CN110885655B - Surface insulation type electromagnetic shielding adhesive and preparation method thereof - Google Patents
Surface insulation type electromagnetic shielding adhesive and preparation method thereof Download PDFInfo
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- CN110885655B CN110885655B CN201911285688.1A CN201911285688A CN110885655B CN 110885655 B CN110885655 B CN 110885655B CN 201911285688 A CN201911285688 A CN 201911285688A CN 110885655 B CN110885655 B CN 110885655B
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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
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/04—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to rubbers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a surface insulation type electromagnetic shielding adhesive and a preparation method thereof, wherein the adhesive comprises the following components in parts by weight: the epoxy resin material comprises, by weight, 300 parts of epoxy resin, 50-150 parts of special resin, 20-80 parts of reactive diluent, 150 parts of curing agent, 10-50 parts of stabilizer, 5-20 parts of coupling agent and 800 parts of metal filler, wherein the special resin is prepared by copolymerizing two or more of acrylate, epoxy acrylate and rubber, the rubber is natural rubber or nitrile rubber, the metal filler is prepared by mixing spherical silver powder with long-chain fatty acid, grinding the mixture to 4-10 mu m particle size by using a three-roll grinder, and drying the mixture for 2-5h at the temperature of 50-70 ℃, and the metal filler accounts for 35-60% of the total mass of the raw materials. The adhesive can be cured within 1 hour at the temperature of 90-100 ℃, has good normal-temperature storage performance, can still have stable viscosity after 72 hours, has insulated surface after curing, and has good electromagnetic shielding performance.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to a surface insulation type electromagnetic shielding adhesive and a preparation method thereof.
Background
With the development of modern electronic information technology, electronic products are continuously developing towards miniaturization, portability and multi-functionalization, and further higher and higher requirements are put forward on assembly processes. Efficient, low-cost assembly solutions are an urgent appeal to every electronic product manufacturing enterprise. The adhesive product which is essential in the assembly process increasingly plays an important role, and the adhesive can not only bear components and parts and connecting circuits in the product assembly process, but also can provide the application of functions such as electric conduction, heat conduction and electromagnetic shielding.
The mobile communication technology is undergoing the spanning development from 4G to 5G, the transmission rate, the frequency, the signal intensity and the like of the smart phone in the age of 5G are obviously improved, and from a core chip to a radio frequency device, from the body material to an internal structure, the parts of the 5G smart phone are new, and the hardware innovation and the upgrade provide new requirements for the electromagnetic shielding and the heat conduction of the smart phone. Because the existing electromagnetic shielding adhesive tape on the market cannot be used in some special structures due to continuous miniaturization and light weight of equipment, the development of the electromagnetic shielding adhesive for assembling 5G communication equipment is imminent, and a low-temperature curing conductive adhesive and a preparation method thereof are provided in application No. 2019101959884 (a low-temperature curing conductive adhesive and a preparation method thereof), wherein the adhesive is cured at low temperature by adding metal fillers accounting for 65-85% of the total mass of raw materials into the raw materials, the curing temperature is 70-75 ℃, the curing is completed within 1hr, and the electronic shielding performance (100um) exceeds 55 dB. How to further improve this performance is a goal of development efforts of those skilled in the art.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the surface insulation type electromagnetic shielding adhesive which has a good electromagnetic shielding effect and can be cured within 1 hour at the temperature of not higher than 100 ℃.
In order to achieve the purpose, the invention adopts the technical scheme that: the surface insulation type electromagnetic shielding adhesive comprises the following components in parts by weight: the epoxy resin material comprises, by weight, 300 parts of epoxy resin, 50-150 parts of special resin, 20-80 parts of reactive diluent, 150 parts of curing agent, 10-50 parts of stabilizer, 5-20 parts of coupling agent and 800 parts of metal filler, wherein the special resin is prepared by copolymerizing two or more of acrylate, epoxy acrylate and rubber, the rubber is natural rubber or nitrile rubber, the metal filler is prepared by mixing spherical silver powder with long-chain fatty acid, grinding the mixture to 4-10 mu m particle size by using a three-roll grinder, and drying the mixture for 2-5h at the temperature of 50-70 ℃, and the metal filler accounts for 35-60% of the total mass of the raw materials.
In a specific embodiment, the long-chain fatty acid is a fatty acid having 12 to 15 carbon atoms.
As a specific embodiment, the special resin is formed by copolymerizing epoxy acrylate and rubber.
As a specific embodiment, the epoxy resin is selected from one or more of bisphenol a epoxy resin, bisphenol F epoxy resin, novolac epoxy resin, and resorcinol epoxy resin.
As a specific embodiment, the reactive diluent is selected from 1, 4-butanediol glycidyl ether, 1, 6-hexanediol diglycidyl ether, benzyl glycidyl ether, butyl glycidyl ether, C12-14One or more of alkyl glycidyl ether, neopentyl glycol diglycidyl ether and p-tert-butylphenyl glycidyl ether.
Here, the reactive diluent is selected from the group consisting of 1, 4-butanediol glycidyl ether, 1, 6-hexanediol diglycidyl ether, benzyl glycidyl ether, butyl glycidyl ether, C12-14One or more of alkyl glycidyl ether, neopentyl glycol diglycidyl ether and p-tert-butylphenyl glycidyl ether; the curing agent is selected from one or more of polyether amine, a composition containing polyether amine, polyamide and an addition product thereof, fatty amine and an addition product thereof, imidazole, dicyanodiamine and hydrazide; the stabilizer is selected from one or a mixture of trimethyl borate, triethyl borate, tributyl borate, p-nitrophenol and m-nitrophenol; the coupling agent is selected from one or a mixture of more of vinyl silane, amino silane, epoxy silane and mercapto silane.
The invention also aims to provide a preparation method of the surface insulation type electromagnetic shielding adhesive, which comprises the following steps:
1) mixing epoxy resin, special resin, an active diluent, a curing agent and a coupling agent according to the mass part ratio, and grinding and dispersing by adopting a three-roll grinder, wherein the temperature is controlled to be 25 +/-10 ℃ in the grinding process so as to uniformly mix the epoxy resin, the special resin, the active diluent, the curing agent and the coupling agent;
2) mixing a metal filler with the mixture obtained in the step 1), adding the mixture into a vacuum double planet, stirring at a high speed and dispersing and stirring at a speed of 1000r/min +/-50 r/min, a vacuum degree of less than 0.2MPa, controlling the temperature to be 25 +/-10 ℃, and fully stirring to obtain a semi-finished product;
3) and standing the semi-finished product at-40 deg.C for 24hr to obtain the desired adhesive.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: according to the adhesive, the special resin is introduced, the directional surface migration is formed in the curing process, the insulating property of the surface of a cured product is realized, meanwhile, a stable conductive network is formed inside, the contents of all components of the adhesive are reasonably controlled, so that all the components are mutually promoted and matched, in the process of preparing the adhesive, the temperature is always controlled to be 25 +/-10 ℃, the prepared adhesive can be cured within 1 hour at the temperature lower than 100 ℃, the normal-temperature storage performance is good, the adhesive still has stable viscosity after 72 hours, the surface is insulated after curing, and the electromagnetic shielding performance is good.
Detailed Description
The technical solution of the present invention is further illustrated below with reference to specific examples.
The metal fillers used in the following examples are commercially available spherical silver powders mixed with long-chain fatty acids, ground to 4-10um particle size using a three-roll grinder, and dried at 50-70 ℃. The long-chain fatty acid is a fatty acid having 12 to 15 carbon atoms.
Example 1
The example provides a surface insulation type electromagnetic shielding adhesive, which is composed of the following raw materials in parts by weight: 200 parts of bisphenol A epoxy resin, 100 parts of acrylate-styrene butadiene rubber copolymer, 80 parts of 1, 6-hexanediol glycidyl ether, 100 parts of polyether amine, 15 parts of triethyl borate, 6 parts of epoxy silane and 700 parts of metal filler.
Example 2
The example provides a surface insulation type electromagnetic shielding adhesive, which is composed of the following raw materials in parts by weight: 80 parts of bisphenol F epoxy resin, 80 parts of novolac epoxy resin, 80 parts of epoxy acrylate and natural rubber copolymer, 30 parts of 1,6 hexanediol glycidyl ether, 130 parts of polyamide and addition product thereof, 30 parts of triethyl borate, 10 parts of epoxy silane and 650 parts of metal filler.
Example 3
The example provides a surface insulation type electromagnetic shielding adhesive, which is composed of the following raw materials in parts by weight: 100 parts of bisphenol F epoxy resin, 200 parts of novolac epoxy resin, 150 parts of epoxy acrylate and natural rubber copolymer, 20 parts of 1, 4-butanediol glycidyl ether, 80 parts of polyether amine, 20 parts of a composition containing the polyether amine, 30 parts of imidazole, 50 parts of triethyl borate, 5 parts of vinyl silane and 500 parts of metal filler.
Example 4
The example provides a surface insulation type electromagnetic shielding adhesive, which is composed of the following raw materials in parts by weight: 100 parts of phenolic epoxy resin, 50 parts of epoxy acrylate and styrene butadiene rubber copolymer, 25 parts of benzyl glycidyl ether, 80 parts of aliphatic amine and addition product thereof, 30 parts of dicyandiamide, 10 parts of p-nitrophenol, 5 parts of epoxy silane and 350 parts of metal filler.
Comparative example 1
The example provides a conductive adhesive which is composed of the following raw materials in parts by mass: 300 parts of bisphenol F epoxy resin, 180 parts of 1, 4-butanediol glycidyl ether, 10 parts of dicyanodiamine, 20 parts of hydrazide, 10 parts of trimethyl borate, 10 parts of vinyl silane and 900 parts of metal filler.
Comparative example 2
The example provides a surface insulation type electromagnetic shielding adhesive, which is composed of the following raw materials in parts by weight: 300 parts of bisphenol A epoxy resin, 100 parts of 1,6 hexanediol glycidyl ether, 120 parts of polyetheramine, 30 parts of triethyl borate, 20 parts of epoxy silane and 300 parts of metal filler.
Here, there is also provided a surface insulation type electromagnetic shielding adhesive, which is prepared by using the formulations in examples 1 to 4, and the specific preparation process is as follows:
1) mixing epoxy resin, special resin, an active diluent, a curing agent and a coupling agent according to the mass part ratio, and grinding and dispersing by adopting a three-roll grinder, wherein the temperature is controlled to be 25 +/-10 ℃ in the grinding process so as to uniformly mix the epoxy resin, the special resin, the active diluent, the curing agent and the coupling agent;
2) mixing a metal filler with the mixture obtained in the step 1), adding the mixture into a vacuum double planet, stirring at a high speed and dispersing and stirring at a speed of 1000r/min +/-50 r/min, a vacuum degree of less than 0.2MPa, controlling the temperature to be 25 +/-10 ℃, and fully stirring to obtain a semi-finished product;
3) and standing the semi-finished product at-40 deg.C for 24hr to obtain the desired adhesive.
The adhesives prepared by the above preparation method in combination with the formulations of examples 1 to 4 and comparative example were subjected to performance tests, and the test results are shown in table 1.
And (4) testing standard:
(II) resistivity: four-probe resistance tester
Viscosity test: the Bohler-Fei HBTVV 2TCP cone-plate viscometer is adopted to test at 25 DEG C
(III) electromagnetic shielding: agilent E5071C (100M-8.5GHz)
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | |
| Viscosity cps at 25 deg.C/4 hr | 25000 | 25000 | 20000 | 30000 | 18000 | 14000 |
| Viscosity cps at 25 deg.C/72 hr | 24000 | 24000 | 20000 | 31000 | 18000 | 14000 |
| Thixotropic property | 4 | 4 | 4 | 4 | 6 | 5 |
| Curing conditions | 90℃*1hr | 100℃*1hr | 100℃*1hr | 100℃*1hr | 75℃*1hr | 70℃*1hr |
| Surface volume resistivity omega cm | ＞4*104 | ＞4*104 | ＞4*104 | ＞4*104 | 0.1 | ＞4*104 |
| Thickness um of insulating layer | 10 | 15 | 20 | 30 | - | - |
| Internal volume resistivity Ω. cm | 0.1 | 0.5 | 0.8 | 1.0 | 0.1 | ＞4*104 |
| Electromagnetic shielding dB (300um) | 20 | 18 | 15 | 15 | 30 | 0 |
As can be seen from table 1, the adhesives prepared by the formulations of examples 1 to 4 according to the above method can be cured at a low temperature and for 1 hour, and the cured adhesives have insulated surfaces and form a stable conductive network inside, so as to achieve a good electromagnetic shielding effect, and particularly, the formulations of example 1 have optimal properties, and compared with comparative examples, the adhesives have good internal volume resistivity and better electromagnetic shielding performance, and as can be seen from comparative example 2, if the addition amount of the metal filler is too low, the adhesives do not have electromagnetic shielding performance; from the comparison of the comparative example with the examples, it can be seen that the addition of the special resin while adjusting the proportion of the metal filler enables the curing conditions of the adhesive to be more excellent.
According to the adhesive, the special resin is introduced, the metal filler is prepared by mixing the spherical silver powder with the long-chain fatty acid, so that the prepared adhesive has good internal conductivity while the surface is insulated, the contents of all the components are reasonably controlled to mutually promote and jointly cooperate, in the process of preparing the adhesive, the temperature is always controlled to be 25 +/-10 ℃, so that the prepared adhesive can be cured within 1 hour at the temperature of 90-100 ℃, and meanwhile, the adhesive also has good normal-temperature storage performance, and has good viscosity, electromagnetic shielding performance and thixotropic performance after 72 hours.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (4)
1. The surface insulation type electromagnetic shielding adhesive is characterized by comprising the following components in parts by weight: the epoxy resin comprises, by weight, 300 parts of epoxy resin, 50-150 parts of special resin, 20-80 parts of reactive diluent, 150 parts of curing agent, 10-50 parts of stabilizing agent, 5-20 parts of coupling agent and 800 parts of metal filler, wherein the special resin adopts any one of acrylate and styrene-butadiene rubber copolymer, epoxy acrylate and natural rubber copolymer and epoxy acrylate and styrene-butadiene rubber copolymer, the metal filler is prepared by mixing spherical silver powder with long-chain fatty acid, grinding the mixture to 4-10 mu m particle size by using a three-roll grinder, and drying the mixture for 2-5h at the temperature of 50-70 ℃, the metal filler accounts for 35-60% of the total mass of the raw materials, and the long-chain fatty acid is fatty acid with 12-15 carbon atoms.
2. The surface-insulating electromagnetic shielding adhesive according to claim 1, wherein the epoxy resin is selected from one or more of bisphenol a epoxy resin, bisphenol F epoxy resin, novolac epoxy resin and resorcinol epoxy resin.
3. The surface insulation type electromagnetic shielding adhesive according to claim 1, wherein the reactive diluent is selected from 1, 4-butanediol glycidyl ether, 1, 6-hexanediol diglycidyl ether, benzyl glycidyl ether, butyl glycidyl ether, C12-14One or more of alkyl glycidyl ether, neopentyl glycol diglycidyl ether and p-tert-butylphenyl glycidyl ether.
4. A method for preparing the surface insulation type electromagnetic shielding adhesive according to any one of claims 1 to 3, comprising the steps of:
1) mixing epoxy resin, special resin, an active diluent, a curing agent and a coupling agent according to the mass part ratio, and grinding and dispersing by adopting a three-roll grinder, wherein the temperature is controlled to be 25 +/-10 ℃ in the grinding process so as to uniformly mix the epoxy resin, the special resin, the active diluent, the curing agent and the coupling agent;
2) mixing a metal filler with the mixture obtained in the step 1), adding the mixture into a vacuum double-planet stirrer for high-speed dispersion stirring, wherein the stirring speed is 1000r/min +/-50 r/min, the vacuum degree is less than 0.2MPa, the temperature is controlled to be 25 +/-10 ℃, and fully stirring to obtain a semi-finished product;
3) and standing the semi-finished product for 24 hours at the temperature of-40 ℃ to obtain the required adhesive finished product.
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| CN201911285688.1A CN110885655B (en) | 2019-12-13 | 2019-12-13 | Surface insulation type electromagnetic shielding adhesive and preparation method thereof |
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| CN110885655B true CN110885655B (en) | 2021-09-03 |
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| CN102719199A (en) * | 2012-04-23 | 2012-10-10 | 苏州异导光电材料科技有限公司 | Preparation method of three-dimensional anisotropic conductive film |
| CN104968746A (en) * | 2012-12-27 | 2015-10-07 | 学校法人关西大学 | Thermally-conductive, electrically-conductive adhesive composition |
| CN106961826A (en) * | 2017-03-27 | 2017-07-18 | 保定乐凯新材料股份有限公司 | The electromagnetic wave proof film that a kind of repeatable attachment is used |
| CN208609256U (en) * | 2017-07-20 | 2019-03-15 | 信越聚合物株式会社 | The printed circuit board of electromagnetic shielding film and charged magnetic shielding film |
| KR20190054024A (en) * | 2017-11-11 | 2019-05-21 | 이종영 | Composition that combines Electromagnetic wave absorption, electromagnetic interference, antistatic, flame resistance, non-combustibility, antimicrobial, antifungal, anti-condensation, anti-foaming and applications using the composition |
-
2019
- 2019-12-13 CN CN201911285688.1A patent/CN110885655B/en active Active
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| CN102719199A (en) * | 2012-04-23 | 2012-10-10 | 苏州异导光电材料科技有限公司 | Preparation method of three-dimensional anisotropic conductive film |
| CN104968746A (en) * | 2012-12-27 | 2015-10-07 | 学校法人关西大学 | Thermally-conductive, electrically-conductive adhesive composition |
| CN106961826A (en) * | 2017-03-27 | 2017-07-18 | 保定乐凯新材料股份有限公司 | The electromagnetic wave proof film that a kind of repeatable attachment is used |
| CN208609256U (en) * | 2017-07-20 | 2019-03-15 | 信越聚合物株式会社 | The printed circuit board of electromagnetic shielding film and charged magnetic shielding film |
| KR20190054024A (en) * | 2017-11-11 | 2019-05-21 | 이종영 | Composition that combines Electromagnetic wave absorption, electromagnetic interference, antistatic, flame resistance, non-combustibility, antimicrobial, antifungal, anti-condensation, anti-foaming and applications using the composition |
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| 各向异性导电胶粘剂膜的制备及其性能研究;黎文部等;《功能材料》;20080120(第01期);第57-63页 * |
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