CN105086873A - Isotropous thermosetting conductive adhesive film and preparation method thereof - Google Patents
Isotropous thermosetting conductive adhesive film and preparation method thereof Download PDFInfo
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- CN105086873A CN105086873A CN201510481199.9A CN201510481199A CN105086873A CN 105086873 A CN105086873 A CN 105086873A CN 201510481199 A CN201510481199 A CN 201510481199A CN 105086873 A CN105086873 A CN 105086873A
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- conductive adhesive
- adhesive film
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Abstract
The invention relates to isotropous thermosetting conductive adhesive film and a preparation method thereof. A thermosetting conductive adhesive is composed of, by weight, 3%-5% of polyester resin, 4%-7% of hydroxy acrylic resin, 2.5%-6% of epoxy resin, 12%-19.5% of conducting media, 0.1%-0.5% of thixotropic agents and 62%-77.7% of solvent. The preparation method of the adhesive film comprises the steps that a release liner is coated with the prepared thermosetting conductive adhesive liquid, the temperature of a drying channel is controlled to be 80 DEG C to 120 DEG C, coating speed ranges from 10 m/min to 15 m/min, the thickness of the adhesive ranges from 25 microns to 30 microns, and the isotropous thermosetting conductive adhesive film is obtained by attaching the release liner to the thermosetting conductive adhesive film in the winding process. The conductive adhesive film is good in conductivity, small in resistance change rate, large in peeling strength and good in operating performance, and can be stored for more than 30 days at room temperature.
Description
Technical field
The present invention relates to a kind of thermoset conductive adhesive film, be specifically related to a kind of isotropy thermoset conductive adhesive film and preparation method thereof.This conductive adhesive film is applied to consumption electronic products as smart mobile phone, panel computer, and the parts such as camera module, liquid-crystal display module of digital camera, belong to electronic chemical product field.
Background technology
Thermoset conductive adhesive film be a kind of be heating and curing under certain temperature condition after there is the thermosetting glued membrane of certain conductivity, it is main moiety with matrix resin and conducting medium and conducting particles usually, by the bonding effect of matrix resin, conducting particles medium is sticked together formation conductive path, the conduction realized by gluing material connects.Conductive adhesive film comprises two large class, isotropic conductive adhesive film (ICA) and anisotropic conductive films (ACA).ICA refers to the glued membrane that all directions are all conducted electricity; ACA then refers in one direction as Z-direction conduction, and at X and the nonconducting glued membrane of Y-direction.Conductive adhesive film is widely used in the fields such as electronic devices and components, circuit card assembling, liquid-crystal display and lighting industry, communication, automotive electronics, smart card, RF identification, electronic tag.
Chinese patent CN104017511A discloses a kind of preparation method of epoxide resin conductive adhesive film, but matrix resin only adopts epoxy resin in the formula of this conductive adhesive film, the surface viscosity of this glued membrane is very poor, when glued membrane needs when downstream client uses to add heat fixation with flatiron, once occur that contraposition is bad, all right causing is scrapped, and causes consumer product condemnation factor higher.And containing very large materials of toxicity such as polythiol, polymeric amide, formaldehyde in glued membrane formula, in production and use procedure, all can bring harm to work human and environment.This conductive adhesive film generally will could keep necessarily overflowing glue amount through semicure thermal treatment in addition, and the normal temperature shelf-time is general only less than 10 days, but also apt to deteriorately scraps.
Summary of the invention
The object of this invention is to provide a kind of thermoset conductive resin, isotropy thermoset conductive adhesive film and preparation method thereof.This conductive adhesive film has good conductivity, and resistance change rate is little, and stripping strength is large, technique is simple, good operation performance, good stability, and the shelf-time is long, and room temperature can deposit more than 30 days.
For achieving the above object, the technical solution used in the present invention is:
A kind of thermoset conductive resin, by weight percentage, comprises following component:
By such scheme, described Hydroxylated acrylic resin is white or light yellow, and solid content is 60 ~ 70wt%, and hydroxy radical content is 2 ~ 5wt%.The BS-8070 acrylic resin that available acrylic resin has Boshan light industry laboratory to produce.
By such scheme, in described vibrin, optional polyester has: one or more the mixture in polyester 7908, polyester 3550 and polyester 560.Wherein polyester 7908, polyester 3550 are that precious sharp Bond produces, and polyester 560 spins production for Japan.
By such scheme, described epoxy resin is preferably bisphenol A type epoxy resin, wherein: the epoxy equivalent (weight) of liquid-state epoxy resin is 180 ~ 215g/mol, and viscosity is 8000 ~ 15000mPa.s; The epoxy equivalent (weight) of solid epoxy resin is 450 ~ 1000g/mol, and softening temperature is 60 ~ 102 DEG C.Solid epoxy resin and liquid-state epoxy resin are preferably combined into enforcement use by the epoxy resin in the present invention, CYD-014 and CYD-128 as Hunan Ba Ling petrochemical industry epoxy resin company limited produced is used in combination.
By such scheme, described conducting medium is the mixture of several conducting mediums in the silver-bearing copper powder of copper powder, nickel powder, argentiferous 10%.
By such scheme, described thixotropic agent is aerosil.
By such scheme, the median size of described aerosil is 0.5-2 μm, is preferably 0.7-1.0 μm.
By such scheme, described solvent is the mixture of two kinds or more solvents in ethyl acetate, butanone, butylacetate, toluene.
The preparation method of thermoset conductive resin: use dissolution with solvents vibrin, conducting medium is added after dissolving, load in the milling tank of high speed ball mill, high speed dispersion is poured in mix and blend tank after milling and filtering, slowly add the Hydroxylated acrylic resin of formula metering, epoxy resin and thixotropic agent, namely uniform stirring obtains thermoset conductive resin glue.
By such scheme, described high speed dispersion grinding time is 60 ~ 90 minutes, and described being filtered into is filtered with 200-300 mesh filter screen.
By such scheme, described churning time is 20-24h.
Isotropy thermoset conductive adhesive film, is made up of release film and the isotropy thermoset conductive adhesive layer be coated on release film.
The preparation method of isotropy thermoset conductive adhesive film, at release film as BOPP film, PET film etc. applied above-mentioned obtained thermoset conductive resin glue, controlling drying tunnel temperature is 80 DEG C ~ 120 DEG C, coating speed is 10 ~ 15m/min, glue is thick is 25 ~ 30 μm, to fit on thermoset conductive resin glued membrane during rolling release film, be namely prepared into thermoset conductive adhesive film.
The present invention coordinates acrylic resin to use by epoxy resin, in a heated condition epoxy resin can with hydroxyl reaction in acrylic resin, play curing cross-linked effect, strengthen glued membrane stripping strength, coordinate the use of polyester also can increase the surface viscosity of glued membrane simultaneously, in addition the acrylic resin that uses of the present invention for Primary resins also controlled glue film there is stable glue amount of overflowing, a kind of conductive adhesive film of high comprehensive performance that coordinated the interpolation of the interpolation of conducting medium and a small amount of thixotropic agent finally to prepare on this basis again.This conductive adhesive film possesses and has good conductivity, and resistance change rate is little, and stripping strength is large, technique is simple, good operation performance, good stability, and the shelf-time is long, and room temperature can deposit more than 30 days.
Accompanying drawing explanation
Fig. 1 is contact resistance test schematic diagram;
Fig. 2 is connection resistance test schematic diagram.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.Involved by the process for preparation of thermoset conductive resin in the following embodiments, each component consumption is with reference to subordinate list 1.
Embodiment 1
With reference to the formulation ratio of embodiment 1 in subordinate list 1, take the dissolution with solvents vibrin of formula, conducting medium is added after dissolving, load in the milling tank of high speed ball mill, high speed dispersion and milling 60 ~ 90 minutes, pours in mix and blend tank after filtering, slowly add the acrylic resin of formula metering, epoxy resin and thixotropic agent with 300 mesh filter screen, uniform stirring 20 ~ 24 hours again, obtains thermoset conductive resin glue.
Thermoset conductive resin glue obtained in coating step a in BOPP film, controlling drying tunnel temperature is 80 DEG C ~ 120 DEG C, and coating speed is 10 ~ 15m/min, and glue is thick is 25 ~ 30 μm, to fit on thermoset conductive resin glued membrane during rolling release film, be namely prepared into thermoset conductive adhesive film.Carry out performance test.The test performance of sample sees attached list 2.Under testing method is shown in.
Embodiment 2
According to the formulation ratio with reference to embodiment 2 in subordinate list 1, according to joining glue, film and sample preparation way preparation test sample in embodiment 1, the test performance of sample sees attached list 2.
Embodiment 3
According to the formulation ratio with reference to embodiment 3 in subordinate list 1, according to joining glue, film and sample preparation way preparation test sample in embodiment 1, the test performance of sample sees attached list 2.
Embodiment 4
According to the formulation ratio with reference to embodiment 4 in subordinate list 1, according to joining glue, film and sample preparation way preparation test sample in embodiment 1, the test performance of sample sees attached list 2.
Embodiment 5
According to the formulation ratio with reference to embodiment 5 in subordinate list 1, according to joining glue, film and sample preparation way preparation test sample in embodiment 1, the test performance of sample sees attached list 2.
Table 1: the formula constituent table of thermoset conductive resin
Table 2: the performance test table of conductive adhesive film test sample
Each performance test methods is as follows:
(1) conductive adhesive film contact resistance testing method:
First use the circular hole that die-cut for 13umPI film diameter is 1.0mm by punch tool, by on the PI film after conductive adhesive film sample composite transferring to punching, two-layer all use is greater than aperture but the 35um electrolytic copper foil light face attaching being less than PI film up and down, afterwards sample is placed in fast press with 175 DEG C, hot pressing 120s under 90Mpa pressure condition, resistance meter two end electrodes chuck is used to clamp the upper and lower two panels electrolytic copper foil of sample respectively, test resistance size is the contact resistance that aperture is the test sample of φ 1.0mm, and Fig. 1 is shown in by contact resistance test schematic diagram.
(2) conductive adhesive film connection resistance testing method:
2 electrolytic copper foil spacing 20mm, cut the long conductive adhesive film sample of the wide 40mm of 20mm, are pressed between two Copper Foils.The resistance between two copper foil electrodes measured by use DC digital resistance instrument, is connection resistance.Fig. 2 is shown in by connection resistance test schematic diagram.
(3) resistance change rate (resistance change of sample before and after resistance to soldering)
Resistance before resistance change rate=(resistance before the resistance-Nai soldering after resistance to soldering)/resistance to soldering.
(4) resistance to tin-welding, the test of stripping strength and resistance to acids and bases
By the conductive adhesive film laminating Copper Foil and flexibility coat copper plate prepared, fast pressure 3 minutes under 2MPa and 170 DEG C condition, 160 DEG C of bakings 60 ~ 120 minutes, namely the test sample of conductive adhesive film is prepared into, test resistance to tin-welding, stripping strength and resistance to acids and bases, resistance to tin-welding: according to IPC-TM-650, NO.2.4.139 testing method; Stripping strength: according to IPC-TM-650, NO.2.4.9 testing method; Resistance to acids and bases: testing method consults JIS-9.2 in Japanese Industrial Standards' " flexible printed wiring board copper-clad plate experimental technique ".
(5) testing method of preservation period
By conductive adhesive film temperature 6 ~ 10 DEG C, relative humidity 60%, stores certain hour, then tests resistance to tin-welding, stripping strength and resistance to acids and bases by as above method.If test item middle finger mark now a certain defective time, be exactly the maximum storage phase under this condition, i.e. preservation period.
Claims (10)
1. a thermoset conductive resin, is characterized in that: by weight percentage, comprises following component:
2. thermoset conductive resin according to claim 1, is characterized in that: described Hydroxylated acrylic resin is white or light yellow, and solid content is 60 ~ 70wt%, and hydroxy radical content is 2 ~ 5wt%.
3. thermoset conductive resin according to claim 1, is characterized in that: the optional polyester of described vibrin has: one or more the mixture in polyester 7908, polyester 3550 and polyester 560.
4. thermoset conductive resin according to claim 1, is characterized in that: described epoxy resin is bisphenol A type epoxy resin, wherein: the epoxy equivalent (weight) of liquid-state epoxy resin is 180 ~ 215g/mol, and viscosity is 8000 ~ 15000mPa.s; The epoxy equivalent (weight) of solid epoxy resin is 450 ~ 1000g/mol, and softening temperature is 60 ~ 102 DEG C.
5. thermoset conductive resin according to claim 1, is characterized in that: solid epoxy resin and liquid-state epoxy resin are combined into exercise and use by the epoxy resin in the present invention.
6. thermoset conductive resin according to claim 1, is characterized in that: described conducting medium is the mixture of several conducting mediums in the silver-bearing copper powder of copper powder, nickel powder, argentiferous 10%; Described thixotropic agent is aerosil; Described solvent is the mixture of two kinds or more solvents in ethyl acetate, butanone, butylacetate, toluene.
7. the preparation method of thermoset conductive resin according to claim 1, it is characterized in that: use dissolution with solvents vibrin, conducting medium is added after dissolving, load in the milling tank of high speed ball mill, high speed dispersion is poured in mix and blend tank after milling and filtering, slowly add the Hydroxylated acrylic resin of formula metering, epoxy resin and thixotropic agent, namely uniform stirring obtains thermoset conductive resin glue.
8. the preparation method of thermoset conductive resin according to claim 7, is characterized in that: described high speed dispersion grinding time is 60 ~ 90 minutes, and described being filtered into is filtered with 200-300 mesh filter screen; Described churning time is 20-24h.
9. isotropy thermoset conductive adhesive film, is characterized in that: it is made up of release film and the thermoset conductive adhesive layer according to claim 1 be coated on release film.
10. the preparation method of isotropy thermoset conductive adhesive film according to claim 9, release film applies above-mentioned obtained thermoset conductive resin glue, controlling drying tunnel temperature is 80 DEG C ~ 120 DEG C, coating speed is 10 ~ 15m/min, glue is thick is 25 ~ 30 μm, to fit on thermoset conductive resin glued membrane during rolling release film, be namely prepared into thermoset conductive adhesive film.
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| CN201510481199.9A CN105086873A (en) | 2015-08-07 | 2015-08-07 | Isotropous thermosetting conductive adhesive film and preparation method thereof |
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| CN201510481199.9A CN105086873A (en) | 2015-08-07 | 2015-08-07 | Isotropous thermosetting conductive adhesive film and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883786A (en) * | 2017-02-24 | 2017-06-23 | 深圳市金晖科技有限公司 | A kind of preparation method of comprehensive thermal setting conductive glue |
| CN108130032A (en) * | 2017-12-23 | 2018-06-08 | 苏州佳亿达电器有限公司 | A kind of high temperature resistant conductive silver glue for producing LED |
| CN112831296A (en) * | 2021-01-11 | 2021-05-25 | 东莞市迪奥顺水性涂料有限公司 | Glue for bonding glass and metal and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392154A (en) * | 2007-09-20 | 2009-03-25 | 第一毛织株式会社 | Anisotropic conductive adhesive composition and anisotropic conductive film comprising the same |
| CN103468159A (en) * | 2013-03-11 | 2013-12-25 | 苏州牛剑新材料有限公司 | Silver coated nickel powder conductive adhesive and preparation method thereof |
-
2015
- 2015-08-07 CN CN201510481199.9A patent/CN105086873A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392154A (en) * | 2007-09-20 | 2009-03-25 | 第一毛织株式会社 | Anisotropic conductive adhesive composition and anisotropic conductive film comprising the same |
| CN103468159A (en) * | 2013-03-11 | 2013-12-25 | 苏州牛剑新材料有限公司 | Silver coated nickel powder conductive adhesive and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883786A (en) * | 2017-02-24 | 2017-06-23 | 深圳市金晖科技有限公司 | A kind of preparation method of comprehensive thermal setting conductive glue |
| CN108130032A (en) * | 2017-12-23 | 2018-06-08 | 苏州佳亿达电器有限公司 | A kind of high temperature resistant conductive silver glue for producing LED |
| CN112831296A (en) * | 2021-01-11 | 2021-05-25 | 东莞市迪奥顺水性涂料有限公司 | Glue for bonding glass and metal and preparation method thereof |
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