CN102040761A - High-heat-conductivity composite material and preparation method thereof - Google Patents
High-heat-conductivity composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-heat-conductivity composite material and a preparation method thereof. The preparation method comprises the following steps: evenly mixing fibrous heat-conduction filler and high-heat-conductivity filler graphene in a mass ratio of 1:1-1:200 with thermoplastic polymer, dispersing for 0.5-24 hours, granulating to obtain high-heat-conductivity composite grains, and putting the grains in a die to carry out hot molding at 170-280 DEG C under the pressure of 10-18 MPa. The thermoplastic polymer is any one of polyethylene, polypropylene, polyvinylidene fluoride, polytetrafluoroethylene, polyperfluoroalkoxy ester, nylon, polymethyl methacrylate, polycarbonate and polyvinyl chloride. The fibrous heat-conduction filler is carbon fiber or carbon nanotube, and the high-heat-conductivity filler accounts for 5-35 wt% of the high-heat-conductivity composite material. The high-heat-conductivity composite material has the advantages of excellent heat-conduction property, low consumption of heat-conduction filler, favorable mechanical properties, simple preparation technique and low cost.
Description
Technical field
The present invention relates to a kind of heat-conductive composite material, be specifically related to a kind of high-heat-conductive composite material and preparation method thereof with excellent heat conducting performance and excellent mechanical performances.
Background technology
Along with industrial growing, the etching problem of equipment is more and more outstanding in fields such as chemical industry, oil, machinery, weaving, metallurgy, space flight and aviation, national defence, especially in heat exchange occasions such as interchanger, heat pipes.Corrosion not only brings enormous economic loss to society, causes catastrophic failure and jeopardizes personnel safety, exhausts the valuable resource and the energy, contaminate environment, and hindered high-tech normal development.Traditional metal materials can not satisfy requirements such as it is corrosion-resistant, high heat conduction.
Polymkeric substance has the superior corrosion resistance energy, but low heat conductivity can limit its application in heat-exchange equipment.Use high heat conductive filler polymkeric substance is carried out the effective way that blending and modifying is a raising polymkeric substance heat conductivility, prepared matrix material has corrosion-resistant, cheap, light weight, is easy to advantages such as machine-shaping.Existing bibliographical information has prepared good matrix material (polymer material science and the engineering of heat conductivility by different high heat conductive fillers (such as graphite, carbon nanotube, carbon fiber) to polymer blending modification, 2005,21 (6): 170-173, Mater.Res.Soc.Symp.Proc., 2005, Vol.858E, HH3.31.1-HH3.31.5, Poly.Eng.﹠amp; Sci., 2008,2474-2481; J. Chemical Manufacture and technology, 2001,8 (2): 17-19), still, the subject matter that existing composite heat conducting material exists: (1) under the situation of the low loading level of heat conductive filler, the heat conductivility of matrix material is not high; (2) under the high filler loading capacity situation, though heat conductivility significantly improves, comprehensive mechanical performance sharply significantly descends, and such as the graphite that adds 30% in the tetrafluoroethylene, its tensile strength only is 0.44 times of tetrafluoroethylene; The graphite mass content is 40% o'clock, and the tensile strength of thermally conductive material has only 5SMPa, can not satisfy the service requirements on the engineering fully.By contrast, though the matrix material of carbon nanotube or carbon fiber preparation can keep good mechanical property, heat conductivility is still waiting further raising.In a word, existing composite heat conducting material can not reach the heat conductivility height simultaneously, comprehensive mechanical property is good, is difficult to satisfy the use properties of actual needs, thus the widespread use of restriction heat-conductive composite material.
Therefore, need a kind of high-heat-conductive composite material badly, when guaranteeing material mechanical performance, possess good heat conductivility, really solve the equipment corrosion problem that the heat exchange occasion exists.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, a kind of high-heat-conductive composite material and preparation method thereof is provided.
High-heat-conductive composite material provided by the invention comprises high heat conductive filler and thermoplastic polymer, and described high heat conductive filler is the mixture of Graphene and fibrous heat conductive filler, and the mass ratio of wherein fibrous heat conductive filler and Graphene is 1: 1～1: 200.Graphene is main high heat conductive filler, and fibrous heat conductive filler is auxilliary high heat conductive filler.Wherein high heat conductive filler accounts for 5%～35% of total mass in the high-heat-conductive composite material.
High-heat-conductive composite material preparation method provided by the invention specifically is achieved through the following technical solutions:
The mixture and the thermoplastic polymer uniform mixing of above-mentioned Graphene and fibrous heat conductive filler were disperseed 0.5～24 hour; to disperse back gained mixture forcing machine extruding pelletization or crusher in crushing granulation; form the high-heat-conductive composite material pellet, it is hot-forming under 170 ℃～280 ℃, 10～18MPa more prepared pellet to be put into mould.Above-mentioned blending dispersion can adopt mechanical dispersion, ultra-sonic dispersion or solution to disperse.
Above-mentioned thermoplastic polymer is any in polyethylene (PE), polypropylene (PP), polyvinylidene difluoride (PVDF) (PVDF), polytetrafluoroethylene (PTFE), poly-perfluoro alkoxy ester (PFA), nylon (PA), polymethylmethacrylate (PMMA), polycarbonate (PC) or the polyvinyl chloride (PVC).
Above-mentioned fibrous heat conductive filler is carbon fiber or carbon nanotube, and carbon fiber is preferably asphalt base carbon fiber.
Because of high heat conductive filler Graphene of the present invention is the nano-sheet structure, not only heat conductivility is superpower, and has the effect that strengthens the polymkeric substance mechanical property; In addition, two heat conductive fillers of sheet structure heat conductive filler or sheet structure and filamentary structure form the heat conduction network easily in polymkeric substance, significantly improve the heat conductivility of polymkeric substance.Therefore, high-heat-conductive composite material provided by the invention has heat conductivility excellence, amount of filler is few, comprehensive mechanical property is good advantage.
Compare with prior art, the present invention has following advantage:
1, high-heat-conductive composite material provided by the invention has heat conductivility excellence and the little advantage of heat conductive filler consumption.Graphene is the nano-sheet structure, not only has superpower heat conductivility, and two heat conductive fillers of sheet structure heat conductive filler or sheet structure and filamentary structure easy heat conduction network that forms in polymeric substrate, therefore under the situation of low loading level, can make matrix material have excellent heat conductivility.
2, the mechanical property of high-heat-conductive composite material provided by the invention is good.Graphene is the heat conductivility excellence not only, and has the effect that strengthens the polymkeric substance mechanical property; And the present invention is high, and the heat conductive filler consumption is low, and the auxilliary filler of the high heat conduction of adding can not reduce the mechanical property of polymkeric substance.
3, high-heat-conductive composite material provided by the invention all can adopt conventional polymer blend method to obtain, and need not harsh synthesis condition, and preparation technology is simple; Polymkeric substance involved in the present invention, fibrous heat conductive filler all can directly be bought, and the convenient preparation of graphite that related Graphene can be cheap is therefore, with low cost.
Embodiment
In order to understand the present invention better, the present invention is done to describe further below in conjunction with embodiment.
High-heat-conductive composite material of the present invention comprises high heat conductive filler and thermoplastic polymer, and wherein Graphene is that high heat conduction master filler, fibrous heat conductive filler are that the auxilliary filler of high heat conduction, thermoplastic polymer are base material.Heat conductive filler is dispersed in the thermoplastic polymer.High heat conductive filler accounts for 5%～35% of high-heat-conductive composite material total mass.The mass ratio of wherein fibrous heat conductive filler and Graphene is 1: 1～1: 200.
Adopt the high-heat-conductive composite material that the Hotdisk thermal conductivity coefficient measurement instrument makes each embodiment and the heat conductivility of contrast thermally conductive material to test, the high-heat-conductive composite material that each embodiment is made by GB/T528 1992 methods and the tensile strength of contrast thermally conductive material detect.Table 1 is The performance test results (K
mBe the thermal conductivity of each heat-conductive composite material, a is the thermal conductivity ratio of each heat-conductive composite material and original copolymer; Data in the tensile strength bracket are the tensile strength values of the unmodified original copolymer of each heat-conductive composite material).
High-heat-conductive composite material that various embodiments of the present invention make and contrast heat-conductive composite material all adopt the method for expressing of A-B-D or A-B (b)-C (c)-D, and wherein A is expressed as thermoplastic polymer, B and C and is expressed as respectively that the high heat conduction master filler of interpolation and the auxilliary filler of Gao Re, b and c are expressed as the high heat conduction master filler that added and mass ratio, the D of the auxilliary filler of high heat conduction is expressed as the mass content percentage ratio of high heat conductive filler in high-heat-conductive composite material.
Embodiment 1
2g Graphene (xGnP) and 0.02g carbon fiber (CF) are joined in the 500mL Virahol,, obtain graphene suspension through ultra-sonic dispersion 20 hours; 18.18g new LDPE (film grade) (LDPE) powder is added in the suspension, high-speed stirring was removed Virahol through reduction vaporization after 10 hours, obtained mixed powder again; The mixed powder that makes is joined in the mould, the hot-forming high-heat-conductive composite material (being called for short LDPE-xGnP-10) that promptly obtains under 170 ℃, 10MPa, wherein high heat conductive filler is 10% in the mass content of matrix material.Cut test specimens according to the specimen size.
Wherein, preparation method of graphene is pressed document (J.Mater.Chem.2010,20,8496-8505; Carbon 2010,48,2361-2380), the 10g nano-graphite under agitation joined in the mixing solutions of the 270mL vitriol oil and nitrosonitric acid (volume ratio is 2: 1), obtain uniform suspension; In suspension, slowly add the 110g potassium perchlorate again, stir after 96 hours, obtain solid after filtration; With the solid of gained successively with 5% twice of salt pickling, be washed to filtrate neutrality, drying is pulverized and is obtained graphite oxide.With graphite oxide in nitrogen atmosphere, 900 ℃ down heating promptly obtained graphene powder in 50 seconds.Identical method is all adopted in Graphene preparation in following examples.
The heat conductivility and the tensile strength of prepared high-heat-conductive composite material the results are shown in Table 1.In addition, as a comparison case, adopt same procedure that thermal conductivity and the tensile strength of PP-CNT-15 are tested.PP-CNT-15 is to be heat conductive filler with the carbon nanotube, and polypropylene is the heat-conductive composite material (preparation method presses document J.Appl.Phys.2006, and A85:25-28 is described) of base material, and the mass content of carbon nanotube is 15%.
The result shows that the thermal conductivity of LDPE-xGnP-10 is apparently higher than PP-CNT-15, and its tensile strength is suitable with the pure new LDPE (film grade) that does not add heat conductive filler.
Embodiment 2
Behind 12g Graphene and 2g carbon nanotube and 26g polypropylene (PP) usefulness homogenizer premix, with the twin screw extruder granulation of the mixture of gained, wherein, the mass content of high heat conductive filler in matrix material is 35% to form high-heat-conductive composite material (being called for short PP-xGnP (6)-CNT (1)-35).It is hot-forming under 190 ℃, 18MPa that the pellet that makes is put into mould, cuts test specimens according to the specimen size.
Heat conductivility and the tensile strength of PP-xGnP (6)-CNT (1)-35 the results are shown in Table shown in 1.In addition, as a comparison case, adopt same procedure that thermal conductivity and the tensile strength of PP-Gn-40 are tested.PP-Gn-40 is to be heat conductive filler with graphite, and polypropylene is that (preparation method such as document J. Chemical Manufacture and technology, 2001,8 (2): 17-19), the mass content of graphite is 40% for the heat-conductive composite material of base material.
The result shows that the thermal conductivity of PP-xGnP (6)-CNT (1)-35 is 2.09 times of PP-Gn-40, and its tensile strength is 1.88 times of PP-Gn-40.
Embodiment 3
500mg Graphene and 500mg asphalt base carbon fiber (CF) and 19g polyvinylidene difluoride (PVDF) (PVDF) joined carry out ball milling in the ball mill and obtained mixed powder in 0.5 hour, to make mixed powder joins in the mould, the hot-forming high-heat-conductive composite material (being called for short PVDF-xGnP (1)-CF (1)-5) that promptly obtains under 200 ℃, 15MPa, wherein high heat conductive filler is 5% at the total mass content of matrix material.Cut test specimens according to the specimen size.
Heat conductivility and the tensile strength of PVDF-xGnP (1)-CF (1)-5 the results are shown in Table 1.In addition, as a comparison case, adopt same procedure that thermal conductivity and the tensile strength of PP-CNT-15 are tested.PP-CNT-15 is to be that heat conductive filler, polypropylene are the heat-conductive composite material of base material with the carbon nanotube, and the mass content of carbon nanotube is 15%.
The result shows, heat conductive filler content be PVDF-xGnP (1)-CF (1)-5 of 5% the unmodified original copolymer PVDF of thermal conductivity ratio raising 3 times, and heat conductive filler content is that the thermal conductivity of 15% PP-CNT-15 is only than 1.99 times of the raisings of unmodified original copolymer PP.
Embodiment 4
2g Graphene and 0.2g asphalt base carbon fiber and 17.8g nylon 66 (PA66) joined carried out ball milling in the ball mill 1 hour, obtain mixed powder; Mixed powder is joined in the mould, the hot-forming high-heat-conductive composite material (PA66-xGnP (10)-CF (1)-11) that promptly obtains under 280 ℃, 15MPa, wherein high heat conductive filler is 11% at the total mass content of matrix material.Cut test specimens according to the specimen size.
PA66-xGnP (10)-CF (1)-11 sees Table 1 with heat conductivility and the tensile strength detected result of contrast thermally conductive material PTFE-Gn-30.PTFE-Gn-30 is to be that heat conductive filler, polytetrafluoroethylene (PTFE) are that (preparation method such as document J. Chemical Manufacture and technology, 2001,8 (2): 17-19), the mass content of graphite is 30% for the heat-conductive composite material of base material with graphite.
The result shows, high heat conductive filler mass content is that the tensile strength of PA66-xGnP (10)-CF (1)-11 of 11% is suitable with unmodified PA66, and it is 30% PTFE-Gn-30 that the amplitude that thermal conductivity increases is higher than the heat conductive filler mass content; And the tensile strength of PTFE-Gn-30 only is 0.44 times of unmodified PTFE.
Embodiment 5
5g Graphene and 15g polytetrafluorethylepowder powder (PTFE) are carried out mechanically mixing, then with the twin screw extruder granulation of the mixed powder of gained, obtain high-heat-conductive composite material (being called for short PTFE-xGnP-25), wherein Graphene is 25% in the mass content of high-heat-conductive composite material.It is hot-forming that the pellet that makes is put into mould.Cut test specimens according to the specimen size.
Heat conductivility and the tensile strength of PTFE-xGnP-25 and contrast heat-conductive composite material PTFE-Gn-30 are tested, and the gained experimental result sees Table 1.The result shows that the thermal conductivity of PTFE-xGnP-25 is 1.63 times of PTFE-Gn-30, and its tensile strength is 2.27 times of PTFE-Gn-30.
Embodiment 6
600mg Graphene and 300mg carbon nanotube are joined in the 800mL Virahol,, obtain graphene suspension through ultra-sonic dispersion 24 hours; 29.1g polymethylmethacrylate (PMMA) powder is added in the suspension, high-speed stirring was removed Virahol through reduction vaporization after 6 hours, obtained the mixture of Graphene, carbon nanotube and polymethylmethacrylate again; Graphene and poly mixture are joined in the mould, under 170 ℃, the hot-forming high-heat-conductive composite material (be called for short PMMA-xGnP (2)-CNT (1)-10) that promptly obtains of 14MPa, wherein, the total mass content of high heat conductive filler in matrix material is 10%.Cut test specimens according to the specimen size.
The heat conductivility of PMMA-xGnP (2)-CNT (1)-10 and contrast heat-conductive composite material PP-CNT-15 and the detected result of tensile strength see Table 1.The result shows, the heat conductive filler mass content is that the unmodified original copolymer PMMA of thermal conductivity ratio of PMMA-xGnP (2)-CNT (1)-10 of 10% has increased by 6.2 times, and the heat conductive filler mass content is that the thermal conductivity of 15% PP-CNT-15 only increases by 1.99 times than unmodified original copolymer PP; The tensile strength of PMMA-xGnP (2)-CNT (1)-10 is suitable with unmodified PMMA.
Embodiment 7
4.5g Graphene and 1.5g asphalt base carbon fiber and 34g polyvinyl chloride (PVC) joined carried out ball milling in the ball mill 1 hour, obtain mixed powder; Mixed powder is joined in the mould, the hot-forming high-heat-conductive composite material (PVC-xGnP (3)-CF (1)-11) that promptly obtains under 250 ℃, 18MPa, wherein heat conductive filler is 11% at the total mass content of matrix material.
Heat conductivility and the tensile strength of PVC-xGnP (3)-CF (1)-11 and contrast heat-conductive composite material PP-CNT-15 are tested, and the gained experimental result sees Table 1.The result shows, the heat conductive filler mass content is that the unmodified PVC of thermal conductivity ratio of PVC-xGnP (3)-CF (1)-11 of 10% compares and improved 6.3 times, has only improved 1.99 times than unmodified PP and the heat conductive filler mass content is the thermal conductivity of 15% PP-CNT-15; And the tensile strength of PVC-xGnP (3)-CF (1)-11 is suitable with unmodified PVC.
Embodiment 8
Behind 6g Graphene and 0.03g carbon nanotube and 34g polypropylene powder usefulness homogenizer premix, the mixed powder of gained is plastified with mixing with driving plastics processing mill down at 200 ℃, directly take off mixing material through the crusher in crushing granulation then from mill, high-heat-conductive composite material (PP-xGnP-15), wherein the mass content of heat conductive filler in matrix material is 15%.With the pellet that makes put under 200 ℃ on the mould, 14MPa pressure forming machine compression moulding, cut test specimens according to the specimen size.
Heat conductivility and the tensile strength of PP-xGnP-15 and contrast heat-conductive composite material PP-CNT-15 are tested, and the gained experimental result sees Table 1.The result shows that under the identical situation of heat conductive filler mass content, the thermal conductivity of PP-xGnP-15 is 2.33 times of PP-CNT-15, and tensile strength is a little more than unmodified PP.
Embodiment 9
8g Graphene and 0.16g carbon nanotube and poly-perfluoro alkoxy ester (PFA) powder of 32.64g joined carried out ball milling in the ball mill 1 hour, then just the mixed powder of gained put under 280 ℃ on the mould, 16MPa pressure forming machine compression moulding, promptly obtain high-heat-conductive composite material (being called for short PFA-xGnP-20), the total mass content of wherein high heat conductive filler in matrix material is 20%.Cut test specimens according to the specimen size.
Heat conductivility and the tensile strength detected result of PFA-xGnP-20 and contrast heat-conductive composite material PP-Gn-40 see Table 1.The result shows, the heat conductive filler mass content is that the unmodified PFA of thermal conductivity ratio of 20% PFA-xGnP-20 has improved 8.5 times, only improved 6.3 times than unmodified PP and the heat conductive filler mass content is the thermal conductivity of 40% PP-Gn-40; The tensile strength of PFA-xGnP-20 is suitable with unmodified PFA, and the tensile strength of PP-Gn-40 only is 0.53 times of unmodified PP.
Embodiment 10
Behind 5g Graphene, 1g carbon nanotube and 34g high density polyethylene(HDPE) (HDPE) powder usefulness homogenizer premix, the mixed powder of gained is plastified with mixing with driving plastics processing mill down at 200 ℃, then with the mixing material that makes through the crusher in crushing granulation, obtain high-heat-conductive composite material (being called for short HDPE-xGnP (5)-CNT (1)-15), the total mass content of wherein high heat conductive filler in matrix material is 15%.The pellet that makes is put into mould compression moulding under 190 ℃, 12MPa, cut test specimens according to the specimen size.
Thermal conductivity and the tensile strength detected result of HDPE-xGnP (5)-CNT (1)-15 and contrast heat-conductive composite material HDPE-CNT-38 see Table 1.HDPE-CNT-38 is to be heat conductive filler with the carbon nanotube, and high density polyethylene(HDPE) (HDPE) is that (J.Appl.Phys.2006, A85:25-28), the carbon nanotube mass content is 38% for the matrix material of base material.The result shows, high heat conductive filler mass content is that the thermal conductivity of HDPE-xGnP (5)-CNT (1)-15 of 15% is that high heat conductive filler mass content is 2.26 times of 38% HDPE-CNT-38.
Embodiment 11
Behind 6g Graphene and 2g carbon nanotube and 34g polypropylene usefulness homogenizer premix, the mixed powder of gained is plastified with mixing with driving plastics processing mill down at 200 ℃, directly take off mixing material through the crusher in crushing granulation then from mill, promptly obtain high-heat-conductive composite material (being called for short PP-xGnP (3)-CNT (1)-20), the total mass content of wherein high heat conductive filler in matrix material is 20%.It is hot-forming under 230 ℃, 15MPa that the pellet that makes is put into mould, cuts test specimens according to the specimen size.
Heat conductivility and the tensile strength detected result of PP-xGnP (3)-CNT (1)-20 and contrast heat-conductive composite material PP-Gn-40 see Table 1.The result shows, high heat conductive filler mass content is that the thermal conductivity of PP-xGnP (3)-CNT (1)-20 of 20% is that high heat conductive filler quality is 1.35 times of 40% PP-Gn-40, and its tensile strength is 1.88 times of PP-Gn-40.
Embodiment 12
8g Graphene, 1g asphalt base carbon fiber and 15g polycarbonate (PC) powder are carried out mechanically mixing, then with the twin screw extruder granulation of the mixed powder of gained, obtain high-heat-conductive composite material (being called for short PC-xGnP (8)-CF (1)-30), the total mass content of wherein high heat conductive filler in matrix material is 30%.With the pellet that makes put into 250 ℃ on mould, 14MPa is hot-forming, cuts test specimens according to the specimen size.
Heat conductivility and the tensile strength detected result of PC-xGnP (8)-CF (1)-30 and contrast heat-conductive composite material PTFE-Gn-30 see Table 1.Under the identical situation of high heat conductive filler mass content, the thermal conductivity of PC-xGnP (8)-CF (1)-30 is 12 times of the preceding PC of modification, and the thermal conductivity of PTFE-Gn-30 only is 6 times of the preceding PTFE of modification; Tensile strength and the PC of PC-xGnP (8)-CF (1)-30 are suitable, and the tensile strength of PTFE-Gn-30 only is 0.44 times of PTFE.
The thermal conductivity of the high-heat-conductive composite material that makes from above each embodiment and contrast heat-conductive composite material and the test result analysis of tensile strength be as can be seen: under the situation of low sizing consumption, the thermal conductivity of high-heat-conductive composite material of the present invention i.e. original copolymer before the modification; Under the identical situation of high heat conductive filler consumption, the thermal conductivity of high-heat-conductive composite material provided by the invention is far above existing thermally conductive material; Along with the increase of heat conductive filler consumption, the tensile strength and the original copolymer of highly heat-conductive material provided by the invention are suitable, and the tensile strength of existing thermally conductive material then significantly descends, and only are 0.44 times of original copolymer.Therefore, high-heat-conductive composite material provided by the invention has heat conductivility excellence, amount of filler is few, comprehensive mechanical property is good advantage.
Table 1
Claims (6)
1. a high-heat-conductive composite material comprises high heat conductive filler and thermoplastic polymer, it is characterized in that described high heat conductive filler is the mixture of Graphene and fibrous heat conductive filler, and the mass ratio of wherein fibrous heat conductive filler and Graphene is 1: 1～1: 200.
2. root high-heat-conductive composite material according to claim 1 is characterized in that described high heat conductive filler accounts for 5%～35% of high-heat-conductive composite material total mass.
3. high-heat-conductive composite material according to claim 1 is characterized in that described thermoplastic polymer is any in polyethylene, polypropylene, polyvinylidene difluoride (PVDF), tetrafluoroethylene, poly-perfluoro alkoxy ester, nylon, polymethylmethacrylate, polycarbonate or the polyvinyl chloride.
4. high-heat-conductive composite material according to claim 1 is characterized in that described fibrous heat conductive filler is carbon fiber or carbon nanotube.
5. high-heat-conductive composite material according to claim 4 is characterized in that described carbon fiber is preferably asphalt base carbon fiber.
6. the preparation method of the described high-heat-conductive composite material of claim 1, it is characterized in that described high heat conductive filler and thermoplastic polymer uniform mixing were disperseed 0.5～24 hour, to disperse back gained mixture pelleting, form the high-heat-conductive composite material pellet, it is hot-forming under 170 ℃～280 ℃, 10～18MPa more described high-heat-conductive composite material pellet to be put into mould.
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