CN113201271A - Preparation method and application of high-voltage insulation silicon carbide-epoxy resin composite coating - Google Patents

Preparation method and application of high-voltage insulation silicon carbide-epoxy resin composite coating Download PDF

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CN113201271A
CN113201271A CN202110439093.8A CN202110439093A CN113201271A CN 113201271 A CN113201271 A CN 113201271A CN 202110439093 A CN202110439093 A CN 202110439093A CN 113201271 A CN113201271 A CN 113201271A
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silicon carbide
epoxy resin
resin composite
composite material
voltage
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梅云辉
梁玉
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Tianjin Polytechnic University
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Tianjin Polytechnic University
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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
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/69—Particle size larger than 1000 nm
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
    • H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
    • 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
    • C08K2201/005—Additives being defined by their particle size in general
    • 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
    • C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts

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Abstract

The invention discloses a preparation method and application of a high-voltage insulation silicon carbide-epoxy resin composite coating, wherein the silicon carbide-epoxy resin composite coating comprises modified silicon carbide with nonlinear conductivity, bisphenol A epoxy resin and a low-molecular polyamide curing agent, and the mass ratio of the modified silicon carbide to the epoxy resin is 1: 3-3: 2; the mass ratio of the epoxy resin to the curing agent is 3: 1. The preparation process provided by the invention is simple, and the prepared silicon carbide-epoxy resin composite material has the advantages of good fluidity, non-linearity of conductivity and high insulation and pressure resistance, the conductivity of the silicon carbide-epoxy resin composite material is very small when the electric field intensity is low, but the conductivity of the silicon carbide-epoxy resin composite material is increased sharply when the field intensity is increased to a certain degree, and the silicon carbide-epoxy resin composite material has the potential of homogenizing the electric field distribution and reducing partial discharge. The material is applied to the weak three-phase point of the substrate, and the silicon gel is encapsulated outside the substrate, so that the voltage is uniform, the raw material is saved, and the dielectric loss is reduced. The invention solves the problem of module breakdown failure caused by high-voltage working condition and over-high partial discharge of the silicon carbide power electronic device, and creates conditions for popularization and use of high-voltage performance of the silicon carbide power electronic device.

Description

Preparation method and application of high-voltage insulation silicon carbide-epoxy resin composite coating
Technical Field
The invention belongs to the technical field of power electronic device packaging, and relates to a preparation method and application of a high-voltage insulating silicon carbide-epoxy resin composite coating.
Background
The third generation wide bandgap semiconductor material represented by silicon carbide (SiC) has the characteristics of high breakdown electric field intensity (about 10 times of that of silicon-based materials) and low intrinsic carrier concentration (10-20 of that of the silicon-based materials at normal temperature), and becomes a new development direction of power electronic devices under the condition that the performance of the silicon-based devices is close to the molar limit. The high breakdown field strength means that the silicon carbide power electronic device can have superior high-voltage characteristics and smaller on-resistance than a silicon-based device and can bear higher blocking voltage. In addition, the silicon carbide material has high saturation migration velocity and low dielectric coefficient, and good high-frequency characteristics are brought to the device. Therefore, the silicon carbide device has a wide prospect in the application of high voltage, large capacity, high temperature and high frequency, and the modularization of the device is very necessary for realizing the application of the silicon carbide power device in a high-voltage large-capacity circuit.
The module package is filled in the module by using an insulating material under the condition of air removal, so that the module circuit board can be effectively prevented from being damaged in severe environments such as vibration, humidity, corrosion and the like. The filling materials are various, and various synthetic polymers, namely epoxy resin, polyurethane elastomer and organic silicon polymer are widely used. The epoxy resin has the advantages of corrosion resistance, high bonding strength, low shrinkage, high strength, excellent bonding performance and the like, is easy to obtain raw materials, low in price and easy to machine and form, is widely applied to a plurality of industrial fields in the forms of composite materials, potting materials, adhesives and the like, and is one of the most widely applied packaging insulating materials at present. With the continuous development of electronic devices, the requirements for the comprehensive performance of electronic packaging materials are also continuously improved. However, the current module packaging material cannot meet the use requirements of silicon carbide power electronic devices on high breaking voltage and high switching frequency.
Disclosure of Invention
In the power module, the bonding interface edge (triple point) of the ceramic substrate of the substrate and the metal copper layer thereof is the weakest position, and the position is the position which is most easily damaged and failed in the actual working state due to the large difference of the dielectric properties of materials at the interface and the uneven distribution of an electric field. The invention provides a preparation method and application of a high-voltage insulation silicon carbide-epoxy resin composite coating, wherein a nonlinear composite coating material is added to homogenize an electric field at a three-phase point, so that the problem that a module packaging material in the prior art cannot meet the high-voltage and high-frequency requirements of a silicon carbide power electronic device is solved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a high-voltage insulation silicon carbide-epoxy resin composite coating comprises modified silicon carbide, bisphenol A epoxy resin and a low-molecular polyamide curing agent.
The grain diameter of the silicon carbide powder is 5 mu m.
The modified silicon carbide is modified with a KH-550 silane coupling agent but is not limited to KH-550 silane coupling agent.
The epoxy resin and the curing agent were weighed in a mass ratio of 3: 1.
The mass ratio of the modified silicon carbide to the epoxy resin is 1: 3-3: 2.
A preparation method of a high-voltage insulation silicon carbide-epoxy resin composite coating comprises the following steps:
s1, dispersing the silicon carbide powder and the silane coupling agent in absolute ethyl alcohol, and performing ultrasonic dispersion to obtain modified silicon carbide;
s2, uniformly mixing bisphenol A type epoxy resin and modified silicon carbide to obtain a high-voltage insulation silicon carbide-epoxy resin composite material;
s3, the mixed composite material is taken and put into a vacuum de-bubbling chamber to be subjected to vacuum de-bubbling treatment.
S4 the low molecular polyamide curing agent is added into the composite material and mixed evenly for vacuum defoaming treatment.
In the step S1, the mass ratio of the KH-550 silane coupling agent to the silicon carbide powder to the absolute ethyl alcohol is 1: 199-1: 19, and the ultrasonic vibration dispersion time of the nano silicon carbide powder, the KH-550 silane coupling agent and the absolute ethyl alcohol solution is 1-2 h; in the step S2, the mixing process is high-speed centrifugal mixing of a high-speed mixer for 20-30 min; in the step S3, the composite material is subjected to vacuum defoaming for 10-20 min; in the step S4, the mixing process is high-speed centrifugal mixing for 5-10min by a high-speed mixer, and the vacuum defoaming treatment time of the composite material is 5-10 min.
The application of the high-voltage insulation silicon carbide-epoxy resin composite coating in the packaging of high-power silicon carbide power electronic devices.
The application method comprises the steps of coating the high-voltage insulation silicon carbide-epoxy resin composite material on three phase points of a substrate of a high-power silicon carbide power electronic device packaging module, and curing at a high temperature, wherein the high-temperature curing treatment temperature is 90 ℃, and the heat preservation time is 2 hours.
The invention has the advantages that: the invention relates to a high-voltage insulation silicon carbide-epoxy resin composite material for packaging a high-power silicon carbide power electronic device, which has obvious conductivity nonlinearity, has the potential of homogenizing electric field distribution under a high-voltage working condition, and obviously improves the voltage resistance of a module. And the material is applied to the weak three-phase point of the substrate, and the silicon gel is encapsulated outside the substrate, so that the voltage is uniform, the raw material is saved, and the dielectric loss is reduced. The invention solves the problem of module breakdown failure caused by high-voltage working condition and over-high partial discharge of the silicon carbide power electronic device, and creates conditions for popularization and use of high-voltage performance of the silicon carbide power electronic device.
Drawings
Fig. 1 is a non-linear conductivity test chart of example 1.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
The embodiment provides a high-voltage insulation silicon carbide-epoxy resin composite material for packaging a high-power silicon carbide power electronic device, which comprises the following preparation steps: 0.5 percent of KH-550 silane coupling agent and 30 parts of nano silicon carbide with the particle size of 5 mu m by mass are mixed in absolute ethyl alcohol, and the mixture is dispersed for 1 hour by ultrasonic vibration to obtain modified silicon carbide; mixing 100 parts by mass of epoxy resin with silicon carbide, and mixing at a high speed of 2000r/min for 20min to obtain a silicon carbide-epoxy resin composite material, placing the obtained material in a vacuum de-bubbling chamber, vacuumizing and placing for 20min to remove bubbles; adding 33 parts by mass of curing agent into the composite material, coating the curing agent on the three phase points of the packaging module substrate, and keeping the temperature of 90 ℃ for 2 hours in the nitrogen-hydrogen atmosphere. Encapsulating silicon gel outside, and keeping the temperature in an oven at 100 ℃ for 1 h.
Example 2
The embodiment provides a high-voltage insulation silicon carbide-epoxy resin composite material for packaging a high-power silicon carbide power electronic device, which comprises the following preparation steps: 0.5 percent of KH-550 silane coupling agent and 60 parts of nano silicon carbide with the particle size of 5 mu m by mass are mixed in absolute ethyl alcohol, and the mixture is dispersed for 1 hour by ultrasonic vibration to obtain modified silicon carbide; mixing 100 parts by mass of epoxy resin with silicon carbide, and mixing at a high speed of 2000r/min for 20min to obtain a silicon carbide-epoxy resin composite material, placing the obtained material in a vacuum de-bubbling chamber, vacuumizing and placing for 20min to remove bubbles; adding 33 parts by mass of curing agent into the composite material, coating the curing agent on the three phase points of the packaging module substrate, and keeping the temperature of 90 ℃ for 2 hours in the nitrogen-hydrogen atmosphere. Encapsulating silicon gel outside, and keeping the temperature in an oven at 100 ℃ for 1 h.
Example 3
The embodiment provides a high-voltage insulation silicon carbide-epoxy resin composite material for packaging a high-power silicon carbide power electronic device, which comprises the following preparation steps: mixing 0.5 mass percent of KH-550 silane coupling agent and 90 mass parts of nano silicon carbide with the particle size of 5 mu m in absolute ethyl alcohol, and performing ultrasonic vibration dispersion for 1h to obtain modified silicon carbide; mixing 100 parts by mass of epoxy resin with silicon carbide, and mixing at a high speed of 2000r/min for 20min to obtain a silicon carbide-epoxy resin composite material, placing the obtained material in a vacuum de-bubbling chamber, vacuumizing and placing for 20min to remove bubbles; adding 33 parts by mass of curing agent into the composite material, coating the curing agent on the three phase points of the packaging module substrate, and keeping the temperature of 90 ℃ for 2 hours in the nitrogen-hydrogen atmosphere. Encapsulating silicon gel outside, and keeping the temperature in an oven at 100 ℃ for 1 h.
Example 4
The embodiment provides a high-voltage insulation silicon carbide-epoxy resin composite material for packaging a high-power silicon carbide power electronic device, which comprises the following preparation steps: 0.5 percent of KH-550 silane coupling agent and 120 parts of nano silicon carbide with the particle size of 5 mu m by mass are mixed in absolute ethyl alcohol, and the mixture is dispersed for 1 hour by ultrasonic vibration to obtain modified silicon carbide; mixing 100 parts by mass of epoxy resin with silicon carbide, and mixing at a high speed of 2000r/min for 20min to obtain a silicon carbide-epoxy resin composite material, placing the obtained material in a vacuum de-bubbling chamber, vacuumizing and placing for 20min to remove bubbles; adding 33 parts by mass of curing agent into the composite material, coating the curing agent on the three phase points of the packaging module substrate, and keeping the temperature of 90 ℃ for 2 hours in the nitrogen-hydrogen atmosphere. Encapsulating silicon gel outside, and keeping the temperature in an oven at 100 ℃ for 1 h.
The conductivity performance of the high-voltage insulation silicon carbide-epoxy resin composite material for packaging the high-power silicon carbide power electronic device in the embodiment is tested by a three-electrode method, and the test result (as shown in fig. 1) shows that the test current value starts to be obviously increased after the field strength is higher than 3kV/mm, and the current value still keeps stably increasing along with the increase of the field strength after the field strength is higher than 3kV/mm, which shows that the conductivity of the high-voltage insulation silicon carbide-epoxy resin composite material for packaging the high-power silicon carbide power electronic device in the embodiment obviously increases along with the increase of the field strength, namely the high-voltage insulation silicon carbide-epoxy resin composite material has obvious conductivity nonlinearity, has the function of homogenizing the distribution of an internal electric field of the high-power silicon carbide power electronic device under a high-voltage working condition, and obviously improves the high-voltage resistance. And the material is applied to the weak three-phase point of the substrate, and the silicon gel is encapsulated outside the substrate, so that the voltage is uniform, the raw material is saved, and the dielectric loss is reduced.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.

Claims (10)

1. The high-voltage insulation silicon carbide-epoxy resin composite coating material is characterized by comprising modified silicon carbide, bisphenol A epoxy resin and a low-molecular polyamide curing agent.
2. The high voltage insulating silicon carbide-epoxy composite material according to claim 1, wherein the nano silicon carbide powder has a particle size of 5 μm.
3. The high voltage insulating silicon carbide-epoxy composite coating material according to claim 1, wherein the modified silicon carbide is modified with but not limited to KH-550 silane coupling agent.
4. The high voltage insulating silicon carbide-epoxy composite coating material according to claim 1, wherein the bisphenol a epoxy resin and the low molecular polyamide curing agent are weighed in a mass ratio of 3: 1.
5. The high-voltage insulation silicon carbide-epoxy resin composite coating material according to claim 1, wherein the mass ratio of the modified silicon carbide to the organic epoxy resin is 1: 3-3: 2.
6. A preparation method of a high-voltage insulation silicon carbide-epoxy resin composite coating material is characterized by comprising the following steps:
s1, dispersing the nano silicon carbide powder and the silane coupling agent in absolute ethyl alcohol, and performing ultrasonic dispersion to obtain modified silicon carbide;
s2, uniformly mixing bisphenol A type epoxy resin and modified silicon carbide to obtain a high-voltage insulation silicon carbide-epoxy resin composite material;
s3 the composite material after mixing is put into a vacuum de-bubbling chamber to be subjected to vacuum de-bubbling.
7. The method for preparing the high-voltage insulation silicon carbide-epoxy resin composite coating material according to claim 6, wherein the mass ratio of the KH-550 silane coupling agent, the nano silicon carbide powder and the absolute ethyl alcohol in the step S1 is 1: 199-1: 19.
8. The method for preparing a high-voltage insulation silicon carbide-epoxy resin composite material according to claim 6, wherein in step S1, the nano silicon carbide powder, the KH-550 silane coupling agent powder and the absolute ethanol solution are subjected to ultrasonic vibration for 1-2 h; in the step S2, the mixing process is high-speed centrifugal mixing of a high-speed mixer for 20-30 min; in the step S3, the composite material is subjected to vacuum defoaming for 10-20 min; in the step S4, the mixing process is high-speed centrifugal mixing for 5-10min by a high-speed mixer, and the vacuum defoaming treatment time of the composite material is 5-10 min.
9. The application of the high-voltage insulation silicon carbide-epoxy resin composite material in the packaging of high-power silicon carbide power electronic devices.
10. The application of the high-power silicon carbide power electronic device packaging module as claimed in claim 9, wherein the high-voltage insulation silicon carbide-epoxy resin composite material is injected into the high-power silicon carbide power electronic device packaging module, coated on the triple junction of the substrate, and cured at high temperature in nitrogen-hydrogen atmosphere, wherein the high-temperature curing treatment temperature is 90 ℃ and the heat preservation time is 2 hours. Then encapsulating silicon gel outside, and preserving heat for 1h in an oven at 100 ℃.
CN202110439093.8A 2021-04-23 2021-04-23 Preparation method and application of high-voltage insulation silicon carbide-epoxy resin composite coating Pending CN113201271A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117106286A (en) * 2023-10-19 2023-11-24 聚灿光电科技（宿迁）有限公司 LED composite packaging material and preparation method thereof

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CN107266863A (en) * 2017-07-25 2017-10-20 南方电网科学研究院有限责任公司 nonlinear conductivity epoxy resin composite insulating material and preparation method thereof
CN107418146A (en) * 2017-07-25 2017-12-01 南方电网科学研究院有限责任公司 Insulator material, insulator and preparation method
WO2019113699A1 (en) * 2017-12-13 2019-06-20 HYDRO-QUéBEC Composite, crossarm coated with the composite and use thereof in an electricity grid
CN111777840A (en) * 2020-07-14 2020-10-16 浙江大学 Epoxy resin micro-nano blending composite material for packaging power electronic high-power device and preparation method thereof
CN112063262A (en) * 2020-06-18 2020-12-11 武汉大学 Epoxy nonlinear conductive coating and preparation process thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107266863A (en) * 2017-07-25 2017-10-20 南方电网科学研究院有限责任公司 nonlinear conductivity epoxy resin composite insulating material and preparation method thereof
CN107418146A (en) * 2017-07-25 2017-12-01 南方电网科学研究院有限责任公司 Insulator material, insulator and preparation method
WO2019113699A1 (en) * 2017-12-13 2019-06-20 HYDRO-QUéBEC Composite, crossarm coated with the composite and use thereof in an electricity grid
CN112063262A (en) * 2020-06-18 2020-12-11 武汉大学 Epoxy nonlinear conductive coating and preparation process thereof
CN111777840A (en) * 2020-07-14 2020-10-16 浙江大学 Epoxy resin micro-nano blending composite material for packaging power electronic high-power device and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117106286A (en) * 2023-10-19 2023-11-24 聚灿光电科技（宿迁）有限公司 LED composite packaging material and preparation method thereof
CN117106286B (en) * 2023-10-19 2024-03-22 聚灿光电科技（宿迁）有限公司 LED composite packaging material and preparation method thereof

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Application publication date: 20210803