CN113980624B - Low-viscosity epoxy potting material for silicon carbide power module packaging and preparation method and application thereof - Google Patents

Low-viscosity epoxy potting material for silicon carbide power module packaging and preparation method and application thereof Download PDF

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CN113980624B
CN113980624B CN202111369879.3A CN202111369879A CN113980624B CN 113980624 B CN113980624 B CN 113980624B CN 202111369879 A CN202111369879 A CN 202111369879A CN 113980624 B CN113980624 B CN 113980624B
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CN113980624A (en
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曾亮
柯攀
戴小平
刘洋
刘亮
黄蕾
杜隆纯
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Hunan Guoxin Semiconductor Technology Co ltd
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    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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    • C08G59/00Polycondensates 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
    • C08G59/18Macromolecules 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
    • C08G59/40Macromolecules 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
    • C08G59/4007Curing agents not provided for by the groups C08G59/42 - C08G59/66
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    • C08G59/00Polycondensates 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
    • C08G59/18Macromolecules 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
    • C08G59/40Macromolecules 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
    • C08G59/42Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
    • C08G59/4284Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof together with other curing agents
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    • C08G59/00Polycondensates 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
    • C08G59/18Macromolecules 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
    • C08G59/40Macromolecules 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
    • C08G59/50Amines
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    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • 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
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    • H01L23/295Organic, e.g. plastic containing a filler

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Abstract

The invention discloses a low-viscosity epoxy potting material for silicon carbide power module encapsulation, a preparation method and application thereof, wherein the epoxy potting material is prepared by mixing a component A and a component B, and the component A is as follows: the epoxy resin comprises low-viscosity alicyclic epoxy resin, high-purity bisphenol A epoxy resin, a nano core-shell toughening agent, a coupling agent, silica micropowder and carbon black, wherein the component B comprises the following components: curing agent A, curing agent B, latency accelerator and silica micropowder. The epoxy potting material has the advantages of very low viscosity and CTE value, long operation time, good manufacturability, capability of directly potting the silicon carbide power module, capability of improving the integrity and impact resistance of the module, very important significance for better meeting the packaging process requirement of the silicon carbide power module and expanding the popularization and application of the epoxy potting material in the packaging of the silicon carbide power module, high use value, good application prospect, simple preparation method, convenient operation and the like, can realize large-scale preparation, and is suitable for industrial production.

Description

Low-viscosity epoxy potting material for silicon carbide power module packaging and preparation method and application thereof
Technical Field
The invention belongs to the field of materials, and relates to a low-viscosity epoxy potting material for silicon carbide power module encapsulation, and a preparation method and application thereof.
Background
The epoxy tree has excellent electrical insulation property and is widely applied to the potting field of power electronic devices, for example, encapsulation is generally carried out on high-voltage high-current IGBT modules of 3300V and 6500V such as rail traction, the epoxy glue is filled and sealed after silicone gel filling and sealing is finished, and a layer of high-density and hard protective layer is formed on the silicone gel after curing, so that the effect of improving the integrity of the module is improved, and the epoxy tree has good practical significance for improving the mechanical impact resistance of the module. However, with the development of silicon carbide power modules, new challenges are presented to conventional silicone gels. The silicon carbide power module has the characteristics of high frequency, high voltage and high junction temperature (175 ℃) and has higher performance requirements on packaging materials, organic silicon gel is easy to bubble and crack at high temperature, epoxy pouring sealant prepared by common bisphenol A epoxy resin is contracted and cracked at low temperature of-40 ℃, so that packaging failure is caused, and therefore, many problems exist in packaging the silicon carbide power module with the running temperature of more than 175 ℃.
At present, a technical route for directly applying epoxy encapsulation and abandoning silica gel encapsulation has been developed, and a certain application experience is obtained. Such as direct potting resin (DP resin), which is essentially an epoxy potting material (SMC) with high heat resistance and low Coefficient of Thermal Expansion (CTE) value, through the DP resin potting module, solder cracks under the chip can be reduced, greatly improving thermal cycle test life. The packaging mode is greatly different from the traditional packaging mode, and opens up a new opportunity for the application of epoxy resin encapsulation on the power semiconductor module. However, the existing epoxy potting material still has the defect of larger viscosity, so that the resin and the module can meet the requirements of the potting process by preheating, and the operation process is complex. Therefore, the obtained epoxy potting material has low viscosity, good thermal stability, low thermal expansion coefficient, long operation time and good manufacturability, and has very important significance for better meeting the packaging process requirements of the silicon carbide power module and expanding the popularization and application of the epoxy potting material in the packaging of the silicon carbide power module.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and providing the low-viscosity epoxy potting material for the encapsulation of the silicon carbide power module, which has the advantages of low viscosity, good thermal stability, low expansion coefficient, long operation time and good manufacturability, and the preparation method and the application thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
the low-viscosity epoxy potting material for the encapsulation of the silicon carbide power module comprises a component A and a component B, wherein the component A is mainly prepared from the following raw materials in parts by weight:
40-65 parts of low-viscosity alicyclic epoxy resin, wherein the epoxy equivalent of the low-viscosity alicyclic epoxy resin is 126-140 g/eq, and the average viscosity of the low-viscosity alicyclic epoxy resin is less than 800 mPa.s at 25 ℃;
35-60 parts of high-purity bisphenol A epoxy resin;
5-10 parts of nano core-shell toughening agent which is spherical nano particles with core-shell structure and the average particle diameter is less than 200nm;
1-5 parts of a coupling agent, wherein the coupling agent is a modified silane coupling agent;
35-70 parts of silicon micropowder;
1 to 3 parts of carbon black;
the component B is mainly prepared from the following raw materials in parts by weight:
40-60 parts of curing agent A, wherein the curing agent A is high-purity low-viscosity modified anhydride, and the average viscosity of the curing agent A is less than 200 mPa.s at 25 ℃;
40-50 parts of curing agent B, wherein the curing agent B is modified polyaromatic amine, the amine value equivalent is 420-480 mg KOH/g, and the average viscosity is less than 4000 mPa.s at 25 ℃;
1-10 parts of a latent accelerator, wherein the latent accelerator is an adduct of modified imidazole and triamine;
46-80 parts of silicon micropowder.
The low-viscosity epoxy potting material for packaging the silicon carbide power module is further improved, wherein the low-viscosity alicyclic epoxy resin is at least one of 3, 4-epoxy cyclohexylmethyl 3, 4-epoxy cyclohexylformate, bis ((3, 4-epoxy cyclohexyl) methyl) adipate, bis (7-oxabicyclo [4.1.0] 3-heptylmethyl) adipate and 3,3' - [ oxybismethylene ] bis [ 3-ethyl ] oxetane.
The low-viscosity epoxy potting material for silicon carbide power module encapsulation is further improved, the epoxy equivalent of the high-purity bisphenol A epoxy resin is 171 g/eq-177 g/eq, the hydrolyzable chlorine is lower than 300ppm, and the average viscosity is lower than 3000 mPa.s at 25 ℃.
The low-viscosity epoxy potting material for packaging the silicon carbide power module is further improved, and the nano core-shell toughening agent is a Wake GENIOPERL P52 nano core-shell toughening agent.
The low-viscosity epoxy potting material for packaging the silicon carbide power module is further improved, and the coupling agent is at least one of UM-636, UM-996, UM-998 and UM-HV 0571.
The low-viscosity epoxy potting material for packaging the silicon carbide power module is further improved, wherein the curing agent A is a mixture of methyl tetrahydrophthalic anhydride and methyl nadic anhydride; the mass ratio of the methyl tetrahydrophthalic anhydride to the methyl nadic anhydride is 1-3:1; the curing agent B is liquefied diaminomethane; the latency promoter is at least one of AJCURE PN-23, AJCURE PN-23J, and AJCURE MY-24.
The low-viscosity epoxy potting material for packaging the silicon carbide power module is further improved, and the mass ratio of the component A to the component B is 1:1-5:1.
The invention also provides a preparation method of the low-viscosity epoxy potting material for packaging the silicon carbide power module, which comprises the following steps of:
(1) Preparing a component A: mixing low-viscosity alicyclic epoxy resin, high-purity bisphenol A epoxy resin and nano core-shell toughening agent at 40-60 ℃, adding coupling agent, silica micropowder and carbon black for high-speed shearing dispersion, cooling, and removing impurities by vacuum defoaming to obtain a component A;
and (3) preparing a component B: mixing a curing agent A, a curing agent B and a latent accelerator, adding silicon micropowder for high-speed shearing and dispersing, cooling, and removing impurities by vacuum defoaming to obtain a component B;
(2) And (3) mixing the component A and the component B obtained in the step (1), and stirring to obtain the low-viscosity epoxy potting material for packaging the silicon carbide power module.
In the step (1), the high-speed shearing dispersion is carried out at the rotating speed of 2500 rpm-3000 rpm, and the time of the high-speed shearing dispersion is 20 min-30 min;
according to the preparation method of the low-viscosity epoxy potting material for packaging the silicon carbide power module, which is further improved, in the preparation process of the component B, the high-speed shearing dispersion is carried out at the rotating speed of 2500 rpm-3000 rpm, and the high-speed shearing dispersion time is 20 min-30 min.
The preparation method of the low-viscosity epoxy potting material for packaging the silicon carbide power module is further improved, and in the step (2), the stirring time is 25-35 min.
The invention also provides an application of the low-viscosity epoxy potting material for the silicon carbide power module package or the low-viscosity epoxy potting material for the silicon carbide power module package prepared by the preparation method in the silicon carbide power module package as a general technical conception.
Compared with the prior art, the invention has the advantages that:
(1) The invention provides a low-viscosity epoxy potting material for silicon carbide power module encapsulation, which comprises a component A and a component B, wherein the mutual promotion relation between the raw materials in the component A and the component B is as follows:
(1.1) the epoxy potting material has very low viscosity, excellent thermal stability and extremely low curing shrinkage rate by using low-viscosity cycloaliphatic epoxy resin and high-purity low-viscosity bisphenol A epoxy resin and using a nano core-shell toughening agent, and can meet the packaging process requirements of silicon carbide power module packaging.
In the invention, (1.2) on the premise of ensuring the crosslinking density of the resin, the low-viscosity modified anhydride curing agent and the modified polyaramid are adopted, so that the crosslinking density of the resin can be further ensured, the thermal stability of the epoxy potting material can be improved, and the thermal expansion coefficient of the epoxy potting material is prepared, so that the difference between the thermal expansion coefficient and the silicon carbide chip and the copper is small, and the reliability of the module is improved.
(1.3) in the invention, the adduct of modified imidazole and triamine is adopted as a latency accelerator, and the stability is good at 60-80 ℃, so that the epoxy potting material has longer operation time; can be quickly cured at 120 ℃ and reduce the heat of curing reaction.
Therefore, the low-viscosity epoxy potting material for the encapsulation of the silicon carbide power module has very low viscosity and CTE value, long operation time and good manufacturability, can directly encapsulate the silicon carbide power module without encapsulating organic silicon gel, can well improve the integrity and the shock resistance of the module, has high use value and good application prospect, is beneficial to the popularization and the application of special epoxy potting material on the encapsulation of the silicon carbide power module, and provides an effective technical route for the encapsulation of novel power modules.
(2) The invention also provides a preparation method of the low-viscosity epoxy potting material for the encapsulation of the silicon carbide power module, which has the advantages of simple process, convenient operation and the like, can realize large-scale preparation, and is suitable for industrial production.
Detailed Description
The invention is further described below in connection with specific preferred embodiments, but it is not intended to limit the scope of the invention.
The materials and instruments used in the examples below are all commercially available; the equipment and the preparation process adopted are conventional equipment and conventional process unless otherwise specified.
Examples
The low-viscosity epoxy potting material for the encapsulation of the silicon carbide power module comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1:1-5:1.
In the invention, the component A is mainly prepared from the following raw materials in parts by weight: 40-65 parts of low-viscosity alicyclic epoxy resin, 35-60 parts of high-purity bisphenol A type epoxy resin, 5-10 parts of nano core-shell toughening agent, 1-5 parts of coupling agent, 35-70 parts of silica micropowder and 1-3 parts of carbon black.
In the component A, the epoxy equivalent of the low-viscosity alicyclic epoxy resin is 126 g/eq-140 g/eq, and the average viscosity of the low-viscosity alicyclic epoxy resin is less than 800 mPa.s at 25 ℃; more specifically, the low viscosity alicyclic epoxy resin is at least one of 3, 4-epoxycyclohexylmethyl 3, 4-epoxycyclohexylformate, bis ((3, 4-epoxycyclohexyl) methyl) adipate, bis (7-oxabicyclo [4.1.0] 3-heptylmethyl) adipate, 3' - [ oxybis methylene ] bis [ 3-ethyl ] oxetane, but is not limited thereto.
In the component A, the epoxy equivalent of the high-purity bisphenol A epoxy resin is 171 g/eq-177 g/eq, the hydrolyzable chlorine is lower than 300ppm, and the average viscosity is lower than 3000 mPa.s at 25 ℃; more specifically, the high purity bisphenol a type epoxy resin is at least one of DER331 and DER332, but is not limited thereto.
In the component A, the nanometer core-shell toughening agent is spherical nanometer particles with a core-shell structure, and the average particle size is smaller than 200nm; more specifically, the nano core-shell toughening agent is a Wake GeniOPERL P52 nano core-shell toughening agent, but is not limited thereto.
In the component A, the coupling agent is a modified silane coupling agent; more specifically, the coupling agent is at least one of UM-636, UM-996, UM-998, UM-HV0571, available from Wohan An Ruike materials, inc., but is not limited thereto.
In the invention, the component B is mainly prepared from the following raw materials in parts by weight: 40-60 parts of curing agent A, 40-50 parts of curing agent B, 1-10 parts of latent accelerator and 46-80 parts of silica powder.
In the component B, the curing agent A is high-purity low-viscosity modified anhydride, and the average viscosity of the curing agent A is less than 200 mPa.s at 25 ℃; more specifically, the curing agent A is a mixture of methyl tetrahydrophthalic anhydride and methyl nadic anhydride, wherein the mass ratio of the methyl tetrahydrophthalic anhydride to the methyl nadic anhydride is 1-3:1, but the curing agent A is not limited to the mixture;
in the component B, the curing agent B is modified polyaromatic amine, the amine value equivalent is 420-480 mg KOH/g, and the average viscosity is less than 4000 mPa.s at 25 ℃; more specifically, the curing agent B is liquefied diaminomethane, but is not limited thereto;
in the component B, the latent accelerator is an adduct of modified imidazole and triamine; more specifically, the latency accelerator is at least one of AJCURE PN-23, AJCURE PN-23J, AJCURE MY-24, which is used for Japanese taste.
The invention discloses a preparation method of a low-viscosity epoxy potting material for packaging a silicon carbide power module, which comprises the following steps:
(1) Preparing a component A: mixing 40-65 parts of alicyclic epoxy resin, 35-60 parts of high-purity bisphenol A type epoxy resin and 5-10 parts of nano toughening agent at 40-60 ℃, adding 1-5 parts of coupling agent, 35-70 parts of silica micropowder and 1-3 parts of carbon black, performing high-speed shearing dispersion for 20-30 min at the rotating speed of 2500-3000 rpm, cooling to room temperature, and performing vacuum defoaming and impurity removal to obtain a component A;
and (3) preparing a component B: mixing 40-60 parts of curing agent A, 40-50 parts of curing agent B and 1-10 parts of latent accelerator, adding 46-80 parts of silicon micropowder, performing high-speed shearing dispersion for 20-30 min at the rotating speed of 2500-3000 rpm, cooling to room temperature, and performing vacuum defoaming and impurity removal to obtain a component B;
(2) Mixing the component A and the component B obtained in the step (1) according to the mass ratio of the component A to the component B of 1:1-5:1, and stirring for 30min to obtain the low-viscosity epoxy potting material for packaging the silicon carbide power module.
Example 1
The low-viscosity epoxy potting material for the encapsulation of the silicon carbide power module comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1:1; the component A comprises the following raw material components in parts by weight:
Figure BDA0003361913220000051
the component B is mainly prepared by mixing the following components in parts by weight:
Figure BDA0003361913220000052
Figure BDA0003361913220000061
in this example, the mass ratio of methyl tetrahydrophthalic anhydride to methyl nadic anhydride was 1:1.
The preparation method of the low-viscosity epoxy potting material for silicon carbide power module encapsulation in the embodiment comprises the following steps:
(1) The preparation process of the component A comprises the following steps: uniformly mixing 40 parts of 3, 4-epoxycyclohexylmethyl 3, 4-epoxycyclohexylformate, 35 parts of high-purity epoxy DER331 and 5 parts of Watt-gram GENIOPERL P52 nanometer core-shell toughening agent at 40 ℃, adding 1 part of UM-636, 35 parts of silica micropowder and 1 part of carbon black, carrying out high-speed shearing and dispersing at the rotating speed of 2500rpm for 20min, cooling to room temperature, and carrying out vacuum defoaming and impurity removal to obtain the component A.
(2) The preparation process of the component B comprises the following steps: adding 40 parts of a mixture of methyl tetrahydrophthalic anhydride and methyl nadic anhydride, 40 parts of liquefied DDM and 1 part of AJCURE PN-23 into a stirring kettle, uniformly mixing, adding 46 parts of silicon micropowder, carrying out high-speed shearing and dispersing at the rotating speed of 2500rpm for 20min, cooling to room temperature, and carrying out vacuum defoaming and impurity removal to obtain a component B.
(3) 100g of the prepared component A and 100g B are accurately weighed and stirred for 30min to obtain the low-viscosity epoxy potting material for packaging the silicon carbide power module. The performance of the low viscosity epoxy potting compound for silicon carbide power module encapsulation was tested and the results are shown in table 1 below.
The application of the low-viscosity epoxy potting material for the encapsulation of the silicon carbide power module in the embodiment in the encapsulation of the silicon carbide power module.
Example 2
The low-viscosity epoxy potting material for the encapsulation of the silicon carbide power module comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 5:1; the component A comprises the following raw material components in parts by weight:
Figure BDA0003361913220000062
the component B is mainly prepared by mixing the following components in parts by weight:
Figure BDA0003361913220000063
in this example, the mass ratio of methyl tetrahydrophthalic anhydride to methyl nadic anhydride was 3:1.
The preparation method of the low-viscosity epoxy potting material for silicon carbide power module encapsulation in the embodiment comprises the following steps:
(1) The preparation process of the component A comprises the following steps: uniformly mixing 65 parts of bis ((3, 4-epoxycyclohexyl) methyl) adipate, 60 parts of high-purity epoxy DER332 and 10 parts of Wake GENIOPERL P52 nanometer core-shell toughening agent at 60 ℃, adding 5 parts of UM-996, 70 parts of silica micropowder and 3 parts of carbon black, carrying out high-speed shearing and dispersing at a rotating speed of 3000rpm for 30min, cooling to room temperature, and carrying out vacuum defoaming and impurity removal to obtain a component A;
(2) The preparation process of the component B comprises the following steps: adding 60 parts of methyl tetrahydrophthalic anhydride and methyl nadic anhydride mixture, 50 parts of liquefied DDM and 10 parts of AJCURE MY-24 into a stirring kettle, uniformly mixing, adding 80 parts of silicon micro powder, carrying out high-speed shearing and dispersing at a rotating speed of 3000rpm for 30min, cooling to room temperature, and carrying out vacuum defoaming and impurity removal to obtain a component B.
(3) Accurately weighing 500g of the prepared component A and 100g B components, and stirring for 30min to obtain the low-viscosity epoxy potting material for packaging the silicon carbide power module. The performance of the low viscosity epoxy potting compound for silicon carbide power module encapsulation was tested and the results are shown in table 1 below.
Example 3
The low-viscosity epoxy potting material for the encapsulation of the silicon carbide power module comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 3:1; the component A comprises the following raw material components in parts by weight:
Figure BDA0003361913220000071
the component B is mainly prepared by mixing the following components in parts by weight:
Figure BDA0003361913220000072
in this example, the mass ratio of methyl tetrahydrophthalic anhydride to methyl nadic anhydride was 2:1.
The preparation method of the low-viscosity epoxy potting material for silicon carbide power module encapsulation in the embodiment comprises the following steps:
(1) The preparation process of the component A comprises the following steps: uniformly mixing 50 parts of bis (7-oxabicyclo [4.1.0] 3-heptylmethyl) adipate, 55 parts of high-purity epoxy DER332 and 8 parts of Wake GENIOPERL P52 nanometer core-shell toughening agent at 50 ℃, adding 1 part of UM-998, 60 parts of silica micropowder and 2 parts of carbon black, carrying out high-speed shearing dispersion at the rotating speed of 2700rpm for 25min, cooling to room temperature, and carrying out vacuum defoaming and impurity removal to obtain a component A;
(2) The preparation process of the component B comprises the following steps: adding 60 parts of a mixture of methyl tetrahydrophthalic anhydride and methyl nadic anhydride, 45 parts of liquefied DDM and 5 parts of AJCURE PN-23 into a stirring kettle, uniformly mixing, adding 64 parts of silicon micropowder, carrying out high-speed shearing dispersion at the rotating speed of 2700rpm for 25min, cooling to room temperature, and carrying out vacuum defoaming and impurity removal to obtain a component B.
(3) 300g of the prepared component A and 100g B are accurately weighed and stirred for 30min to obtain the low-viscosity epoxy potting material for packaging the silicon carbide power module. The performance of the low viscosity epoxy potting compound for silicon carbide power module encapsulation was tested and the results are shown in table 1 below.
Comparative example 1
An epoxy potting material comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1:1; the component A comprises the following raw material components in parts by weight:
Figure BDA0003361913220000081
the component B is mainly prepared by mixing the following components in parts by weight:
Figure BDA0003361913220000082
in comparative example 1, the mass ratio of methyl tetrahydrophthalic anhydride to methyl nadic anhydride was 3:1.
In comparative example 1, the epoxy potting material was prepared in the same manner as in example 1, wherein the performance test results of the prepared epoxy potting material are shown in the following table 1.
Comparative example 2
An epoxy potting material comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1:1; the component A comprises the following raw material components in parts by weight:
Figure BDA0003361913220000083
Figure BDA0003361913220000091
the component B is mainly prepared by mixing the following components in parts by weight:
Figure BDA0003361913220000092
in comparative example 2, the mass ratio of methyl tetrahydrophthalic anhydride to methyl nadic anhydride was 2:1.
In comparative example 2, the epoxy potting material was prepared in the same manner as in example 1, wherein the performance test results of the prepared epoxy potting material are shown in the following table 1.
TABLE 1 Performance test results of the low viscosity epoxy potting compound for silicon carbide power module encapsulation prepared in examples 1-3
Project Unit (B) Example 1 Example 2 Example 3 Comparative example 1 Comparative example 2
Viscosity of A component mPa·s/25℃ 12085 12115 11895 9876 14568
Viscosity of the B component mPa·s/25℃ 5676 5320 5426 5897 5756
Viscosity of the mixture mPa·s/25℃ 7885 7659 7784 6758 9456
Operating time at 60-80 DEG C min 120 87 102 183 37
Gel time @120℃150g min 35 43 39 71 18
Hardness, short D / 92 92 92 87 85
Glass transition temperature 178.6 184.9 187.3 179.5 155.9
Heat distortion temperature 167 156 163 154 143.1
Tensile Strength N/mm 2 49 53 58 43 37
Coefficient of thermal expansion K -1 17×10 -6 18×10 -6 17×10 -6 11×10 -5 9×10 -5
Dielectric breakdown strength kV/mm 18.5 19.2 18.0 16.7 16.2
Volume resistor ohm/cm 7.6×10 13 8.3×10 13 9.2×10 13 3.2×10 13 4.5×10 13
As can be seen from Table 1, the low-viscosity epoxy potting compound for silicon carbide power module encapsulation prepared in the embodiments 1-3 has excellent glass transition temperature and thermal decomposition temperature, low viscosity at room temperature, low coefficient of thermal expansion (CTE value), long operation time and good manufacturability, can directly encapsulate the silicon carbide power module, does not need to encapsulate organic silicon gel, and can well improve the integrity and impact resistance of the module, so that the low-viscosity epoxy potting compound for silicon carbide power module encapsulation has important significance for improving the reliability of the silicon carbide power module, and has high use value and good application prospect. Meanwhile, as shown in table 1, based on different types and amounts of components in the epoxy potting materials, the epoxy potting materials in comparative examples 1 and 2 still have the defect of higher thermal expansion coefficient, have larger difference with silicon carbide chips and copper, and are not beneficial to improving the reliability of the silicon carbide power module.
The above examples are only preferred embodiments of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the concept of the invention belong to the protection scope of the invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.

Claims (8)

1. The low-viscosity epoxy potting material for the encapsulation of the silicon carbide power module is characterized by comprising a component A and a component B, wherein the component A is mainly prepared from the following raw materials in parts by weight:
40-65 parts of low-viscosity alicyclic epoxy resin, wherein the epoxy equivalent of the low-viscosity alicyclic epoxy resin is 126-140 g/eq, and the average viscosity of the low-viscosity alicyclic epoxy resin is less than 800 mPa.s at 25 ℃; the low-viscosity alicyclic epoxy resin is at least one of 3, 4-epoxycyclohexylmethyl 3, 4-epoxycyclohexylformate and bis ((3, 4-epoxycyclohexyl) methyl) adipate;
35-60 parts of high-purity bisphenol A epoxy resin; the high-purity bisphenol A type epoxy resin is at least one of DER331 and DER 332;
5-10 parts of nano core-shell toughening agent which is spherical nano particles with a core-shell structure and has an average particle size smaller than 200nm;
1-5 parts of a coupling agent, wherein the coupling agent is a modified silane coupling agent;
35-70 parts of silicon micropowder;
1 to 3 parts of carbon black;
the component B is mainly prepared from the following raw materials in parts by weight:
40-60 parts of curing agent A, wherein the curing agent A is high-purity low-viscosity modified anhydride, and the average viscosity of the curing agent A is less than 200 mPa.s at 25 ℃; the curing agent A is a mixture of methyl tetrahydrophthalic anhydride and methyl nadic anhydride; the mass ratio of the methyl tetrahydrophthalic anhydride to the methyl nadic anhydride is 1-3:1;
40-50 parts of curing agent B, wherein the curing agent B is modified polyaromatic amine, the amine value equivalent is 420-480 mg KOH/g, and the average viscosity is less than 4000 mPa.s at 25 ℃; the curing agent B is liquefied diaminomethane;
1-10 parts of a latent accelerator, wherein the latent accelerator is an adduct of modified imidazole and triamine;
46-80 parts of silicon micropowder.
2. The low viscosity epoxy potting material for silicon carbide power module packaging of claim 1, wherein the nano-core-shell toughener is a wack geniopl P52 nano-core-shell toughener.
3. The low viscosity epoxy potting material for silicon carbide power module encapsulation of claim 2, wherein the coupling agent is at least one of UM-636, UM-996, UM-998, UM-HV 0571.
4. A low viscosity epoxy potting material for silicon carbide power module encapsulation according to any of claims 1 to 3 wherein the latency accelerator is at least one of AJCURE PN-23, AJCURE PN-23J, AJCURE MY-24.
5. A low viscosity epoxy potting material for silicon carbide power module encapsulation according to any one of claims 1 to 3, wherein the mass ratio of the a component to the B component is 1:1 to 5:1.
6. A method for preparing the low-viscosity epoxy potting material for silicon carbide power module encapsulation according to any one of claims 1 to 5, comprising the following steps:
(1) Preparing a component A: mixing low-viscosity alicyclic epoxy resin, high-purity bisphenol A epoxy resin and nano core-shell toughening agent at 40-60 ℃, adding coupling agent, silica micropowder and carbon black for high-speed shearing dispersion, cooling, and removing impurities by vacuum defoaming to obtain a component A;
and (3) preparing a component B: mixing a curing agent A, a curing agent B and a latent accelerator, adding silicon micropowder for high-speed shearing and dispersing, cooling, and removing impurities by vacuum defoaming to obtain a component B;
(2) And (3) mixing the component A and the component B obtained in the step (1), and stirring to obtain the low-viscosity epoxy potting material for packaging the silicon carbide power module.
7. The method of manufacturing a low viscosity epoxy potting material for silicon carbide power module encapsulation according to claim 6, wherein in the step (1), the high speed shearing dispersion is performed at a rotation speed of 2500rpm to 3000rpm, and the time of the high speed shearing dispersion is 20min to 30min; in the preparation process of the component B, the high-speed shearing dispersion is carried out at the rotating speed of 2500 rpm-3000 rpm, and the high-speed shearing dispersion time is 20-30 min;
in the step (2), the stirring time is 25-35 min.
8. Use of the low-viscosity epoxy potting material for silicon carbide power module packaging according to any one of claims 1 to 5 or the low-viscosity epoxy potting material for silicon carbide power module packaging prepared by the preparation method according to claim 6 or 7 in silicon carbide power module packaging.
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