CN108690324A - A kind of micro-nano composite insulating material of high-thermal-conductivity epoxy resin base alumina-boron nitride - Google Patents
A kind of micro-nano composite insulating material of high-thermal-conductivity epoxy resin base alumina-boron nitride Download PDFInfo
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- CN108690324A CN108690324A CN201710232591.9A CN201710232591A CN108690324A CN 108690324 A CN108690324 A CN 108690324A CN 201710232591 A CN201710232591 A CN 201710232591A CN 108690324 A CN108690324 A CN 108690324A
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- Prior art keywords
- epoxy resin
- heat
- thermal
- insulation material
- deaeration
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4215—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof cycloaliphatic
-
- 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
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
-
- 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
- C08K7/00—Use of ingredients characterised by shape
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/40—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes 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
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
Abstract
The present invention discloses a kind of micro-nano composite insulating material of high-thermal-conductivity epoxy resin base alumina-boron nitride, filler constitutes high heat conduction filler systems, pad bearing ball class formation is formed in epoxy resin-base, the thermal conductivity of material is excellent, it disclosure satisfy that needed for power component heat dissipation, have the characteristics that electrical insulation properties stabilization simultaneously, can ensure that electric/electronic device lasting security is run.This method processing technology is simple, and universality is good, can conveniently make high-thermal-conductivity epoxy resin base composite insulating material.
Description
Technical field
The present invention relates to a kind of High-heat-conductiviinsulation insulation materials, and it is micro- to be specifically related to a kind of epoxy resin-matrix alumina-boron nitride
The preparation method of nano-composite insulating material, filler constitute the high heat conduction filler systems with bearing ball structure.
Background technology
Epoxy resin is due to corrosion resistance, excellent caking property, excellent dielectric properties and can processing technology etc.
Advantage and be widely used in insulation of electrical installation and microelectronic device package.However, the thermal conductivity of pure epoxy resin is very low, only about
For 0.18W/ (mK).Therefore, electrically electric using the high power density of epoxy resin as insulating materials or encapsulating material to improve
The heat-sinking capability of sub- equipment must just be modified epoxy resin to improve its thermal conductivity.With variety classes, different shape ruler
Very little inorganic heat filling fills epoxy resin, can improve composite material heat conductivility, and ensure its electrical insulation properties.Cause
This, it is desirable to provide a kind of insulating materials of high heat conduction.
Invention content
The present invention provides a kind of by being combined with bearing ball structure high heat conduction filler systems and epoxy resin
High-heat-conductiviinsulation insulation material.The insulating materials can be applied to electric/electronic device, enhance electric/electronic device heat-sinking capability, ensure
Effective operation of electric/electronic device.
The present invention uses following technical proposals:
The preparation method of a kind of High-heat-conductiviinsulation insulation material, the insulating materials includes the following steps:
1) dry bisphenol f type epoxy resin, curing agent methyl hexahydrophthalic anhydride, accelerating agent benzyl dimethylamine, inorganic particle and
Silane coupling agent;
2) blending epoxy and curing agent methyl hexahydrophthalic anhydride, add silane coupling agent, are stirred using planetary vacuum
The machine of mixing is sufficiently stirred rear deaeration processing;
3) high heat conduction filler systems uniformly mixed in advance, are added in the mixture of step 2), using planetary vacuum
Blender is sufficiently stirred rear deaeration processing;
4) mixture of ultrasonic vibration step 3);
5) it is fully stirred using planetary de-airing mixer after accelerating agent benzyl dimethylamine being added in the mixture of step 4)
Mix rear deaeration processing;
6) mixture of step 5) is poured into mold, is heating and curing in drying box, solidification temperature be followed successively by 80 DEG C of 2h,
120 DEG C of 2h and 150 DEG C of 4h;
The mass fraction of wherein raw material is as follows:
The epoxy resin is bisphenol f type epoxy resin;
The high heat conduction filler systems are aluminum oxide micron piece, boron nitride particle.High heat conduction filler systems:Aluminium oxide is micro-
Rice piece, tri- kinds of grain sizes of 100um, 20um and 3-5um are weighed according to 1: 3: 7 ratio;The grain size of boron nitride particle is 50-100nm, nitrogen
Change the 3%-5% that boron accounts for filler systems.
Preferably, the filler particles are the inorganic particle of surface conditioning agent processing, and the filler particles are through silane idol
Join the filler particles of agent processing.
In one embodiment, the drying condition of the filler particles is:It is small in 70-80 DEG C of drying 2 in drying box
When.
The drying condition of the epoxy resin is:It is 15~30 minutes dry in 60 DEG C in drying box, so that its viscosity drops
It is low.
The drying condition of the curing agent and accelerating agent is:It is 15~30 minutes dry in 60 DEG C in drying box.
Preferably, deaeration processing is carried out in planetary vacuum stirring deaeration machine.
In one embodiment, corresponding epoxy resin and curing agent are weighed with precision electronic balance, be sufficiently stirred, put
Enter progress deaeration processing in planetary vacuum stirring deaeration machine.
In one embodiment, the oscillation step 3 in KQ2200 type ultrasonic cleaners) mixture, put after oscillation
Enter in planetary vacuum stirring deaeration machine and carries out deaeration processing again.
Preferably, hardening time is 1.5-2.5 hours.In one embodiment, hardening time is 2 hours, and cooling is about
It is taken out after 10 hours.
Beneficial effects of the present invention are as follows:
The high heat conduction modified epoxy prepared with the preparation method, the high heat conduction filling body with bearing ball structure
System, heat conductivility is excellent, disclosure satisfy that needed for power component heat dissipation, while having the characteristics that electrical insulation properties stabilization,
It can ensure that electric/electronic device lasting security is run.This method processing technology is simple, and universality is good, can conveniently make high heat conduction
Epoxy resin composite insulating material.
Specific implementation mode
In order to illustrate more clearly of the present invention, with reference to preferred embodiment, the present invention is described further.Ability
Field technique personnel should be appreciated that following specifically described content is illustrative and be not restrictive, this should not be limited with this
The protection domain of invention.
Embodiment 1:Prepare the micro-nano composite insulating material of high-thermal-conductivity epoxy resin base aluminium oxide
Specific preparation method is as follows:
1) aluminum oxide micron piece and boron nitride particle are placed in drying box dries 2 hours in 80 DEG C, weighs corresponding amount and incites somebody to action
It is uniformly mixed, and epoxy resin is 15~30 minutes dry in 60 DEG C in drying box, so that viscosity reduces;
2) epoxy resin and curing agent are weighed with precision electronic balance, mixes and be thoroughly mixed object, adds silane
Then mixture is put into progress deaeration processing in planetary vacuum stirring deaeration machine by coupling agent;
3) uniformly mixed high heat conduction filler systems are added in the mixture of step 2), add after being sufficiently stirred again
Enter accelerating agent;
4) oscillation step 3 in KQ2200 type ultrasonic cleaners) mixture, mixture is put into after oscillation planetary
It is stirred under vacuum in deaeration machine and carries out deaeration processing again;
5) mixture of step 4) is poured into mold, is put into drying box and is heating and curing, solidification temperature be followed successively by 80 DEG C,
120 DEG C and 150 DEG C, hardening time is 2 hours, and cooling is taken out after 10 hours.
Embodiment 2:Prepare the micro-nano composite insulating material of high-thermal-conductivity epoxy resin base aluminium oxide
The preparation method is the same as that of Example 1 for embodiment 2.
Embodiment 3:Prepare the micro-nano composite insulating material of high-thermal-conductivity epoxy resin base aluminium oxide
The preparation method is the same as that of Example 1.
Embodiment 4:High-thermal-conductivity epoxy resin based micro-nano composite insulating material thermal conductivity is tested
Thermal conductivity survey is carried out with the embodiment 1-3 micro-nano composite insulating materials of high-thermal-conductivity epoxy resin base boron nitride prepared
Examination, the results are shown in Table 1.
Table 1:The thermal conductivity test result of embodiment 1-3 high-thermal-conductivity epoxy resin based micro-nano composite insulating materials
The result shows that:
1. with the increase of filler doping content, the thermal conductivity of composite material gradually increases, when filler doping content reaches
After to a certain degree, the thermal conductivity of composite material increased dramatically;
2. the filler of more than kinds of variety classes grain size is combined with each other doping, is filled out to reach maximum under identical loading
Rate is filled, general principle is grain size ratio >=8 of filler, and the gap between large particle size filler will be effectively embedded in compared with small particle size filler
In, high heat conduction filler systems are constituted, effective heat conduction network is formed, improve the thermal conductivity of material.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical solution is extended out still in protection scope of the present invention.
Claims (6)
1. a kind of High-heat-conductiviinsulation insulation material, which is characterized in that the preparation method of the insulating materials includes the following steps:
1) dry bisphenol f type epoxy resin, curing agent methyl hexahydrophthalic anhydride, accelerating agent benzyl dimethylamine, filler and silane coupled
Agent;
2) blending epoxy and curing agent methyl hexahydrophthalic anhydride, add silane coupling agent, are sufficiently stirred rear deaeration;
3) high heat conduction filler systems are added in the mixture of step 2), and deaeration processing is carried out after being sufficiently stirred;
4) mixture of ultrasonic vibration step 3);
5) it carries out being sufficiently stirred deaeration after accelerating agent benzyl dimethylamine being added in the mixture of step 4);
6) mixture of step 5) is poured into mold, is heating and curing in drying box, solidification temperature be followed successively by 80 DEG C, 120 DEG C and
150℃;
The mass fraction of wherein raw material is as follows:
The epoxy resin is bisphenol f type epoxy resin;
The high heat conduction filler systems are one or more in aluminum oxide micron piece and boron nitride particle.High heat conduction filling body
System:Aluminum oxide micron piece, tri- kinds of grain sizes of 100um, 20um and 3-5um are weighed according to 1: 3: 7 ratio, the grain size of boron nitride particle
For 50-100nm.
2. High-heat-conductiviinsulation insulation material as claimed in claim 1, which is characterized in that the inorganic filler is that silane coupling agent carries out surface
The inorganic particle of processing, coupling agent are 1/20~1/10 with packing quality ratio.
3. High-heat-conductiviinsulation insulation material as claimed in claim 1, which is characterized in that the drying condition of the inorganic filler is:In drying
Dried 10 hours in 100-120 DEG C in case or more.
4. High-heat-conductiviinsulation insulation material as claimed in claim 1, which is characterized in that the epoxy resin, curing agent methyl hexahydrophthalic anhydride
Drying condition with accelerating agent benzyl dimethylamine is:It is 15~30 minutes dry in 60 DEG C in drying box.
5. High-heat-conductiviinsulation insulation material as claimed in claim 1, which is characterized in that be stirred by planetary vacuum stirring deaeration machine
It is handled with deaeration.
6. High-heat-conductiviinsulation insulation material as claimed in claim 1, which is characterized in that in step 5), hardening time is 1.5-2.5 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710232591.9A CN108690324A (en) | 2017-04-11 | 2017-04-11 | A kind of micro-nano composite insulating material of high-thermal-conductivity epoxy resin base alumina-boron nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710232591.9A CN108690324A (en) | 2017-04-11 | 2017-04-11 | A kind of micro-nano composite insulating material of high-thermal-conductivity epoxy resin base alumina-boron nitride |
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| CN108690324A true CN108690324A (en) | 2018-10-23 |
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| CN201710232591.9A Pending CN108690324A (en) | 2017-04-11 | 2017-04-11 | A kind of micro-nano composite insulating material of high-thermal-conductivity epoxy resin base alumina-boron nitride |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112175351A (en) * | 2020-08-24 | 2021-01-05 | 安徽众博新材料有限公司 | Epoxy resin composite material for photoelectron encapsulation |
| CN112961469A (en) * | 2021-04-08 | 2021-06-15 | 厦门稀土材料研究所 | Epoxy resin-based high-thermal-conductivity insulating material and preparation method thereof |
| WO2021128895A1 (en) * | 2019-12-26 | 2021-07-01 | 苏州巨峰电气绝缘系统股份有限公司 | High-thermal-conductivity insulating layer material, metal substrate, and preparation method |
| CN113061321A (en) * | 2021-03-26 | 2021-07-02 | 清华大学 | Composite material and preparation method thereof |
| CN113549301A (en) * | 2021-08-26 | 2021-10-26 | 北京高科宏烽电力技术有限公司 | Epoxy resin ultrahigh-thermal-conductivity insulating material and preparation method thereof |
| CN113583388A (en) * | 2021-06-29 | 2021-11-02 | 福建师范大学泉港石化研究院 | Heat-conducting epoxy resin composite material and preparation method thereof |
-
2017
- 2017-04-11 CN CN201710232591.9A patent/CN108690324A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021128895A1 (en) * | 2019-12-26 | 2021-07-01 | 苏州巨峰电气绝缘系统股份有限公司 | High-thermal-conductivity insulating layer material, metal substrate, and preparation method |
| CN112175351A (en) * | 2020-08-24 | 2021-01-05 | 安徽众博新材料有限公司 | Epoxy resin composite material for photoelectron encapsulation |
| CN113061321A (en) * | 2021-03-26 | 2021-07-02 | 清华大学 | Composite material and preparation method thereof |
| CN113061321B (en) * | 2021-03-26 | 2022-07-29 | 清华大学 | Composite material and preparation method thereof |
| CN112961469A (en) * | 2021-04-08 | 2021-06-15 | 厦门稀土材料研究所 | Epoxy resin-based high-thermal-conductivity insulating material and preparation method thereof |
| CN112961469B (en) * | 2021-04-08 | 2023-03-31 | 厦门稀土材料研究所 | Epoxy resin-based high-thermal-conductivity insulating material and preparation method thereof |
| CN113583388A (en) * | 2021-06-29 | 2021-11-02 | 福建师范大学泉港石化研究院 | Heat-conducting epoxy resin composite material and preparation method thereof |
| CN113549301A (en) * | 2021-08-26 | 2021-10-26 | 北京高科宏烽电力技术有限公司 | Epoxy resin ultrahigh-thermal-conductivity insulating material and preparation method thereof |
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Application publication date: 20181023 |