CN113416332A - Preparation method of high-thermal-conductivity three-phase composite film under assistance of electric field - Google Patents
Preparation method of high-thermal-conductivity three-phase composite film under assistance of electric field Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 50
- 239000000945 filler Substances 0.000 claims abstract description 37
- 239000011159 matrix material Substances 0.000 claims abstract description 29
- 229920000642 polymer Polymers 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000011231 conductive filler Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 16
- 229910052582 BN Inorganic materials 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 5
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- 238000007872 degassing Methods 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229920001296 polysiloxane Polymers 0.000 claims 1
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 description 27
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 27
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 27
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 24
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 24
- 229910052593 corundum Inorganic materials 0.000 description 5
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K7/00—Use of ingredients characterised by shape
Abstract
The invention belongs to the field of polymer heat-conducting composite materials, and particularly relates to a preparation method of a three-phase heat-conducting composite film of electric field auxiliary oriented filler particles, which specifically comprises the following steps: (1) simultaneously adding at least two kinds of heat-conducting filler particles with larger size difference into a polymer matrix, uniformly mixing to obtain a mixed solution, and adding a curing agent into the mixed solution; (2) pouring the mixed solution into a sealed conductive mold, providing a certain electric field for the mixed solution, enabling corresponding particles to be aligned in a matrix under the regulation and control of an external field, and curing or crosslinking the polymer matrix in a proper mode to obtain a three-phase composite membrane; the thermally conductive filler particles include at least one micron-sized and one nano-sized particle. The heat conductivity of the composite film is obviously increased due to the synergistic effect of the heat-conducting filler particles with different sizes; after the two filler particles are oriented and arranged under an external electric field, heat conduction paths formed in the system are increased, and the heat conductivity is further improved.
Description
Technical Field
The invention belongs to the field of polymer heat-conducting composite materials, and particularly relates to a preparation method of a three-phase heat-conducting composite material with electric field auxiliary oriented filler particles.
Technical Field
With the rapid development of science and technology, the increase of power density of electronic, photoelectric and microwave equipment makes effective heat dissipation a key problem; for various electronic devices, it is important to develop thermally conductive composites with higher thermal conductivity. Because the traditional heat-conducting composite material is difficult to machine and form, poor in solvent resistance, high in price, poor in performance and the like, the application field is severely limited, and the increasingly developed material requirements are difficult to meet, so that high polymer materials are researched and developed to replace the traditional heat-conducting materials. However, the polymer material itself is a poor thermal conductor and has a low thermal conductivity, which severely limits the use of the polymer material in electronic devices that generate a large amount of heat energy. Therefore, how to improve the thermal conductivity of the polymer is considered as a key application problem, and the method has wide prospects. At present, the addition of highly thermally conductive fillers to polymers has proven to be a simple and feasible way to increase the thermal conductivity of polymers. Researchers mostly adopt external fields such as a shear field, a magnetic field and the like (non-electric field) to orient two heat-conducting fillers in a matrix, or adopt an external electric field to orient a single heat-conducting filler in the matrix, so as to improve the heat-conducting property of the high polymer material. And little research has been done on the use of an applied electric field to orient two types of thermally conductive filler particles to improve thermal conductivity.
Disclosure of Invention
The invention aims to provide a preparation method of a high-thermal-conductivity three-phase composite film under the assistance of an electric field, aiming at the defects in the prior art.
The invention can be realized by the following technical scheme:
a preparation method of a high-thermal-conductivity three-phase composite film under the assistance of an electric field specifically comprises the following steps:
(1) adding at least two kinds of heat-conducting filler particles with larger size difference into a polymer matrix with fluidity, uniformly mixing to obtain a mixed solution, then adding a certain amount of curing agent into the mixed solution, uniformly mixing and removing bubbles;
(2) pouring the mixed solution into a sealed conductive mold, providing a certain electric field for the mixed solution, enabling corresponding particles to be aligned in a matrix under the regulation and control of an external field, and curing or crosslinking the polymer matrix in a proper mode to obtain a three-phase composite membrane;
the at least two types of thermally conductive filler particles having a large size difference include at least one type of micron-sized and one type of nano-sized thermally conductive filler particles.
Further, the polymer matrix is silica gel or epoxy resin, preferably PDMS or SR silicone rubber.
Further, the electric field is a sinusoidal electric field of 2000Vp-p/mm and 5Hz, the electric field is provided by electric field equipment, the electric field equipment is composed of an arbitrary waveform generator, a high-voltage amplifier and an oscilloscope, and the waveform, the voltage and the frequency of the electric field can be adjusted arbitrarily.
Further, the mass sum of the at least two heat-conducting filler particles with larger size difference accounts for 10-40% of the mass of the polymer matrix, and the mass of the heat-conducting filler particles with larger size is 1-5 times of that of the heat-conducting filler particles with smaller size, and the most preferable is that: the mass sum of the at least two heat-conducting filler particles with larger size difference accounts for 20% of the mass of the polymer matrix, wherein the mass of the heat-conducting filler particles with larger size is 3 times that of the heat-conducting filler particles with small size.
Further, the heat-conducting filler particles comprise 5 mu m flaky hexagonal boron nitride serving as a large-size high heat-conducting filler and alumina with the particle size of 800nm serving as a small-size heat-conducting filler.
Further, the curing agent is contained in an amount of (5-15) wt%, preferably 10 wt% of the polymer matrix, and the curing agent may be a curing agent conventionally used in the art.
Further, in the step (1), in the step of uniformly mixing and degassing, the mixed solution is stirred by using a non-intrusive homogenizer, and then vacuum degassing and stirring treatment are performed.
Further, in the step (2), curing is performed by heating or crosslinking is performed by light irradiation.
Further, the specific operation in the step (2) is as follows:
and (3) placing the die on a hot table, starting electric field equipment to assist in orienting the filler particles for 2min, then starting heating, setting the temperature of the hot table at 90 ℃, heating at 90 ℃ for 30min, then closing the electric field equipment, stopping heating, cooling, and taking out to obtain the three-phase composite film.
Compared with the prior art, the application has the following advantages and beneficial effects:
the synergistic effect between the two heat-conducting filler particles with different sizes can obviously increase the heat conductivity of the composite material; meanwhile, the two filler particles are oriented under an external electric field, so that after the particles are oriented, heat conduction paths formed in a system are increased, and the heat conductivity is further improved.
The small-sized nano alumina particles are inserted between the large-sized hexagonal boron nitride sheets and are oriented under the action of an electric field to form a high-heat-conduction percolation network, so that the heat-conduction performance of the material is greatly improved.
The flexible heat-conducting composite material can be prepared according to different selected matrixes.
The three-phase composite material prepared by the method has high thermal conductivity and has wide application prospect in the application fields of electronic packaging, LED illumination and the like.
Drawings
Fig. 1 is an external view of an oriented and non-oriented three-phase heat conductive composite film prepared in example 1 (the left drawing is an oriented three-phase heat conductive composite film).
FIG. 2 shows BN/Al in example 12O3The two filler particles are oriented in PDMS matrix under a sinusoidal electric field of 2000Vp-p/mm and 5Hz for 2min, and then the oriented structure of the particles is shown by an in-situ observation in an optical microscope.
Fig. 3 is a heat conduction mechanism diagram of the oriented three-phase heat conduction composite film of the present invention. When the two fillers are randomly dispersed in the PDMS matrix, the formed heat conduction path is less; when an applied electric field is used to orient both filler particles, the thermal conductivity path formed is increased, which can further improve the thermal conductivity of the polymer.
Fig. 4 is a graph comparing thermal conductivities of samples prepared in example 1 and comparative example, from left to right: PDMS matrix-Al2O3a/PDMS two-phase heat-conducting composite membrane-BN/PDMS two-phase heat-conducting composite membrane-non-oriented three-phase heat-conducting composite membrane.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific embodiments. The following examples are only preferred embodiments of the present invention and are not intended to limit the present invention, and the present invention may be variously modified and changed. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
In the following examples, ITO conductive glass was purchased from zhahiki, a photoelectric technology ltd, model number: ITO-P001, the electric field device is composed of an arbitrary waveform generator (HDG2012B Hantek), a high voltage amplifier (AMJ-2B10 Matsusada), and an oscilloscope (DSO5072P Hantek), the waveform, voltage, frequency and the like of the electric field can be adjusted at will, and the electric field device in the embodiment 1 adopts the arbitrary waveform generator HDG2012B of Hantek company.
Embodiment 1 a method for preparing a three-phase composite film with high thermal conductivity under the assistance of an electric field, comprising the following steps:
in this embodiment, 5 μm hexagonal plate-shaped hexagonal boron nitride is used as a large-sized high thermal conductive filler, alumina with a particle size of 800nm is used as a small-sized low-cost thermal conductive filler, dow corning SYLGARD184 polydimethylsiloxane is used as a matrix, dow corning SYLGARD184 is a two-component kit product composed of liquid components, and comprises a basic component (PDMS matrix) and a curing agent, wherein the weight ratio of the basic component (PDMS) to the curing agent is 10:1, and the selected external field is an electric field.
Preparation of BN/Al from PDMS matrix2O3The preparation method comprises the following steps of mixing a PDMS matrix, hexagonal Boron Nitride (BN), alumina and a curing agent, wherein the mass of the hexagonal Boron Nitride (BN) accounts for 15% of that of the PDMS matrix, the mass of the alumina accounts for 5% of that of the PDMS matrix, adding the curing agent, stirring the reaction solution for 3min by using a non-intrusive homogenizer for achieving the purposes of uniform mixing and bubble removal, and then carrying out vacuum defoaming and stirring for 2 min.
Mixing BN/Al2O3the/PDMS mixed liquid is led into a sealed conductive mould (the mould is obtained by using common glass to stick on one piece of ITO to obtain a glass groove with the depth of about 1mm and covering the other piece of ITO glass), and meanwhile, the ITO conductive glass is also used as an upper electrode and a lower electrode to be connected with electric field equipment so as to ensure that a sinusoidal electric field with the frequency of 2000Vp-p/mm and the frequency of 5Hz can be provided for the mixed liquid.
And (3) placing the die on a hot table, starting electric field equipment to assist in orienting the filler particles for 2min, then starting heating, setting the temperature of the hot table at 90 ℃, heating for 30min, then closing the electric field equipment, and stopping heating. And (3) placing the die in water for cooling, opening the die and taking out the die to obtain the high-thermal-conductivity three-phase composite film.
The non-oriented three-phase heat-conducting composite membrane is prepared by directly heating a sample to 90 ℃ after adding the sample into a mould without an electric field orientation process, then heating and curing at 90 ℃ for 30min, cooling and opening the mould.
Comparative example 1:
preparing a hexagonal boron nitride/PDMS mixed solution with the mass fraction of 20% of hexagonal boron nitride by using polydimethylsiloxane, preparing an alumina/PDMS mixed solution with the mass fraction of 20% of alumina by using the polydimethylsiloxane, respectively adding respective samples into a mould, directly heating to 90 ℃, heating and curing at 90 ℃ for 30min, and opening the mould to respectively obtain the comparative two-phase heat-conducting composite membrane BN/PDMS and Al2O3/PDMS。
Fig. 1 is a sample diagram of a high thermal conductivity three-phase composite film prepared in example 1, wherein the left diagram is an oriented composite film, and the right diagram is a non-oriented composite film.
The alignment structure of the three-phase alignment composite film prepared in example 1 is shown in fig. 2, and the alignment structure is observed in situ by an optical microscope, and it can be seen that: under the electric field condition of 2000Vp-p/mm and 5Hz, the boron nitride and alumina particles are oriented and arranged in the PDMS matrix along the electric field direction to form a chain structure.
FIG. 3 is a diagram illustrating the mechanism of improved thermal conductivity after orientation; firstly, the synergistic effect among the fillers with different sizes is mainly embodied in the embedding of small-sized nano alumina particles among large-sized hexagonal boron nitride sheets, so that more heat conduction paths are formed; secondly, a high-thermal-conductivity percolation network is formed after the particles are oriented and arranged; the existence of more heat conduction paths and high-heat-conduction percolation networks can greatly improve the heat conductivity coefficient of the material.
The thermal conductivity of each of the sample films of example 1 and comparative example is shown in FIG. 4 (from left to right: PDMS matrix-Al, respectively)2O3a/PDMS two-phase heat-conducting composite membrane-BN/PDMS two-phase heat-conducting composite membrane-non-oriented three-phase heat-conducting composite membrane), and the analysis can be known; the thermal conductivity of the PDMS matrix without filler filling is 0.141W/mK, and the mass fraction is 20 percent of BN/PDMS and Al2O3The thermal conductivity of the/PDMS two-phase heat-conducting composite membrane is 0.196W/mK and 0.172W/mK respectively; and is filled with 15 percent of BN and 5 percent of alumina (the mass fraction of the total filling filler is also 20 percent, the BN: Al2O3The thermal conductivity of the non-oriented three-phase heat conduction composite film is 0.215W/mK, and compared with the thermal conductivity of a two-phase composite film with the same filling amount, the thermal conductivity of the non-oriented three-phase heat conduction composite film is allThe synergistic effect between two heat-conducting filler particles with size difference is verified, so that the heat conductivity of the composite material can be remarkably increased. In addition, the thermal conductivity of the oriented three-phase heat-conducting composite film is 0.228W/mK, and compared with the thermal conductivity of the unoriented three-phase composite film, the thermal conductivity of the oriented three-phase heat-conducting composite film is also obviously improved; it is thus possible to verify: the two filler particles are oriented and arranged under an external electric field, and after the particles are oriented, heat conduction paths formed in a system are increased, so that the heat conductivity is further improved. This also indicates that the method of the present invention is effective.
The above-mentioned thermal conductivity was measured by a DTC-300 type thermal conductivity meter of the American TA company.
Claims (10)
1. A preparation method of a high-thermal-conductivity three-phase composite film under the assistance of an electric field specifically comprises the following steps:
(1) adding at least two kinds of heat-conducting filler particles with larger size difference into a polymer matrix with fluidity, uniformly mixing to obtain a mixed solution, then adding a certain amount of curing agent into the mixed solution, uniformly mixing and removing bubbles;
(2) pouring the mixed solution into a sealed conductive mold, providing a certain electric field for the mixed solution, enabling corresponding particles to be aligned in a matrix under the regulation and control of an external field, and curing or crosslinking the polymer matrix in a proper mode to obtain a three-phase composite membrane;
the at least two types of thermally conductive filler particles having a large size difference include at least one type of micron-sized and one type of nano-sized thermally conductive filler particles.
2. The method of claim 1, wherein the polymer matrix is a silicone or an epoxy resin.
3. The preparation method of claim 1, wherein the electric field is provided by an electric field device, the electric field device comprises an arbitrary waveform generator, a high voltage amplifier and an oscilloscope, the waveform, the voltage and the frequency of the electric field can be arbitrarily adjusted, and the electric field is a sinusoidal electric field of 2000Vp-p/mm and 5 Hz.
4. The method according to claim 1, wherein the total mass of the at least two kinds of the heat-conducting filler particles with larger size difference accounts for 10-40% of the mass of the polymer matrix, and the mass of the heat-conducting filler particles with larger size is 1-5 times that of the heat-conducting filler particles with smaller size.
5. The method according to claim 4, wherein the sum of the masses of the at least two kinds of the heat-conducting filler particles having the larger size difference accounts for 20% of the mass of the polymer matrix, and the mass of the heat-conducting filler particles having the larger size is 3 times that of the heat-conducting filler particles having the smaller size.
6. The production method according to claim 4, wherein the thermally conductive filler particles comprise large-sized highly thermally conductive filler 5 μm flaky hexagonal boron nitride and small-sized thermally conductive filler having a particle size of 800nm of alumina.
7. The method for preparing the polymer of claim 1, wherein the curing agent is present in an amount of (5-15) wt% based on the polymer matrix, and the curing agent may be a curing agent conventionally used in the art.
8. The method according to claim 1, wherein in the step (1), the step of uniformly mixing and degassing the bubbles comprises stirring the mixed solution with a non-intrusive homogenizer, and then performing vacuum defoaming stirring treatment.
9. The method according to claim 1, wherein the step (2) is carried out by curing with heat or crosslinking with light irradiation.
10. The preparation method according to claim 1, wherein the specific operation in the step (2) is: and (3) placing the die on a hot table, starting electric field equipment to assist in orienting the filler particles for 2min, then starting heating, setting the temperature of the hot table at 90 ℃, heating at 90 ℃ for 30min, then closing the electric field equipment, stopping heating, cooling and taking out to obtain the three-phase composite film.
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|---|---|---|---|---|
| WO2023064932A1 (en) * | 2021-10-14 | 2023-04-20 | Saint-Gobain Ceramics & Plastics, Inc. | Composite body having high thermal conductivity and method of making the composite body |
| WO2023064939A1 (en) * | 2021-10-14 | 2023-04-20 | Saint-Gobain Ceramics & Plastics, Inc. | Composite body having high thermal conductivity and method of making the composite body |
| CN114318931A (en) * | 2021-12-20 | 2022-04-12 | 北京交通大学 | Method for preparing high-thermal-conductivity mica paper based on electric field orientation |
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| CN113416332B (en) | 2023-03-24 |
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