CN110282974A - Oriented alignment magnetic carbon fiber graphene composite film and its preparation method and application - Google Patents

Oriented alignment magnetic carbon fiber graphene composite film and its preparation method and application Download PDF

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CN110282974A
CN110282974A CN201910575761.2A CN201910575761A CN110282974A CN 110282974 A CN110282974 A CN 110282974A CN 201910575761 A CN201910575761 A CN 201910575761A CN 110282974 A CN110282974 A CN 110282974A
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carbon fiber
magnetic
magnetic carbon
graphene
composite film
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CN110282974B (en
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李静
雷汝白
陈燕
康梓彬
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South China University of Technology SCUT
Zhuhai Institute of Modern Industrial Innovation of South China University of Technology
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South China University of Technology SCUT
Zhuhai Institute of Modern Industrial Innovation of South China University of Technology
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Abstract

The invention discloses oriented alignment magnetic carbon fiber graphene composite films and its preparation method and application.Preparation method is first to carry out the magnetic loading of carbon fiber; then by magnetic carbon fiber powder ultrasonic disperse in a solvent; it pours into two sides and is fixed in the suction funnel of the opposite magnetite of magnetic pole and stand, after magnetic carbon fiber is stablized under magnetic fields, filter film forming; composite membrane is removed from filter membrane; and be put into mold after pressurization, it is put into tube furnace, protective gas is added; it is warming up to 1000-1500 DEG C and keeps the temperature, obtain magnetic carbon fiber graphene composite film.For parallelly distribute in graphene sheet layer, parallel rate reaches 85%-95% to magnetic carbon fiber of the present invention under external magnetic field.Fibre reinforced in the composite membrane mechanical property of composite membrane, and the graphene sheet layer in composite membrane is efficiently separated, lamella quality is improved, the heating conduction of composite membrane is increased.

Description

Oriented alignment magnetic carbon fiber graphene composite film and its preparation method and application
Technical field
The present invention relates to Heat Conduction Material technical field, in particular to a kind of oriented alignment magnetic carbon fiber graphene composite film Preparation method and application.Oriented alignment magnetic carbon fiber graphene composite film of the invention can be applied to great-power electronic member Device, LED, battery component heat dissipation in.
Background technique
The general radiating mode of prior art high heat flux density system is to obtain the metal wings such as copper, aluminium by machining Piece, and fin is installed at heat source.Since the thermal conductivity of metal only has hundred grades of W/mK, reach cooling requirements generally require it is high-quality The fin realization of amount, large volume, and it often increases system gross weight, occupies more volumes.
In thermally conductive field, graphene becomes the high heat conducting nano carbon material after diamond, carbon nanotube, thermal conductivity in face Up to 5300W/mK.However, no matter being by mechanically pulling off, liquid phase removing, redox, the methods of chemical vapor deposition obtain original Beginning graphene, excellent properties are based on nanoscale more, and without very high commercial value, and graphene product is mostly with graphene Composite material is made for substrate or packing factor to play the excellent properties of graphene.In heat management system, with graphene system At composite material have thermal conductivity high, the features such as stability is strong, good mechanical properties, light weight, become the high collection of solution At the important means of degree cooling electronic component problem.It is necessary to have more compared to conventional thermal conductive material for NEW TYPE OF COMPOSITE Heat Conduction Material High thermal conductivity, lighter quality, and require certain flexibility.Carbon carbon composite heat conducting material light weight, and its thermal conductivity, Mechanical strength and its microscopic appearance are closely related, its mechanical property and heat-conducting effect can be improved by adjusting its internal structure.
TGC series multilayer high thermal conductivity graphite film is produced by carbon source Science and Technology Ltd., and civilian high-end electricity is mainly used in Sub- device, LED chip material, commercial plant radiator, first wall of fusion reactor etc..The preparation of TGC series of products Method is generally required using polymeric membranes such as polyimides, polyamide as presoma, first pass through 600-1000 DEG C of carbonization, 2600-3200 DEG C is graphitized and keeps the temperature, and then finally obtains product by roll-in, not only complex process, energy consumption are huge for this process Greatly, simultaneously as product is that graphene film stacks, interlayer slip phenomenon is obvious when by tensile stress, and tensile strength is lower, And increase with the stacking number of graphene, thermal conductivity decline is obvious.
Summary of the invention
A kind of tension it is an object of the invention to overcome the deficiencies of the prior art and provide composite membrane along carbon fiber direction is strong Degree reaches 35-37MPa, and thermal conductivity is more than oriented alignment magnetic carbon fiber graphene composite film of 600W/mK and preparation method thereof.
Another object of the present invention is to provide the oriented alignment magnetic carbon fiber graphene composite film in LED heat dissipation Using.
The present invention guides building parallel arrangement carbon fiber skeleton and the deposited oxide graphene on skeleton by external magnetic field, leads to The mode for crossing Low Temperature Thermal reduction obtains composite film material, on the one hand, the fibre reinforced mechanical property of composite membrane, another party Face, carbon fiber efficiently separate graphene sheet layer, reduce the leakage of interlayer phonon, improve the thermal conductivity of film.Meanwhile the preparation Method effectively has adjusted the fiber orientation of chopped carbon fiber, and avoids hot pressing graphite merely through low-temperature carbonization in preparation process Change process effectively reduces the energy consumption in preparation process.In order to improve the comprehensive performance of graphene film,
The present invention separates what graphene sheet layer reduction graphene stacking generated by introducing the magnetic carbon fiber of oriented alignment Interlayer phon scattering, meanwhile, magnetic carbon fiber increases the tensile strength of graphene film, and the present invention as good reinforcement Preparation process need not move through graphitization processing, reduce the energy consumption of preparation process.High thermal conductivity prepared by the present invention, high-strength complex Conjunction film is high-power electronic component, the heat dissipation of LED, battery component provides better solution.
The composite film heat conductance that the present invention is prepared is high, and light weight, small in size, is attached to heat source surface conduct Uniform temperature material, the heat sink material quality and the occupied volume of heat sink material for reaching identical heat dissipation effect needs all obviously drop It is low.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of oriented alignment magnetic carbon fiber graphene composite film, comprising the following steps:
1) magnetic loading of carbon fiber: being added dispersing agent stirring for carbon fiber, be ultrasonically treated, be filtered by vacuum, dry;It will dry Solid is stirred at reflux in 80-90 DEG C of oil bath with the first mixed liquor afterwards, is filtered after dilution in deionized water, is washed to during filtrate is Property, it is dry;Resulting solid is mixed with the second mixed liquor after will be dry, and after immersion, alkaline solution is added dropwise in 80-90 DEG C of oil bath Until a large amount of precipitatings of generation, stand, being washed to filtrate with deionized water suction filtration is neutrality, dry, obtains magnetic carbon fiber powder;Institute The first mixed liquor stated is that nitric acid and sulfuric acid are 1:1-3:2 mixing gained in mass ratio;Second mixed liquor is tri-chlorination Ferrous solution and solution of ferrous chloride, wherein Fe3+With Fe2+Mass ratio be 2:1-3:1;
2) preparation of magnetic carbon fiber graphene oxide composite membrane: by magnetic carbon fiber powder ultrasonic disperse in a solvent, It pours into two sides and is fixed in the suction funnel of the opposite magnetite of magnetic pole and stand, after magnetic carbon fiber is stablized under magnetic fields, take out It filters and washs, the graphene oxide dispersion that concentration is 2-6mg/ml is added dropwise, continue to filter to film forming, it is dry;
3) thermal reduction of composite membrane: composite membrane is removed from filter membrane, and is put into mold after pressurization, and tube furnace is put into In, protective gas is added, is warming up to 1000-1500 DEG C and keeps the temperature, obtain magnetic carbon fiber graphene composite film.
To further realize purpose of the invention, it is preferable that in step 1), the dispersing agent is acetone, methanol and benzene At least one of phenol;The alkaline solution is at least one of ammonium hydroxide, sodium hydroxide and potassium hydroxide;
In step 2), the magnetite is ferrite magnetite, samarium-cobalt alloy magnetite or rubidium cesium alloy magnetite;The oxidation Graphene dispersing solution is prepared by improving Hummmers method.
Preferably, in step 1), the Fe of carbon fiber and generation is controlled3O4Mass ratio be 2:1-5:1.
Preferably, in step 1), in terms of mass fraction, the carbon fiber is 10-40 parts, dispersing agent 1000-1200 Part.
Preferably, in step 1), all dryings are all dry to constant weight in 50-70 DEG C of temperature condition;In step 1), institute The time that dispersing agent stirring is added in the carbon fiber stated is 36-48h;The time of the ultrasonic treatment is 1-2h;The standing Time be 1-2h;The time being stirred at reflux is 6-8h, and the time of the immersion is 12-24h.
Preferably, in step 2), the mass ratio of the magnetic carbon fiber and graphene oxide is 1:3-1:20;Described Solvent is N-Methyl pyrrolidone or N,N-dimethylformamide;The time of the ultrasonic disperse is 10-20 minutes;Described The time of standing is 10-20 minutes, and the drying is to be dried under vacuum to constant weight in 50-60 DEG C of temperature condition.
Preferably, in step 3), the pressure of the pressurization is 10-50MPa;The protective gas is argon gas or nitrogen Gas;It is described that be warming up to 1000-1500 DEG C be to be started to warm up with 3-5 DEG C/min heating rate from room temperature;The heat preservation when Between be 2-3h.
A kind of oriented alignment magnetic carbon fiber graphene composite film, is made by above-mentioned preparation method, resulting orientation row Cloth magnetic carbon fiber graphene composite film with a thickness of 50-220 μm, thermal coefficient 600-800W/mK, side parallel with carbon fiber To tensile strength be 35-37MPa.
Preferably, composite membrane is made of magnetic carbon fiber and graphene, and by percentage to the quality, magnetic carbon fiber content is 10%-40%, graphene content are 60%-90;The diameter of composite membrane is 40-80mm;The magnetic carbon fiber is in external magnetic field Lower parallelly distribute on is acted in graphene sheet layer, parallel rate reaches 85%-95%.
Application of the oriented alignment magnetic carbon fiber graphene composite film in LED heat dissipation.
In step 3), the mold fixes two pieces of ceramic wafers by high temperature screw or graphite plate is realized.
The present invention uses for reference co-precipitation preparation magnetic Fe3O4The method of fluid, by magnetic Fe3O4Particle is supported on carbon fiber, And be arranged in carbon fiber in magnetic field with same orientation under outer introduction by magnetic field and constituted skeleton, graphene oxide is deposited on carbon fiber It ties up in skeleton, heat-treats to obtain oriented alignment magnetic carbon fiber graphene composite film by low temperature.Since carbon fiber has well Mechanical performance, carbon fiber and graphene form clad structure, the nanometer Fe of carbon fiber surface load in composite membrane3O4Particle The surface roughness for increasing carbon fiber reduces the sliding being likely to occur between carbon fiber and graphene, to enhance compound The tensile strength and flexibility of film.Meanwhile carbon fiber efficiently separates the lamella of graphene, the phonon reduced in diabatic process is let out Leakage, to improve the thermal conductivity of composite membrane.
The present invention has the following advantages and effects with respect to the prior art:
The present invention is by magnetic Fe3O4Particle is supported on carbon fiber, and makes carbon fiber with same orientation under outer introduction by magnetic field It is arranged in magnetic field and constitutes parallel skeleton, then pass through deposited oxide graphene and obtain in a manner of thermal reduction oriented alignment magnetic Property carbon fiber and graphite alkene composite membrane.On the one hand, the magnetic carbon fiber of oriented alignment effectively enhances composite membrane along carbon fiber direction Tensile strength, reach 35-37MPa.On the other hand, magnetic carbon fiber is distributed in the different-thickness of graphene sheet layer, from And efficiently separate graphene sheet layer, it is mainly realized and is conducted heat by phonon transmission due to graphene, and with the graphene film number of plies The increase of amount, phonon is obviously increased in the scattering of interlayer with leakage phenomenon, to reduce its thermal conductivity.Therefore, graphene sheet layer The increase of spacing reduces the phon scattering and leakage of interlayer, improves the heating conduction of composite membrane, makes its thermal conductivity be more than 600W/mK.Compared to TGC series multilayer high thermal conductivity graphite film, the present invention increases composite membrane since magnetic carbon fiber is added Heating conduction and mechanical property, while the huge graphitization of energy consumption is avoided, effectively reduce production cost.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph that 1 carbon fiber surface of embodiment wraps up the particle containing magnetic ferroferric oxide nanometer.
Fig. 2 is the scanning electron microscope (SEM) photograph of 1 oriented alignment magnetic carbon fiber graphene composite film of embodiment.
Fig. 3 is that embodiment 1 heat-treats die drawing used by oriented alignment magnetic carbon fiber graphene composite film.
It is shown in Fig. 3: screw 1, ceramic wafer 2, composite membrane 3, nut 4.
Specific embodiment
For a better understanding of the invention, the present invention is further illustrated with reference to the accompanying drawings and examples, but implements Example does not constitute the limitation to any protection scope of the invention.
Embodiment 1
A kind of preparation method of oriented alignment magnetic carbon fiber graphene composite film, comprising the following steps:
1) 30 parts of carbon fibers are added in 1000 parts of acetone based on parts by weight and stir 48h by the magnetic loading of carbon fiber, surpass Sound 1h is filtered by vacuum and solid is dry to constant weight in 70 DEG C of conditions.Carbon fiber after drying is added in glassware, is added The nitric acid and sulfuric acid mixture liquid that 500 parts of mass ratios are 3:2 are stirred at reflux 6h in 90 DEG C of oil baths, dilute and in suction funnel It is middle with deionized water suction filtration be washed to filtrate be it is neutral, it is dry to constant weight in 60 DEG C of conditions.Glass is added in solid after drying In vessel, 150 parts of deionized waters and configured liquor ferri trichloridi and solution of ferrous chloride are separately added into, and guarantee m (Fe3 +):m(Fe2+)=2:1, m (carbon fiber): m (Fe3O4After impregnating 12h, 20 parts of sodium hydroxides are added dropwise in)=3:1 in 90 DEG C of oil baths, 2h is stood, being washed to filtrate with deionized water suction filtration in suction funnel is neutrality, is dried under vacuum to constant weight in 60 DEG C of conditions, most Magnetic carbon fiber powder is obtained eventually.Here m indicates quality.It is as shown in Figure 1 the scanning electron microscope shape of magnetic carbon fiber Looks figure has a large amount of ferriferrous oxide nano-particles and generates and be attached to carbon fiber surface after aqueous slkali is added.
2) preparation of magnetic carbon fiber graphene oxide composite membrane: based on parts by weight, the magnetic carbon fiber that will be prepared Dimension powder is dispersed in ultrasound 10 minutes in 500 parts of N-Methyl pyrrolidones, pours into the suction filtration that two sides are fixed with the opposite magnetite of magnetic pole In funnel, 10 minutes are stood, after magnetic carbon fiber is stablized under magnetic fields, filters and washs, 60 parts of concentration, which are added dropwise, is The graphene oxide dispersion of 6mg/ml continues to filter to forming a film, is dried under vacuum to constant weight in 60 DEG C of conditions.Graphene oxide point Dispersion liquid is prepared by improving Hummmers method.Selected magnetite is rubidium cesium alloy magnetite.
3) composite membrane is removed from filter membrane, and is put into mold (Fig. 3) after application 50MPa pressure, is put into tube furnace, Using argon gas as protective gas, 5 DEG C/min heating rate rises to 1500 DEG C and keeps the temperature 2h, and it is compound to obtain magnetic carbon fiber graphene Film.It is illustrated in figure 2 the scanning electron microscope diagram of magnetic carbon fiber graphene composite film, in the composite membrane after reduction, in parallel The carbon fiber of arrangement is distributed in the different thickness of graphene, and is tightly wrapped up by graphene.
Fig. 3 is that embodiment 1 heat-treats die drawing used by oriented alignment magnetic carbon fiber graphene composite film.Such as Fig. 3 It is shown, as shown in figure 3, composite membrane 2 is placed between two pieces of ceramic wafers 2 with unthreaded hole and nut 4, screw 1 are passed through light Hole connection compresses ceramic wafer 2.
Embodiment 2
A kind of preparation method of oriented alignment magnetic carbon fiber graphene composite film, comprising the following steps:
1) 40 parts of carbon fibers are added in 1200 parts of methanol and stir 36h, ultrasonic 2h by the magnetic loading of carbon fiber, are filtered by vacuum And it is solid is dry to constant weight in 65 DEG C of conditions.Carbon fiber after drying is added in glassware, it is 1 that 500 parts of ratios, which are added: 1 nitric acid and sulfuric acid mixture liquid is stirred at reflux 7h in 80 DEG C of oil baths, dilutes and filters water with deionized water in suction funnel Filtrate is washed till for neutrality, in 50 DEG C of conditions dryings to constant weight.Solid after drying is added in glassware, is separately added into 100 parts Deionized water and configured liquor ferri trichloridi and solution of ferrous chloride, and guarantee m (Fe3+):m(Fe2+)=3:1, m (carbon fiber Dimension): m (Fe3O4)=4:1 after impregnating 18h, is added dropwise 30 parts of potassium hydroxide in 80 DEG C of oil baths, stands 2h, use in suction funnel Deionized water suction filtration is washed to filtrate as neutrality, is dried under vacuum to constant weight in 50 DEG C of conditions, finally obtains magnetic carbon fiber powder.
2) the magnetic carbon fiber powder being prepared is dispersed in by the preparation of magnetic carbon fiber graphene oxide composite membrane Ultrasound 15 minutes in 600 parts of N-Methyl pyrrolidones, pour into two sides and are fixed in the suction funnel of the opposite magnetite of magnetic pole and stand 15 Minute, it after magnetic carbon fiber is stablized under magnetic fields, filters and washs, the graphite oxide that 80 parts of concentration are 5mg/ml is added dropwise Alkene dispersion liquid continues to filter to forming a film, is dried under vacuum to constant weight in 60 DEG C of conditions.Graphene oxide dispersion passes through improvement Hummmers method is prepared.Selected magnetite is samarium-cobalt alloy magnetite.
3) composite membrane is removed from filter membrane, and be put into mold after application 30MPa pressure, is put into tube furnace, with argon Gas is protective gas, and 5 DEG C/min heating rate, which rises to 1200 DEG C and keeps the temperature 3h, obtains magnetic carbon fiber graphene composite film.It is adopted Mold is fixed two pieces of graphite plates by high temperature screw and is realized.
Embodiment 3
A kind of preparation method of oriented alignment magnetic carbon fiber graphene composite film, comprising the following steps:
1) magnetic loading of carbon fiber, it is to stir in 6:5 mixed liquor that 1100 parts of methanol phenol ratios, which are added, in 20 parts of carbon fibers 40h, ultrasonic 1.5h are filtered by vacuum and solid is dry to constant weight in 60 DEG C of conditions.Vierics are added in carbon fiber after drying In ware, 500 parts of ratios are added as the nitric acid and sulfuric acid mixture liquid of 5:4 and are stirred at reflux 8h in 85 DEG C of oil baths, dilutes and is simultaneously filtering Being washed to filtrate with deionized water suction filtration in funnel is neutrality, dry to constant weight in 55 DEG C of conditions.Solid after drying is added into glass In glass vessel, 125 parts of deionized waters and configured liquor ferri trichloridi and solution of ferrous chloride are separately added into, and guarantee m (Fe3+):m(Fe2+)=2:1, m (carbon fiber): m (Fe3O4After impregnating 20h, 40 parts of hydrogen-oxygens are added dropwise in)=5:1 in 85 DEG C of oil baths Change ammonium, stand 1.5h, being washed to filtrate with deionized water suction filtration in suction funnel is neutrality, is dried under vacuum in 55 DEG C of conditions Constant weight finally obtains magnetic carbon fiber powder.
2) the magnetic carbon fiber powder being prepared is dispersed in by the preparation of magnetic carbon fiber graphene oxide composite membrane Ultrasound 20 minutes in 550 parts of n,N-Dimethylformamide, pour into two sides and are fixed in the suction funnel of the opposite magnetite of magnetic pole and stand It 20 minutes, after magnetic carbon fiber is stablized under magnetic fields, filters and washs, the oxidation stone that 90 parts of concentration are 2mg/ml is added dropwise Black alkene dispersion liquid continues to filter to forming a film, is dried under vacuum to constant weight in 55 DEG C of conditions.Graphene oxide dispersion passes through improvement Hummmers method is prepared.Selected magnetite is ferrite magnetite.
3) composite membrane is removed from filter membrane, and be put into mold after application 40MPa pressure, is put into tube furnace, with argon Gas is protective gas, and 4 DEG C/min heating rate, which rises to 1300 DEG C and keeps the temperature 2h, obtains magnetic carbon fiber graphene composite film.It is adopted Mold is fixed two pieces of graphite plates by high temperature screw and is realized.
The oriented alignment magnetic carbon fiber graphene composite film that embodiment 1-3 is obtained by scanning electron microscope image The parallel rate detection of carbon fiber is carried out, on the basis of magnetic induction line direction, magnetic carbon fiber is parallel point less than 10 ° with magnetic induction line angle Cloth.The parallel rate of magnetic carbon fiber is as shown in table 1, and the carbon fiber due to having loaded magnetic particle has good under magnetic fields Paramagnetism, therefore loaded the carbon fiber of magnetic particle in embodiment 1-3 and had under outer introduction by magnetic field along magnetic induction line direction The trend of parallelly distribute on, meanwhile, parallel rate is higher, and the paramagnetic performance of magnetic carbon fiber is better.
The parallel rate of table 1 statistics
Type Parallel rate (%)
Embodiment 1 94
Embodiment 2 85
Embodiment 3 89
Composite membrane prepared by the present invention is multi-layer graphene composite membrane, and commercialized multilayer high-thermal conductivity graphite film is with carbon source The TGC series multilayer high thermal conductivity graphite film of Science and Technology Ltd.'s production is most representative, and TGC series is mainly used in civilian high-end Electronic device, LED chip material, commercial plant radiator, first wall of fusion reactor etc..It is prepared by the present invention compound Film is mainly used in the heat dissipation of high-power electronic component, LED, battery component, and reduces system bulk quality simultaneously, with TGC series of products purposes is close.By comparing, choose with bulk density of the present invention similar in TGC-1 product progress piece interlamellar spacing, The comparison of heating conduction, mechanical property and cooling application.
High thermal conductivity graphite to the obtained oriented alignment magnetic carbon fiber graphene composite film of embodiment 1-3 and on the market The graphene of film carries out X-ray diffraction detection, and the piece interlamellar spacing such as table 2 of graphene is calculated by bragg's formula.For the minimum interlamellar spacing of graphite, and compared with the similar product of carbon source science and technology, the graphene film interlamellar spacing of embodiment 1-3 Obviously become larger, it was demonstrated that the carbon fiber of oriented alignment can effectively increase the piece interlamellar spacing of graphene, since graphene mainly passes through Phonon transmission realizes heat transfer, but with the increase of graphene film layer number, phonon in transmission process by the scattering of interlayer with Leakage phenomenon, which obviously increases, reduces its thermal conductivity, and the phonon that the piece interlamellar spacing for increasing graphene can reduce interlayer generation dissipates It penetrates.
2 interlamellar spacing comparisons of table
Using laser heat conducting instrument according to ASTME1461 standard, universl tester is according to ASTMF152 respectively to embodiment 1-3 Obtained oriented alignment magnetic carbon fiber graphene composite film and carbon source science and technology similar product heating conduction and mechanical property is examined It surveys, obtains table 3.It can be seen that the carbon fibre separation lamella of graphene due to oriented alignment by embodiment 1-3, compare Greatly reduce in the phonon leakage of product similar on the market, interlayer, so that its thermal conductivity is also effectively promoted.Meanwhile Carbon fiber effectively improves the tensile strength of graphene film as reinforcement.
3 heating conduction of table and mechanical property compare
Type Thermal coefficient (W/mK) Tensile strength
Embodiment 1 670±35 36MPa
Embodiment 2 600±30 37MPa
Embodiment 3 630±30 35MPa
TGC-1 300-350 15-20MPa
By the obtained oriented alignment magnetic carbon fiber graphene composite film of embodiment 1-3 and the similar product of carbon source science and technology It is applied in 24W LED heat dissipation as uniform temperature material, is made into samming film and is attached on LED light backboard, by infrared camera mirror Head alignment LED light tergal position, detects the temperature after attaching different samming films after LED light back plate surface thermal balance and obtains table 4.? After reaching thermal balance, LED light backboard temperature is lower, illustrates that the samming film heat dissipation effect used is more preferable, due to the face of embodiment 1-3 Interior thermal conductivity is apparently higher than carbon source science and technology similar product, therefore embodiment 1-3 is equally shown preferably in application process Temp effect.
4 thermal interfacial material surface temperature of table
Type Surface temperature (DEG C)
Embodiment 1 62
Embodiment 2 68
Embodiment 3 66
TGC-1 73
Oriented alignment magnetic carbon fiber graphene composite film of the invention can be applied to high-power electronic component, LED, Instead of metal fins such as traditional copper, aluminium used in the heat dissipation of battery component.Since the thermal conductivity of metal only has hundred grades of W/mK, Reach the fin realization that cooling requirements generally require high quality, large volume, and it often increases system gross weight, occupies more Volume.The composite film heat conductance that the present invention is prepared is high, and light weight, small in size, is attached to heat source surface conduct Uniform temperature material, the heat sink material quality and the occupied volume of heat sink material for reaching identical heat dissipation effect needs all obviously drop Low, this provides good solution for the heat dissipation of high heat flux density system.Compared to TGC series multilayer high thermal conductivity graphite Film, the composite membrane that the present invention is prepared have better heat dissipation effect in identical LED light radiation processes, it is thus possible to make LED light keeps lower temperature when stablizing and using, and the service life for improving LED light has highly beneficial.
It should be noted that for those of ordinary skill in the art to which the present invention belongs, not departing from the present invention The embodiment of several alternative or obvious variations is made under the premise of design, these all shall be regarded as belonging to protection model of the invention In enclosing.

Claims (10)

1. a kind of preparation method of oriented alignment magnetic carbon fiber graphene composite film, it is characterised in that the following steps are included:
1) magnetic loading of carbon fiber: being added dispersing agent stirring for carbon fiber, be ultrasonically treated, be filtered by vacuum, dry;It is solid after will be dry Body is stirred at reflux in 80-90 DEG C of oil bath with the first mixed liquor, is filtered after dilution in deionized water, and being washed to filtrate is neutrality, It is dry;Resulting solid is mixed with the second mixed liquor after will be dry, and after immersion, it is straight that alkaline solution is added dropwise in 80-90 DEG C of oil bath To a large amount of precipitatings of generation, stand, being washed to filtrate with deionized water suction filtration is neutrality, it is dry, obtain magnetic carbon fiber powder;It is described The first mixed liquor be nitric acid and sulfuric acid be in mass ratio 1:1-3:2 mixing gained;Second mixed liquor is ferric trichloride Solution and solution of ferrous chloride, wherein Fe3+With Fe2+Mass ratio be 2:1-3:1;
2) preparation of magnetic carbon fiber graphene oxide composite membrane: magnetic carbon fiber powder ultrasonic disperse in a solvent pours into Two sides are fixed in the suction funnel of the opposite magnetite of magnetic pole and stand, and after magnetic carbon fiber is stablized under magnetic fields, filter simultaneously The graphene oxide dispersion that concentration is 2-6mg/ml is added dropwise in washing, continues suction filtration and extremely forms a film, dry;
3) thermal reduction of composite membrane: composite membrane is removed from filter membrane, and is put into mold after pressurization, is put into tube furnace, is added Enter protective gas, be warming up to 1000-1500 DEG C and keep the temperature, obtains magnetic carbon fiber graphene composite film.
2. the preparation method of oriented alignment magnetic carbon fiber graphene composite film according to claim 1, which is characterized in that In step 1), the dispersing agent is at least one of acetone, methanol and phenol;The alkaline solution is ammonium hydroxide, hydrogen At least one of sodium oxide molybdena and potassium hydroxide;
In step 2), the magnetite is ferrite magnetite, samarium-cobalt alloy magnetite or rubidium cesium alloy magnetite;The graphite oxide Alkene dispersion liquid is prepared by improving Hummmers method.
3. the preparation method of oriented alignment magnetic carbon fiber graphene composite film according to claim 1, which is characterized in that In step 1), the Fe of carbon fiber and generation is controlled3O4Mass ratio be 2:1-5:1.
4. the preparation method of oriented alignment magnetic carbon fiber graphene composite film according to claim 1, which is characterized in that In step 1), in terms of mass fraction, the carbon fiber is 10-40 parts, and dispersing agent is 1000-1200 parts.
5. the preparation method of oriented alignment magnetic carbon fiber graphene composite film according to claim 1, which is characterized in that In step 1), all dryings are all dry to constant weight in 50-70 DEG C of temperature condition;In step 1), the carbon fiber is added The time of dispersing agent stirring is 36-48h;The time of the ultrasonic treatment is 1-2h;The time of the standing is 1-2h;Institute The time being stirred at reflux stated is 6-8h, and the time of the immersion is 12-24h.
6. the preparation method of oriented alignment magnetic carbon fiber graphene composite film according to claim 1, which is characterized in that In step 2), the mass ratio of the magnetic carbon fiber and graphene oxide is 1:3-1:20;The solvent is N- methyl pyrrole Pyrrolidone or N,N-dimethylformamide;The time of the ultrasonic disperse is 10-20 minutes;The time of the standing is 10-20 minutes, the drying was to be dried under vacuum to constant weight in 50-60 DEG C of temperature condition.
7. the preparation method of oriented alignment magnetic carbon fiber graphene composite film according to claim 1, which is characterized in that In step 3), the pressure of the pressurization is 10-50MPa;The protective gas is argon gas or nitrogen;Described is warming up to 1000-1500 DEG C is to be started to warm up with 3-5 DEG C/min heating rate from room temperature;The time of the heat preservation is 2-3h.
8. a kind of oriented alignment magnetic carbon fiber graphene composite film, which is characterized in that it is as described in claim any one of 1-7 Preparation method be made, resulting oriented alignment magnetic carbon fiber graphene composite film with a thickness of 50-220 μm, thermal coefficient For 600-800W/mK, the tensile strength with carbon fiber parallel direction is 35-37MPa.
9. oriented alignment magnetic carbon fiber graphene composite film according to claim 8, which is characterized in that composite membrane is by magnetic Property carbon fiber and graphene form, by percentage to the quality, magnetic carbon fiber content is 10%-40%, and graphene content is 60%-90;The diameter of composite membrane is 40-80mm;The magnetic carbon fiber under external magnetic field parallelly distribute in graphene In lamella, parallel rate reaches 85%-95%.
10. application of the oriented alignment magnetic carbon fiber graphene composite film of claim 8 or 9 in LED heat dissipation.
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