CN116102986A - Composite anisotropic conductive film for 5G millimeter wave antenna communication module and preparation method thereof - Google Patents
Composite anisotropic conductive film for 5G millimeter wave antenna communication module and preparation method thereof Download PDFInfo
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- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
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- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/16—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the structure of the carrier layer
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/314—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive layer and/or the carrier being conductive
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
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Abstract
The invention relates to the field of new materials, in particular to a composite anisotropic conductive film for a 5G millimeter wave antenna communication module and a preparation method thereof. The adhesive film has the advantages that a plurality of adhesive compound systems are adopted, special-shaped particles with different shapes, wherein continuous carbon nanotubes are distributed on the surfaces of the special-shaped particles under different temperature conditions, are used as conductive particles, the bonding process range of the obtained anisotropic conductive adhesive film is wider, the adhesive force is reliable, the low on-resistance stability performance can be realized according to the bonding requirements of the surfaces of different materials, and the adhesive film can be suitable for some severe environments of different 5G modules in the actual use process and the working environment of the components.
Description
Technical Field
The invention relates to the field of new materials, in particular to a composite anisotropic electro-adhesive film for a 5G millimeter wave antenna communication module and a preparation method thereof.
Background
Along with the development of 5G mobile phones, the development of 5G millimeter wave small-sized base stations in the design of wireless access systems and front-end modules is driven, and great opportunities and challenges are faced in the development and verification of 5G millimeter wave front-end modules in the future: how to realize the integration of the intelligent antenna, and the miniaturization, cost and performance optimization of the radio frequency front end will put higher and higher requirements on the design of the electronic equipment. At present, an LDS and an FPC antenna are mainly adopted by the smart phone, and the size of the antenna is sharply reduced in the millimeter wave range due to the great improvement of the 5G frequency. The design of electronic equipment also tends to be miniaturized and refined more and more, the arrangement of internal components of the equipment is more precise, the reserved bonding area is gradually reduced, and the complicated design requires more excellent grounding and shielding schemes. Therefore, there is a need to develop new generation of conductive paste series solutions.
The system of the conductive adhesive film disclosed at present mainly concentrates an epoxy system, and the adopted conductive particles are basically spherical particles, so that many problems such as poor adhesion, unstable on-resistance and the like exist, and the stability and the service life of the 5G millimeter wave antenna communication module are affected. Therefore, it is urgent to develop a composite anisotropic conductive film for a 5G millimeter wave antenna communication module.
Disclosure of Invention
The invention discloses a conductive adhesive system, which adopts a plurality of adhesive compound systems, and takes special-shaped particles with different shapes derived under different temperature conditions as conductive particles to prepare a composite anisotropic conductive adhesive film for a 5G millimeter wave antenna communication module. The conductive adhesive film realizes a wider temperature and pressure construction range, the processing temperature is about 85-350 ℃, the pressure is 50-600N, the requirement of a wide process is met, and the bonding of various base materials such as aluminum alloy, stainless steel, titanium alloy, copper foil, nano carbon copper film and the like is met.
The invention aims to solve the following technical problems: aiming at the bonding requirements of the surfaces of different materials, such as titanium alloy, copper foil base materials or base materials of stainless steel parts and the like, the conductive adhesive film can realize the performances of reliable adhesive force, low on-resistance and stability. The bonding process under the conditions of 85-350 ℃ and 50-600N is realized, the requirements of different structure applications of the 5G module can be met, the intelligent antenna integration is realized, and the miniaturization, cost and performance optimization of the radio frequency front end are realized.
The invention provides a composite anisotropic conductive film for a 5G millimeter wave antenna communication module.
The conductive adhesive film layer comprises the following components in parts by weight:
according to the conductive adhesive film, the selected resin base material is a mixed system of the silicon-based adhesive and the acrylic adhesive in any proportion, and the specific mixing proportion is adjusted according to the bonding temperature.
The silicon-based adhesive is a cross-linked polymer based on silane-terminated polyether, is odorless, and mainly has a curing mode of hydrolysis, dealcoholization and condensation with moisture in air in the process of sizing and can realize the adhesion among various base materials. Such as 609-PC, primer607C, primer608, 712-PC, primer607B.F, etc. may be used.
Acrylate adhesives such as perfluorohexyl ethyl methacrylate, perfluoroalkyl ethyl acrylate, and the like.
The special-shaped conductive particles are metal-organic framework polymers, metal oxides or alloy oxides of different metal sources which are derived under different temperatures or different atmosphere conditions, and the like. The conductive particles prepared by the method have strong structural designability, the material has a porous structure, and the conductive particles are also used for preparing the anisotropic conductive adhesive film for the first time, and the derived conductive particles have higher structural flexibility in the use process, can cope with the complex environment of the conductive adhesive film in the use process, and improve the reliability of the conductive adhesive film.
The special-shaped conductive particles mainly comprise spherical shapes, irregular cubes and rod shapes, and continuous carbon nanotubes are distributed on the surfaces of the special-shaped conductive particles. The irregular shape of the conductive material is in the resin matrix, and when the conductive material is subjected to dispersion filling, a stable continuous conductive path can be formed, and a stable binding force can be formed between the conductive material and the base material. The irregular structural characteristics of the adhesive form a cross-linked network-like stable structure in the conductive adhesive film. Stable conductive paths can be formed in the conductive adhesive film.
The preparation method of the special-shaped conductive particles comprises the following steps:
(1) Weighing a certain amount of metal salt and organic ligand respectively, dissolving the metal salt and the organic ligand in a solvent respectively, and dissolving the metal salt and the organic ligand respectively by ultrasonic; slowly adding the solution containing the organic ligand into the solution containing the metal salt, stirring for 10-12min, aging for 40-60min, washing with deionized water for several times, and vacuum drying to obtain solid powder, namely the metal organic framework polymer.
The metal salt can comprise nitrate, sulfate and acetate of metal elements such as Zn, fe, co, ni, ag, cd, bi, au, cu, wherein the metal salt can be single metal or multi-metal for compounding, and the compounding proportion is not limited.
The organic ligand is imidazole and benzoic acid compounds, mainly 2-methylimidazole, 3', 5' -biphenyl tetracarboxylic acid and ethynyl biphenyl-3, 3',5,5' -tetracarboxylic acid, 1, 2-tetra (4-carboxyphenyl) ethylene, terphenyl-3, 3', 5' -tetracarboxylic acid, 1,2,4, 5-tetra (4-carboxyphenyl) benzene, 3,4', 5-biphenyltricarboxylic acid, 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine, and the like.
Wherein the molar ratio of the metal salt to the organic ligand is between 1:1 and 1:12.
(2) And (3) derivatizing the metal organic framework polymer prepared in the first step under the condition of nitrogen or argon to obtain the special-shaped conductive particles with different morphologies.
The derivative process comprises the following steps: the temperature is 400-600 ℃, and the heat preservation is carried out for 2-4 hours.
(3) And (3) carrying out activation treatment on the special-shaped conductive particles prepared in the second step, wherein the activating agent is 1-5 mMol/L of potassium hydroxide or sodium hydroxide aqueous solution, soaking for 12-24h, centrifuging and washing to obtain the final special-shaped conductive particles.
The surfactant is a fluorine-containing surfactant, can effectively improve the surface tension of a conductive adhesive film system, and can also strengthen the wetting, dispersing, leveling and improving the adhesive property between conductive particles and different base materials in the adhesive film system. Common are Zonyl FSG, 8857A, capsule FS-22.
The leveling agent is mainly used for enabling the conductive adhesive film to form a layer of even, smooth and uniform adhesive film layer on the surface of the base material in the curing process. Effectively reduces the surface tension between the adhesive film and the base material. The main components are organic silicon for compounding, including polyether polyester modified organic siloxane and alkyl modified organic siloxane. The polyether polyester modified organosiloxane is mainly based on a comb structure, can form an interlocking firm structure with the structure of the conductive particles, and is preferably 1000-150000 in molecular weight according to different molecular weights, so that the conductive adhesive film is endowed with excellent temperature resistance. Such as 1070, 1071, 1080, 1090, etc. The alkyl modified organosiloxane has smaller molecular weight, and can make up the defect of poor thermal stability of the polyether polyester modified organosiloxane in the actual use process, wherein the polyether polyester modified organosiloxane is 1073, 1074 and the like.
Curing agents are a class of substances or mixtures that enhance or control the curing reaction. The resin curing is a process of irreversibly changing the thermosetting resin through chemical reactions such as condensation, ring closure, addition or catalysis. The type of curing agent has great influence on the performance of the adhesive film, such as thermal stability, conductive stability and the like. Therefore, the invention adopts the curing agent for compound use, so that the adhesive film meets the use requirement of a wider 5G module. Peroxides such as benzoyl peroxide, cumene hydroperoxide and tert-butyl hydroperoxide are mainly adopted, and the intermediate double bond of the methacrylate in the acrylic resin is subjected to bond opening reaction to form a three-dimensional cross-linked structure (curing).
The structure for the 5G millimeter wave antenna communication module is that the outer layer is a glue layer protection layer, the next layer is a metal thin layer, the next layer is a copper foil, and the innermost layer is a conductive glue film layer.
The conductive adhesive film adopts a plurality of adhesive compound systems, and special-shaped particles with different shapes are derived under different temperature conditions to serve as conductive particles, so that the composite anisotropic conductive film for the 5G millimeter wave antenna communication module is prepared. The conductive adhesive film realizes a wider temperature and pressure construction range, the processing temperature is about 85-350 ℃, the pressure is 50-600N, and the bonding of various base materials such as aluminum alloy, stainless steel, titanium alloy, copper foil, nano carbon copper film and the like is met by the requirement of a wide process.
Drawings
FIG. 1 is a graph showing the morphology of the shaped conductive particles prepared in examples 1-6 of the present invention.
Fig. 2 is a morphology diagram of the shaped conductive particles prepared in example 7 of the present invention.
Fig. 3 is a morphology diagram of the shaped conductive particles prepared in example 8 of the present invention.
Detailed Description
In order to more clearly illustrate the present disclosure, the present invention will be described in detail with reference to examples.
Volume resistivity test: the volume resistivity is an important evaluation index of the conductive adhesive film, and a direct measurement method is adopted for testing.
Shear strength test: the shear strength of the conductive adhesive film was measured by referring to GB/T7124-2008 "measurement of tensile shear Strength of adhesive".
Thermal conductivity testing: the thermal conductivity of the conductive adhesive film was tested with reference to ASTM E1461-07 method for testing thermal diffusivity and thermal conductivity by flash method.
The preparation method of the special-shaped conductive particles comprises the following steps:
(1) The metal salt (see table 2) and the organic ligand (see table 2) (the molar ratio of the two is see table 2) are respectively weighed, and are completely dissolved in deionized water, and ultrasonic is completely dissolved; slowly adding the aqueous solution containing the organic ligand into the aqueous solution containing the metal salt, stirring for 10min, aging for 40min, washing with deionized water, and vacuum drying to obtain purple powder, namely the metal organic framework polymer.
(2) And (3) derivatizing the metal organic framework polymer prepared in the first step under the nitrogen condition to obtain the special-shaped conductive particles. The derivatization conditions are shown in Table 2.
(3) And (3) carrying out activation treatment (see table 2 in detail) on the special-shaped conductive particles prepared in the second step, soaking for 12 hours, centrifuging and washing to obtain the final special-shaped conductive particles.
The composition of the conductive adhesive film is shown in Table 1.
The specific formulations of examples 1-8 and comparative examples 1-4 are shown in Table 1.
Table 1 specific formulations of examples 1-8 and comparative examples 1-4:
table 2: the formula and the derivative process of the special-shaped conductive particles are as follows:
| metal compound | Organic ligands | Molar ratio of | Derivatization temperature/. Degree.C | Atmosphere of | ||
| Example 1 | Cobalt nitrate | 2-methylimidazole | 1:2 | 400 | Nitrogen gas | 1m Mol/L KOH |
| Example 2 | Cobalt nitrate | 2-methylimidazole | 1:2 | 400 | Nitrogen gas | 5m Mol/L KOH |
| Example 3 | Cobalt nitrate | 2-methylimidazole | 1:2 | 400 | Nitrogen gas | 1m Mol/L KOH |
| Example 4 | Cobalt nitrate | 2-methylimidazole | 1:2 | 400 | Nitrogen gas | 1m Mol/L KOH |
| Example 5 | Cobalt nitrate | 2-methylimidazole | 1:2 | 400 | Nitrogen gas | 1m Mol/L KOH |
| Example 6 | Cobalt nitrate | 2-methylimidazole | 1:2 | 400 | Nitrogen gas | 1m Mol/L KOH |
| Example 7 | Cobalt nitrate/nickel nitrate (1:1) | 2-methylimidazole | 1:2 | 400 | Nitrogen gas | 1m Mol/L KOH |
| Example 8 | Cobalt nitrate | 2-methylimidazole | 1:2 | 500 | Nitrogen gas | 1m Mol/L KOH |
| Comparative example 1 | Cobalt nitrate | 2-methylimidazole | 1:2 | 400 | Nitrogen gas | 1m Mol/L KOH |
| Comparative example 2 | Cobalt nitrate | 2-methylimidazole | 1:2 | 400 | Nitrogen gas | 1m Mol/L KOH |
| Comparative example 3 | Cobalt nitrate | 2-methylimidazole | 1:2 | 400 | Nitrogen gas | Without any means for |
| Comparative example 4 | Micron silver particles |
Table 3: performance test of examples 1-8 and comparative examples 1-4:
Claims (10)
1. a composite anisotropic conductive film is characterized in that: the composite anisotropic conductive adhesive film comprises the following components in parts by weight:
2. the composite anisotropic conductive film of claim 1, wherein: the silicon-based adhesive is 609-PC, primer607C, primer608, 712-PC or primer607B.F.
3. The composite anisotropic conductive film of claim 1, wherein: the acrylate adhesive is perfluorohexyl ethyl methacrylate or perfluoroalkyl ethyl acrylate.
4. The composite anisotropic conductive film of claim 1, wherein: the preparation method of the special-shaped conductive particles comprises the following steps:
(1) Respectively weighing metal salt and organic ligand, respectively completely dissolving the metal salt and the organic ligand in deionized water, respectively carrying out ultrasonic treatment to completely dissolve the metal salt and the organic ligand; slowly adding the aqueous solution containing the organic ligand into the aqueous solution containing the metal salt, stirring for 10-12min, aging for 40-60min, washing with deionized water, and vacuum drying to obtain purple powder, namely the metal organic framework polymer;
(2) Derivatizing the metal organic framework polymer prepared in the step (1) under the condition of nitrogen or argon to obtain special-shaped conductive particles with different morphologies;
(3) And (3) carrying out activation treatment, centrifugation and washing on the special-shaped conductive particles with different shapes prepared in the step (2) to obtain the final special-shaped conductive particles.
5. The composite anisotropic conductive film of claim 4, wherein: the molar ratio of the metal salt to the organic ligand in the step (1) is 1:1-1:12.
6. the composite anisotropic conductive film of claim 4, wherein: the metal salt in the step (1) is nitrate, sulfate or acetate of Zn, fe, co, ni, ag, cd, bi, au, cu metal elements; the organic ligand is 2-methylimidazole, 3', 5' -biphenyl tetracarboxylic acid, ethynyl biphenyl-3, 3', 5' -tetracarboxylic acid, 1, 2-tetra (4-carboxybenzene) ethylene, terphenyl-3, 3",5,5" -tetracarboxylic acid, 1,2,4, 5-tetrakis (4-carboxyphenyl) benzene, 3,4', 5-biphenyltricarboxylic acid or 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine.
7. The composite anisotropic conductive film of claim 4, wherein: and (3) the derivatization temperature in the step (2) is 500-600 ℃, and the temperature is kept for 2-4h.
8. The composite anisotropic conductive film of claim 4, wherein: the activator in the step (3) is 1-5 mMol of potassium hydroxide or sodium hydroxide aqueous solution, and the activator is soaked for 12-24h.
9. The composite anisotropic conductive film of claim 1, wherein: the surfactant is Zonyl FSG, 8857A or capstone FS-22, the leveling agent is 1070, 1071, 1080 or 1090, and the curing agent is benzoyl peroxide, cumene hydroperoxide or tert-butyl hydroperoxide.
10. The utility model provides a be used for 5G millimeter wave antenna communication module which characterized in that: the communication module is characterized in that the outer layer is a glue layer protection layer, the next layer is a metal foil layer, the next layer is a copper foil, and the innermost layer is a conductive glue film layer according to any one of claims 1-9.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102989432A (en) * | 2012-12-28 | 2013-03-27 | 南开大学 | Preparation of solid-phase microextraction (SPME) fiber and extraction device assembled by same |
| CN112521881A (en) * | 2020-11-23 | 2021-03-19 | 东莞市鸿亿导热材料有限公司 | High-thermal-conductivity graphene heat dissipation film for 5G communication equipment and preparation method thereof |
| CN113620349A (en) * | 2021-09-01 | 2021-11-09 | 合肥工业大学 | One-dimensional iron-based wave-absorbing material derived from metal organic framework and preparation method thereof |
| CN113736087A (en) * | 2021-09-13 | 2021-12-03 | 北京天山新材料技术有限公司 | Organic silicon resin and preparation method thereof, organic silicon conductive adhesive composition and organic silicon conductive adhesive |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102989432A (en) * | 2012-12-28 | 2013-03-27 | 南开大学 | Preparation of solid-phase microextraction (SPME) fiber and extraction device assembled by same |
| CN112521881A (en) * | 2020-11-23 | 2021-03-19 | 东莞市鸿亿导热材料有限公司 | High-thermal-conductivity graphene heat dissipation film for 5G communication equipment and preparation method thereof |
| CN113620349A (en) * | 2021-09-01 | 2021-11-09 | 合肥工业大学 | One-dimensional iron-based wave-absorbing material derived from metal organic framework and preparation method thereof |
| CN113736087A (en) * | 2021-09-13 | 2021-12-03 | 北京天山新材料技术有限公司 | Organic silicon resin and preparation method thereof, organic silicon conductive adhesive composition and organic silicon conductive adhesive |
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