CN116176075A - Preparation method of polymer-based heat-conducting composite material with sandwich structure - Google Patents
Preparation method of polymer-based heat-conducting composite material with sandwich structure Download PDFInfo
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- CN116176075A CN116176075A CN202310068403.9A CN202310068403A CN116176075A CN 116176075 A CN116176075 A CN 116176075A CN 202310068403 A CN202310068403 A CN 202310068403A CN 116176075 A CN116176075 A CN 116176075A
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Abstract
The invention discloses a preparation method of a polymer-based heat-conducting composite material with a sandwich structure, and belongs to the technical field of heat-conducting composite material preparation. The heat-conducting composite material is formed by alternately and thermally pressing heat-conducting filler layers and polymer layers. And depositing the sheet-shaped heat-conducting filler with the functionalized surface on the polymer fiber felt prepared by electrostatic spinning in a vacuum filtration mode, and preparing the composite material with the sandwich structure through multi-layer lamination and hot pressing. The surface functionalized flaky heat conducting filler improves the compatibility with the polymer matrix and reduces the interface thermal resistance between the heat conducting fillers and the matrix. By constructing the continuous heat-conducting filler layer in the polymer matrix, the heat-conducting property of the polymer-based heat-conducting composite material is effectively improved. The polymer-based heat-conducting composite material with the sandwich structure also has good flexibility and mechanical strength, and has wide application prospects in the heat dissipation fields of electronic components, communication equipment and the like.
Description
Technical Field
The invention relates to a preparation method of a polymer-based heat-conducting composite material with a sandwich structure, and belongs to the technical field of heat-conducting composite material preparation.
Background
In recent years, with the rapid development of electronic integration technology, electronic products are continually tending to be miniaturized and highly integrated. The heat generated by the high power operation of these products severely affects the reliability and life of the electronic components. At the same time, high requirements are placed on the characteristics of advanced thermal management materials, including excellent electrical insulation, good flexibility, light weight, and strong mechanical and thermal properties. Compared with metal and ceramic materials, the polymer composite material has light weight, easy molding and excellent flexibility, and is convenient to prepare into various shapes. Therefore, the development of polymer composite materials with high heat conducting property has great application value.
Compared to metals, inorganic materials, polymeric materials are poor conductors of heat, and pure polymeric materials have very low intrinsic thermal conductivities, mostly less than 0.5W/(m·k). Researchers have often incorporated various thermally conductive fillers (e.g., carbon materials, ceramic particles, and metal materials) with high thermal conductivity into polymer matrices to improve the thermal conductivity of polymer matrix composites. The key to preparing polymer-based composites with high thermal conductivity is to rationally design the filler structure, i.e., to form a continuous heat transfer path for more filler in the polymer matrix. With the gradual increase of the heat conducting filler, the heat conductivity of the composite material can be effectively improved, but the enhancement effect is reduced after the content exceeds a certain threshold value, because the interface thermal resistance becomes a main factor for limiting the improvement of the heat conductivity of the composite material.
Therefore, it is a key to improve the heat conducting performance of the composite material to study how to reasonably distribute the heat conducting filler in the polymer matrix and reduce the heat resistance between the filler and the polymer matrix.
Disclosure of Invention
The invention solves the main technical problems that: aiming at the problems of agglomeration among fillers and larger interfacial thermal resistance among filler-polymer matrixes in the polymer-based heat-conducting composite material prepared at present, the invention provides a preparation method of a polymer-based heat-conducting composite material with a sandwich structure. The polymer matrix composite is composed of a thermally conductive filler layer and a polymer layer. By virtue of the surface functionalization of the heat conducting filler and the construction of a continuous heat conducting filler layer in the polymer matrix, the heat conducting performance of the composite material is effectively improved.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
in the invention, the polymer layer is a polymer fiber felt prepared by solution electrostatic spinning.
The polymer in the polymer fiber felt is selected from polyvinyl alcohol, polyacrylonitrile and polyvinylidene fluoride. One or more of polyimide and polystyrene.
In the invention, the heat-conducting filler layer is prepared by depositing the dispersion liquid of the heat-conducting filler on the surface of the polymer fiber mat through vacuum filtration.
The heat conducting filler is a sheet-shaped structure heat conducting filler with a functionalized surface.
The sheet-structure heat-conducting filler is one or more selected from boron nitride nano-sheets, graphite sheets, graphene oxide nano-sheets and nitrides (MXene).
The surface functionalization refers to that dopamine is self-polymerized into polydopamine, and a polydopamine layer is coated on the surface of the sheet-shaped structural filler.
In the invention, the addition mass of the heat conducting filler in the polymer-based heat conducting composite material with the sandwich structure is 10-40wt%.
The invention also relates to a preparation method of the polymer-based heat-conducting composite material with the sandwich structure, which comprises the following steps of;
step one: and dissolving the polymer in the solvent A to form a spinning solution, and preparing the polymer fiber felt from the spinning solution through electrostatic spinning.
Step two: dispersing the heat conducting filler with the surface functionalized sheet structure in the solvent B, and depositing the heat conducting filler on the surface of the polymer fiber felt prepared in the step one through vacuum filtration to obtain the composite fiber felt.
And thirdly, stacking and drying the composite fiber felt layer by layer, hot-pressing and forming the composite fiber felt at a temperature higher than the melting point or softening point of the polymer, and annealing to obtain the polymer-based heat-conducting composite material with the sandwich structure.
In the first step, the solvent A comprises one or more of deionized water, acetone, tetrahydrofuran, N-dimethylformamide, N-dimethylacetamide and ethyl acetate.
In the first step, the spinning voltage is 15-30kV, the spinning distance is 15-20cm, the temperature is 20-25 ℃, and the environmental humidity is 20% -50%.
In the first step, the concentration of the polymer spinning solution is 8-15wt% and the spinning capacity is 0.6-1.0ml.
In the second step, the solvent B is required to follow the principle of being a poor polymer solvent in the first step, and includes one or more of isopropanol, acetone, ethanol and chloroform.
In the second step, the surface functionalization adopts polydopamine coating: adding dopamine into a sheet-shaped heat-conducting filler dispersion solution with the pH of 8.5, and polymerizing the dopamine to form polydopamine and coating the polydopamine on the surface of the sheet-shaped heat-conducting filler; the mass ratio of the dopamine to the platy heat-conducting filler is 1:1-2:1.
According to the invention, the surface functionalized sheet-shaped heat-conducting filler is deposited on the polymer fiber felt prepared by electrostatic spinning in a vacuum filtration mode, and the composite material with a sandwich structure is prepared by multi-layer stacking and hot pressing. The surface functionalized flaky heat conducting filler improves the compatibility between the heat conducting filler and the polymer matrix, and reduces the interface thermal resistance between the heat conducting filler and the polymer matrix, thereby improving the heat conductivity of the polymer matrix composite. Thanks to the direct construction of the heat conduction path of the heat conducting filler in the polymer matrix, the in-plane thermal conductivity is as high as 16.6W/(m·k) when the content of the sheet-like heat conducting filler after surface functionalization of the polymer matrix composite is 35wt% in the first embodiment. At the same time, the polymer matrix composites also exhibit a content of more than 10 14 Bulk resistivity of Ω·cm, and good tensile strength of 23 MPa.
Drawings
FIG. 1 is an SEM image of a fibrous mat made according to an embodiment of the invention;
FIG. 2 is a cross-sectional SEM image of a polymer-based thermally conductive composite material prepared according to an embodiment of the present invention;
FIG. 3 is a graph of thermal conductivity of a polymer-based thermally conductive composite material prepared in accordance with an embodiment of the present invention;
FIG. 4 shows the variation data of the highest temperature of the surface of the LED lamp when the polymer-based heat-conducting composite material and the pure polyvinyl alcohol material prepared by the embodiment of the invention are used as the heat dissipation material of the thermal interface of the LED lamp set to conduct the actual heat dissipation effect comparison experiment;
FIG. 5 is a graph showing the bulk resistivity of a polymer-based thermally conductive composite material and a pure polyvinyl alcohol material prepared in accordance with an embodiment of the present invention;
FIG. 6 is a stress-strain curve of a polymer-based thermally conductive composite material prepared in accordance with an embodiment of the present invention.
Detailed Description
In order to more fully explain the preparation method of the polymer-based heat-conducting composite material with the sandwich structure, the following specific examples of the preparation method are provided, but the invention is not limited to these examples. The embodiment adopts the platy heat-conducting filler boron nitride nano-sheet and polymer polyvinyl alcohol as examples.
Examples:
(1) Preparing a boron nitride nano sheet (BNNS@PDA) with a polydopamine layer coated on the surface: firstly, adding 0.4g of boron nitride nano-sheets (BNNS) with the particle size of 2 mu M into a beaker filled with 300ml of deionized water, fully dispersing the boron nitride nano-sheets by ultrasonic treatment for 30min, then adding 0.3g of Tris (hydroxymethyl) aminomethane (Tris) and dropwise adding 9ml of HCl solution (0.1M) to adjust the pH value of the solution to 8.5; next, after stirring the dispersion in which BNNS is dispersed and adding 0.6g of Dopamine (DA) at 60 ℃, the reaction was maintained for 12 hours, DA was polymerized to form Polydopamine (PDA) and coated on the surface of BNNS, bnns@pda was collected by filtration and dried at 60 ℃ for 12 hours.
(2) Preparing a polyvinyl alcohol (PVA) electrostatic spinning fiber felt: adding PVA particles with the molecular weight of 20 ten thousand into deionized water according to the mass fraction of 8wt%, and continuously stirring for 2 hours at 90 ℃ until a uniform electrostatic spinning precursor solution is obtained; PVA solution was loaded into the syringe and spun at a push rate of 0.8 ml/h. The rotary receiver is connected with a direct current power supply of +15KV, the filament outlet is connected with a direct current power supply of-5 KV, the spinning environment condition is 25 ℃, the relative environment humidity is 30%, the diameter of the rotary receiver is 20cm, and the spinning amount of each layer of PVA fiber felt is 0.8ml.
(3) Preparing a polymer-based heat-conducting composite material with a sandwich structure: dispersing BNNS@PDA prepared in the step (1) in isopropanol serving as a solvent by ultrasonic for 30 minutes to form BNNS@PDA dispersion liquid with uniform dispersion concentration of 0.5 mg/ml; taking the PVA fiber felt prepared in the step (2) as a filtering membrane of a suction filtration device with the caliber of 5cm, and depositing 4ml BNNS@PDA dispersion liquid on the PVA fiber felt through vacuum suction filtration; the PVA fiber felt deposited with BNNS@PDA is laminated by 11 layers, then dried for 12 hours at 60 ℃, and finally hot-pressed for 20 minutes at 120 ℃ and 15MPa to prepare the polymer-based heat-conducting composite material with a sandwich structure.
And (3) carrying out Scanning Electron Microscope (SEM) characterization on the PVA fiber mat prepared by electrostatic spinning in the step (2). As shown in FIG. 1, the PVA fiber prepared in the examples has a uniform morphology and a smooth surface, and is free from the condition of beads or crosslinking. And fiber diameter distributionIs very narrow, about 400nm. And (3) preparing the polymer-based heat-conducting composite material with the sandwich structure in the step (3), and observing the cross-section structure of the composite material by adopting SEM. Results as shown in fig. 2, PVA fiber mat deposited with bnns@pda showed a distinct sandwich structure after multi-layer stacked hot pressing, and the bnns@pda layer was highly oriented in the horizontal direction. FIG. 3 shows the polymer-based heat conductive composite material with sandwich structure prepared in the step (3), wherein the plane heat conductivity coefficient is as high as 16.6W/(m.K) at 25 ℃. Fig. 4 is data of variation of the surface maximum temperature of the LED lamp when the polymer-based heat conductive composite material with the sandwich structure and the pure PVA material prepared in the step (3) are used as the thermal interface heat dissipation material of the LED lamp set to perform an actual heat dissipation effect comparison experiment. After the LED lamp set runs for 4 minutes, the polymer-based heat conduction composite material with the sandwich structure prepared in the step (3) is 38.7 ℃ lower than the pure PVA material in an actual heat dissipation performance test. FIG. 5 shows the insulating properties of the polymer-based thermally conductive composite material with sandwich structure prepared in step (3), showing a value higher than 10 14 The volume resistivity of omega cm is far higher than the standard (10 9 Omega cm). Fig. 6 is a stress-strain curve of the polymer-based heat conductive composite material with a sandwich structure prepared in step (3), with a good tensile strength of 23 MPa.
Claims (7)
1. A preparation method of a polymer-based heat-conducting composite material with a sandwich structure is characterized by comprising the following steps: the polymer matrix composite is formed by alternately and thermally pressing a heat-conducting filler layer and a polymer layer; the method comprises the following steps:
the polymer layer is a polymer fiber felt prepared by solution electrostatic spinning;
the polymer in the polymer fiber felt is one or more of polyvinyl alcohol, polyacrylonitrile, polyvinylidene fluoride, polyimide and polystyrene;
the heat-conducting filler layer is prepared by depositing a heat-conducting filler dispersion liquid on the surface of the polymer fiber felt through vacuum suction filtration;
the heat-conducting filler is a heat-conducting filler with a surface-functionalized sheet structure;
the sheet-structure heat-conducting filler is one or more of boron nitride nano-sheets, graphite sheets, graphene oxide nano-sheets and nitrides (MXene);
the surface functionalization is that dopamine is self-polymerized into polydopamine, and a polydopamine layer is coated on the surface of the sheet-shaped structural filler;
the addition mass of the heat conducting filler in the polymer-based heat conducting composite material with the sandwich structure is 10-40wt%.
2. The method for preparing the polymer-based heat-conducting composite material with the sandwich structure according to claim 1, which comprises the following steps of;
step one: dissolving a polymer in a solvent A to form a spinning solution, and preparing the spinning solution into a polymer fiber felt through electrostatic spinning;
step two: dispersing the heat conducting filler with the surface functionalized sheet structure in a solvent B, and depositing the heat conducting filler on the surface of the polymer fiber felt prepared in the step one through vacuum filtration to obtain a composite fiber felt;
and thirdly, stacking and drying the composite fiber felt layer by layer, hot-pressing and forming the composite fiber felt at a temperature higher than the melting point or softening point of the polymer, and annealing to obtain the polymer-based heat-conducting composite material with the sandwich structure.
3. The method for preparing a polymer-based heat-conducting composite material with a sandwich structure according to claim 1, wherein in the first step, the solvent a comprises one or more of deionized water, acetone, tetrahydrofuran, N-dimethylformamide, N-dimethylacetamide and ethyl acetate.
4. The method for preparing a polymer-based heat-conducting composite material with a sandwich structure according to claim 1, wherein in the first step, the spinning voltage is 15-30kV, the spinning distance is 15-20cm, the temperature is 20-25 ℃, and the ambient humidity is 20% -50%.
5. The method for preparing a polymer-based heat-conducting composite material with a sandwich structure according to claim 1, wherein in the first step, the concentration of the polymer spinning solution is 8-15wt% and the spinning capacity is 0.6-1.0ml.
6. The method for preparing a polymer-based heat-conducting composite material with a sandwich structure according to claim 1, wherein in the second step, the solvent B is required to follow the poor solvent principle of the polymer in the first step, and comprises one or more of isopropanol, acetone, ethanol and chloroform.
7. The method for preparing a polymer-based heat-conducting composite material with a sandwich structure according to claim 1, wherein in the second step, the surface functionalization is coated with polydopamine: adding dopamine into a sheet-shaped heat-conducting filler dispersion solution with the pH of 8.5, and polymerizing the dopamine to form polydopamine and coating the polydopamine on the surface of the sheet-shaped heat-conducting filler; the mass ratio of the dopamine to the platy heat-conducting filler is 1:1-2:1.
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