CN107794388A - A kind of preparation method of high heat conduction graphene doped and compounded sheet material - Google Patents
A kind of preparation method of high heat conduction graphene doped and compounded sheet material Download PDFInfo
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- CN107794388A CN107794388A CN201710755339.6A CN201710755339A CN107794388A CN 107794388 A CN107794388 A CN 107794388A CN 201710755339 A CN201710755339 A CN 201710755339A CN 107794388 A CN107794388 A CN 107794388A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/20—Use of vacuum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The present invention relates to a kind of preparation method of high heat conduction graphene doped and compounded sheet material, comprise the following steps：Graphene powder is prepared, graphene powder and metal-powder ball milling mixing are then obtained into mixed powder, mixed powder is finally placed in grinding tool into the sintering in vacuum sintering funace is prepared graphene doped composite metal sheet material.The method that the present invention is molded by powder mixed sintering prepares composite sheet, simple process, and other impurities are free of in sheet material, excellent thermal conductivity, and changes graphene orientation using hot-pressing sintering technique, further lifts heat conductivility.
Description
Technical field
The present invention relates to field of nanocomposite materials, and in particular to a kind of preparation of high heat conduction graphene doped and compounded sheet material
Method.
Background technology
Graphene (Graphene) is the only one layer of atomic thickness for being stripped out from graphite material, being made up of carbon atom
Two dimensional crystal.2004, Univ Manchester UK physicist An Deliegaimu and Constantine's Nuo Woxiao loves,
Graphene is isolated in success from graphite, it was demonstrated that therefore it can also obtain Nobel's thing in 2010 jointly with individualism, two people
Neo-Confucianism prize.Graphene is both most thin material, and most tough material, 200 times more taller than best steel of fracture strength.
It has good elasticity again simultaneously, and stretch range can reach the 20% of own dimensions.It is that current nature is most thin, intensity highest
Material, if making hammock with the graphene of one piece of 1 square metre of area, weight itself can be to bear one less than 1 milligram
One kilogram of cat.Graphene most potential application at present is the substitute as silicon, ultra micro transistor npn npn is manufactured, for producing
Following supercomputer.Substitute silicon with graphene, the speed of service of computer processor will be fast hundreds times.In addition, graphite
Alkene is almost fully transparent, only absorbs 2.3% light.On the other hand, it is very fine and close, even minimum gas atom
(helium atom) can not also penetrate.These features cause it to be highly suitable as the raw material of transparent electron product, such as transparent touch
Display screen, luminescent screen and solar panel.
A kind of novel nano-material most strong as the most thin, maximum intensity, electrical and thermal conductivity performance that have now been found that, graphene
It is referred to as " dark fund ", is " king of new material ", scientist even foretells that graphene " will thoroughly change 21 century ".
In general graphene and metallic composite panel are being passed through by the way that graphene and metal are respectively prepared after sheet
Gluing is compound, the complex process, and adhesive therebetween be present, influences product heat conductivility.
The content of the invention
It is existing to solve it is an object of the invention to provide a kind of preparation method of high heat conduction graphene doped and compounded sheet material
There is the problem of graphene composite sheet preparation technology in technology is complicated and properties of product are poor.
The invention provides a kind of preparation method of high heat conduction graphene doped and compounded sheet material, comprise the following steps：
(1) native graphite is mixed with acid solution, stirring at normal temperature 5min；Catalyst and expansion intercalator are successively added,
After continuing 5~10min of stirring, reaction 5min~1h is stored at room temperature, obtains graphene presoma；Graphene presoma water is more
Secondary flushing, it is subsequently placed in ultrasound in ultrasonic wave and peels off 5min~1h, obtain graphene dispersing solution；At graphene dispersing solution centrifugation
Reason, obtains primary graphene, and primary graphene is washed to multiple, then progress In-situ condensation drying, stone is obtained after moisture of going out
Black alkene powder；
(2) graphene powder that metal-powder and step (1) obtain is placed in ball grinder by a certain percentage, added quantitative
Absolute ethyl alcohol carry out ball milling 4-6h, by the mixed liquor after ball milling using Rotary drying instrument carry out vacuum rotating drying, mixed
Close powder；
(3) mixed powder that step (2) obtains is placed in graphite grinding tool, the sinter molding in vacuum sintering funace,
Obtain graphene doping metals composite sheet.
Further, the sintering temperature is 800-1600 DEG C, and sintering pressure is 20MPa~40Mpa, sintering time 1-
2h。
Further, the mass fraction of graphene powder described in step (2) is 2%-40%, the matter of the metal-powder
Amount fraction is 60%-98%.
Further, the metal is one or more of compositions in silver, copper, aluminium and iron.
Beneficial effect using the invention described above technical scheme is：
The method that the present invention is molded by powder mixed sintering prepares composite sheet, simple process, and is free of in sheet material
Other impurities, excellent thermal conductivity；The present invention finally uses hot-pressing sintering method, applies in composite sheet sintering process
20MPa~40Mpa, it is easy to graphene being more preferably orientated in sheet material, further lifts heat conductivility.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described, it is clear that described embodiment is part of the embodiment of the present invention, rather than
Whole embodiments.
Embodiment 1
The preparation method of graphene doped and compounded sheet material, comprises the following steps：
(1) native graphite is mixed with acid solution, stirring at normal temperature 5min；Catalyst and expansion intercalator are successively added,
Continue after stirring 5min, be stored at room temperature reaction 20min, obtain graphene presoma；Graphene presoma is rinsed 3 times with water,
It is subsequently placed in ultrasound in ultrasonic wave and peels off 20minh, obtains graphene dispersing solution；By graphene dispersing solution centrifugal treating, obtain just
Level graphene, primary graphene is washed 3 times, then carries out In-situ condensation drying, graphene powder is obtained after moisture of going out；
(2) graphene powder that copper powder and step (1) obtain is placed in ball grinder, adds quantitative absolute ethyl alcohol and carry out
Ball milling 4h, the mixed liquor after ball milling is subjected to vacuum rotating drying using Rotary drying instrument, obtains mixed powder；
(3) mixed powder that step (2) obtains is placed in graphite grinding tool, the sinter molding in vacuum sintering funace,
Sintering temperature is 1300 DEG C, sintering pressure 20MPa, sintering time 1h, obtains graphene doping metals composite sheet.
Embodiment 2
The preparation method of graphene doped and compounded sheet material, comprises the following steps：
(1) native graphite is mixed with acid solution, stirring at normal temperature 5min；Catalyst and expansion intercalator are successively added,
Continue after stirring 10min, be stored at room temperature reaction 1h, obtain graphene presoma；By graphene presoma with water rinse 3 times, so
After be placed in ultrasonic wave ultrasound and peel off 1h, obtain graphene dispersing solution；By graphene dispersing solution centrifugal treating, primary graphite is obtained
Alkene, primary graphene is washed 3 times, then carry out In-situ condensation drying, graphene powder is obtained after moisture of going out；
(2) graphene powder that silver powder and step (1) obtain is placed in ball grinder, adds quantitative absolute ethyl alcohol and carry out
Ball milling 6h, the mixed liquor after ball milling is subjected to vacuum rotating drying using Rotary drying instrument, obtains mixed powder；
(3) mixed powder that step (2) obtains is placed in graphite grinding tool, the sinter molding in vacuum sintering funace,
Sintering temperature is 1100 DEG C, sintering pressure 40MPa, sintering time 1h, obtains graphene doping metals composite sheet.
Embodiment 3
The preparation method of graphene doped and compounded sheet material, comprises the following steps：
(1) native graphite is mixed with acid solution, stirring at normal temperature 5min；Catalyst and expansion intercalator are successively added,
Continue after stirring 5min, be stored at room temperature reaction 30min, obtain graphene presoma；Graphene presoma is rinsed 3 times with water,
It is subsequently placed in ultrasound in ultrasonic wave and peels off 30min, obtains graphene dispersing solution；By graphene dispersing solution centrifugal treating, obtain just
Level graphene, primary graphene is washed to multiple, then progress In-situ condensation drying, graphene powder is obtained after moisture of going out；
(2) graphene powder that iron powder and step (1) obtain is placed in ball grinder, adds quantitative absolute ethyl alcohol and carry out
Ball milling 5h, the mixed liquor after ball milling is subjected to vacuum rotating drying using Rotary drying instrument, obtains mixed powder；
(3) mixed powder that step (2) obtains is placed in graphite grinding tool, the sinter molding in vacuum sintering funace,
Sintering temperature is 1600 DEG C, sintering pressure 40MPa, sintering time 2h, obtains graphene doping metals composite sheet.
Following table is the thermal conductivity of graphene doping metals composite sheet obtained by embodiment 1-3, and the method for testing of thermal conductivity is
Laser shines method：
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, either which part or all technical characteristic are entered
Row equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (4)
1. a kind of preparation method of high heat conduction graphene doped and compounded sheet material, it is characterised in that comprise the following steps：
(1) native graphite is mixed with acid solution, stirring at normal temperature 5min；Catalyst and expansion intercalator are successively added, is continued
After stirring 5~10min, reaction 5min~1h is stored at room temperature, obtains graphene presoma；Graphene presoma is repeatedly rushed with water
Wash, be subsequently placed in ultrasound in ultrasonic wave and peel off 5min~1h, obtain graphene dispersing solution；By graphene dispersing solution centrifugal treating,
Primary graphene is obtained, primary graphene is washed to multiple, then progress In-situ condensation drying, graphene is obtained after moisture of going out
Powder；
(2) graphene powder that metal-powder and step (1) obtain is placed in ball grinder by a certain percentage, adds quantitative nothing
Water-ethanol carries out ball milling 4-6h, and the mixed liquor after ball milling is carried out into vacuum rotating drying using Rotary drying instrument, obtains mixed powder
Body；
(3) mixed powder that step (2) obtains is placed in graphite grinding tool, the sinter molding in vacuum sintering funace, obtained
Graphene doping metals composite sheet.
2. the preparation method of graphene doped and compounded sheet material according to claim 1, it is characterised in that the sintering temperature
For 800-1600 DEG C, sintering pressure is 20MPa~40Mpa, sintering time 1-2h.
3. the preparation method of graphene doped and compounded sheet material according to claim 1, it is characterised in that institute in step (2)
The mass fraction for stating graphene powder is 2%-40%, and the mass fraction of the metal-powder is 60%-98%.
4. the preparation method of graphene doped and compounded sheet material according to claim 1, it is characterised in that the metal is
One or more of compositions in silver, copper, aluminium and iron.
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| CN201710755339.6A CN107794388A (en) | 2017-08-29 | 2017-08-29 | A kind of preparation method of high heat conduction graphene doped and compounded sheet material |
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| CN201710755339.6A CN107794388A (en) | 2017-08-29 | 2017-08-29 | A kind of preparation method of high heat conduction graphene doped and compounded sheet material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108950281A (en) * | 2018-08-22 | 2018-12-07 | 哈尔滨工业大学 | A kind of polyethylene glycol repairs the preparation method of graphene reinforced aluminum matrix composites |
| CN111365681A (en) * | 2020-04-18 | 2020-07-03 | 江西瀚霖智能车灯有限公司 | Vehicle headlamp and manufacturing method thereof |
| CN112852389A (en) * | 2021-03-23 | 2021-05-28 | 依润特工业智能科技(苏州)有限公司 | High-strength heat conduction material for 5G communication and preparation method thereof |
| CN117680676A (en) * | 2024-02-02 | 2024-03-12 | 深圳市绚图新材科技有限公司 | Preparation method of antioxidant high-conductivity graphene-copper composite powder |
-
2017
- 2017-08-29 CN CN201710755339.6A patent/CN107794388A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108950281A (en) * | 2018-08-22 | 2018-12-07 | 哈尔滨工业大学 | A kind of polyethylene glycol repairs the preparation method of graphene reinforced aluminum matrix composites |
| CN108950281B (en) * | 2018-08-22 | 2020-08-21 | 哈尔滨工业大学 | Preparation method of polyethylene glycol-repaired graphene-reinforced aluminum-based composite material |
| CN111365681A (en) * | 2020-04-18 | 2020-07-03 | 江西瀚霖智能车灯有限公司 | Vehicle headlamp and manufacturing method thereof |
| CN111365681B (en) * | 2020-04-18 | 2023-09-22 | 江西瀚霖智能车灯有限公司 | Headlight and manufacturing method thereof |
| CN112852389A (en) * | 2021-03-23 | 2021-05-28 | 依润特工业智能科技(苏州)有限公司 | High-strength heat conduction material for 5G communication and preparation method thereof |
| CN117680676A (en) * | 2024-02-02 | 2024-03-12 | 深圳市绚图新材科技有限公司 | Preparation method of antioxidant high-conductivity graphene-copper composite powder |
| CN117680676B (en) * | 2024-02-02 | 2024-05-14 | 深圳市绚图新材科技有限公司 | Preparation method of antioxidant high-conductivity graphene-copper composite powder |
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