CN109943075A - A kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning - Google Patents
A kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the graphene thermally conductive silicone rubber composite material of magnetic aligning, belong to heat-conductivity polymer composite field.The composite material is made of the graphene and liquid silastic of magnetic aligning.Graphene surface is adsorbed by electrostatic interaction using the magnetic ferroferric oxide nano-particles of chemical coprecipitation preparation first, then magnetic/functionalized graphene uniform filling is distributed in liquid silica gel.It handled, be heating and curing by magnetic aligning, the graphene thermally conductive silicone rubber composite material of magnetic aligning is prepared.Since magnetic aligning acts on, heating conduction in the face of graphene superelevation is efficiently utilized, to form efficient heat conduction network in differently- oriented directivity, significantly improves the thermal conductivity of silicon rubber.The simple process of the graphene thermally conductive silicone rubber composite material of magnetic aligning prepared by the present invention, favorable repeatability, it is easy to accomplish industrialized production has a good application prospect in field of heat management.
Description
Technical field
The invention belongs to heat-conductivity polymer composite fields, more particularly to a kind of graphene thermal conductive silicon rubber of magnetic aligning
The preparation method of glue composite material.
Background technique
With the development of the emerging fields such as communication, energy stores, Internet of Things, electronic component constantly tends to miniaturization and collection
Cheng Hua, efficient heat management, which has become, maintains equipment life and the stable key factor of performance.Thermal interfacial material is a kind of normal
With and important thermal management component, effect be the gap for substituting air and being filled between heat source (such as chip) and heat dissipation equipment,
To play the role of thermally conductive medium.
Silicon rubber heat resistance with higher, excellent electrical insulation capability, good transparency, minimum hygroscopicity etc.
Excellent properties are a kind of widely used thermal interfacial material matrixes.However, since the thermal conductivity of silicon rubber is only 0.12 W/
(mK), the cooling requirements being unable to satisfy under electronic component high power density.It is thus typically necessary to add heat filling raising
Its thermal conductivity.Currently used heat filling mainly includes metal, boron nitride, aluminium nitride, aluminium oxide, silicon carbide etc., to realize
Ideal thermal conductivity needs the additive amount (50 vol% or more) of high load, this has seriously affected the mechanical performance of composite material, has added
Work performance, limits its scope of application.In order to realize the relatively high thermal conductivity under low sizing load, while meeting required mechanicalness
Can, processing performance requirement, need to develop the thermally conductive silicone rubber composite material of a kind of low-density, low sizing load.
The unique two-dimensional structure of graphene assigns the thermal conductivity (5300 W/ (mK)) and theoretical Young's modulus of its superelevation
Numerous excellent properties such as (1.0TPa), therefore, graphene, which can be used as high thermal conductivity filler, directly to be added in polymeric matrix with significant
Improve the heating conduction of composite material.Research about graphene thermally conductive silicone rubber composite material at present have been achieved for centainly into
Exhibition, patent CN104910625A discloses a kind of heat-conducting silicon rubber interface material producing method containing graphene, prepared
Not only contain the graphene of low component in composite material, but also is added to the micron grade aluminum oxide of high component (50-80 wt%).Though
Right this method achieves preferable heat-conducting effect, but the specific gravity for causing composite material increases sharply, processing performance decline.There is researcher
The quasi- orientation by material prepares the composite material of the low filling of one kind, high thermal conductivity.For example, patent CN108976606A is disclosed
A kind of anisotropic conductive thermal conductive polymer composite material and preparation method, (outer layer is molten by polymeric matrix for the composite material
Body) and two-dimentional conductive and heat-conductive filler (internal layer melt) it is obtained by the molding of more melt multiple injections, but this method is not suitable for
The preparation of low-viscosity liquid silicon rubber composite material.Entitled " a kind of high thermal conductivity, stretchable silicon rubber/graphene nanometer sheet
The multilayered film material and preparation method thereof of layer-by-layer assembled formation " (Jianan Song et al. High thermal
conductivity and stretchability of layer-by-layer assembled silicone rubber/
graphene nanosheets multilayered films. Composites Part A: Applied Science
And Manufacturing, 2018,105:1-8.) document in disclose: using rotation auxiliary layer-by-layer assemble method system
For silicon rubber/graphene nanometer sheet plural layers of 40 assembling circulations, to realize the level side of 2.03 W/ (mK)
To thermal conductivity, 325% elongation at break.However this method forming process is complicated, lacks scalability.
Since the particle with magnetic responsiveness can be orientated under the action of externally-applied magnetic field along magnetic direction, magnetic is used
Oriented padding method can make full use of thermal conductivity in the face of graphene superelevation and form perfect thermal conducting path, to be expected to reality
High thermal conductivity under existing low sizing load.Based on this, the present invention is assigned using the method for coated magnetic ferriferrous oxide nano-particle
Graphene magnetic responsiveness, and then apply external magnetic field to prepare the graphene thermally conductive silicone rubber composite material of magnetic aligning.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning, with
Overcome the deficiencies in the prior art, efficiently uses thermally conductive in the face of graphene superelevation, to form efficient thermal conducting path, realizes reason
The heating conduction thought.
To achieve the above object, the present invention provides the following technical solutions.
A kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning, the composite material is by magnetic function
The graphene of change and the compound preparation of liquid silastic, the magnetic/functionalized graphene make it in silicone rubber matrix through magnetic field processing
In be orientated along magnetic direction.
In the preferred embodiment of the present invention, the magnetic/functionalized graphene is to be aoxidized by electrostatic adsorption by four
Three Fe nanometer particles are coated on graphene surface and are made.
In the preferred embodiment of the present invention, the graphene is removed by liquid phases such as ultrasound, ball milling, electrochemical strippings
Method is made.
In the preferred embodiment of the present invention, the liquid silastic is Si―H addition reaction type silicon rubber, the liquid silicon
The viscosity of rubber is 100-5000 cs.
In the preferred embodiment of the present invention, the magnetic field strength is 0.5-2 T, and the magnetic treatment time is 0.5-6 h.
The preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning described in any of the above embodiments, including following step
It is rapid:
(1) cationic polyelectrolyte is coated on the surface of graphene, then receives ferroso-ferric oxide prepared by chemical coprecipitation
Rice corpuscles is coated on graphene surface, obtains magnetic/functionalized graphene；
(2) magnetic/functionalized graphene uniform obtained in step (1) is distributed in liquid silastic, after being magnetically oriented processing
Precuring, removes to be warming up to behind magnetic field and is fully cured, so that the graphene thermally conductive silicone rubber composite material of magnetic aligning be made.
In the preferred embodiment of the present invention, cationic polyelectrolyte described in step (1) can be polydiene propyl
At least one of quaternary ammonium salts such as alkyl dimethyl ammonium chloride, dodecyl trimethyl ammonium chloride.
In the preferred embodiment of the present invention, the cladding of ferriferrous oxide nano-particle and graphene described in step (1)
Mass ratio is 0.5:1-5:1.
In the preferred embodiment of the present invention, precuring temperature described in step (2) is 50-80 DEG C, when the precuring
Between be 1-3 h, the solidification temperature be 90-120 DEG C, the curing time be 1-6 h.
Compared with prior art, present invention has an advantage that
(1) orientation by magnetic/functionalized graphene in silicone rubber matrix realizes the high thermal conductivity under low sizing load, and
And magnetic aligning method is applicable to squeeze out the molding modes such as drawing and forming, calendering formation；
(2) compared with the method for alignment such as traditional extrusion molding, injection moulding, the magnetic aligning method under externally-applied magnetic field can be long-range
Controlling filler, any direction is orientated in a polymer matrix；
(3) graphene is magnetic/functionalized simple and easy, and experiment has expansibility, and the graphene for the magnetic aligning being prepared is led
Hot silicon rubber composite material has a good application prospect in field of heat management such as Electronic Packagings.
Detailed description of the invention
Fig. 1 a is the transmission electron microscope picture of the graphene as made from liquid phase ball grinding method in embodiment 1.
Fig. 1 b is the scanning electron microscope (SEM) photograph of the ferriferrous oxide nano-particle prepared in embodiment 1 by chemical coprecipitation.
Fig. 2 a is the transmission electron microscope picture of the magnetic/functionalized graphene prepared in embodiment 1.
Fig. 2 b, Fig. 2 c, Fig. 2 d are the elemental distribution figures of the magnetic/functionalized graphene prepared in embodiment 1.
Fig. 3 a is the profile scanning electricity of the graphene thermally conductive silicone rubber composite material without magnetic field orientating processing in embodiment 1
Mirror figure.
Fig. 3 b is the profile scanning electricity of the graphene thermally conductive silicone rubber composite material in embodiment 1 by magnetic field orientating processing
Mirror figure.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It is necessarily pointed out that following specific embodiments are only to explain the present invention, without
Composition is defined the spirit and scope of the present invention, and field technical staff makes various according to the technique and scheme of the present invention
Non-intrinsically safe modifications and adaptations, still fall within protection scope of the present invention.
Embodiment 1
(1) magnetic/functionalized graphene is prepared
The water that 1 g graphene dispersion prepared by liquid phase ball-milling method contains 1 wt% diallyl dimethyl ammoniumchloride to 200g
Dispersion liquid mixes 6 h, is filtered, washes to obtain the graphene of diallyl dimethyl ammoniumchloride cladding；Then with contain 3 g
The aqueous dispersions of ferriferrous oxide nano-particle mix, and adjusting PH with ammonium hydroxide is 12, with promote ferriferrous oxide nano-particle with
The Electrostatic Absorption of graphene obtains ferriferrous oxide nano-particle then using Magnetic Isolation, water cleaning, 60 DEG C of vacuum drying
The magnetic/functionalized graphene for being 3:1 with graphene coated mass ratio.
The transmission electron microscope picture of the graphene as made from liquid phase ball grinding method is as shown in Figure 1a in the present embodiment, from liquid phase ball
It grinds the obtained transmission electron microscope picture of graphene to find out, the lateral dimension of graphene is 1-2 μm, sub-translucent and show accordion.
Scanning electron microscope (SEM) photograph such as Fig. 1 b of the ferriferrous oxide nano-particle prepared in the present embodiment by chemical coprecipitation
It is shown, find out from the scanning electron microscope (SEM) photograph of ferriferrous oxide nano-particle, ferriferrous oxide nano-particle forms small aggregation.
The transmission electron microscope picture and elemental distribution figure such as Fig. 2 a of the magnetic/functionalized graphene prepared in the present embodiment,
Fig. 2 b, Fig. 2 c, shown in Fig. 2 d, it can be seen from the figure that Fe, O, C element are uniformly distributed, show ferriferrous oxide nano-particle at
Function and it is uniformly coated on graphene surface.
(2) the graphene thermally conductive silicone rubber composite material of magnetic aligning is prepared
By in the silicon rubber (viscosity is 1000 cs) of 4g magnetic/functionalized graphene dispersion to 16g Si―H addition reaction, stir evenly
Afterwards, vacuum defoamation is then transferred into PP mold, be put into intensity be 1 T magnetic field condition under be orientated 2 h, then 80 DEG C it is pre- solid
Change 2 h of processing.Magnetic field is removed, is warming up to 110 DEG C, 2 h are fully cured, and obtain the magnetic aligning that graphene mass fraction is 5 wt%
Graphene thermally conductive silicone rubber composite material.
Thermal conductivity test is carried out using graphene thermally conductive silicone rubber composite material of the heat conduction coefficient tester to magnetic aligning, is measured
The thermal coefficient of the composite material is 0.64 W/ (mK).
In order to compare the heat-conducting effect before and after magnetic aligning, it is compound to be prepared for the graphene heat-conducting silicon rubber handled without magnetic field
Material, through thermal conductivity test, the thermal coefficient for measuring the composite material is 0.22 W/ (mK).
Without magnetic field orientating processing and the graphene heat-conducting silicon rubber composite wood by magnetic field orientating processing in the present embodiment
The profile scanning electron microscope difference of material is as shown in Figure 3a, 3b, it can be seen from the figure that the composite material without magnetic field processing,
Magnetic/functionalized graphene is evenly dispersed in silicone rubber matrix.And treated in magnetic field composite material, magnetic/functionalized graphite
Alkene is orientated along magnetic direction, and forms chain beam.
Embodiment 2
The preparation process of the graphene thermally conductive silicone rubber composite material of magnetic/functionalized graphene, magnetic aligning is same as Example 1,
The magnetic field processing time need to only be reduced to 0.5 h.
Thermal conductivity test is carried out using graphene thermally conductive silicone rubber composite material of the heat conduction coefficient tester to magnetic aligning, is measured
The thermal coefficient of the composite material is 0.53 W/ (mK).
Embodiment 3
Prepare magnetic/functionalized graphene
The process of magnetic/functionalized graphene is prepared with embodiment 1, only cationic polyelectrolyte need to be changed to trimethyl
The mass ratio of ammonium chloride, ferriferrous oxide nano-particle and graphene is changed to 0.5:1.
(2) the graphene thermally conductive silicone rubber composite material of magnetic aligning is prepared
By in the silicon rubber (viscosity is 2500 cs) of 1.5g magnetic/functionalized graphene dispersion to 12.8g Si―H addition reaction, stirring is equal
After even, vacuum defoamation is then transferred into PP mold, is put under the magnetic field condition that intensity is 1T and is orientated 3 h, then 60 DEG C it is pre-
1 h of curing process.Magnetic field is removed, is warming up to 90 DEG C, 1 h is fully cured, and obtains the magnetic that graphene mass fraction is 7 wt% and takes
To graphene thermally conductive silicone rubber composite material.
Thermal conductivity test is carried out using graphene thermally conductive silicone rubber composite material of the heat conduction coefficient tester to magnetic aligning, is measured
The thermal coefficient of the composite material is 0.59 W/ (mK).
In order to compare the heat-conducting effect before and after magnetic aligning, it is compound to be prepared for the graphene heat-conducting silicon rubber handled without magnetic field
Material, through thermal conductivity test, the thermal coefficient for measuring the composite material is 0.38 W/ (mK).
Embodiment 4
The preparation process of the graphene thermally conductive silicone rubber composite material of magnetic/functionalized graphene, magnetic aligning is same as Example 3,
Magnetic field strength need to be only reduced to 0.5 T.
Thermal conductivity test is carried out using graphene thermally conductive silicone rubber composite material of the heat conduction coefficient tester to magnetic aligning, is measured
The thermal coefficient of the composite material is 0.49 W/ (mK).
Embodiment 5
Prepare magnetic/functionalized graphene
The process of magnetic/functionalized graphene is prepared with embodiment 1, it only need to be by the quality of ferriferrous oxide nano-particle and graphene
Than being changed to 1:1.
(2) the graphene thermally conductive silicone rubber composite material of magnetic aligning is prepared
By in 2g magnetic/functionalized graphene dispersion to 31.3g Si―H addition reaction type silicon rubber (viscosity is 5000 cs), stir evenly
Afterwards, vacuum defoamation is then transferred into PP mold, be put into intensity be 1 T magnetic field condition under be orientated 2 h, then 70 DEG C it is pre- solid
Change 1 h of processing.Magnetic field is removed, is warming up to 100 DEG C, 3 h are fully cured, and obtain the magnetic aligning that graphene mass fraction is 3 wt%
Graphene thermally conductive silicone rubber composite material.
Thermal conductivity test is carried out using graphene thermally conductive silicone rubber composite material of the heat conduction coefficient tester to magnetic aligning, is measured
The thermal coefficient of the composite material is 0.36 W/ (mK).
In order to compare the heat-conducting effect before and after magnetic aligning, it is compound to be prepared for the graphene heat-conducting silicon rubber handled without magnetic field
Material, through thermal conductivity test, the thermal coefficient for measuring the composite material is 0.17 W/ (mK).
Embodiment 6
The preparation process of the graphene thermally conductive silicone rubber composite material of magnetic/functionalized graphene and magnetic aligning and 5 phase of embodiment
Together, only amount graphene-supported in composite material need to be changed to 5 wt%.
(2) the graphene thermally conductive silicone rubber composite material of magnetic aligning is prepared
By in 2g magnetic/functionalized graphene dispersion to 18g Si―H addition reaction type silicon rubber (viscosity is 5000 cs), stir evenly
Afterwards, vacuum defoamation is then transferred into PP mold, be put into intensity be 1 T magnetic field condition under be orientated 2 h, then 70 DEG C it is pre- solid
Change 1 h of processing.Magnetic field is removed, is warming up to 100 DEG C, 3 h are fully cured, and obtain the magnetic aligning that graphene mass fraction is 5 wt%
Graphene thermally conductive silicone rubber composite material.
Thermal conductivity test is carried out using graphene thermally conductive silicone rubber composite material of the heat conduction coefficient tester to magnetic aligning, is measured
The thermal coefficient of the composite material is 0.53 W/ (mK).
In order to compare the heat-conducting effect before and after magnetic aligning, it is compound to be prepared for the graphene heat-conducting silicon rubber handled without magnetic field
Material, through thermal conductivity test, the thermal coefficient for measuring the composite material is 0.26 W/ (mK).
Embodiment 7
Prepare magnetic/functionalized graphene
The process of magnetic/functionalized graphene is prepared with embodiment 1, only cationic polyelectrolyte need to be changed to trimethyl
The mass ratio of ammonium chloride, ferriferrous oxide nano-particle and graphene is changed to 5:1.
(2) the graphene thermally conductive silicone rubber composite material of magnetic aligning is prepared
By in 6g magnetic/functionalized graphene dispersion to 27.3g Si―H addition reaction type liquid silica gel (viscosity is 100 cs), stirring is equal
After even, vacuum defoamation is then transferred into PP mold, is put under the magnetic field condition that intensity is 2 T and is orientated 6 h, then 80 DEG C it is pre-
3 h of curing process.Magnetic field is removed, is warming up to 120 DEG C, 6 h are fully cured, and obtain the magnetic that graphene mass fraction is 3 wt% and take
To graphene thermally conductive silicone rubber composite material.
Thermal conductivity test is carried out using graphene thermally conductive silicone rubber composite material of the heat conduction coefficient tester to magnetic aligning, is measured
The thermal coefficient of the composite material is 0.42 W/ (mK).
In order to compare the heat-conducting effect before and after magnetic aligning, it is compound to be prepared for the graphene heat-conducting silicon rubber handled without magnetic field
Material, through thermal conductivity test, the thermal coefficient for measuring the composite material is 0.24 W/ (mK).
Embodiment 8
The preparation process of the graphene thermally conductive silicone rubber composite material of magnetic aligning is same as Example 7, and precuring temperature is changed to
50℃。
Thermal conductivity test is carried out using graphene thermally conductive silicone rubber composite material of the heat conduction coefficient tester to magnetic aligning, is measured
The thermal coefficient of the composite material is 0.28 W/ (mK).
Claims (10)
1. a kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning, which is characterized in that the composite wood
Material by magnetic/functionalized graphene and the compound preparation of liquid silastic, the magnetic/functionalized graphene through magnetic field processing make its
It is orientated in silicone rubber matrix along magnetic direction.
2. a kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning according to claim 1, special
Sign is that the magnetic/functionalized graphene is that ferriferrous oxide nano-particle is coated on graphene by electrostatic adsorption
Surface is made.
3. according to claim 1 to a kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning described in 2,
It is characterized in that, the graphene is made by ultrasound, ball milling or electrochemical stripping.
4. a kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning according to claim 1, special
Sign is that the liquid silastic is Si―H addition reaction type silicon rubber, viscosity 100-5000cs.
5. a kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning according to claim 1, special
Sign is that the intensity in the magnetic field is 0.5-2 T, and the magnetic treatment time is 0.5-6 h.
6. a kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning according to claim 1, special
Sign is, this method specifically includes the following steps:
(1) cationic polyelectrolyte is coated on the surface of graphene, then receives ferroso-ferric oxide prepared by chemical coprecipitation
Rice corpuscles is coated on graphene surface, obtains magnetic/functionalized graphene；
(2) magnetic/functionalized graphene uniform obtained in step (1) is distributed in liquid silastic, after being magnetically oriented processing
Precuring, removes to be warming up to behind magnetic field and is fully cured, so that the graphene thermally conductive silicone rubber composite material of magnetic aligning be made.
7. a kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning according to claim 6, special
Sign is that cationic polyelectrolyte described in step (1) is quaternary ammonium salt.
8. a kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning according to claim 7, special
Sign is that cationic polyelectrolyte described in step (1) is diallyl dimethyl ammoniumchloride, trimethyl chlorine
Change at least one of ammonium.
9. a kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning according to claim 6, special
Sign is that the cladding mass ratio of ferriferrous oxide nano-particle described in step (1) and graphene is 0.5:1-5:1.
10. a kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning according to claim 6, special
Sign is that the temperature of precuring described in step (2) is 50-80 DEG C, and the time of precuring is 1-3 h, the cured temperature
It is 90-120 DEG C, the cured time is 1-6 h.
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| CN113075803A (en) * | 2021-03-10 | 2021-07-06 | 西安交通大学 | Graphene nanosheet-based magnetic response intelligent optical material and preparation method thereof |
| CN113416420A (en) * | 2021-06-25 | 2021-09-21 | 厦门大学 | Preparation method of high-orientation-arrangement graphene sheet thermal interface material |
| CN113956663A (en) * | 2021-10-26 | 2022-01-21 | 中节能太阳能科技（镇江）有限公司 | Directional high-thermal-conductivity silica gel for improving heat dissipation of photovoltaic module junction box and preparation method thereof |
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| CN115157714A (en) * | 2022-08-24 | 2022-10-11 | 浙江工业大学 | Foam metal/oriented graphene laminated composite high-thermal-conductivity flexible interface material and preparation method thereof |
| CN117467333A (en) * | 2023-11-28 | 2024-01-30 | 济南市雋瀚电子材料有限公司 | High-heat-conductivity breakdown-voltage-resistant circuit board material, circuit board and preparation method thereof |
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| CN114989613A (en) * | 2022-06-30 | 2022-09-02 | 哈尔滨理工大学 | Preparation method of heat-conducting silicon rubber filled with highly-oriented silicon carbide whiskers |
| CN115157714A (en) * | 2022-08-24 | 2022-10-11 | 浙江工业大学 | Foam metal/oriented graphene laminated composite high-thermal-conductivity flexible interface material and preparation method thereof |
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