CN114456757B - Pouring sealant and preparation method and application thereof - Google Patents
Pouring sealant and preparation method and application thereof Download PDFInfo
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- CN114456757B CN114456757B CN202210098546.XA CN202210098546A CN114456757B CN 114456757 B CN114456757 B CN 114456757B CN 202210098546 A CN202210098546 A CN 202210098546A CN 114456757 B CN114456757 B CN 114456757B
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- pouring sealant
- modified filler
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on 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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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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
- C08K2201/001—Conductive additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
- Conductive Materials (AREA)
Abstract
The invention provides pouring sealant and a preparation method and application thereof. The pouring sealant comprises a component A and a component B, wherein the component A comprises epoxy resin, a diluent, spherical modified filler and flake silver powder; the component B comprises a curing agent and a curing accelerator; the spherical modified filler comprises a glass powder core body, and a graphene layer and a silver deposition layer which are sequentially coated on the glass powder core body. The invention adds ball-shaped modified filler and flake silver powder into the system to improve the electric conductivity and heat conductivity of the pouring sealant, the heat conductivity coefficient is 1.6W/(m.k) at the minimum, and the resistivity is 6 multiplied by 10 at the maximum ‑4 (Ω·cm), the potting adhesive can be used for packaging electronic components.
Description
Technical Field
The invention belongs to the technical field of pouring sealants, and particularly relates to a pouring sealant, and a preparation method and application thereof.
Background
The cured epoxy resin has good physical and mechanical properties, bonding properties and insulating properties, and is widely applied to various industrial production fields in various forms such as composite materials, adhesives, potting materials and the like. The epoxy potting material has the characteristics of good permeability, long pot life and good performance, and is widely applied to the fields of electronics, automobiles, aerospace and the like. The thermal conductivity of the common epoxy potting material is only 0.2-0.3W/m.k, and along with the rapid development of high-performance and high-density packaging technology of the potting device, in some occasions with high antistatic requirements, the insulating property of the potting material is too good, but is a defect, and the potting material cannot effectively remove static electricity, so that the potting adhesive capable of meeting the requirements of high heat conduction and high electric conduction is required. At present, in order to improve the heat conduction performance, a heat conduction filler is generally added into a system, and in order to improve the electric conduction performance, an electric conduction filler is generally added. Meanwhile, the addition of the heat-conducting filler and the electric-conducting filler improves the electric conductivity and the heat conductivity to a certain extent, but has limited reinforcing effect and unsatisfactory effect.
Therefore, it is necessary to develop a pouring sealant with high electrical conductivity and high thermal conductivity.
Disclosure of Invention
The present invention aims to solve at least one of the above technical problems in the prior art. For this purpose, the invention provides a pouring sealant.
The invention also provides a preparation method of the pouring sealant.
The invention also provides application of the pouring sealant.
The first aspect of the invention provides a pouring sealant, which comprises an A component and a B component, wherein the A component comprises epoxy resin, a diluent, spherical modified filler and flake silver powder; the component B comprises a curing agent and a curing accelerator;
the spherical modified filler comprises a glass powder core body, and a graphene layer and a silver deposition layer which are sequentially coated on the glass powder core body.
The invention relates to one of the technical schemes of pouring sealant, which has at least the following beneficial effects:
the spherical modified filler and the flake silver powder are added into the system to improve the electric conduction and heat conduction properties of the pouring sealant, wherein the spherical modified filler obtained by silver plating on the surface of the graphene coated glass powder has high heat conduction property and electric conduction property, the graphene coated glass powder aims to enable the graphene to promote the heat conduction property of the glass powder and improve the electric conduction property, the silver deposition layer aims to further improve the electric conduction property, and when the spherical modified filler and the flake silver powder are mixed with the flake silver powder, more spherical-surface lap joints can be generated on a microstructure to further improve the electric conduction and heat conduction properties of the pouring sealant, the heat conduction coefficient is at least 1.6W/(m.k), and the resistivity is at most 6 multiplied by 10 -4 (Ω·cm)。
According to some embodiments of the invention, the spherically modified filler is prepared by the following method:
preparing graphene coated glass powder: preparing a mixed solvent of water and isopropanol, adding glass powder, dispersing uniformly, sequentially adding a silane coupling agent and graphene suspension, performing ultrasonic dispersion, heating, and washing and drying to obtain graphene coated glass powder;
preparing spherical modified filler: adding the prepared graphene coated glass powder into silver nitrate solution under the actions of ultrasound and stirring, dispersing uniformly, adding a reducing agent, depositing silver on the surface of the powder, and washing and drying to obtain the graphene coated glass powder.
According to some embodiments of the present invention, the surface of the plate-like silver powder is subjected to an acid treatment for the purpose of preventing the silver powder from settling or agglomerating in the epoxy matrix.
According to some embodiments of the invention, the average particle size of the plate-like silver powder is 2um to 20um, preferably 5um to 10um.
According to some embodiments of the invention, the a component comprises the following components in parts by weight: 25-40 parts of epoxy resin; 3-5 parts of diluent; 30-50 parts of spherical modified filler; 15-50 parts of flake silver powder; the component B comprises the following components in parts by weight: 30-40 parts of curing agent; the curing accelerator is 0.05 to 0.1 part.
According to some embodiments of the invention, the mass ratio of the spherically modified filler to the plate-like silver powder is 1: (0.5-1).
The research shows that the mass ratio of the spherical modified filler to the flake silver powder is 1: (0.5-1) has better electric conductivity and heat conductivity, and if the mass ratio of the spherical modified filler to the flake silver powder is more than 1:0.5, the electric conductivity is not improved enough; if the mass ratio of the spherical modified filler to the flake silver powder is less than 1:1, the heat conducting property is not obviously improved.
According to some embodiments of the invention, the silver coating comprises 10-20% of the total mass of the spherically modified filler.
When the silver coating content in the spherical modified filler of the present invention is less than 10%, the electric conductivity is lowered, and when the silver coating content exceeds 20%, the heat conductivity is lowered.
According to some embodiments of the invention, the diluent comprises at least one of polypropylene glycol diglycidyl ether, cyclohexanediol diglycidyl ether, diethylene glycol diglycidyl ether, or neopentyl glycol diglycidyl ether.
According to some embodiments of the invention, the epoxy resin comprises bisphenol a epoxy resin.
According to some embodiments of the invention, the curing agent comprises at least one of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, methyl nadic anhydride, tetrahydrophthalic anhydride, or hexahydrophthalic anhydride.
According to some embodiments of the invention, the curing accelerator comprises at least one of DMP-30, N-dimethylbenzylamine, 2-methylimidazole, or 2-ethyl-4-methylimidazole.
The second aspect of the invention provides a preparation method of a pouring sealant with high electric conductivity and high thermal conductivity, which comprises the following steps:
s1, uniformly mixing epoxy resin, a diluent, spherical modified filler and flake silver powder to obtain a component A;
s2, uniformly mixing the curing agent and the curing accelerator to obtain the component B.
According to some embodiments of the invention, in step S1, the stirring speed during the mixing is 800-1200 r/min; stirring time is 20-60 min.
According to some embodiments of the invention, in step S2, the stirring speed during the mixing is 1000-1500 r/min; stirring time is 20-40 min.
The third aspect of the invention provides an electronic component, which is encapsulated by the pouring sealant.
Detailed Description
Technical solutions in the embodiments of the present invention will be clearly and completely described below, but the embodiments of the present invention are not limited thereto.
The reagents, methods and apparatus employed in the present invention, unless otherwise specified, are all conventional in the art.
The raw materials used in the examples and comparative examples of the present invention are as follows:
epoxy resin: bisphenol a epoxy resin, mitsubishi bisphenol a epoxy resin JER1256 in japan;
flake silver powder a: the average grain diameter is 5-8 mu m; HW-FB11701; guangzhou Hongwu materials science and technology Co., ltd;
flake silver powder B: the average grain diameter is 1-3 mu m; HW-FB11501; guangzhou Hongwu materials science and technology Co., ltd;
spherical modified filler a: the mass of the silver deposition layer accounts for 15wt% of the total mass of the spherical modified filler A, and the spherical modified filler A is self-made;
spherical modified filler B: the mass of the silver deposition layer accounts for 10 weight percent of the total mass of the spherical modified filler B, and the spherical modified filler B is self-made;
spherical modified filler C: the mass of the silver deposition layer accounts for 20 weight percent of the total mass of the spherical modified filler C, and the spherical modified filler C is self-made;
spherical modified filler D: the mass of the silver deposition layer accounts for 5 weight percent of the total mass of the spherical modified filler D, and the spherical modified filler D is self-made;
spherical modified filler E: the mass of the silver deposition layer accounts for 30 weight percent of the total mass of the spherical modified filler E, and the spherical modified filler E is self-made;
the preparation method of the spherical modified filler comprises the following steps: dispersing graphene in water to prepare graphene suspension;
preparing a mixed solvent of water and isopropanol (volume ratio is 1:9), adding glass powder (lead-free glass powder, particle size is 1-4 mu m) for uniform dispersion, then adding a silane coupling agent KH550, wherein the dosage is 3% of the weight of the glass powder, then adding graphene suspension prepared in the previous step, performing ultrasonic dispersion, heating to 60-70 ℃, maintaining for 60min, and then filtering, washing and drying to obtain graphene coated glass powder;
adding the prepared graphene coated glass powder into 1mol/L silver nitrate solution under the action of ultrasound and stirring, dispersing uniformly, maintaining the ultrasound stirring action unchanged, adding ascorbic acid to deposit silver on the surface of the powder, and washing and drying to obtain modified glass powder, wherein the weight ratio of the glass powder to the graphene to the silver nitrate is 1:0.05 (0.2-0.6), and regulating and controlling the content of the silver nitrate to obtain a series of spherical modified fillers.
Diluents, curing agents and curing accelerators are commercially available.
Examples 1 to 7
Examples 1-7 provide a series of pouring sealants prepared as follows, with the composition contents shown in Table 1.
S1, mixing epoxy resin, a diluent, spherical modified filler and flake silver powder, wherein the stirring speed is 1000r/min, and the stirring time is 40min to obtain a component A;
s2, uniformly mixing the curing agent and the curing accelerator, wherein the stirring speed is 1300r/min, and the stirring time is 30min, so that the component B is obtained.
TABLE 1 content (parts) of Components of examples 1 to 7
Examples 8 to 12
Examples 8-12 provide a series of pouring sealants prepared in the same manner as in example 1, with the composition contents shown in Table 2.
TABLE 2 content (parts) of Components of examples 8 to 12
Comparative example 1
Comparative example 1 provides a pouring sealant, the preparation method and the component content are the same as those of example 1, except that the flake silver powder is not added.
Comparative example 2
Comparative example 2 provides a pouring sealant, the preparation method and the component content are the same as in example 1, except that no spherical modified filler is added.
Comparative example 3
Comparative example 3 provides a pouring sealant, the preparation method and the component content are the same as in example 1, except that the spherical modified filler is not silvered.
Performance testing
The components A, B of the above examples and comparative examples were mixed in proportions and tested at a curing temperature of 80℃for a curing time of 1 hour, and the following performance tests were performed, and the data are shown in Table 3.
Conductivity: testing the heat conductivity of the pouring sealant after curing by adopting a heat conductivity coefficient tester;
thermal conductivity: and testing the conductivity of the cured pouring sealant by adopting a surface resistivity tester.
Table 3 data for examples and comparative examples
As can be seen from the above embodiments, the pouring sealant provided by the embodiment of the invention has high heat conduction performance and high electric conduction performance, and is particularly suitable for packaging electronic components due to the excellent characteristics.
It can be seen from examples 1 to 5 of the present invention that when the mass ratio of the spherically modified filler to the plate-like silver powder is 1: in the range of (0.5-1), the heat conductive property and the electric conductive property are high.
From examples 8 to 9 of the present invention, when silver in the spherical modified filler accounts for 10 to 20% of the total mass of the spherical modified filler, it has high heat conductive property and high electric conductive property.
As can be seen from comparative examples 1 to 3, when no spherical modified filler or no flake silver powder is added to the system, both the electric conductivity and the heat conductivity are lowered, and the requirements are not satisfied.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (9)
1. The pouring sealant is characterized by comprising a component A and a component B, wherein the component A comprises the following components in parts by weight: 25-40 parts of epoxy resin; 3-5 parts of diluent; 30-50 parts of spherical modified filler; 15-50 parts of flake silver powder; the component B comprises the following components in parts by weight: 30-40 parts of curing agent; 0.05 to 0.1 part of curing accelerator;
the spherical modified filler comprises a glass powder core body, and a graphene layer and a silver deposition layer which are sequentially coated on the glass powder core body.
2. The pouring sealant according to claim 1, wherein the mass ratio of the spherical modified filler to the plate-like silver powder is 1: (0.5-1).
3. The pouring sealant according to claim 1, wherein the mass of the silver deposit layer accounts for 10-20% of the total mass of the spherically modified filler.
4. The pouring sealant according to claim 1, wherein the diluent comprises at least one of polypropylene glycol diglycidyl ether, cyclohexanediol diglycidyl ether, diethylene glycol diglycidyl ether, or neopentyl glycol diglycidyl ether.
5. The casting glue of claim 1, wherein the epoxy resin comprises bisphenol a epoxy resin.
6. The pouring sealant according to claim 1, wherein the curing agent comprises at least one of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, methyl nadic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride.
7. The pouring sealant according to claim 1, wherein the curing accelerator comprises at least one of DMP-30, N-dimethylbenzylamine, 2-methylimidazole, 2-ethyl-4-methylimidazole.
8. The method for preparing the pouring sealant according to any one of claims 1 to 7, comprising the steps of:
s1, uniformly mixing epoxy resin, a diluent, spherical modified filler and flake silver powder to obtain a component A;
s2, uniformly mixing the curing agent and the curing accelerator to obtain the component B.
9. An electronic component, characterized in that potting is performed by using the potting adhesive according to any one of claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210098546.XA CN114456757B (en) | 2022-01-27 | 2022-01-27 | Pouring sealant and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210098546.XA CN114456757B (en) | 2022-01-27 | 2022-01-27 | Pouring sealant and preparation method and application thereof |
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| CN114456757A CN114456757A (en) | 2022-05-10 |
| CN114456757B true CN114456757B (en) | 2023-10-17 |
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Citations (7)
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|---|---|---|---|---|
| CN103160232A (en) * | 2013-03-31 | 2013-06-19 | 广东普赛特电子科技股份有限公司 | Pouring sealant containing modified magnesium powder and preparation method of pouring sealant |
| CN105368362A (en) * | 2015-11-23 | 2016-03-02 | 苏州盖德精细材料有限公司 | Two-component epoxy resin pouring sealant and preparation method thereof |
| CN108018010A (en) * | 2017-10-27 | 2018-05-11 | 什邡市太丰新型阻燃剂有限责任公司 | A kind of high thermal conductivity, no halogen expandable flame retardant epoxy resin embedding adhesive and preparation method thereof |
| CN109192357A (en) * | 2018-09-07 | 2019-01-11 | 储军 | graphene composite conductive silver paste |
| CN110590167A (en) * | 2019-09-30 | 2019-12-20 | 湖南诺尔得材料科技有限公司 | Preparation method and application of hybrid glass powder |
| CN110706842A (en) * | 2019-09-30 | 2020-01-17 | 湖南诺尔得材料科技有限公司 | Front silver paste and preparation method thereof |
| CN111944469A (en) * | 2020-07-28 | 2020-11-17 | 湖南创瑾科技有限公司 | High-flame-retardance epoxy resin pouring sealant, and preparation method and application thereof |
-
2022
- 2022-01-27 CN CN202210098546.XA patent/CN114456757B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103160232A (en) * | 2013-03-31 | 2013-06-19 | 广东普赛特电子科技股份有限公司 | Pouring sealant containing modified magnesium powder and preparation method of pouring sealant |
| CN105368362A (en) * | 2015-11-23 | 2016-03-02 | 苏州盖德精细材料有限公司 | Two-component epoxy resin pouring sealant and preparation method thereof |
| CN108018010A (en) * | 2017-10-27 | 2018-05-11 | 什邡市太丰新型阻燃剂有限责任公司 | A kind of high thermal conductivity, no halogen expandable flame retardant epoxy resin embedding adhesive and preparation method thereof |
| CN109192357A (en) * | 2018-09-07 | 2019-01-11 | 储军 | graphene composite conductive silver paste |
| CN110590167A (en) * | 2019-09-30 | 2019-12-20 | 湖南诺尔得材料科技有限公司 | Preparation method and application of hybrid glass powder |
| CN110706842A (en) * | 2019-09-30 | 2020-01-17 | 湖南诺尔得材料科技有限公司 | Front silver paste and preparation method thereof |
| CN111944469A (en) * | 2020-07-28 | 2020-11-17 | 湖南创瑾科技有限公司 | High-flame-retardance epoxy resin pouring sealant, and preparation method and application thereof |
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