CN109912912B - Flexible and electric-insulation fluorinated graphene heat-conducting composite film and preparation and application thereof - Google Patents
Flexible and electric-insulation fluorinated graphene heat-conducting composite film and preparation and application thereof Download PDFInfo
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Abstract
The invention relates to a flexible and electric-insulation fluorinated graphene heat-conducting composite film, and a preparation method and application thereof. Preparation: and (3) orderly accumulating fluorinated graphene nanosheets on the base membrane by a reduced-pressure auxiliary filtration membrane forming method of the uniformly dispersed solution of polyvinyl alcohol/fluorinated graphene. The fluorinated graphene composite film obtained by the method has high in-plane thermal conductivity, and simultaneously keeps good electrical insulation and bendability, so that the fluorinated graphene composite film has potential application value in the thermal management of future flexible electronic devices. The method is convenient to operate, relatively simple in preparation conditions, low in production cost, easy for batch and large-scale production, and has a good industrial production basis and a wide application prospect.
Description
Technical Field
The invention belongs to the field of heat-conducting composite films and preparation and application thereof, and particularly relates to a flexible and electric-insulation fluorinated graphene heat-conducting composite film and preparation and application thereof.
Background
In the past decade, rapid development of various portable devices (mobile phones, tablet computers and other intelligent devices) towards multi-functionalization, light weight and flexibility has made higher requirements on indexes such as integration, miniaturization and high power of internal electronic components. In such cases, the increase in heat flow per unit area will inevitably lead to serious heat dissipation problems, which in turn are strongly related to the lifetime and operational reliability of the electronic device. The use of an anisotropic heat conductive film having high in-plane direction thermal conductivity, good electrical insulation, and flexibility as a heat dissipating material is considered to be an effective method for solving overheating of highly integrated electronic devices.
Graphene, the two-dimensional material of most current interest, has an ultra-high thermal conductivity (-5300W m-1K-1) Excellent flexibility and high aspect ratio. These excellent combinations of properties make them an excellent alternative to traditional thermally conductive fillers in the preparation of thermally conductive materials. Among many heat-conducting composite materials, the flexible graphene heat-conducting film prepared by the high-temperature graphitization treatment of the graphene oxide film has ultrahigh macroscopic thermal conductivity (more than 1000W m)-1K-1) But has received a great deal of attention from both academic and business circles (adv.2014,24, 4542; small,2018,14, 1801346; adv.mater.2017,29,1700589). For example, Liu et al report that graphene thermal conductive film is obtained by natural volatilization drying of GO aqueous solution on aluminum plate and high-temperature graphitization treatment, and its in-plane thermal conductivity can reach 3200W m-1K-1(Small,2018,14, 1801346). There are also a number of literature reports of compounding commercial graphene micro-sheets or reduced graphene oxide with some polymer molecules to directly prepare self-supporting, thermally conductive composite films (ACS appl.mater.interfaces,2018,10, 41690; j.mater.chem.c,2016,4, 305; composite.sci.technol., 2017,138,179). Unfortunately, although these graphene-based thermally conductive films have excellent in-plane thermal conductivity, the excellent electrical conductivity of graphene itself also leads to generally poor electrical insulation of the composite films, which greatly limits their application in some electronic devices with high integration degree. Although the introduction of some insulating nanomaterials such as boron nitride (chem.mater.,2016,28, 1049-. Furthermore, in view of the need for electrical insulation, boron nitride, which also has a higher thermal conductivity while having excellent electrical insulation properties, is considered as an effective substitute for graphene as a thermally conductive filler. To date, boron nitride films reported in the literature have been constructed with certain strength mainly by introducing small amounts of organic macromolecules as interlayer adhesives (ACS appl. mater. interfaces,2017,9, 30035; 2D mater, 2017,4, 025047; comp. sci. technol.,2018,160,199). However, the in-plane thermal conductivity of the currently reported boron nitride heat-conducting film is less than 60W m-1K-1。
Fluorination of graphene can bond carbon-carbon bonds from sp2To sp3And converting to realize effective regulation and control of the forbidden band width of the graphene. As reflected in intrinsic performance, the conductivity of graphene shows a rapid decrease, i.e., a rapid change from a conductive state to an insulator state, as the degree of fluorination increases. However, graphiteThe thermal conductivity of alkenes varies greatly with the degree of fluorination. Simulation experiments show that the thermal conductivity of the graphene shows a U-shaped change trend along with the increase of the fluorination degree. When the degree of fluorination reaches 100%, the thermal conductivity of the fluorinated graphene may reach 35% of the initial value. That is, perfluorinated graphene may be able to maintain over 1800W m while possessing good electrical insulation and flexibility-1K-1The theoretical thermal conductivity of (1). Therefore, we can imagine that the preparation of a thermally conductive film using perfluorinated or highly fluorinated graphene nanoplatelets as a thermally conductive filler is expected to achieve both high thermal conductivity and excellent electrical insulation. At present, no literature or patent report exists on the application of fluorinated graphene as a heat conducting filler in the preparation of heat dissipation materials.
Disclosure of Invention
The invention aims to solve the technical problem of providing a flexible and electrically-insulating fluorinated graphene heat-conducting composite film and preparation and application thereof, and overcomes the defects of poor heat conductivity and non-insulating graphene film of a boron nitride composite film obtained in the prior art.
The fluorinated graphene heat-conducting composite film comprises fluorinated graphene nanosheets and interlayer adhesive polyvinyl alcohol, wherein polyvinyl alcohol molecular chains are distributed among the layers of the fluorinated graphene nanosheets which are arranged in an ordered orientation manner and are bonded with adjacent layers.
The fluorinated graphene nanosheets are highly oriented along the in-plane direction of the membrane, so that heat transfer along the in-plane direction of the membrane can be effectively promoted, and the polyvinyl alcohol has the effects of bonding adjacent lamellar layers, reducing interlayer interface thermal resistance and improving the mechanical property of the membrane.
As used herein, "ordered orientation" refers to the phenomenon of a one-dimensional or two-dimensional nanofiller having a large aspect ratio, which is regularly distributed in a certain order along a certain direction in space in the radial or axial direction.
The mass ratio of the fluorinated graphene to the polyvinyl alcohol is 5-14: 1 to 2.
The highly ordered anisotropic film is prepared by a reduced pressure assisted filtration film-forming process.
The preparation method of the fluorinated graphene heat-conducting composite membrane comprises the following steps:
(1) dispersing fluorinated graphene in a solvent, performing ultrasonic treatment and centrifuging to obtain an exfoliated fluorinated graphene nanosheet;
(2) dispersing the fluorinated graphene nanosheets in water, adding a polyvinyl alcohol aqueous solution, performing ultrasonic treatment to obtain a fluorinated graphene dispersion solution, and performing reduced pressure filtration to obtain the fluorinated graphene heat-conducting composite membrane.
The preferred mode of the above preparation method is as follows:
the solvent in the step (1) is one or more of N, N-dimethylformamide, isopropanol, N-methylpyrrolidone and dichloromethane.
The ultrasound in the step (1) is performed by a water bath ultrasound instrument with the power of 150- & lt500 & gt W and the ultrasound time of 8-24 h; centrifuging: centrifuging for 5-20min at the rotating speed of 1000-.
Further, the ultrasonic power in the step (1) is one of 150W, 250W and 500W.
The molecular weight of the polyvinyl alcohol in the step (2) is 47-205 kg/mol.
Further, the molecular weight of the polyvinyl alcohol in the step (2) is one of 47kg/mol, 67kg/mol, 145kg/mol and 205 kg/mol.
Dispersing fluorinated graphene nanoplatelets in water in the step (2), wherein the mass-to-volume ratio of the fluorinated graphene nanoplatelets to the water is 20-40 mg: 100-; the concentration of the polyvinyl alcohol aqueous solution is 6 wt%; the mass ratio of the fluorinated graphene nanosheet to the polyvinyl alcohol is 20-40 mg: 3-40 mg.
The ultrasonic time in the step (2) is 20-60 min; the reduced pressure filtration is carried out by adopting a reduced pressure filtration device using mixed cellulose acetate as a filtration membrane.
The application of the fluorinated graphene heat-conducting composite film provided by the invention has a great potential application value in the aspect of heat management of portable or flexible electronic equipment.
Advantageous effects
(1) The invention mainly utilizes the characteristics of high thermal conductivity, electrical insulation and two-dimensional flexibility of the highly fluorinated graphene to solve the problems of low thermal conductivity and non-insulation of a graphene film in chemical reduction or low-degree thermal reduction;
(2) according to the method provided by the invention, the anisotropic fluorinated graphene heat-conducting composite film with high heat conductivity, good electrical insulation and good bending property can be obtained, and the fluorinated graphene nanosheets are stacked layer by layer along the in-plane direction of the film by mainly adopting a reduced-pressure auxiliary filtration method to obtain an anisotropic ordered film, so that the heat conductivity of the film in the in-plane direction is greatly improved; in addition, a small amount of polyvinyl alcohol is added to be used as an interlayer adhesive to strengthen the interaction between adjacent sheets and play a role in reducing the thermal resistance of an interlayer interface. The fluorinated graphene heat-conducting composite film prepared by the method has a great potential application value in the heat management of future highly-integrated portable or flexible electronic equipment;
(3) the method has the advantages of convenient operation, relatively simple preparation conditions, lower production cost, easy batch and large-scale production, good industrial production basis and wide application prospect;
(4) in the flexible and electric insulation fluorinated graphene heat-conducting composite film, the fluorinated graphene nanosheets have high orientation arrangement characteristics along the in-plane direction, and the polyvinyl alcohol serving as an interlayer adhesive effectively enhances the interaction between layers, so that the prepared composite film shows good heat conductivity, electric insulation and bending property, when the addition amount of the fluorinated graphene is 93 wt%, the in-plane heat conductivity of the composite film can reach 61.3W/mK, and meanwhile, the good electric insulation property is maintained (the fluorinated graphene is prepared by using polyvinyl alcohol as an interlayer adhesive, the composite film has good heat conductivity, electric insulation property and bending property>1011Ω cm). Although the thermal conductivity of the fluorinated graphene composite film obtained by the invention is smaller than that of the graphene thermal conductive film obtained by graphitizing graphene oxide at high temperature (in the aspect of thermal conductivity)>1000W m-1K-1) But higher than the vast majority of self-supporting materials prepared by compounding graphene nanoplatelets or reduced graphene oxide with some polymer moleculesHeat conductive composite film (<50W m-1K-1) (Nanoscale,2016,8, 19984; ACS appl. mater. interfaces,2018,10, 41690; mate chem.c,2016,4, 305; ). In addition, the fluorinated graphene film prepared by the invention is remarkably higher than the graphene-based heat-conducting composite film in electrical insulation performance.
Drawings
FIG. 1 is a transmission electron microscope photograph of the fluorinated graphene used in examples 1 to 5.
FIG. 2 is an X-ray photoelectron spectrum of the fluorinated graphene used in examples 1 to 5.
FIG. 3 is a scanning electron microscope image of the brittle fracture of fluorinated graphene films with different polyvinyl alcohol contents in examples 1 to 5; wherein a, b, c and d represent the addition amounts of the fluorinated graphene of 93 wt%, 88.6 wt%, 81.8 wt% and 73.3 wt%, respectively.
FIG. 4 is a tensile stress-strain curve of fluorinated graphene films of examples 1-5 with different polyvinyl alcohol content.
Fig. 5 is a graph of the flexibility displays of the fluorinated graphene films with polyvinyl alcohol content of 7 wt% (a) and 26.7 wt% (b) in examples 1 and 5, respectively.
FIG. 6 is a graph of the volume resistivity of fluorinated graphene films of different polyvinyl alcohol content in examples 1-5.
FIG. 7 is a graph of in-plane thermal conductivity for fluorinated graphene films of different polyvinyl alcohol content in examples 1-5.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
And (3) reagent sources: graphite fluoride was purchased from Yucheng science and technology, Inc. of Hubei (size 5-10 microns, fluorine content about 58 wt%); isopropanol was purchased from national pharmaceutical agents; polyvinyl alcohol was purchased from alatin reagent.
Example 1
(1) Dispersing commercial graphite fluoride powder in isopropanol, performing ultrasonic treatment on a water bath ultrasonic instrument for 24h (250W), and centrifuging the mixed dispersion liquid at the rotating speed of 3000rpm for 10min to obtain the peeled fluorinated graphene nanosheet.
(2) Weighing 40mg of the fluorinated graphene obtained in the step (1) and dispersing the fluorinated graphene in 200ml of water, adding 0.05ml of 6 wt% polyvinyl alcohol (molecular weight 145kg/mol) aqueous solution, and carrying out ultrasonic treatment for 30min to obtain uniformly dispersed fluorinated graphene dispersion liquid; and then pouring the dispersion liquid into a reduced pressure filtering device of the mixed cellulose acetate filter membrane to enable the fluorinated graphene nano-sheets to be uniformly deposited layer by layer to obtain the anisotropic composite graphene heat-conducting membrane, wherein the content of the fluorinated graphene under the condition is estimated to be 93 wt% by thermogravimetric analysis.
Transmission electron microscopy of fluorinated graphene as shown in fig. 1 shows that: the exfoliated fluorinated graphene is in a graphene-like sheet shape and has a large diameter-thickness ratio.
The X-ray photoelectron spectrum of fluorinated graphene, as shown in fig. 2, shows: the fluorine content of the exfoliated graphene fluoride was 48.2 at% (atomic%) and the fluorine/carbon atomic ratio was 0.94, indicating that it had a high degree of fluorination.
Example 2
(1) Dispersing commercial graphite fluoride powder in isopropanol, performing ultrasonic treatment on a water bath ultrasonic instrument for 24h (250W), and centrifuging the mixed dispersion liquid at the rotating speed of 3000rpm for 10min to obtain the peeled fluorinated graphene nanosheet.
(2) Weighing 40mg of the fluorinated graphene obtained in the step (1) and dispersing the fluorinated graphene in 200ml of water, adding 0.1ml of 6 wt% polyvinyl alcohol (molecular weight 145kg/mol) aqueous solution, and carrying out ultrasonic treatment for 30min to obtain uniformly dispersed fluorinated graphene dispersion liquid; and then pouring the dispersion liquid into a mixed cellulose acetate filter membrane reduced pressure filtration device, so that the fluorinated graphene nanosheets are uniformly deposited layer by layer to obtain the anisotropic composite graphene heat-conducting membrane, and the content of the fluorinated graphene under the condition is estimated to be 88.6 wt% by thermogravimetric analysis.
Example 3
(1) Dispersing commercial graphite fluoride powder in isopropanol, performing ultrasonic treatment on a water bath ultrasonic instrument for 24h (250W), and centrifuging the mixed dispersion liquid at the rotating speed of 3000rpm for 10min to obtain the peeled fluorinated graphene nanosheet.
(2) Weighing 40mg of the fluorinated graphene obtained in the step (1) and dispersing the fluorinated graphene in 200ml of water, adding 0.2ml of 6 wt% polyvinyl alcohol (molecular weight 145kg/mol) aqueous solution, and carrying out ultrasonic treatment for 30min to obtain uniformly dispersed fluorinated graphene dispersion liquid; and then pouring the dispersion liquid into a mixed cellulose acetate filter membrane reduced pressure filtration device, so that the fluorinated graphene nanosheets are uniformly deposited layer by layer to obtain the anisotropic composite graphene heat-conducting membrane, and the content of the fluorinated graphene under the condition is estimated to be 81.8 wt% by thermogravimetric analysis.
Example 4
(1) Dispersing commercial graphite fluoride powder in isopropanol, performing ultrasonic treatment on a water bath ultrasonic instrument for 24h (250W), and centrifuging the mixed dispersion liquid at the rotating speed of 3000rpm for 10min to obtain the peeled fluorinated graphene nanosheet.
(2) Weighing 40mg of the fluorinated graphene obtained in the step (1) and dispersing the fluorinated graphene in 200ml of water, adding 0.3ml of 6 wt% polyvinyl alcohol (molecular weight 145kg/mol) aqueous solution, and carrying out ultrasonic treatment for 30min to obtain uniformly dispersed fluorinated graphene dispersion liquid; and then pouring the dispersion liquid into a mixed cellulose acetate filter membrane reduced pressure filtration device, so that the fluorinated graphene nanosheets are uniformly deposited layer by layer to obtain the anisotropic composite graphene heat-conducting membrane, and the content of the fluorinated graphene under the condition is estimated to be 78.1 wt% by thermogravimetric analysis.
Example 5
(1) Dispersing commercial graphite fluoride powder in isopropanol, performing ultrasonic treatment on a water bath ultrasonic instrument for 24h (250W), and centrifuging the mixed dispersion liquid at the rotating speed of 3000rpm for 10min to obtain the peeled fluorinated graphene nanosheet.
(2) Weighing 40mg of the fluorinated graphene obtained in the step (1) and dispersing the fluorinated graphene in 200ml of water, adding 0.5ml of 6 wt% polyvinyl alcohol (molecular weight 145kg/mol) aqueous solution, and carrying out ultrasonic treatment for 30min to obtain uniformly dispersed fluorinated graphene dispersion liquid; and then pouring the dispersion liquid into a mixed cellulose acetate filter membrane reduced pressure filtration device, so that the fluorinated graphene nanosheets are uniformly deposited layer by layer to obtain the anisotropic composite graphene heat-conducting membrane, and the content of the fluorinated graphene under the condition is estimated to be 73.3 wt% by thermogravimetric analysis.
The brittle cross-section scanning electron microscope images of fluorinated graphene films of different polyvinyl alcohol content are shown in fig. 3, which shows that: and tightly orienting and stacking the fluorinated graphene nanosheets in the obtained fluorinated graphene film along the in-plane direction. However, as the addition amount of polyvinyl alcohol increases, the degree of orientation stacking order of the fluorinated graphene nanosheets gradually decreases, and the distance between adjacent sheets gradually increases due to filling of polyvinyl alcohol.
The tensile stress-strain curves for fluorinated graphene films of different polyvinyl alcohol content are shown in fig. 4, indicating that: the tensile strength of the composite film with the content of the fluorinated graphene of 93 wt% is 27.3MPa, and the tensile strength and the elongation at break of the composite film are increased along with the increase of the content of the polyvinyl alcohol.
The flexibility of the fluorinated graphene film is shown in fig. 5, indicating that: the fluorinated graphene composite membrane has good flexibility. The composite film having a fluorinated graphene content of 73.3 wt% has an excellent folding type and can be folded into a complicated shape even without being broken.
The volume resistivity of fluorinated graphene films of different polyvinyl alcohol content is shown in fig. 6, indicating that: the composite film still has excellent electrical insulation (the volume resistivity is always more than 10) even under the condition of high addition amount of the fluorinated graphene11Ωcm)。
The in-plane thermal conductivity of fluorinated graphene films of different polyvinyl alcohol content is shown in fig. 7, indicating that: with the increase of the addition of the fluorinated graphene, the in-plane thermal conductivity of the composite film is gradually improved, and when the content of the fluorinated graphene is 93 wt%, the in-plane thermal conductivity of the composite film can reach 61.3W m-1K-1Higher than the boron nitride-based electric insulation and heat conduction film reported in the literature at present: (<60W m-1K-1)(ACS Appl.Mater.Interfaces,2017,9,30035；2D Mater.,2017,4,025047；Compos.Sci.Technol.,2018,160,199；ACS Appl.Nano Mater.2018,1,4875)。
Comparative example 1
Zheng et al recently published in the journal of advanced functional materials (adv. funct. mater.2014,24,4542) first dissolved in water by graphene oxideThe graphene oxide film is prepared by a liquid low-temperature 50 ℃ drying method, and then the final graphene heat-conducting film is obtained by high-temperature graphitization operation at 2000 ℃. The graphene film has the in-plane thermal conductivity of 1100W m in terms of thermal conductivity-1K-1. In addition, the conductivity of the graphene composite membrane can reach 1000S cm-1Indicating that they have extremely excellent conductivity, which limits their use in some electronic devices to some extent. The fluorinated graphene film obtained in the invention has excellent electrical insulation and flexibility.
Comparative example 2
Drzal et al, published in Carbon journal (Carbon 2011,49,773), prepared thermally conductive composite films of thermally exfoliated graphene nanoplatelets and polyethyleneimine. The in-plane thermal conductivity of the composite film can reach 178W m-1K-1And the thermal conductivity of the fluorinated graphene thermal conductive composite film is relatively higher than that of the fluorinated graphene thermal conductive composite film. The electrical insulation of the composite films is still poor, which also limits their use in some electronic devices to some extent. The fluorinated graphene film obtained in the invention has excellent electrical insulation and flexibility.
Comparative example 3
Song et al recently published in journal of materials chemistry C (J.Mater.chem.C,2016,4,305) prepared a reduced graphene oxide (rGO) dispersion liquid with water-soluble cellulose Nanofibers (NFC) co-dispersed by a method of membrane extraction through reduced pressure filtration. The in-plane thermal conductivity of the NFC/rGO composite membrane is 6.17W m-1K-1And it is also electrically non-insulating. Therefore, the fluorinated graphene film prepared by the work is the NFC/rGO composite film in thermal conductivity and electrical insulation.
Comparative example 4
Xie et al recently published in the american chemical society for applied materials and journal of interfaces (j. mater. chem.c,2016,4,305) prepared a thermally conductive composite film of Oxidized Cellulose Nanocrystals (OCNC) and Graphene (GNS) nanoplatelets from a dispersion by a natural drying method. The in-plane thermal conductivity of the composite film can reach 25.66W m when the graphene content is 4.1 vol%-1K-1. Also, the fluorinated graphene film prepared in this work is due to the OCNC/GNS composite film in terms of both thermal conductivity and electrical insulation.
Comparative example 5
Li et al, recently published on composite science and technology (composite.sci.technol., 2017,138,179), produced thermally conductive composite films of cellulose Nanofibers (NFC) and Graphene Nanoplatelets (GNPs) by a method of membrane extraction by reduced pressure filtration. The in-plane thermal conductivity of the NFC/GNPs composite film can reach 59.46W m when the content of GNPs is 75 wt%-1K-1But it also has a better conductivity. Therefore, the fluorinated graphene film prepared by the work is better than the NFC/GNPs composite film in thermal conductivity and electrical insulation.
Claims (8)
1. The fluorinated graphene heat-conducting composite film is characterized by comprising fluorinated graphene nanosheets and polyvinyl alcohol, wherein polyvinyl alcohol molecular chains are distributed among the fluorinated graphene nanosheets which are arranged in an ordered orientation manner and are bonded with adjacent layers; wherein the mass ratio of the fluorinated graphene to the polyvinyl alcohol is 5-14: 1-2; wherein the fluorine/carbon atom ratio is 0.94.
2. A preparation method of the fluorinated graphene heat-conducting composite film according to claim 1, comprising the following steps:
(1) dispersing graphite fluoride in a solvent, performing ultrasonic treatment and centrifuging to obtain a stripped graphite fluoride nanosheet;
(2) dispersing the fluorinated graphene nanosheets in water, adding a polyvinyl alcohol aqueous solution, performing ultrasonic treatment to obtain a uniformly fluorinated graphene dispersion liquid, and performing reduced pressure filtration to obtain the fluorinated graphene heat-conducting composite membrane.
3. The preparation method according to claim 2, wherein the solvent in the step (1) is one or more of N, N-dimethylformamide, isopropanol, N-methylpyrrolidone and dichloromethane.
4. The preparation method according to claim 2, wherein the ultrasound in step (1) is performed by a water bath ultrasound instrument with a power of 150-; centrifuging: centrifuging for 5-20min at the rotating speed of 1000-.
5. The method according to claim 2, wherein the polyvinyl alcohol in the step (2) has a molecular weight of 47 to 205 kg/mol.
6. The preparation method according to claim 2, wherein the fluorinated graphene nanoplatelets are dispersed in water in step (2), wherein the mass-to-volume ratio of fluorinated graphene nanoplatelets to water is 20-40 mg: 100-; the concentration of the polyvinyl alcohol aqueous solution is 6 wt%; the mass ratio of the fluorinated graphene nanosheet to the polyvinyl alcohol is 20-40 mg: 3-40 mg.
7. The preparation method according to claim 2, wherein the ultrasonic time in the step (2) is 20-60 min; the reduced pressure filtration is carried out by adopting a reduced pressure filtration device using mixed cellulose acetate as a filtration membrane.
8. Use of the fluorinated graphene thermally conductive composite membrane of claim 1 in thermal management of portable or flexible electronic devices.
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