CN111777840A - Epoxy resin micro-nano blending composite material for packaging power electronic high-power device and preparation method thereof - Google Patents

Epoxy resin micro-nano blending composite material for packaging power electronic high-power device and preparation method thereof Download PDF

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CN111777840A
CN111777840A CN202010673989.8A CN202010673989A CN111777840A CN 111777840 A CN111777840 A CN 111777840A CN 202010673989 A CN202010673989 A CN 202010673989A CN 111777840 A CN111777840 A CN 111777840A
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micro
aluminum nitride
nano
epoxy resin
composite material
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CN111777840B (en
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陈向荣
戴超
孟繁博
江铁
刘斌
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Zhejiang Tianji Instrument Transformer Co ltd
Zhejiang University ZJU
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Zhejiang Horizon Transformer Co ltd
Zhejiang University ZJU
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/28Nitrogen-containing compounds
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00Details of semiconductor or other solid state devices
    • H01L23/28Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/29Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00Details of semiconductor or other solid state devices
    • H01L23/28Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/29Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
    • H01L23/293Organic, e.g. plastic
    • H01L23/295Organic, e.g. plastic containing a filler
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/28Nitrogen-containing compounds
    • C08K2003/282Binary compounds of nitrogen with aluminium
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts

Abstract

The invention discloses an epoxy resin micro-nano blending composite material for packaging a power electronic high-power device and a preparation method thereof, belonging to the crossing field of high voltage and insulation technology and composite materials. In the process of preparing the composite material, firstly, the silane coupling agent surface modified nano aluminum nitride is prepared as the heat conducting filler, the nano aluminum nitride is uniformly dispersed in the epoxy resin by utilizing ultrasound, and the micro-nano blended composite material is prepared by the processes of vacuum degassing, infusion molding and the like. The micro-nano blended composite material has excellent heat conductivity and electrical insulating property, and can be used as a packaging material for power electronic high-power devices. The preparation method of the micro-nano blended composite material is simple, easy to operate, low in cost and suitable for industrial production.

Description

Epoxy resin micro-nano blending composite material for packaging power electronic high-power device and preparation method thereof
Technical Field
The invention belongs to the crossing field of high voltage and insulation technology and composite materials, and particularly relates to an epoxy resin micro-nano blending composite material for packaging a power electronic high-power device and a preparation method thereof.
Background
With the development of new energy in the 21 st century, the demand of global energy interconnection and the introduction of ubiquitous power internet of things, power electronics are gradually developed from a first-generation controllable rectifier (SCR), and pass through a second-generation Bipolar Junction Transistor (BJT), a turn-off transistor (GTO), a semiconductor field effect transistor (MOSFET), a third-generation Insulated Gate Bipolar Transistor (IGBT) to a fourth-generation intelligent integrated circuit and intelligent power module power electronic devices. The power electronic technology is developed dramatically in a period as short as 50 years, and the performance of power electronic devices based on silicon (Si) is restricting the development of power electronic devices towards high voltage, high temperature and high frequency. Accordingly, power devices such as silicon carbide (SiC), gallium nitride (GaN), and the like based on Wide Band Gap (WBG) materials have begun to attract attention from power electronics engineers. Compared with the traditional silicon power device, the SiC power device has lower intrinsic carrier concentration (10-35 times of order), higher breakdown electric field (4-20 times), higher thermal conductivity (3-13 times) and larger saturated electron drift velocity (2-2.5 times). Meanwhile, the SiC power device can bear higher breakdown voltage, higher current, higher working temperature (200 ℃ C. and 300 ℃ C.), higher switching speed and lower switching loss. The SiC power device puts higher requirements on the heat resistance and electricity resistance of an external packaging tube shell when bearing high temperature and high pressure, and according to the IEC JEDEC standard, the device test items relate to the maximum energy/current of the tube shell, so the packaging material of the SiC power device seriously restricts the development of the power device.
The rise of new generation power electronic devices has put higher demands on the encapsulation insulating material. The thermal conductivity and electrical properties of the insulating material are critical to the safe operation of power electronics and the stability of electrical equipment. Epoxy is one of the major packaging materials at present. However, the development of devices is always restricted by the heat conducting performance and the thermal stability of the epoxy resin, and heat generated during the operation of equipment cannot be dissipated in time, so that the dielectric strength and the insulation life of the epoxy resin are reduced. Therefore, it is important to study the thermal and electrical properties of epoxy resins to improve the reliability of devices.
Since the concept of "nano dielectric" was proposed formally in 1994, many researchers at home and abroad have focused on improving the thermal conductivity and electrical properties of polymer insulation materials by adding nanoparticles, and there are a lot of documents reporting that the addition of inorganic nano-oxide particles or metal nanoparticles can effectively improve the capabilities of polymer insulation materials such as breakdown characteristics, electrical conductivity and space charge characteristics. The thermal conductivity and electrical performance of epoxy resins are key factors that limit the performance and reliability of SiC power devices. Therefore, it is necessary to improve the thermal conductivity and electrical properties of epoxy resins using nanotechnology. Relatively more research is conducted on improving the thermal conductivity of epoxy resins, and many different nanoparticles can be added to epoxy resins to improve the thermal conductivity thereof. Since the thermal conductivity of epoxy resins is very low (-0.2W/mK), it is very useful for aluminum nitride (AIN), aluminum oxide (Al)2O3) Silicon carbide (SiC) and silicon nitride (Si)3N4) Particles with high thermal conductivity such as Boron Nitride (BN) and Graphene (GO) are doped into the epoxy resin matrix, so that the heat-conducting property of the composite material can be obviously improved. The mechanism of action of thermal conductivity results from the transport of phonons within the material. The addition of the filler promotes the formation of a heat-conducting network, can reduce the scattering of phonons to a certain extent, and realizes the improvement of heat conductivity. And the formation of the heat-conducting network is closely related to the heat conductivity coefficient, size and content of the filler. However, the nano-particles promote the epoxy resin composite materialIs very limited. Microparticles can more easily establish a stable thermally conductive network than nanoparticles, but can cause a large number of defects and voids between the filler and the matrix, resulting in insulation problems such as increased dielectric loss and reduced dielectric strength. Proper nanoparticle loading can improve the dielectric properties of the material by inhibiting charge injection and trapping mobile charges by deep traps. However, the addition of nanoparticles increases the interface between the filler and the matrix, limiting the electrical conductivity of the composite. Increasingly, hybrid fillers have been applied to epoxy composites combining the advantages of microparticles and nanoparticles to develop composites with high electrical conductivity and excellent dielectric breakdown strength. AIN is also a commonly used inorganic filler because of its relatively high thermal conductivity (150-. High particle loading can increase the thermal conductivity of the epoxy resin. Furthermore, surface modification of the filler is essential to reduce the thermal resistance between the filler and the matrix. The silane coupling agent has low price and simple operation, can realize industrialized treatment, and is widely applied to the modification of surface fillers.
In summary, micro-nano blended composite materials prepared by adding micro-nano materials into epoxy resin at home and abroad are in the laboratory research stage, and have made certain progress in recent years. The utilization of the high-thermal-conductivity and high-electrical-property nano material to improve the thermal conductivity and the electrical property of the epoxy resin becomes one of key technologies for breaking through the bottleneck of a new generation of power electronic devices, and the research on the application of the high-thermal-conductivity and high-electrical-property epoxy resin micro-nano blended composite material to the packaging of the power electronic devices at present is less at home and abroad, so that the high-thermal-conductivity and high-electrical-property epoxy resin micro-nano blended composite material has wide research prospect and engineering significance.
Disclosure of Invention
The invention aims to provide a surface modification process of aluminum nitride for packaging a power electronic high-power device.
The invention also aims to provide an aluminum nitride reinforced high-thermal conductivity epoxy resin composite material for packaging a power electronic high-power device and a preparation process thereof.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
the invention firstly discloses a preparation method of an epoxy resin micro-nano blending composite material for packaging a power electronic high-power device, which comprises the following steps:
step 1: mixing 20 parts by mass of micron aluminum nitride and 2-4 parts by mass of nanometer aluminum nitride to obtain micro-nano aluminum nitride particles, and drying the micro-nano aluminum nitride particles; mixing absolute ethyl alcohol and distilled water according to the mass ratio of 15-20: 3-4 parts by mass of a mixture, and then adding the dried micro-nano aluminum nitride particles into an ethanol water solution to perform a hydration reaction at 40-50 ℃;
step 2: adding a silane coupling agent into the solution reacted in the step 1, performing ultrasonic oscillation, then performing centrifugal separation on the micro-nano aluminum nitride and the solution, drying and grinding the micro-nano aluminum nitride obtained by separation to obtain modified micro-nano aluminum nitride particles;
and step 3: adding the modified micro-nano aluminum nitride particles into epoxy resin for ultrasonic dispersion, and standing the mixed solution after the ultrasonic dispersion is completed at room temperature to fully mix the mixed solution to obtain a mixed solution;
and 4, step 4: adding a curing agent into the mixed solution, uniformly stirring, adding an accelerant, uniformly stirring, and then carrying out vacuum degassing;
and 5: spraying a release agent on the mold in advance, drying, cooling to room temperature, pouring the solution subjected to vacuum degassing in the step (4) into the mold, pre-curing at 70-90 ℃, and then curing at 130-150 ℃; and finally, moving out the die to room temperature, standing, and demolding to obtain the micro-nano blended composite material.
As a preferable scheme of the invention, the mass part ratio of the micron aluminum nitride to the nanometer aluminum nitride is preferably 20: 3.
In one embodiment, the particle size of the micron aluminum nitride is 10 μm; the grain diameter of the nano aluminum nitride is 50 nm.
In one embodiment, the drying described in steps 1 and 2 is performed under vacuum at 130 ℃ for 1-3 h.
In one embodiment, the silane coupling agent is KH560, and the amount of the silane coupling agent is 1.3-1.5 parts by mass.
In one embodiment, the epoxy resin is bisphenol A epoxy resin, and the using amount of the epoxy resin is 42-44 parts by mass.
In one embodiment, the curing agent is methyl hexahydrophthalic anhydride and is used in an amount of 33-35 parts by mass.
In one embodiment, the promoter is tris (dimethylaminomethyl) phenol, and the amount of the promoter is 0.8-1 part by mass.
In one embodiment, the pre-curing time is 3-5 hours, and the curing time is 3-5 hours.
The invention also discloses an epoxy resin micro-nano blending composite material for packaging the power electronic high-power device, which is prepared by the method.
The mixing process in the preparation method can adopt mechanical stirring, and the dispersing process can adopt ultrasonic oscillation dispersion; in general, the mechanical stirring and the ultrasonic oscillation dispersion can be combined to achieve the purpose of uniformly mixing the materials, and the rotating speed of the mechanical stirring and the power of the ultrasonic oscillation can be selected according to actual needs.
The mould drying is vacuum drying at 130 ℃, and the drying time is 1-3 h; the mould is preferably poured in vacuum, the vacuum pouring can avoid air in the epoxy resin, and the prepared material has better effect.
In one embodiment, the vacuum degassing temperature is 40-50 ℃, the vacuum degassing time is 30-60 min, and the vacuum degree can be less than 0.1 kPa. The temperature is selected to be 40-50 ℃, so that air and impurities in the epoxy resin can be removed in vacuum degassing, the fluidity in the pouring process is increased, and the operation is not suitable due to overhigh temperature.
The invention has the following beneficial effects:
the filler micrometer aluminum nitride and nanometer aluminum nitride are used as functional phases, because the nitride is not rich in hydroxyl on the surface of oxide, the aluminum nitride particle surface is hydroxylated by reasonably preparing hydrous ethanol to perform hydration reaction with the particles, then the aluminum nitride particles and the epoxy resin generate synergistic effect through silane reaction, the dispersibility of the aluminum nitride particles in the epoxy resin is promoted, and the high specific surface of the aluminum nitride after silanization can also promote the dispersibility in the epoxy resin. After chemical blending, the micro-nano aluminum nitride has strong compatibility, very uniform distribution and no obvious agglomeration and precipitation phenomena. The addition of the micron aluminum nitride promotes the formation of a heat conducting network, can reduce the scattering of phonons to a certain extent, and realizes the improvement of heat conductivity. Microparticles can more easily establish a stable thermally conductive network, but can cause a large number of defects and voids between the filler and the matrix, leading to insulation problems such as increased dielectric loss, reduced dielectric strength, and the like. And the proper content of the nano particles can fill defects and cavities existing between the filler and the epoxy resin, and can improve the electrical performance of the composite material by inhibiting charge injection and generating deep traps to capture mobile charges so as to enhance the electric resistance of the composite material. Therefore, the micro-nano mixed composite material with high conductivity and excellent dielectric property can be obtained by preparing the micro-nano filling epoxy resin with a proper proportion. The preparation method has the advantages of simple operation process, low cost and easy industrial production no matter the modification process of the particles or the preparation process of the materials. The invention belongs to the technical field of high voltage and insulation, and is mainly used for insulating high-power equipment devices such as power electronics, high-voltage electricity, aerospace and the like, in particular to packaging with higher requirements on thermal performance and electric resistance.
Drawings
FIG. 1 is a schematic diagram of a process for preparing a micro-nano blended composite material according to the present invention.
FIG. 2 is an infrared spectrum of nano aluminum nitride before and after surface treatment according to the present invention.
Figure 3 is a differential scanning calorimetry analysis of four cases of the invention.
Fig. 4 is a graph of thermal conductivity for four cases of the present invention.
Fig. 5 is a graph of dc breakdown field strength for four cases of the present invention.
Detailed Description
The present invention will be described in detail with reference to examples, which are only preferred embodiments of the present invention and are not intended to limit the present invention.
Example 1:
an epoxy resin micro-nano blending composite material for packaging a power electronic high-power device is prepared by the following steps in parts by weight:
1, putting 45.5 parts of micron aluminum nitride into a vacuum drying oven at 130 ℃ for drying, and adding 34.2 parts of absolute ethyl alcohol and distilled water: 11.4 parts of the mixture is placed into a beaker and mechanically stirred for 1 minute, and then the dried micro-nano aluminum nitride particles are subjected to hydration reaction in an ethanol aqueous solution at 40 ℃;
2, adding 3 parts of silane coupling agent KH560 into the solution, ultrasonically oscillating for 30min, separating the micro-nano aluminum nitride from the solution by using a centrifugal machine, drying the micro-nano aluminum nitride in a vacuum drying oven at 130 ℃ for 2h, and grinding and drying to obtain modified micro-nano aluminum nitride particles;
3, placing the micro-nano aluminum nitride into 100 parts of epoxy resin, performing ultrasonic dispersion on the mixed solution at 40 ℃ for 1 hour, and standing the mixed solution after the ultrasonic dispersion is completed for 2-4 hours at room temperature to fully mix the mixed solution to obtain a mixed solution;
4 adding 80 parts of curing agent into the mixed solution, mechanically stirring for 30min at 40 ℃, adding 2 parts of accelerator, mechanically stirring for 30min, and then vacuum degassing for 60min at 40 ℃;
5, spraying a release agent in advance on the mold, placing the mold at 130 ℃, drying for 2h, cooling to room temperature, pouring the solution subjected to vacuum pumping into the mold, pre-curing for 3h at 80 ℃, and curing for 3h at 130 ℃; and finally, moving the die out to room temperature, standing, and demolding to obtain the micron composite material (marked as M20N0) with the micron aluminum nitride content of 20%.
Example 2:
an epoxy resin micro-nano blending composite material for packaging a power electronic high-power device is prepared by the following steps in parts by weight:
1, mixing micrometer aluminum nitride and nanometer aluminum nitride particles in 46 parts: 2.3 parts of the mixture is put into a vacuum drying oven at 130 ℃ for drying, and absolute ethyl alcohol and distilled water are added according to the proportion of 36.3 parts: 12.1 parts of the mixture is placed into a beaker and mechanically stirred for 1 minute, and then the dried micro-nano aluminum nitride particles are subjected to hydration reaction in an ethanol aqueous solution at 40 ℃;
2, adding 3.1 parts of silane coupling agent KH560 into the solution, ultrasonically oscillating for 30min, separating the micro-nano aluminum nitride from the solution by using a centrifugal machine, drying the micro-nano aluminum nitride in a vacuum drying oven at 130 ℃ for 2h, and grinding and drying to obtain modified micro-nano aluminum nitride particles;
3, placing the micro-nano aluminum nitride into 100 parts of epoxy resin, performing ultrasonic dispersion on the mixed solution at 40 ℃ for 1 hour, and standing the mixed solution after the ultrasonic dispersion is completed for 2-4 hours at room temperature to fully mix the mixed solution to obtain a mixed solution;
4 adding 80 parts of curing agent into the mixed solution, mechanically stirring for 30min at 40 ℃, adding 2 parts of accelerator, mechanically stirring for 30min, and then vacuum degassing for 60min at 40 ℃;
5, spraying a release agent in advance on the mold, placing the mold at 130 ℃, drying for 2h, cooling to room temperature, pouring the solution subjected to vacuum pumping into the mold, pre-curing for 3h at 80 ℃, and curing for 3h at 130 ℃; and finally, moving the die out to room temperature, standing, and demolding to obtain the micro-nano blended composite material (marked as M20N1) with the mass fraction of the micro-aluminum nitride being 20% and the mass fraction of the nano-aluminum nitride being 1%.
Example 3:
an epoxy resin micro-nano blending composite material for packaging a power electronic high-power device is prepared by the following steps in parts by weight:
1, mixing 47.5 parts of micron aluminum nitride and nano aluminum nitride particles: 7.1 parts of the mixture is put into a vacuum drying oven at 130 ℃ for drying, and the absolute ethyl alcohol and the distilled water are added according to the proportion of 42 parts: putting 13 parts of the mixture into a beaker, mechanically stirring for 1 minute, and then carrying out hydration reaction on the dried micro-nano aluminum nitride particles in an ethanol aqueous solution at 40 ℃;
2, adding 3.5 parts of silane coupling agent KH560 into the solution, ultrasonically oscillating for 30min, separating the micro-nano aluminum nitride from the solution by using a centrifugal machine, drying the micro-nano aluminum nitride in a vacuum drying oven at 130 ℃ for 2h, and grinding and drying to obtain modified micro-nano aluminum nitride particles;
3, placing the micro-nano aluminum nitride into 100 parts of epoxy resin, performing ultrasonic dispersion on the mixed solution at 40 ℃ for 1 hour, and standing the mixed solution after the ultrasonic dispersion is completed for 2-4 hours at room temperature to fully mix the mixed solution to obtain a mixed solution;
4 adding 80 parts of curing agent into the mixed solution, mechanically stirring for 30min at 40 ℃, adding 2 parts of accelerator, mechanically stirring for 30min, and then vacuum degassing for 60min at 40 ℃;
5, spraying a release agent in advance on the mold, placing the mold at 130 ℃, drying for 2h, cooling to room temperature, pouring the solution subjected to vacuum pumping into the mold, pre-curing for 3h at 80 ℃, and curing for 3h at 130 ℃; and finally, moving the die out to room temperature, standing, and demolding to obtain the micro-nano blended composite material (marked as M20N3) with the mass fraction of the micro-aluminum nitride being 20% and the mass fraction of the nano-aluminum nitride being 3%.
Example 4:
an epoxy resin micro-nano blending composite material for packaging a power electronic high-power device is prepared by the following steps in parts by weight:
1, mixing micron aluminum nitride particles and nano aluminum nitride particles in parts by weight of 48.4: 12.1 parts of the mixture is put into a vacuum drying oven at 130 ℃ for drying, and the absolute ethyl alcohol and the distilled water are mixed according to the weight ratio of 45.6 parts: 15.2 parts of the mixture is placed into a beaker and mechanically stirred for 1 minute, and then the dried micro-nano aluminum nitride particles are subjected to hydration reaction in an ethanol aqueous solution at 40 ℃;
2, adding 3.5 parts of silane coupling agent KH560 into the solution, ultrasonically oscillating for 30min, separating the micro-nano aluminum nitride from the solution by using a centrifugal machine, drying the micro-nano aluminum nitride in a vacuum drying oven at 130 ℃ for 2h, and grinding and drying to obtain modified micro-nano aluminum nitride particles;
3, placing the micro-nano aluminum nitride into 100 parts of epoxy resin, performing ultrasonic dispersion on the mixed solution at 40 ℃ for 1 hour, and standing the mixed solution after the ultrasonic dispersion is completed for 2-4 hours at room temperature to fully mix the mixed solution to obtain a mixed solution;
4 adding 80 parts of curing agent into the mixed solution, mechanically stirring for 30min at 40 ℃, adding 2 parts of accelerator, mechanically stirring for 30min, and then vacuum degassing for 60min at 40 ℃;
5, spraying a release agent in advance on the mold, placing the mold at 130 ℃, drying for 2h, cooling to room temperature, pouring the solution subjected to vacuum pumping into the mold, pre-curing for 3h at 80 ℃, and curing for 3h at 130 ℃; and finally, moving the die out to room temperature, standing, and demolding to obtain the micro-nano blended composite material (marked as M20N5) with the micro-aluminum nitride content of 20% and the nano-aluminum nitride content of 5%.
The flow of sample preparation for each example is shown in FIG. 1. FIG. 2 shows the infrared spectra of the micro-nano aluminum nitride surface before and after the treatment in steps 1 and 2 of the example, it can be seen that the transmission peaks of Si-O and N-H are obvious, which indicates that the silane treatment is effective. FIG. 3 is a differential scanning thermogram obtained for four case samples, which can be seen to yield: 119.6,121.1,132.1,126.2. The glass transition temperature of the sample of M20N3 was significantly increased, contributing to the thermal stability of the material. Fig. 4 is the thermal conductivity of the four sample cases, from which it can be seen that the thermal conductivity distribution of the four sample case samples is 0.671, 0725, 0.745, 0737W/mk. If the thermal conductivity of the pure epoxy sold in the market is 0.2W/mk as a standard, the respective lifting rates are as follows: 198%, 222%, 231%, 227%. The weibull distribution of the breakdown field strengths obtained by the four case samples is shown in fig. 5, and the breakdown field strengths obtained by the four case samples with the national standard 63.2% breakdown probability are respectively: 91.2, 113.02, 171.58, 155.53 MV/m.
As can be seen from fig. 3, fig. 4 and fig. 5, in example 3, the micro-nano blended composite material (i.e., M20N3) with the micro-aluminum nitride mass fraction of 20% and the nano-aluminum nitride mass fraction of 3% has significantly better thermal performance (thermal conductivity and thermal stability) and electrical performance.
The above-mentioned embodiments only express the embodiments of the present invention, and the related descriptions are more specific and detailed, but not understood as the limitation of the patent scope of the present invention, but all the technical solutions obtained by using the equivalent substitution or equivalent transformation should be within the protection scope of the present invention.

Claims (10)

1. A preparation method of an epoxy resin micro-nano blending composite material for packaging a power electronic high-power device is characterized by comprising the following steps:
step 1: mixing 20 parts by mass of micron aluminum nitride and 2-4 parts by mass of nanometer aluminum nitride to obtain micro-nano aluminum nitride particles, and drying the micro-nano aluminum nitride particles; mixing absolute ethyl alcohol and distilled water according to the mass ratio of 15-20: 3-4 parts by mass of a mixture, and then adding the dried micro-nano aluminum nitride particles into an ethanol water solution to perform a hydration reaction at 40-50 ℃;
step 2: adding a silane coupling agent into the solution reacted in the step 1, performing ultrasonic oscillation, then performing centrifugal separation on the micro-nano aluminum nitride and the solution, drying and grinding the micro-nano aluminum nitride obtained by separation to obtain modified micro-nano aluminum nitride particles;
and step 3: adding the modified micro-nano aluminum nitride particles into epoxy resin for ultrasonic dispersion, and standing the mixed solution after the ultrasonic dispersion is completed at room temperature to fully mix the mixed solution to obtain a mixed solution;
and 4, step 4: adding a curing agent into the mixed solution, uniformly stirring, adding an accelerant, uniformly stirring, and then carrying out vacuum degassing;
and 5: spraying a release agent on the mold in advance, drying, cooling to room temperature, pouring the solution subjected to vacuum degassing in the step (4) into the mold, pre-curing at 70-90 ℃, and then curing at 130-150 ℃; and finally, moving out the die to room temperature, standing, and demolding to obtain the micro-nano blended composite material.
2. The method according to claim 1, wherein the micron aluminum nitride has a particle size of 10 μm; the grain diameter of the nano aluminum nitride is 50 nm.
3. The method according to claim 1, wherein the drying in steps 1 and 2 is carried out under vacuum at 130 ℃ for 1-3 h.
4. The method according to claim 1, wherein the silane coupling agent is KH560 and is used in an amount of 1.3 to 1.5 parts by mass.
5. The method according to claim 1, wherein the epoxy resin is bisphenol A epoxy resin and is used in an amount of 42 to 44 parts by mass.
6. The method according to claim 1, wherein the curing agent is methyl hexahydrophthalic anhydride and is used in an amount of 33 to 35 parts by mass.
7. The process according to claim 1, wherein the accelerator is tris (dimethylaminomethyl) phenol and the amount thereof is 0.8 to 1 part by mass.
8. The method according to claim 1, wherein the vacuum degassing is performed at a temperature of 40 to 50 ℃ for 30 to 60 min.
9. The method according to claim 1, wherein the pre-curing time is 3 to 5 hours and the curing time is 3 to 5 hours.
10. An epoxy resin micro-nano blended composite material for packaging a power electronic high-power device, which is prepared by the method of claim 1.
CN202010673989.8A 2020-07-14 2020-07-14 Epoxy resin micro-nano blending composite material for packaging power electronic high-power device and preparation method thereof Active CN111777840B (en)

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CN113201271A (en) * 2021-04-23 2021-08-03 天津工业大学 Preparation method and application of high-voltage insulation silicon carbide-epoxy resin composite coating
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CN113881190A (en) * 2021-10-19 2022-01-04 合肥工业大学 Epoxy resin composite material for packaging power electronic transformer and preparation method thereof
CN114350110A (en) * 2021-12-02 2022-04-15 西安理工大学 Nano-grade filler and liquid rubber co-modified epoxy composite material and preparation method thereof
CN114958004A (en) * 2022-07-06 2022-08-30 浙江大学杭州国际科创中心 Organic silicon elastomer composite material with high nonlinear conductivity and breakdown characteristics, and preparation process and application thereof

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