auxiliary agent is dilute
Release one or more of agent, defoaming agent, stabilizer, levelling agent, preservative, crosslinking agent, film forming agent or tackifier.
10. the graphene heat dissipation slurry being prepared according to the described in any item methods of claim 1-9.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110157266A (en) * | 2019-05-21 | 2019-08-23 | 常州威斯双联科技有限公司 | A kind of high thermal conductivity graphene Wave suction composite material and preparation method |
| CN111003706A (en) * | 2019-11-25 | 2020-04-14 | 苏州盈顺绝缘材料有限公司 | Preparation method of graphene heat conduction and dissipation material |
| CN113088037A (en) * | 2021-04-13 | 2021-07-09 | 珠海昌意新材料科技有限公司 | Heat dissipation material with high heat conductivity coefficient and high radiation coefficient and preparation method thereof |
| CN113717702A (en) * | 2021-08-31 | 2021-11-30 | 中钢天源股份有限公司 | Graphene composite radiating fin and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110157266A (en) * | 2019-05-21 | 2019-08-23 | 常州威斯双联科技有限公司 | A kind of high thermal conductivity graphene Wave suction composite material and preparation method |
| CN111003706A (en) * | 2019-11-25 | 2020-04-14 | 苏州盈顺绝缘材料有限公司 | Preparation method of graphene heat conduction and dissipation material |
| CN113088037A (en) * | 2021-04-13 | 2021-07-09 | 珠海昌意新材料科技有限公司 | Heat dissipation material with high heat conductivity coefficient and high radiation coefficient and preparation method thereof |
| CN113717702A (en) * | 2021-08-31 | 2021-11-30 | 中钢天源股份有限公司 | Graphene composite radiating fin and preparation method thereof |
| CN113717702B (en) * | 2021-08-31 | 2023-09-29 | 中钢天源股份有限公司 | Graphene composite cooling fin and preparation method thereof |
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Application publication date: 20181130 |