CN105542728A - Method for preparing vertical orientation graphene sheet/high polymer thermal interface material - Google Patents
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Abstract
The invention provides a method for preparing a vertical orientation graphene sheet/high polymer thermal interface material, and belongs to the field of preparation of heat radiation materials. The method comprises the steps that a graphene nanosheet with superhigh thermal conductivity is firstly prepared; then a hot press molding process is utilized for preparing the graphene nanosheet into a thin film with certain thickness; finally, a layer of polymer (such as PDMS) is infiltrated into the surface of the thin film, then the thin film is wound into a cylinder, and the graphene thin film is vertically arranged in the cylinder. The process is simple, the procedure is easy to control, industrial production is convenient, and the method is suitable for bath production. Due to the fact that the hot press process is adopted, graphene cannot be agglomerated, a continuous structure is formed in graphene, a thermal conduction network is formed, and heat can fast pass. The vertical orientation graphene sheet/high polymer thermal interface material has the superhigh thermal conductivity, and can be widely applied to the fields of LED illumination, electromagnetic shielding, electronic information, communication equipment, aerospace, automobiles, household appliances and the like.
Description
Technical field
The invention belongs to the preparation field of heat-conducting interface material, be specially the preparation method of a kind of high heat conductance vertical orientated graphene film/superpolymer heat interfacial material.
Background technology
Heat interfacial material (ThermalInterfaceMaterials, TIMs) be widely used in electronic element radiating field, it can be filled between electronic component and scatterer with expulsion air wherein, the heat that electronic component is produced can be delivered to scatterer by heat interfacial material more quickly, reaches the vital role reducing working temperature, increase the service life.Integrated level along with chip improves constantly and constantly increases with power dissipation density, the heat produced during chip operation gets more and more, if can not be shed by scatterer by these heats in time, the temperature of electronic component will not stop to rise, and has a strong impact on reliability and the work-ing life of electronic component.Electronic component is only relied on to contact with the direct of scatterer, effectively cannot carry out heat conduction, this is because always there is gully or the space of a lot of microcosmic between heat source surface and scatterer, wherein 80% volume is air---hot poor conductor, so had a strong impact on radiating efficiency.Therefore, need to use the air in the heat interfacial material eliminating gap of high heat conduction, enlarge active surface, sets up the green channel of quick conductive between electronic component and scatterer.Semi-conductor, electronic devices and components are usually all very sensitive to heat, and too high heat or for a long time heat all bring secure context and the actual problem used.Show that reason 50% that electronics lost efficacy is that temperature exceedes limit value and causes according to statistical information, electronic devices and components temperature often raises 1 DEG C in 70-80 DEG C of level, and reliability will decline 5%; Often raise 10 DEG C, failure rate exponentially increases an order of magnitude (i.e. " 10 DEG C of rules ").
Current most of heat interfacial material is thermal conductive polymer, and this material generally can be divided into eigenmode and filled-type two kinds.Wherein eigenmode thermal conductive polymer common are polyaniline, polyacetylene, polypyrrole etc., passage of heat is formed mainly through polymkeric substance super large conjugated system own or height-oriented property, but at present its electroconductibility is paid close attention to more to the research of this base polymer, fewer to the research of its heat conduction aspect, and this base polymer preparation and fabrication complex process, is difficult to accomplish scale production; Another kind of filled polymer preparation is compared and is easily realized, and namely by filling high heat conductive filler in the polymer, this is the modal preparation method of heat-conducting interface material.Heat-conducting interface material is made up of matrix and heat conductive filler two portions substantially, wherein filler to heat conduction network be formed to close important, at present, common heat conductive filler by its composition primarily of following: 1, inorganic non-metallic compound: Al
2o
3, BeO, MgO, ZnO, BN, AlN, Si
3n
4, SiC; 2, inorganic non-metallic simple substance: carbon black, graphite flake, carbon fiber, carbon nanotube, Graphene etc.; 3, metal-powder: copper, gold and silver, aluminium etc.
The high molecular heat conductivility of filled-type is determined jointly by macromolecule matrix and filler.When amount of filler is less time, dispersed filler is in the base separated by matrix, and between filler, not contact or interaction, little to the contribution of matrix material heat conductivility.When filler addition reaches a certain threshold value, contact with each other between filler, define chain or netted conductive structure, be called heat conduction network, now the heat conductivility of matrix material is able to effective raising.The factor such as thermal conductivity, loading level, size, geometrical shape, filler accumulation mode in the base, filling surface process, polymer-matrix interphase interaction of the heat conductivility of thermal conductive polymer matrix material and filler itself is closely related.
Carbon material has higher thermal conductivity because of it, causes the concern of investigator.Common carbon material has graphite (2000W/ (mK)), diamond (2300W/ (mK)), carbon black, carbon nanotube (CNT) (3000 ~ 3500W/ (mK)), Nano graphite lamella etc.Carbon nanotube has excellent heat conductivility, and thermal conductivity is 3000 ~ 3500W/ (mK), can be used as heat conductive filler.But carbon nanotube in use faces many problems.Although there are some researches show, carbon nanotube is when packing volume f≤7%, and thermal conductivity improves 50% ~ 250%.But carbon nanotube can not with matrix good coupling, its thermal boundary resistance reaches 10
-7m2K/W, causes thermal conductivity do not increase with addition and significantly improve.And the cost of carbon nanotube in industrial application is still very high, be difficult to reach aligning of carbon nanotube, thus effectively improve the thermal conductivity of material.
Graphene is the bi-dimensional cellular shape crystalline network that carbon atom becomes with sp2 key close-packed arrays, and its heat conductivility is better than carbon nanotube.Graphene has high thermal conductivity, and the thermal conductivity of single-layer graphene can reach 5300W/ (mK), and has good thermostability.And except there being high heat conductivity value, the two-dimentional geometrical shape of Graphene, with tight coupling and the low cost of body material, all makes Graphene become the ideal filler of boundary material.Research shows, the relative traditional interface thermally conductive material of thermal conductivity of graphene-based interface thermally conductive material can significantly improve.
Summary of the invention
The present invention proposes the preparation method of a kind of ultra-high conducting heating rate vertical orientated graphene film/superpolymer heat interfacial material.
Technical scheme of the present invention is as follows:
The first step take graphite as raw material, adopts liquid phase stripping method to prepare graphene oxide, and then high temperature reduction becomes Graphene (thickness is Nano grade, and size is hundreds of nanometer to several microns not etc.);
Second step, adopts hot press forming technology to prepare graphene film (having thermal conductivity in higher face, ~ 1800/W/mK);
3rd step, craft or mechanical means is adopted to be infiltrated by graphene film in polymkeric substance (as PDMS), make film surface cover the uncured polymkeric substance of one deck, then utilize centreless quilling that film is rolled into right cylinder, wherein the content of polymkeric substance can by the pressure-controlling in volume membrane process;
4th step, is placed in baking oven and carries out hot setting (set time is relevant with temperature) by products obtained therefrom, can cut into desired shape as required after product cooling.
Advantage of the present invention and positively effect:
Present invention process condition is simple, and flow process easily controls, and cost is low, is easy to suitability for industrialized production, and yield rate is high, and products obtained therefrom has higher thermal conductivity.Graphene can make full use of thermal conductivity in its higher face in conduction process, and graphene film is also continuous structure at product, can not affect heat conduction network, improve a lot to matrix material thermal conduction because of segmental defect.In addition the content of Graphene also can be controlled by technological process, thus obtains the product of different thermal conductivity.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is material structure figure.
Embodiment
Here be the experimentally room existence conditions related experiment of carrying out.
1, the preparation of graphene oxide
Main is basic raw material with natural flake graphite, and utilize and improve Hummers legal system for graphene oxide, its operation steps prepared is as follows:
(1) vitriol oil 200ml is placed in Erlenmeyer flask, adds 4g SODIUMNITRATE, Erlenmeyer flask is placed in water-bath (adding room temperature water), be stirred to SODIUMNITRATE and be dissolved completely in the vitriol oil;
(2) slowly add 4g graphite in whipping process, period controls the temperature of water-bath below 8 DEG C;
(3) slowly add 18g potassium permanganate in whipping process, control the temperature of water-bath below 8 DEG C;
(4) utilize sealed membrane to be sealed by Erlenmeyer flask, add appropriate ice cube in a water bath and maintain the temperature at about 0 DEG C, keep 2 hours;
(5) reaction unit is moved in the water-bath of 35 DEG C, stir simultaneously.Add 500ml deionized water, slowly add with dropper when just starting, keep temperature in Erlenmeyer flask to be no more than 80 DEG C;
(6) slowly add 40ml superoxol, stir a night;
(7) remove supernatant liquid after calmness, slowly add deionized water to 900ml, adding concentrated hydrochloric acid 100mlm, stir;
(8) repeating step (7) 2-3 time.
2, the reduction of Graphene
In order to obtain reducing the graphene powder of rear good dispersity, adopting freeze-drying instead of general heated drying here, more dried graphene oxide is reduced.General heated drying process, Graphene is easily reunited, thus causes bad dispersibility, and the uneven film thickness made is even.
Thermal reduction step is as follows:
(1) by gained graphene oxide solution centrifugal treating, unnecessary moisture is removed;
(2) graphene solution of high density is placed in refrigerator and cooled to freeze, and then carries out lyophilize in freeze drier;
(3) dried graphene oxide is placed in carries out thermal reduction (temperature rise rate 0.5 DEG C/min) with tube furnace.
3, the preparation of graphene film:
(1) weigh a certain amount of graphene powder, join in hot pressing die, constantly vibration makes graphene powder be uniformly dispersed, then hot pressing die is placed in tabletting machine and raises whole pressure and temperature;
(2) graphene film sample is taken out after keeping the temperature and pressure of certain hour;
(3) graphene film of taking-up is heated and is placed on two roll calender roll, repeatedly can thermal conductivity is higher in forming surface graphene film after calendering.
4, the preparation of vertical orientated graphene film/superpolymer heat interfacial material
Graphene film is cut into wide rectangular, and is immersed in PDMS solution and goes.Current employing be that the mode of manual winding is rolled into a certain thickness right cylinder by rectangular for Graphene, be then placed in baking oven and carry out hot setting, after cooling, be cut into suitable shape according to actual needs.
Describe preparation method provided by the present invention by specific embodiment above, it will be understood by those of skill in the art that in the scope not departing from essence of the present invention, certain conversion or amendment can be made to the present invention; Be not limited to content disclosed in embodiment.
Claims (7)
1. the preparation method of vertical orientated graphene film/superpolymer heat interfacial material:
The first step take graphite as raw material, adopts liquid phase stripping method to prepare graphene oxide, and then high temperature reduction becomes Graphene (thickness is Nano grade, and size is hundreds of nanometer to several microns not etc.);
Second step, adopts hot press forming technology to prepare graphene film (having thermal conductivity in higher face, ~ 1800/W/mK)
3rd step, craft or mechanical means is adopted to be infiltrated by graphene film in polymkeric substance (as PDMS), make film surface cover the uncured polymkeric substance of one deck, then utilize centreless quilling that film is rolled into right cylinder, wherein the content of polymkeric substance can by the pressure-controlling in volume membrane process;
4th step, is placed in baking oven and carries out hot setting (set time is relevant with temperature) by products obtained therefrom, can cut into desired shape as required after product cooling.
2. the method for claim 1, is characterized in that, in order to obtain the graphene powder of good dispersity in the first step, have employed the method for oxidation-centrifugal-lyophilize-reduction.
3. method as claimed in claim 2, is characterized in that, utilize graphite to obtain the lamellar graphite alkene of Nano grade.
4. the method for claim 1, is characterized in that, second step adopts heat pressing process that the lamellar graphite alkene of Nano grade is made graphene film (thickness is between hundreds of nanometer is to several millimeters).
5. the method for claim 1, is characterized in that, the 3rd step adopts the step of infiltration-winding-solidification to prepare vertical orientated Graphene/polymer composites.
6. method as claimed in claim 5, it is characterized in that, above-mentioned straight polymer can be: polypropylene, polyethylene, polystyrene, polycarbonate, acrylonitrile-butadiene-styrene copolymer, polymeric amide, be commonly called as nylon, Polybutylene Terephthalate, polyethylene terephthalate, polyphenylene oxide, polyphenylene sulfide, rigid polyvinyl chloride, polymethylmethacrylate, polyoxymethylene, polysulfones, polyimide, tetrafluoroethylene, voltalef, perfluoroethylene-propylene, polybutylene terephthalate, penton, styrene-butadiene rubber(SBR), nitrile rubber, silicon rubber, cis-1,4-polybutadiene rubber, polyisoprene, ethylene-propylene rubber(EPR), two kinds and two or more mixing of chloroprene rubber or above-mentioned superpolymer.
7. method as claimed in claim 5, it is characterized in that, in the 3rd step, the massfraction of Graphene can control according to technique, and scope is at 0%-100%, and when not infiltrating polymkeric substance, massfraction is 100%.
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Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106433133A (en) * | 2016-08-23 | 2017-02-22 | 广东工业大学 | Polymer matrix/three-dimensional graphene thermal interface composite material, and preparation method and application thereof |
| CN107325542A (en) * | 2017-07-14 | 2017-11-07 | 上海大学 | Graphene nanocomposite material of nylon 6/ of anisotropic thermal and preparation method thereof |
| CN107334633A (en) * | 2017-07-06 | 2017-11-10 | 青岛卓护医疗用品有限公司 | A kind of graphene skeleton Chinese mugwort processs the manufacture method of patch |
| CN108011180A (en) * | 2017-11-24 | 2018-05-08 | 武汉理工大学 | A kind of preparation method of graphene antenna for mobile phone |
| CN108864685A (en) * | 2018-06-12 | 2018-11-23 | 四川大学 | A kind of interfacial assembly structure and method improving thermoplasticity carbon fibre composite mechanical property |
| CN109285761A (en) * | 2018-09-19 | 2019-01-29 | 北京石墨烯研究院 | A kind of preparation method of aluminium nitride film |
| CN110358298A (en) * | 2019-07-11 | 2019-10-22 | 苏州仁甬得物联科技有限公司 | A kind of carbon nanowalls/macromolecule composite construction thermal interfacial material and preparation method thereof |
| CN110589810A (en) * | 2019-09-30 | 2019-12-20 | 曾功昶 | Production process of high-thermal-conductivity flexible graphene film gasket |
| CN110709353A (en) * | 2017-06-08 | 2020-01-17 | 斯马特高科技有限公司 | Method and apparatus for manufacturing graphene film |
| CN110776737A (en) * | 2018-07-31 | 2020-02-11 | 天津大学 | Graphene-polyimide resin heat-conducting composite material and preparation method thereof |
| US10870749B2 (en) | 2017-07-05 | 2020-12-22 | The University Of Akron | Thermally conductive polymers and methods for making |
| CN112679765A (en) * | 2020-12-08 | 2021-04-20 | 中国科学院深圳先进技术研究院 | Preparation method of heat conduction gasket with high normal thermal conductivity and high elasticity |
| CN113130810A (en) * | 2019-12-30 | 2021-07-16 | Tcl集团股份有限公司 | Packaging structure, packaging method thereof and display device |
| CN113502143A (en) * | 2021-06-28 | 2021-10-15 | 浙江大学 | Production device and preparation method of graphene thermal interface material |
| CN114029494A (en) * | 2021-11-11 | 2022-02-11 | 西北有色金属研究院 | Preparation method of spiral graphene film/copper laminated composite material |
| CN114554815A (en) * | 2020-11-25 | 2022-05-27 | 纳米及先进材料研发院有限公司 | Electromagnetic interference shielding device containing flame retardant thermal interface material composite |
| US11349163B2 (en) | 2017-03-25 | 2022-05-31 | Huawei Technologies Co., Ltd. | Battery electrode, method for producing battery electrode, and battery |
| CN114891485A (en) * | 2022-06-28 | 2022-08-12 | 湖南大学 | Graphene framework heat-conducting composite material based on three-dimensional vertical arrangement and preparation method thereof |
| CN115092916A (en) * | 2022-06-23 | 2022-09-23 | 湖南大学 | Graphene-based thermal interface material with sandwich structure and preparation method thereof |
| CN115231564A (en) * | 2021-04-22 | 2022-10-25 | 宁波材料所杭州湾研究院 | Graphene thermal interface material and preparation method and application thereof |
| CN115895262A (en) * | 2022-05-19 | 2023-04-04 | 华中科技大学 | Thermal interface material with vertical orientation structure and preparation method thereof |
| WO2023231990A1 (en) * | 2022-05-31 | 2023-12-07 | 合肥学院 | Polyoxymethylene nanosheet or polyoxymethylene copolymer nanosheet and preparation method therefor |
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Application publication date: 20160504 |