CN107541013A - A kind of micro-nano composite insulating material of high-thermal-conductivity epoxy resin base boron nitride - Google Patents
A kind of micro-nano composite insulating material of high-thermal-conductivity epoxy resin base boron nitride Download PDFInfo
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- CN107541013A CN107541013A CN201610464311.2A CN201610464311A CN107541013A CN 107541013 A CN107541013 A CN 107541013A CN 201610464311 A CN201610464311 A CN 201610464311A CN 107541013 A CN107541013 A CN 107541013A
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Abstract
The present invention discloses a kind of micro-nano composite insulating material of high-thermal-conductivity epoxy resin base boron nitride, and its preparation method is as follows：1) 44 ' diamino-dicyclohexyl methanes (PACM), diglycidyl ether, inorganic nanoparticles and epoxy resin are dried；2) blending epoxy and diglycidyl ether, add 44 ' diamino-dicyclohexyl methane, it is sufficiently stirred rear deaeration；3) inorganic nanoparticles 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) by the mixture deaeration of step 4)；6) mixture of step 5) is poured into mould, be heating and curing in drying box.The composite insulating material heat conductivility is excellent, disclosure satisfy that needed for power component radiating, while has the characteristics of electrical insulation properties are stable, 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 composite insulating material.
Description
Technical field
The present invention relates to the present invention relates to a kind of High-heat-conductiviinsulation insulation material, a kind of preparation side of epoxy resin is specifically related to
Method.
Background technology
With electrical equipment to Large Copacity, high voltage, non-oil ultra high vacuum system, high power density and miniaturization development with micro- electricity
Son and integrated circuit develop to high speed, high density direction, and caused heat sharply increases in FU volume, these heat
The continuous accumulation of amount can accelerate the ageing failure of insulation dielectric, greatly reduce electric/electronic device reliability of operation and longevity
Life.In the main materials such as conductor material, magnetic material and the polymer insulation dielectric of composition electric/electronic device, insulated electro
The thermal conductivity of medium is minimum, therefore the thermal conductivity for improving polymeric dielectric is to strengthen the basic way of electric/electronic device radiating
Footpath.
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, it is electrically electric using epoxy resin as the high power density of insulating materials or encapsulating material to improve
The heat-sinking capability of sub- equipment, epoxy resin must be just modified and improve its thermal conductivity.To epoxy resin filling variety classes,
The inorganic nano heat filling of different shape size, it is possible to increase composite heat conductivility, and ensure its electrical insulation properties.
A kind of accordingly, it is desirable to provide insulating materials of high heat conduction.
The content of the invention
The invention solves first technical problem be to provide a kind of insulating materials of high heat conduction.The insulating materials can
Applied to electric/electronic device, enhancing electric/electronic device radiating, effective operation of electric/electronic device is ensured.
In order to solve the above technical problems, the present invention uses following technical proposals：
A kind of High-heat-conductiviinsulation insulation material, the preparation method of the insulating materials comprise the following steps：
1) 4-4 ' diamino-dicyclohexyl methanes, diglycidyl ether, inorganic nanoparticles and epoxy resin are dried；
2) blending epoxy and diglycidyl ether, 4-4 ' diamino-dicyclohexyl methanes are added, after being sufficiently stirred
Deaeration is handled；
3) inorganic nanoparticles 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) by the mixture deaeration of step 4)；
6) mixture of step 5) is poured into mould, is heating and curing in drying box, solidification temperature be followed successively by 80 DEG C, 120
DEG C and 150 DEG C；
The mass fraction of wherein raw material is as follows：
Described epoxy resin is bisphenol A type epoxy resin or bisphenol f type epoxy resin；
Described inorganic nanoparticles are boron nitride nanosheet, boron nitride nano-tube, aluminum oxide.
Reactive diluent diglycidyl ether is added to reduce the viscosity of compound, diglycidyl ether, which adds, to be increased
The loading of big material, improve the thermal conductivity of material.Preferably the mass parts of the addition of diglycidyl ether are 20.In a reality
Apply in scheme, after mixing diglycidyl ether and epoxy resin, add 4-4 ' diamino-dicyclohexyl methanes.
4-4 ' the diamino-dicyclohexyl methanes (PACM) are curing agent；
Preferably, the inorganic nanoparticles that the inorganic nanoparticles are handled for surface conditioning agent, the inorganic nano
Grain is the inorganic nanoparticles handled through silane coupler.
In one embodiment, the drying condition of the PACM and inorganic nanoparticles are：In 70-80 in drying box
DEG C dry 2 hours.
The drying condition of the epoxy resin is：Dried 15~30 minutes in 60 DEG C in drying box, so that viscosity reduces.
The drying condition of the diglycidyl ether is：Dried 15~30 minutes 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 PACM are weighed with precision electronic balance, is sufficiently stirred, is put into
Deaeration processing is carried out in planetary vacuum stirring deaeration machine.
In one embodiment, the oscillation step 3 in KQ2200 type ultrasonic cleaners) mixture, put after vibration
Enter in planetary vacuum stirring deaeration machine and carry 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
Taken out after 10 hours.
The preparation method further comprises applying electric field in the curing process, to promote boron nitride in composite system
Regular arrangement in solidification process.
Preferably, the condition of the electric field is the DC electric field that frequency is 500V.
Beneficial effects of the present invention are as follows：
The high heat conduction modified epoxy prepared with the material, its heat conductivility is excellent, disclosure satisfy that power component dissipates
Needed for heat, while there is the characteristics of electrical insulation properties are stable, 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 composite insulating material.
Brief description of the drawings
The embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 shows the SEM (SEM) of the epoxy resin-matrix boron nitride nanosheet composite insulating material of embodiment 1
Sectional drawing.
Fig. 2 shows to apply uncured insulating materials in SEM (SEM) figure after 500V DC electric fields.
Embodiment
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.Similar part is indicated with identical reference in accompanying drawing.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1：Prepare the micro-nano composite insulating material of high-thermal-conductivity epoxy resin base boron nitride
Specific preparation method is as follows：
1) PACM and boron nitride nanosheet are placed in drying box dries 2 hours in 80 DEG C, epoxy resin and 2-glycidyl
Ether is dried 15~30 minutes in drying box in 60 DEG C, so that viscosity reduces；
2) epoxy resin and PACM are weighed with precision electronic balance, mixes and be thoroughly mixed thing, then by mixture
It is put into planetary vacuum stirring deaeration machine and carries out deaeration processing；
3) boron nitride nanosheet is added in the mixture of step 2), is sufficiently stirred again；
4) oscillation step 3 in KQ2200 type ultrasonic cleaners) mixture, mixture is put into after vibration planetary
It is stirred under vacuum in deaeration machine and carries out deaeration processing again；
5) mixture of step 4) is poured into mould, 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.
The inorganic nanoparticles are the inorganic nanoparticles of surface conditioning agent silane coupler processing.
Embodiment 2：Prepare the micro-nano composite insulating material of high-thermal-conductivity epoxy resin base boron nitride
The preparation method of embodiment 2 is with embodiment 1, and the difference with embodiment 1 is embodiment 2 in step 5), mixture
Promote boron nitride regular arrangement in composite system solidification process by applying electric field during curing molding.Electric field
Intensity is：Frequency is 500V DC electric field.
Embodiment 3：Prepare the micro-nano composite insulating material of high-thermal-conductivity epoxy resin base boron nitride
Preparation method is the same as embodiment 1.
Embodiment 4：Prepare the micro-nano composite insulating material of high-thermal-conductivity epoxy resin base boron nitride
Preparation method is the same as embodiment 1.
Embodiment 5：Prepare the micro-nano composite insulating material of high-thermal-conductivity epoxy resin base boron nitride
Preparation method is the same as embodiment 1.
Embodiment 6：High-thermal-conductivity epoxy resin based micro-nano composite insulating material thermal conductivity is tested
Thermal conductivity survey is carried out with the embodiment 1-5 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 1-5 high-thermal-conductivity epoxy resin based micro-nano composite insulating materials
As a result show：
1. with the increase of filler doping content, the thermal conductivity of composite gradually increases, when filler doping content reaches
After to a certain degree, the thermal conductivity of composite rapidly increases；
2. the different types of filler of kind more than is combined with each other doping, and carrying out rationally accumulation and spatial arrangement can not only effectively solve
The problem of certainly system viscosity is much during single doping, and the formation of thermal conducting path can be effectively improved, so as to improve composite wood
The heat conductivility of material；
3. extra electric field regulation and control can change distribution of the filler in epoxy resin-base, and can significantly improve composite
Thermal conductivity.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, 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 scheme is extended out still in protection scope of the present invention.
Claims (9)
1. a kind of High-heat-conductiviinsulation insulation material, it is characterised in that the preparation method of the insulating materials comprises the following steps：
1) 4-4 ' diamino-dicyclohexyl methanes, diglycidyl ether, inorganic nanoparticles and epoxy resin are dried；
2) blending epoxy and diglycidyl ether, 4-4 ' diamino-dicyclohexyl methanes are added, is sufficiently stirred rear deaeration；
3) inorganic nanoparticles 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) by the mixture deaeration of step 4)；
6) mixture of step 5) is poured into mould, 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：
Described epoxy resin is bisphenol A type epoxy resin or bisphenol f type epoxy resin；
Described inorganic nanoparticles are the one or more in boron nitride nanosheet, boron nitride nano-tube and aluminum oxide.
2. High-heat-conductiviinsulation insulation material as claimed in claim 1, it is characterised in that the inorganic nanoparticles are surface conditioning agent processing
Inorganic nanoparticles.
3. High-heat-conductiviinsulation insulation material as claimed in claim 2, it is characterised in that the inorganic nanoparticles are carried out for silane coupler
The inorganic nanoparticles of surface treatment.
4. High-heat-conductiviinsulation insulation material as claimed in claim 1, it is characterised in that 4-4 ' diamino-dicyclohexyl methanes and inorganic
The drying condition of nano particle is：Dried 2 hours in 70~80 DEG C in drying box.
5. High-heat-conductiviinsulation insulation material as claimed in claim 1, it is characterised in that the drying of the epoxy resin and diglycidyl ether
Condition is：Dried 15~30 minutes in 60 DEG C in drying box.
6. High-heat-conductiviinsulation insulation material as claimed in claim 1, it is characterised in that the deaeration is in planetary vacuum stirring deaeration machine
Carry out deaeration processing.
7. High-heat-conductiviinsulation insulation material as claimed in claim 1, it is characterised in that in step 6), hardening time is 1.5~2.5 hours.
8. High-heat-conductiviinsulation insulation material as claimed in claim 1, it is characterised in that the preparation method further comprises in solidification process
Middle application electric field.
9. High-heat-conductiviinsulation insulation material as claimed in claim 8, it is characterised in that the condition of the electric field is the direct current that frequency is 500V
Electric field.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610464311.2A CN107541013A (en) | 2016-06-23 | 2016-06-23 | A kind of micro-nano composite insulating material of high-thermal-conductivity epoxy resin base boron nitride |
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| CN201610464311.2A CN107541013A (en) | 2016-06-23 | 2016-06-23 | A kind of micro-nano composite insulating material of high-thermal-conductivity epoxy resin base boron nitride |
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| CN109280332A (en) * | 2018-08-03 | 2019-01-29 | 吉林大学 | A kind of preparation method of boron nitride/epoxy resin heat conductive insulating composite material |
| US20190156968A1 (en) * | 2015-12-28 | 2019-05-23 | General Electric Technology Gmbh | Medium-voltage or high-voltage electrical device having low-thickness hybrid insulation |
| CN109852005A (en) * | 2019-01-14 | 2019-06-07 | 国网西藏电力有限公司 | A kind of high thermal conductivity composite insulating material and preparation method based on electric field abduction mechanism |
| CN110922719A (en) * | 2019-11-22 | 2020-03-27 | 中南大学 | High-thermal-conductivity boron nitride/epoxy resin composite material and preparation method and application 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 |
| CN113278163A (en) * | 2020-11-18 | 2021-08-20 | 百色学院 | Method for improving heat conductivity coefficient of flaky alumina/polymer composite sheet material through electric field induction |
| CN117603555A (en) * | 2024-01-24 | 2024-02-27 | 四川大学 | High-heat-conductivity high-toughness epoxy resin composite material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20190156968A1 (en) * | 2015-12-28 | 2019-05-23 | General Electric Technology Gmbh | Medium-voltage or high-voltage electrical device having low-thickness hybrid insulation |
| US11017919B2 (en) * | 2015-12-28 | 2021-05-25 | General Electric Technology Gmbh | Medium-voltage or high-voltage electrical device having low-thickness hybrid insulation |
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| CN109852005B (en) * | 2019-01-14 | 2021-09-07 | 国网西藏电力有限公司 | High-thermal-conductivity composite insulating material based on electric field induction mechanism and preparation method thereof |
| CN110922719A (en) * | 2019-11-22 | 2020-03-27 | 中南大学 | High-thermal-conductivity boron nitride/epoxy resin composite material and preparation method and application thereof |
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| CN113278163A (en) * | 2020-11-18 | 2021-08-20 | 百色学院 | Method for improving heat conductivity coefficient of flaky alumina/polymer composite sheet material through electric field induction |
| CN117603555A (en) * | 2024-01-24 | 2024-02-27 | 四川大学 | High-heat-conductivity high-toughness epoxy resin composite material and preparation method and application thereof |
| CN117603555B (en) * | 2024-01-24 | 2024-03-22 | 四川大学 | High-heat-conductivity high-toughness epoxy resin composite material and preparation method and application thereof |
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