CN111205594A - Preparation method of epoxy resin-based composite material with high-thermal-conductivity ordered structure - Google Patents
Preparation method of epoxy resin-based composite material with high-thermal-conductivity ordered structure Download PDFInfo
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- CN111205594A CN111205594A CN201811389723.XA CN201811389723A CN111205594A CN 111205594 A CN111205594 A CN 111205594A CN 201811389723 A CN201811389723 A CN 201811389723A CN 111205594 A CN111205594 A CN 111205594A
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- epoxy resin
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- liquid crystal
- electric field
- composite material
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 61
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 61
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000945 filler Substances 0.000 claims abstract description 55
- 230000005684 electric field Effects 0.000 claims abstract description 40
- 239000004973 liquid crystal related substance Substances 0.000 claims abstract description 40
- 230000033228 biological regulation Effects 0.000 claims abstract description 28
- 239000004593 Epoxy Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims description 15
- 239000007822 coupling agent Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- 235000010290 biphenyl Nutrition 0.000 claims description 4
- 239000004305 biphenyl Substances 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000010954 inorganic particle Substances 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000004381 surface treatment Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 4
- 239000002114 nanocomposite Substances 0.000 abstract description 3
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- 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
-
- 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
-
- 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
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- 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
-
- 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
- C08K2201/003—Additives being defined by their diameter
-
- 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
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a preparation method of an epoxy resin-based micro-nano composite material with a high-thermal-conductivity ordered structure under electric field regulation. A certain amount of liquid crystal epoxy structure units are introduced while the common epoxy resin is filled with the heat-conducting filler, and the liquid crystal domain and the heat-conducting filler are directionally and orderly configured in the composite material by utilizing electric field regulation, so that the epoxy resin-based micro-nano composite dielectric with high heat conductivity can be obtained at low content.
Description
Technical Field
The invention relates to a preparation method of a composite material, in particular to an electric field regulation and control method for preparing an epoxy resin-based micro-nano composite material with a high-thermal-conductivity ordered structure.
Background
With the development of electric and electronic equipment towards high power density, small size, light weight and high integration, the equipment temperature rise is serious, the aging failure of the insulating dielectric medium can be accelerated, and the operation reliability and the service life of the electric and electronic equipment are greatly reduced. Epoxy resins are widely used in the field of electrical equipment insulation and electronic packaging because of their excellent adhesion, corrosion resistance, dielectric properties, and the like. Pure epoxy resins, however, have very low thermal conductivity and cannot meet the current development requirements. Therefore, in order to improve the heat dissipation capability of high power density electrical and electronic devices using epoxy resins as insulating materials and encapsulating materials, it is necessary to modify the epoxy resin for improving the thermal conductivity thereof. At present, the heat conduction filler is filled with epoxy resin at home and abroad, so that the heat conductivity of the epoxy resin is improved; however, the thermal conductivity of the filled high-thermal-conductivity epoxy resin-based composite material can be obviously improved only when the amount of the filler is continuously increased to a certain critical value, and the viscosity of the composite material is sharply increased along with the increase of the content of the filler, so that the manufacturability, the electrical insulation property, the mechanical property and the like of the composite material are obviously reduced.
This patent combines epoxy body modification and high heat conduction filler filling two kinds of technologies, introduces a certain amount of liquid crystal epoxy constitutional unit when adding heat conduction filler in ordinary epoxy to realize the orientation configuration of liquid crystal domain and heat conduction filler in combined material through electric field regulation and control, thereby obtain to obtain under low content is filled and have epoxy resin based nanometer composite dielectric of high thermal conductivity along electric field configuration direction.
Disclosure of Invention
The invention aims to ensure that a liquid crystal epoxy unit and a heat-conducting filler in an epoxy resin composite material are orderly arranged along the direction of an external electric field by adopting an electric field regulation and control mode, thereby improving the heat conductivity of the composite material.
Technical scheme
In order to solve the technical problems, the invention is realized by the following technical scheme:
1. a method for preparing an epoxy resin-based composite material with a high-thermal-conductivity ordered structure is characterized by comprising the following steps of:
(1) heating the liquid crystal epoxy resin to melt the liquid crystal epoxy resin into liquid;
(2) dry filler, common epoxy resin, curing agent and coupling agent;
(3) adding a certain amount of coupling agent into the high-thermal-conductivity filler, and fully stirring to prepare a high-thermal-conductivity filler system.
(4) Fully stirring the molten liquid crystal epoxy resin and the common epoxy resin by using a planetary stirrer, then adding a filler system into the mixed solution, and stirring by using a planetary stirring defoaming machine.
(5) Heating the mixed solution to make it have good fluidity, adding curing agent into the mixed solution, and stirring thoroughly with a planetary stirrer.
(6) And placing the mixed solution on an electric field regulation and control processing platform, setting the temperature of the platform (the temperature is required to be carried out at the low-temperature end of the temperature required by the reaction of the liquid crystal epoxy compound and the curing agent), regulating the size of an electric field, and setting the electric field regulation and control time according to the viscosity of the composite material so that the liquid crystal domain and the heat-conducting filler are orderly configured along the direction of the external electric field.
(7) And gradually raising the curing temperature to completely cure the composite material.
Wherein the raw materials comprise the following components in parts by weight:
preferably, the coupling agent is a silane coupling agent, but is not limited to a silane coupling agent.
2. The high heat-conducting filler system used in the invention is inorganic particles subjected to surface treatment by using a silane coupling agent, and the mass ratio of the coupling agent to the high heat-conducting filler system in the filler system is 1: 20.
3. The liquid crystal epoxy resin used in the present invention is a biphenyl liquid crystal epoxy resin, but is not limited to a biphenyl liquid crystal epoxy resin.
4. The liquid crystal epoxy resin in the present invention is melted by heating at 150 ℃.
5. The filler used in the invention is dried under the following conditions: drying for 2-3 h at 80 ℃.
6. The common epoxy resin, the curing agent and the coupling agent used in the invention are dried under the following drying conditions: and drying at 60 ℃ for 15-30 minutes.
7. The common epoxy resin used in the invention is modified by liquid crystal epoxy, and the liquid crystal epoxy resin is 0-500% of the common epoxy resin.
8. The common epoxy resin used in the invention is modified by a filler system, and the mass fraction of the filler system is 5-60 wt%.
9. The epoxy resin composite material modified by the liquid crystal epoxy resin and the filler system is orderly configured by electric field regulation.
10. The electric field regulation and control treatment is characterized in that the ordered orientation degree of the liquid crystal domain and the high-thermal-conductivity filler is related to the viscosity, the electric field amplitude, the regulation and control time, the content of the liquid crystal epoxy resin, the polarity of the filler and the shape of the filler.
11. The electric field regulation and control treatment is characterized in that the composite material has good fluidity at the regulated and controlled temperature, and the viscosity is lower than 8000mPa & s.
12. The electric field regulation and control treatment is characterized in that the form of an electric field (alternating current and direct current) and the electric field intensity are 1-30 kV/mm.
13. The electric field regulation and control treatment is characterized in that the time for orderly configuring the filler and the liquid crystal epoxy structural unit is more than 3 hours.
14. The electric field regulation and control treatment is characterized in that the filler is liquid crystal epoxy resin, and the filler is strong-polarity filler or weak-polarity filler.
15. The electric field regulation and control treatment is characterized in that the filler is flocculent and flaky, but not limited to flocculent and flaky.
The invention has the following beneficial effects:
compared with the prior art, the invention has the beneficial effects that: the liquid crystal epoxy units and the heat-conducting filler in the epoxy resin-based composite material are orderly arranged along the direction of an external electric field by adopting an electric field regulation and control mode, so that the heat conductivity of the composite material is greatly improved under the condition of the same filling content, the raw materials can be saved, and the viscosity of the composite material is reduced.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments below:
example 1: preparation of epoxy resin-based composite material with high-thermal-conductivity ordered structure
The preparation method comprises the following steps:
1) heating liquid crystal epoxy at 150 deg.C to melt it into liquid; the drying conditions of the filler are as follows: drying at 80 deg.C for 3h in a drying oven. The epoxy resin curing agent is characterized in that the drying conditions of the common epoxy resin, the curing agent and the coupling agent are as follows: drying at 60 ℃ for 20 minutes to reduce the viscosity;
2) weighing 150 parts of flake-like aluminum oxide by using a precise electronic balance according to a proportion, adding 6 parts of coupling agent, and fully stirring the mixture to obtain a high-thermal-conductivity filler system;
3) fully stirring the molten liquid crystal epoxy resin and the common epoxy resin by using a planetary stirrer, then adding a filler system into the mixed solution, and stirring by using a planetary stirring defoaming machine.
5) Heating the mixed solution at 100 deg.C for 15min to make it have good fluidity, adding curing agent into the mixed solution, and stirring thoroughly with planetary stirrer.
6) Placing the mixed solution on an electric field regulation and control treatment platform, setting the electric field intensity at 10kV/mm, setting the temperature of the platform at 80 ℃, setting the time of first-stage temperature electric field regulation and control at 6h,
7) gradually raising the temperature to 120 ℃ and 150 ℃, and respectively curing for 3 hours to completely cure the composite material. And taking out the composite material after natural cooling, and testing the thermal conductivity.
The results show that:
the filling content of the epoxy resin-based composite material with the high-thermal-conductivity ordered structure prepared in the first embodiment is 37%, and the thermal conductivity is 2.9W/(m.K), which is 16 times that of the common epoxy resin.
The above description is only a possible embodiment of the invention and does not therefore limit the scope of protection of the invention. Various modifications and adaptations made according to the above embodiments are within the scope of the present disclosure.
Claims (15)
1. A method for preparing an epoxy resin-based composite material with a high-thermal-conductivity ordered structure is characterized by comprising the following steps of:
(1) heating the liquid crystal epoxy resin to melt the liquid crystal epoxy resin into liquid;
(2) dry filler, common epoxy resin, curing agent and coupling agent;
(3) adding a certain amount of coupling agent into the high-thermal-conductivity filler, and fully stirring to prepare a high-thermal-conductivity filler system.
(4) Fully stirring the molten liquid crystal epoxy resin and the common epoxy resin by using a planetary stirrer, then adding a filler system into the mixed solution, and stirring by using a planetary stirring defoaming machine.
(5) Heating the mixed solution to make it have good fluidity, adding curing agent into the mixed solution, and stirring thoroughly with a planetary stirrer.
(6) And placing the mixed solution on an electric field regulation and control processing platform, setting the temperature of the platform (the temperature is required to be carried out at the low-temperature end of the temperature required by the reaction of the liquid crystal epoxy compound and the curing agent), regulating the size of an electric field, and setting the electric field regulation and control time according to the viscosity of the composite material so that the liquid crystal domain and the heat-conducting filler are orderly configured along the direction of the external electric field.
(7) And gradually raising the curing temperature to completely cure the composite material.
Wherein the raw materials comprise the following components in parts by weight:
preferably, the coupling agent is a silane coupling agent, but is not limited to a silane coupling agent.
2. The high heat-conducting filler system used in the invention is inorganic particles subjected to surface treatment by using a silane coupling agent, and the mass ratio of the coupling agent to the high heat-conducting filler system in the filler system is 1: 20.
3. The liquid crystal epoxy resin used in the present invention is a biphenyl liquid crystal epoxy resin, but is not limited to a biphenyl liquid crystal epoxy resin.
4. The liquid crystal epoxy resin in the present invention is melted by heating at 150 ℃.
5. The filler used in the invention is dried under the following conditions: drying for 2-3 h at 80 ℃.
6. The common epoxy resin, the curing agent and the coupling agent used in the invention are dried under the following drying conditions: and drying at 60 ℃ for 15-30 minutes.
7. The common epoxy resin used in the invention is modified by liquid crystal epoxy, and the liquid crystal epoxy resin is 0-500% of the common epoxy resin.
8. The common epoxy resin used in the invention is modified by a filler system, and the mass fraction of the filler system is 5-60 wt%.
9. The epoxy resin composite material modified by the liquid crystal epoxy resin and the filler system is orderly configured by electric field regulation.
10. The electric field regulation and control treatment is characterized in that the ordered orientation degree of the liquid crystal domain and the high-thermal-conductivity filler is related to the viscosity, the electric field amplitude, the regulation and control time, the content of the liquid crystal epoxy resin, the polarity of the filler and the shape of the filler.
11. The electric field regulation and control treatment is characterized in that the composite material has good fluidity at the regulated and controlled temperature, and the viscosity is lower than 8000mPa & s.
12. The electric field regulation and control treatment is characterized in that the form of an electric field (alternating current and direct current) and the electric field intensity are 1-30 kV/mm.
13. The electric field regulation and control treatment is characterized in that the time for orderly configuring the filler and the liquid crystal epoxy structural unit is more than 3 hours.
14. The electric field regulation and control treatment is characterized in that the filler is liquid crystal epoxy resin, and the filler is strong-polarity filler or weak-polarity filler.
15. The electric field regulation and control treatment is characterized in that the filler is flocculent and flaky, but not limited to flocculent and flaky.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811389723.XA CN111205594A (en) | 2018-11-21 | 2018-11-21 | Preparation method of epoxy resin-based composite material with high-thermal-conductivity ordered structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811389723.XA CN111205594A (en) | 2018-11-21 | 2018-11-21 | Preparation method of epoxy resin-based composite material with high-thermal-conductivity ordered structure |
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| Publication Number | Publication Date |
|---|---|
| CN111205594A true CN111205594A (en) | 2020-05-29 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811389723.XA Pending CN111205594A (en) | 2018-11-21 | 2018-11-21 | Preparation method of epoxy resin-based composite material with high-thermal-conductivity ordered structure |
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| CN (1) | CN111205594A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112625215A (en) * | 2020-12-15 | 2021-04-09 | 中科院广州化学所韶关技术创新与育成中心 | Organic-inorganic hybrid intrinsic liquid crystal epoxy resin and preparation method and application thereof |
| CN113262735A (en) * | 2021-04-21 | 2021-08-17 | 华南师范大学 | Preparation method of liquid crystal polymer surface micro-nano structure |
| WO2022206509A1 (en) * | 2021-03-31 | 2022-10-06 | 华为技术有限公司 | Thermally-conductive material and fabrication method therefor, prepreg, laminate, and circuit board |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103906784A (en) * | 2011-08-31 | 2014-07-02 | Lg伊诺特有限公司 | Epoxy resin compound and radiant heat circuit board using the same |
| CN108690325A (en) * | 2017-04-11 | 2018-10-23 | 深圳市圳田科技有限公司 | A kind of high-thermal-conductivity epoxy resin base boron nitride nano-tube composite insulating material prepared by electric field regulation and control |
-
2018
- 2018-11-21 CN CN201811389723.XA patent/CN111205594A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103906784A (en) * | 2011-08-31 | 2014-07-02 | Lg伊诺特有限公司 | Epoxy resin compound and radiant heat circuit board using the same |
| CN108690325A (en) * | 2017-04-11 | 2018-10-23 | 深圳市圳田科技有限公司 | A kind of high-thermal-conductivity epoxy resin base boron nitride nano-tube composite insulating material prepared by electric field regulation and control |
Non-Patent Citations (1)
| Title |
|---|
| 周文英等: "《导热高分子材料》", 31 December 2014, 北京：国防工业出版社, pages: 219 - 220 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112625215A (en) * | 2020-12-15 | 2021-04-09 | 中科院广州化学所韶关技术创新与育成中心 | Organic-inorganic hybrid intrinsic liquid crystal epoxy resin and preparation method and application thereof |
| WO2022206509A1 (en) * | 2021-03-31 | 2022-10-06 | 华为技术有限公司 | Thermally-conductive material and fabrication method therefor, prepreg, laminate, and circuit board |
| CN113262735A (en) * | 2021-04-21 | 2021-08-17 | 华南师范大学 | Preparation method of liquid crystal polymer surface micro-nano structure |
| CN113262735B (en) * | 2021-04-21 | 2023-09-26 | 华南师范大学 | Preparation method of liquid crystal polymer surface micro-nano structure |
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