CN111484832B - Graphene/silicon carbide nanowire composite structure thermal interface material - Google Patents
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Abstract
The application discloses a graphene/silicon carbide nanowire composite structure thermal interface material and a preparation method thereof. The thermal interface material comprises a graphene sheet and a silicon carbide nanowire, wherein the graphene sheet and the silicon carbide nanowire are mutually staggered. The thermal interface material adopts in-situ polymerization of silicon carbide nanowires between graphene sheets at a high temperature to form an interlayer heat conduction path, so that the out-of-plane thermal conductivity of the graphene film is improved, and the problem of low out-of-plane thermal conductivity of the thermal interface material is solved.
Description
Technical Field
The application relates to a graphene/silicon carbide nanowire compound structure thermal interface material, and belongs to the field of chemical materials.
Background
Miniaturization and integration of electronic components put higher demands on heat dissipation performance. The overheated environment affects its service life and operational reliability. Due to the existence of microscopic surface roughness, the actual contact area of the two solids only accounts for 1-2% of the apparent contact area, and the thermal conductivity of the rest is only 0.026 W.m-1K-1The air filling of (2) forms large contact thermal resistance between the heat source and the heat sink, and limits the heat dissipation.
In order to solve the problem, a thermal interface material is used between the heat source and the heat sink to fill an air gap, reduce contact thermal resistance and improve heat dissipation efficiency. The traditional thermal interface material is mainly prepared by mixing some high-heat-conductivity ceramic fillers such as boron nitride, aluminum oxide and the like into a polymer matrixThe conductivity is usually 1 to 5Wm-1K-1And the problem of heat dissipation caused by high-power and high-density packaging in the electronic industry is difficult to solve.
Graphene has been widely used to solve the heat dissipation problem due to its ultra-high thermal conductivity. Lian et al (G.Xin, H.Sun, T.Hu, H.R.Fard, X.Sun, N.Koratkar, T.Borca-Tasciuc, J.Lian.Large-Area fresh Graphene Paper for Superior Thermal Management [ J.]Adv. mater.2014,26,4521.) graphene thin films were prepared by electrospray deposition technique, and the in-plane thermal conductivity could reach 1434W · m by applying pressure after heat treatment at 2850 ℃-1K-1. However, the conventional graphene paper has an out-of-plane thermal conductivity (0.1 to 3.4 W.m)-1K-1) Much lower than the in-plane thermal conductivity. Jiang et al (J.Zhang, G.Shi, C.Jiang, S.Ju, D.Jiang.3D bridge Carbon Nanoring/Graphene Hybrid Paper as a High-Performance coal burner [ J.Zhang, G.Shi, C.Jiang.S.Ju.]Small 2015,11,6197.) the three-dimensional bridged carbon nanoring/graphene hybrid paper is constructed by taking polymethyl methacrylate as a carbon source and nickel acetate as a catalyst and growing carbon nanorings in situ between graphene sheets through thermal reduction, and the out-of-plane thermal conductivity of the three-dimensional bridged carbon nanoring/graphene hybrid paper is 5.81 W.m-1K-1It is still difficult to meet the ever-increasing heat dissipation requirements.
Disclosure of Invention
According to one aspect of the application, a graphene/silicon carbide nanowire composite structure thermal interface material is provided, and the thermal interface material improves the out-of-plane thermal conductivity of a graphene film.
In the present application, the out-of-plane thermal conductivity is the thermal conductivity in the normal direction of the graphene paper.
A graphene/silicon carbide nanowire compound structure thermal interface material comprises graphene sheets and silicon carbide nanowires, wherein the graphene sheets and the silicon carbide nanowires are mutually staggered.
In the thermal interface material provided by the application, graphene forms a sheet structure, and the silicon carbide nanowires are distributed among graphene sheets in a general vertical trend.
Optionally, the width of the silicon carbide nanowire is 20-500 nm.
The silicon carbide nanowires are of a flaky strip structure, and provide out-of-plane heat conduction paths.
Optionally, the thermal interface material has an out-of-plane thermal conductivity greater than 10W · m-1K-1
According to another aspect of the present application, there is also provided a method for preparing the graphene/silicon carbide nanowire composite structure thermal interface material, comprising the following steps: and (3) growing the silicon carbide nanowires in situ between the graphene sheets by adopting a high-frequency heating method to obtain the thermal interface material.
This application adopts high frequency heating at the off-plane thermal conductivity of the laminated normal position growth silicon carbide nano-wire of graphite alkene in order to improve graphite alkene film.
Optionally, the method comprises at least the following steps:
and carrying out high-frequency electric field heating treatment on the film containing the silicon dioxide nanoparticle modified graphene oxide and graphene to obtain the thermal interface material.
Specifically, in one example, the preparation method comprises:
a) drying the mixed solution containing the silicon dioxide nanoparticles and the graphene oxide to obtain silicon dioxide nanoparticle modified graphene oxide;
b) mixing the graphene oxide modified by the silicon dioxide nanoparticles and graphene in ethanol to obtain a dispersion liquid;
c) carrying out suction filtration on the dispersion liquid to obtain a film, namely the composite graphene paper;
d) and (3) carrying out high-frequency electric field heating treatment on the film (composite graphene paper) to obtain the thermal interface material.
In the application, the composite graphene paper is made of SiO2And mixing the nano-particle modified graphene oxide and graphene, and performing suction filtration to obtain the paper-like substance.
Optionally, the silica nanoparticle modified graphene oxide is prepared by a method comprising the following steps:
mixing the dispersion liquid containing the graphene oxide with alkyl silicate and alkaline substances, and performing ultrasonic treatment to obtain the graphene oxide modified by the silicon dioxide-containing nanoparticles;
the alkyl silicate is selected from at least one of compounds having a structural formula shown in formula I:
wherein R is1、R2、R3、R4Independently selected from C1～C5Alkyl groups of (a);
the alkaline substance is selected from organic amine and/or ammonia water.
Specifically, the preparation method of the graphene oxide modified by the silica nanoparticles comprises the following steps: dispersing graphene oxide in an ethanol aqueous solution, adding alkyl silicate and an alkaline substance, performing ultrasonic treatment, hydrolyzing the alkyl silicate in an alkaline environment to generate silicon dioxide nanoparticles, and drying to obtain silicon dioxide nanoparticle modified graphene oxide;
preferably, the alkyl silicate is selected from ethyl orthosilicate and the alkaline substance is selected from ammonia.
The silica nanoparticle-modified graphene oxide in the present application means that the silica nanoparticles are attached to a sheet layer of graphene oxide.
Optionally, the high-frequency heating temperature is 1000-1600 ℃, and the high-frequency heating time is 1-10 min;
preferably, the high-frequency heating temperature is 1300-1500 ℃, and the high-frequency heating time is 2-6 min.
The upper limit of the high-frequency heating temperature is selected from 1300 ℃, 1400 ℃, 1500 ℃, 1600 ℃, and the lower limit of the high-frequency heating temperature is selected from 1000 ℃, 1300 ℃, 1400 ℃, 1500 ℃.
The upper limit of the high-frequency heating time is selected from 2min, 4min, 6min and 10min, and the lower limit of the high-frequency heating time is selected from 1min, 2min, 4min and 6 min.
Optionally, the frequency of the high-frequency heating is 30-300 kHz.
The proportion relationship of graphene oxide, alkyl silicate and graphene can be selected by those skilled in the art according to actual needs.
Preferably, the ratio of the graphene oxide to the alkyl silicate is: mass of graphene oxide: the volume of the alkyl silicate is 200-300: 1 g/L; the mass ratio of the silicon dioxide nanoparticle-modified graphene oxide to graphene is 1: 5 to 15.
Optionally, after the high-frequency electric field heating treatment is performed on the film containing the graphene oxide modified by the silica nanoparticles and the graphene, the method further includes a step of pressurizing the film, so that the thermal interface material is obtained.
In the application, the thin film containing the graphene oxide modified by the silica nanoparticles and the graphene is the composite graphene paper. The thermal interface material can be obtained by carrying out high-frequency electric field heating treatment on the composite graphene paper or carrying out pressurization treatment after the high-frequency electric field heating treatment.
Optionally, the pressure during the pressurization treatment is 50-100 psi.
The silicon carbide nanowire is prepared by uniformly dispersing a nano silicon source between graphene layers and then carrying out high-frequency heat treatment. If the dispersing effect is poor after the nano silicon oxide and the graphene are directly blended, the inventor firstly decorates nano particles on the surface of the graphene oxide, and then mixes the nano particles with the graphene oxide to realize uniform dispersion.
The beneficial effects that this application can produce include:
according to the method, the silicon carbide nanowires are polymerized in situ between graphene sheets by high-frequency heating to form an interlayer heat conduction path, so that the out-of-plane heat conductivity of the graphene film is improved, and the problem of low out-of-plane heat conductivity of a thermal interface material is solved.
The thermal interface material provided by the application has the out-of-plane thermal conductivity higher than 10 W.m-1K-1。
Drawings
Fig. 1 is a scanning electron microscope photograph of graphene oxide modified with silica nanoparticles according to example 1;
FIG. 2 is a scanning electron microscope photograph of a cross section of the graphene sheet/silicon carbide nanowire hybrid paper in example 1;
FIG. 3 is a scanning electron micrograph of a cross section of the graphene paper of comparative example 1;
figure 4 is the XRD pattern of example 1.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples. Unless otherwise specified, the raw materials used in the examples were all purchased commercially and used without further treatment; the instruments and equipment adopted in the embodiment all adopt factory recommended parameters.
Raw materials and reagents used in this application:
graphene sheets: ningbo ink science and technology, Inc.;
graphene oxide sheets: qingdao Huagaoyaomene technologies, Inc.;
ethyl orthosilicate: analytical purity, chemical reagents of national drug group limited;
ethanol: analytical purity, chemical reagents of national drug group limited;
ammonia water: analytically pure, chemical reagents of national drug group, ltd.
The instrument equipment comprises:
in the examples, the out-of-plane thermal conductivity of the samples was determined using LFA 467 laser scintillator (Netzsch, Germany);
the morphology of the sample was determined using a field emission scanning electron microscope (Quanta FEG250, FEI, USA);
the ultrasonic cleaning is performed by using a KQ3200DA type numerical control ultrasonic cleaner (ultrasonic instruments, Inc. of Kunshan city);
electronic balance (aohaus instruments (shanghai) ltd) was used for weighing;
heating by a high-frequency electric field by adopting an XJH-15KW variable frequency welding machine (Shalingsu practice Co., Ltd., Dongguan city);
x-ray diffraction analysis of the samples D8Discover with GADDS (Bruker, Germany) with CuKaradiation
The thermal interface material consists of a graphene sheet and a silicon carbide nanowire, wherein the silicon carbide nanowire is formed by in-situ polymerization of a silicon source and a carbon source between graphene sheets through high-frequency heating.
The silicon carbide nanowires in the thermal interface material provide an out-of-plane thermal conduction path.
The silicon source in the thermal interface material is silicon dioxide nano-particles generated by hydrolyzing tetraethoxysilane in an alkaline environment.
In the preparation process of the thermal interface material, a silicon source is distributed among graphene sheets.
The in-situ polymerization temperature of the silicon carbide nanowires in the thermal interface material is 1000-1600 ℃, and preferably, the in-situ polymerization temperature of the silicon carbide nanowires is 1300-1500 ℃.
The thermal interface material is heated by high frequency for 1-10 min, preferably 2-6 min.
The preparation of the thermal interface material comprises the following steps:
(1) graphene oxide sheets modified by silica nanoparticles and graphene sheets are mixed according to the mass ratio of 1: 10 mixing in ethanol to obtain a dispersion;
(2) filtering the dispersion liquid obtained in the step (1) to obtain a film, namely the composite graphene paper;
(3) and (3) carrying out high-frequency heating treatment on the film (composite graphene paper) in the step (2) to obtain the thermal interface material.
Example 1:
and dispersing 120mg of graphene oxide in a mixed solution of 240mL of ethanol and 24mL of deionized water, and carrying out ultrasonic treatment for 120 min. 4mL of ammonia water and 0.5mL of ethyl orthosilicate are added, and the mixture is subjected to ultrasonic treatment for 180 min. Vacuum filtering, washing with deionized water several times, and oven drying. And weighing 20mg of dried powder and 180mg of graphene sheets, dispersing in ethanol, performing ultrasonic treatment, and performing suction filtration to obtain the composite graphene paper. Heating the filtered film (composite graphene paper) at 1400 ℃ for 4min at high frequency (frequency of 250kHz) to obtain the silicon carbide nanowire/graphene sheet hybrid paper, namely the thermal interface material, and recording the thermal interface material as sample No. 1.
Example 2:
and dispersing 120mg of graphene oxide in a mixed solution of 240mL of ethanol and 24mL of deionized water, and carrying out ultrasonic treatment for 120 min. 4mL of ammonia water and 0.5mL of ethyl orthosilicate are added, and the mixture is subjected to ultrasonic treatment for 180 min. Vacuum filtering, washing with deionized water several times, and oven drying. And weighing 20mg of dried powder and 180mg of graphene sheets, dispersing in ethanol, performing ultrasonic treatment, and performing suction filtration to obtain the composite graphene paper. Heating the vacuum-filtered film (composite graphene paper) at 1400 ℃ and high frequency (frequency 300kHz) for 4min, and then applying 75psi pressure to the film to obtain the silicon carbide nanowire/graphene sheet hybrid paper, namely the thermal interface material, which is recorded as sample No. 2.
Example 3
The difference from the embodiment 1 is that: the vacuum-filtered film was heated at 1000 ℃ for 10min in high frequency, and the result was designated as sample # 3.
Example 4
The difference from the embodiment 1 is that: the vacuum-filtered film was heated at 1600 ℃ for 1min at high frequency, and the result was recorded as sample # 4.
Example 5
The difference from the embodiment 1 is that: the vacuum-filtered film was heated at 1300 ℃ for 6min in high frequency, and the result was recorded as sample # 5.
Example 6
The difference from the embodiment 1 is that: heating the vacuum-filtered film at 1500 deg.C for 2min, and recording as # 6.
Comparative example 1
And dispersing 200mg of graphene in ethanol, performing ultrasonic treatment, and performing suction filtration. The suction-filtered film was heated at 1400 ℃ for 4min with high frequency to obtain a film sample of comparative example 1.
Comparative example 2
And dispersing 200mg of graphene in ethanol, performing ultrasonic treatment, and performing suction filtration. The suction-filtered film was heated at 1400 ℃ for 4min with high frequency, and then a pressure of 75psi was applied to the film to obtain a film sample of comparative example 2.
Example 7 phase and morphology analysis of thermal interface materials
XRD testing and scanning electron microscope analysis were performed on samples # 1 to # 6, respectively, and scanning electron microscope analysis was performed on comparative example 1 and comparative example 2.
The XRD test result shows that: in the XRD patterns of samples 1# to 6#, characteristic peaks (2 θ: 35.6, 60, and 71.8) of 3C — SiC were observed. The XRD pattern of the representative sample No. 1 is shown in FIG. 4, and can be seen from FIG. 4: after the high-frequency heating, characteristic peaks (2 θ ═ 35.6, 60, and 71.8) of 3C — SiC appeared, and it was confirmed that silicon carbide nanowires were produced.
Scanning electron microscope results show that the thermal interface material comprises the graphene sheet and the silicon carbide nanowire, and the width of the silicon carbide nanowire is 20-500 nm. The scanning electron micrograph of the sample # 1, which is typically represented, is shown in FIG. 2.
Taking comparative example 1 as a representative, fig. 3 is a scanning electron microscope photograph of a cross section of the graphene paper in comparative example 1, and as can be seen from fig. 3, the graphene paper has a layered structure.
Example 8
The out-of-plane thermal conductivity tests are respectively carried out on samples 1# to 6# and comparative examples 1 and 2, and the test results show that the samples 1# to 6# have higher out-of-plane thermal conductivity, and the out-of-plane thermal conductivity is higher than 10 W.m-1K-1。
Typical representatives are sample # 1 and sample 2 and comparative example 1 and comparative example 2:
the out-of-plane thermal conductivity of sample No. 1 was 10.9 W.m-1K-1；
The out-of-plane thermal conductivity of sample No. 2 was 17.6 W.m-1K-1；
The out-of-plane thermal conductivity of comparative example 1 was 6.8 W.m-1K-1；
The out-of-plane thermal conductivity of comparative example 2 was 5.8 W.m-1K-1。
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (6)
1. A preparation method of a graphene/silicon carbide nanowire compound structure thermal interface material is characterized in that a high-frequency heating method is adopted, so that silicon carbide nanowires grow in situ between graphene sheets, and the thermal interface material can be obtained;
the method comprises at least the following steps:
carrying out high-frequency electric field heating treatment on the film containing the silicon dioxide nanoparticle modified graphene oxide and graphene to obtain the thermal interface material;
the thermal interface material comprises a graphene sheet and a silicon carbide nanowire, wherein the graphene sheet and the silicon carbide nanowire are mutually staggered;
the silicon dioxide nanoparticle modified graphene oxide is prepared by a method comprising the following steps:
mixing the dispersion liquid containing the graphene oxide with alkyl silicate and alkaline substances, and performing ultrasonic treatment to obtain the graphene oxide modified by the silicon dioxide nanoparticles;
the alkyl silicate is selected from at least one of compounds having a structural formula shown in formula I:
Wherein R is1、R2、R3、R4Independently selected from C1~C5Alkyl groups of (a);
the alkaline substance is selected from organic amine and/or ammonia water;
the ratio of the graphene oxide to the alkyl silicate is:
mass of graphene oxide: the volume of the alkyl silicate is = 200-300: 1 g/L;
the mass ratio of the silicon dioxide nanoparticle-modified graphene oxide to graphene is 1: 5-15;
and after the film containing the silicon dioxide nanoparticle modified graphene oxide and graphene is subjected to high-frequency electric field heating treatment, pressurizing the film to obtain the thermal interface material.
2. The preparation method according to claim 1, wherein the silicon carbide nanowires have a width of 20 to 500 nm.
3. The method of claim 1, wherein the thermal interface material has an out-of-plane thermal conductivity greater than 10W-m-1K-1。
4. The method according to claim 1, wherein the high-frequency heating is performed at a temperature of 1000 to 1600 ℃ for 1 to 10 min.
5. The method according to claim 1, wherein the high-frequency heating is carried out at a temperature of 1300 to 1500 ℃ for 2 to 6 min.
6. The method according to claim 1, wherein the frequency of the high-frequency heating is 30 to 300 kHz.
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| CN113150748B (en) * | 2021-05-18 | 2021-12-21 | 黑龙江科技大学 | Preparation method of graphene heat dissipation composite material |
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