CN110982224A - High-thermal-conductivity gel-free insulating nontoxic new material and processing technology thereof - Google Patents
High-thermal-conductivity gel-free insulating nontoxic new material and processing technology thereof Download PDFInfo
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- CN110982224A CN110982224A CN201911068575.6A CN201911068575A CN110982224A CN 110982224 A CN110982224 A CN 110982224A CN 201911068575 A CN201911068575 A CN 201911068575A CN 110982224 A CN110982224 A CN 110982224A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- 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 novel high-thermal-conductivity gel-free insulating nontoxic material which is prepared from the following components in parts by weight: 100 parts of epoxy resin, 10-20 parts of nitrile rubber, 10-15 parts of aluminum nitride fiber, 10-15 parts of boron nitride and 0.5-1.0 part of silane coupling agent. The preparation method comprises the steps of adding the aluminum nitride fiber and the boron nitride powder into a silane coupling agent, fully reacting, filtering, drying and grinding to obtain the modified composite filler; melting and mixing nitrile rubber and epoxy resin at high temperature; adding the modified composite filler into the mixed resin, stirring at a high speed for 2-3 hours, and adding a curing agent and a defoaming agent to obtain the novel high-thermal-conductivity gel-free insulating nontoxic material. According to the invention, the aluminum nitride fiber and the boron nitride with specific shapes, particle sizes and proportions are selected as the composite filler to be filled in the epoxy resin composite high polymer material, so that the thermal conductivity of the material can be obviously improved, and the novel high-thermal-conductivity gel-free insulating nontoxic material can be applied to the insulating layer of the metal-based copper-clad plate.
Description
Technical Field
The invention relates to the technical field of electronic packaging materials, in particular to a novel high-thermal-conductivity gel-free insulating nontoxic material and a processing technology thereof.
Background
With the development of the electronic industry and the progress of high-density packaging technology, the area of electronic devices is smaller and smaller, the functional integration is more and more, and the operating temperature of circuits is continuously increased, which leads to the higher and higher requirement of electronic products on heat dissipation. In particular, in recent years, third-generation semiconductor materials represented by gallium nitride, silicon carbide, and diamond have been developed, and have characteristics of a large forbidden band width, a high critical breakdown field strength, a large saturated drift rate and mobility of carriers, a very small dielectric constant, and the like, and have a very broad prospect in the fields of high frequency, high voltage, high power, and the like, and electronic devices in these fields have more stringent requirements for heat dissipation.
The metal-based copper-clad plate is a substrate material for a printed circuit board and generally consists of a metal layer, an insulating medium layer and a copper foil. The insulating medium layer is made of a heat-conducting insulating polymer composite material and is the key point for improving the heat-conducting performance of the heat-conducting insulating metal substrate. Improving the thermal conductivity and peel strength of the insulating layer is a major and difficult point of current research. However, most of high molecular materials have extremely low thermal conductivity, generally much less than 1W/(m · K), which limits the application of the materials in the electronic industry.
At present, the most effective method for improving the thermal conductivity of the polymer material is mainly to add a proper amount of high thermal conductive filler into the polymer base material, and generally to select metal oxide, carbide or nitride and the like. The type, shape, size, addition ratio and the like of the heat-conducting filler have great influence on the heat-conducting property of the composite material. The thermal conductivity of the composite material prepared at present is still not high, so that the further application of the composite material is limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a novel high-thermal-conductivity gel-free insulating nontoxic material and a preparation method thereof, and the novel high-thermal-conductivity gel-free insulating nontoxic material has higher thermal conductivity and solves the problem that the thermal conductivity of a high-molecular composite material is generally lower.
The invention aims to provide a novel high-thermal-conductivity gel-free insulating nontoxic material which is prepared from the following components in parts by weight:
preferably, the aluminum nitride fiber is prepared by the following method: mixing aluminum silicate fiber and carbon black according to a weight ratio of 4: 1, mixing, performing ultrasonic dispersion in water, drying, introducing nitrogen into a high-temperature furnace, reacting for 4-6 hours at 1650-1700 ℃, then cooling to 600-700 ℃, continuing to react for 3-5 hours, and cooling to room temperature to obtain the aluminum nitride fiber.
Preferably, the particle size of the boron nitride powder is 3-10 μm.
Preferably, the silane coupling agent is KH-570.
The second purpose of the invention is to provide a preparation method of a novel high-thermal-conductivity gel-free insulating nontoxic material, which comprises the following steps:
adding aluminum nitride fiber and boron nitride powder into a silane coupling agent, stirring in water bath at 60-80 ℃, fully reacting, filtering, drying and grinding to obtain a modified composite filler;
secondly, melting and mixing the nitrile rubber and the epoxy resin at high temperature;
adding the modified composite filler into the mixed resin obtained in the second step, stirring at a high speed for 2-3 hours, and adding a curing agent and a defoaming agent to obtain the novel high-thermal-conductivity gel-free insulating nontoxic material;
wherein the weight parts of the components are as follows:
preferably, the aluminum nitride fiber is prepared by the following method: mixing aluminum silicate fiber and carbon black according to a weight ratio of 4: 1, mixing, performing ultrasonic dispersion in water, drying, introducing nitrogen into a high-temperature furnace, reacting for 4-6 hours at 1650-1700 ℃, then cooling to 600-700 ℃, continuing to react for 3-5 hours, and cooling to room temperature to obtain the aluminum nitride fiber.
Preferably, the particle size of the boron nitride powder is 3-10 μm.
Preferably, in step two, the nitrile rubber and the epoxy resin are mixed at 150-170 ℃ for 2-3 hours.
According to the invention, the aluminum nitride fiber and the boron nitride with specific shapes, particle sizes and proportions are selected as the composite filler to be filled in the epoxy resin composite high polymer material, so that the thermal conductivity of the material can be obviously improved, and the novel high-thermal-conductivity gel-free insulating nontoxic material can be applied to the insulating layer of the metal-based copper-clad plate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless otherwise specified, each raw material is a conventional commercially available product. The silane coupling agent is KH-570, the curing agent is HS-122, and the defoaming agent is Y-686.
Example 1
A novel high-thermal-conductivity gel-free insulating nontoxic material comprises the following components in parts by weight:
the preparation method comprises the following steps:
adding aluminum nitride fiber and boron nitride powder with the particle size of 3 mu m into a silane coupling agent, stirring in water bath at 70 ℃, fully reacting, filtering, drying and grinding to obtain a modified composite filler;
mixing the nitrile rubber and the epoxy resin for 3 hours at the temperature of 170 ℃;
and step three, adding the modified composite filling material into the mixed resin obtained in the step two, stirring at a high speed for 3 hours, and adding a curing agent and a defoaming agent to obtain the novel high-thermal-conductivity gel-free insulating nontoxic material.
The aluminum nitride fiber is prepared by the following method: mixing aluminum silicate fiber and carbon black according to a weight ratio of 4: 1, mixing, performing ultrasonic dispersion in water, drying, introducing nitrogen into a high-temperature furnace, reacting for 6 hours at 1650 ℃, then cooling to 700 ℃, continuing to react for 5 hours, and cooling to room temperature to obtain the aluminum nitride fiber.
The thermal conductivity of the novel high thermal conductivity gel-free insulating nontoxic material prepared in the embodiment is 10.3W/(m.K).
Example 2
A novel high-thermal-conductivity gel-free insulating nontoxic material comprises the following components in parts by weight:
the preparation method comprises the following steps:
adding aluminum nitride fiber and boron nitride powder with the particle size of 10 mu m into a silane coupling agent, stirring in water bath at 60 ℃, fully reacting, filtering, drying and grinding to obtain a modified composite filler;
mixing the nitrile rubber and the epoxy resin for 2 hours at 150 ℃;
and step three, adding the modified composite filling material into the mixed resin obtained in the step two, stirring at a high speed for 2 hours, and adding a curing agent and a defoaming agent to obtain the novel high-thermal-conductivity gel-free insulating nontoxic material.
The aluminum nitride fiber is prepared by the following method: mixing aluminum silicate fiber and carbon black according to a weight ratio of 4: 1, mixing, performing ultrasonic dispersion in water, drying, introducing nitrogen into a high-temperature furnace, reacting for 4 hours at 1700 ℃, then cooling to 600 ℃, continuing to react for 3 hours, and cooling to room temperature to obtain the aluminum nitride fiber.
The thermal conductivity of the novel high thermal conductivity gel-free insulating nontoxic material prepared in the embodiment is measured to be 9.6W/(m.K).
Example 3
A novel high-thermal-conductivity gel-free insulating nontoxic material comprises the following components in parts by weight:
the preparation method comprises the following steps:
adding aluminum nitride fiber and boron nitride powder with the particle size of 5 mu m into a silane coupling agent, stirring in water bath at 70 ℃, fully reacting, filtering, drying and grinding to obtain a modified composite filler;
mixing the nitrile rubber and the epoxy resin for 3 hours at the temperature of 170 ℃;
and step three, adding the modified composite filling material into the mixed resin obtained in the step two, stirring at a high speed for 3 hours, and adding a curing agent and a defoaming agent to obtain the novel high-thermal-conductivity gel-free insulating nontoxic material.
The aluminum nitride fiber is prepared by the following method: mixing aluminum silicate fiber and carbon black according to a weight ratio of 4: 1, mixing, performing ultrasonic dispersion in water, drying, introducing nitrogen into a high-temperature furnace, reacting for 6 hours at 1650 ℃, then cooling to 700 ℃, continuing to react for 5 hours, and cooling to room temperature to obtain the aluminum nitride fiber.
The thermal conductivity of the novel high thermal conductivity gel-free insulating nontoxic material prepared in the embodiment is 10.1W/(m.K).
Comparative example 1
The procedure of example 1 was repeated except that 3 μm aluminum nitride powder was used in place of the aluminum nitride fibers in the first step. The thermal conductivity of the insulation material prepared in this example was determined to be 8.0W/(m · K).
Comparative example 2
The particle size of the boron nitride powder in the first step was changed to 100 μm, and the procedure was otherwise the same as in example 1. The thermal conductivity of the insulation material prepared in this example was determined to be 7.3W/(m · K).
It can be seen from the above embodiments that the thermal conductivity of the material can be significantly improved by selecting the aluminum nitride fiber and boron nitride with specific shapes, particle sizes and proportions as the composite filler to be filled in the epoxy resin composite polymer material.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
2. the new material of high thermal conductivity, gel-free, insulating, and non-toxic material as claimed in claim 1, wherein the aluminum nitride fiber is prepared by the following method: mixing aluminum silicate fiber and carbon black according to a weight ratio of 4: 1, mixing, performing ultrasonic dispersion in water, drying, introducing nitrogen into a high-temperature furnace, reacting for 4-6 hours at 1650-1700 ℃, then cooling to 600-700 ℃, continuing to react for 3-5 hours, and cooling to room temperature to obtain the aluminum nitride fiber.
3. The new material of high thermal conductivity, gel-free, insulating, and non-toxic material as claimed in claim 1, wherein the particle size of the boron nitride powder is 3-10 μm.
4. The new material as claimed in claim 1, wherein the silane coupling agent is KH-570.
5. A preparation method of a novel high-thermal-conductivity gel-free insulating nontoxic material is characterized by comprising the following steps:
adding aluminum nitride fiber and boron nitride powder into a silane coupling agent, stirring in water bath at 60-80 ℃, fully reacting, filtering, drying and grinding to obtain a modified composite filler;
secondly, melting and mixing the nitrile rubber and the epoxy resin at high temperature;
adding the modified composite filler into the mixed resin obtained in the second step, stirring at a high speed for 2-3 hours, and adding a curing agent and a defoaming agent to obtain the novel high-thermal-conductivity gel-free insulating nontoxic material;
wherein the weight parts of the components are as follows:
6. the method of claim 5, wherein the aluminum nitride fibers are prepared by: mixing aluminum silicate fiber and carbon black according to a weight ratio of 4: 1, mixing, performing ultrasonic dispersion in water, drying, introducing nitrogen into a high-temperature furnace, reacting for 4-6 hours at 1650-1700 ℃, then cooling to 600-700 ℃, continuing to react for 3-5 hours, and cooling to room temperature to obtain the aluminum nitride fiber.
7. The method of claim 5, wherein the boron nitride powder has a particle size of 3-10 μm.
8. The method as claimed in claim 5, wherein in step two, the nitrile rubber and the epoxy resin are mixed at 150-170 ℃ for 2-3 hours.
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CN114702788A (en) * | 2022-04-25 | 2022-07-05 | 叶金蕊 | Super-high voltage resistant insulating resin and preparation method thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN114702788A (en) * | 2022-04-25 | 2022-07-05 | 叶金蕊 | Super-high voltage resistant insulating resin and preparation method thereof |
CN114702788B (en) * | 2022-04-25 | 2022-09-27 | 叶金蕊 | Super-high voltage resistant insulating resin and preparation method thereof |
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