CN102719199A - Preparation method of three-dimensional anisotropic conductive film - Google Patents
Preparation method of three-dimensional anisotropic conductive film Download PDFInfo
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- CN102719199A CN102719199A CN2012101200152A CN201210120015A CN102719199A CN 102719199 A CN102719199 A CN 102719199A CN 2012101200152 A CN2012101200152 A CN 2012101200152A CN 201210120015 A CN201210120015 A CN 201210120015A CN 102719199 A CN102719199 A CN 102719199A
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Abstract
The invention discloses a preparation method of a three-dimensional anisotropic conductive film (ACF). The preparation method of the film comprises steps of: mixing an active thermoplastic elastomer, an epoxy resin and a reactive diluent thereof, an antioxidant, a thixotropic agent and a coupling agent; dissolving the mixture in a cyclohexanone / ketone solvent mixture; adding Ni / Au plated conductive particles and latent curing agent to prepare a glue solution; degassing the glue solution and coating on a polyethylene glycol terephthalate release film; and drying to form the film. The film can be applied to the field of photoelectricity.
Description
Technical field
The invention belongs to field of photoelectric technology, be specifically related to a kind of preparation method of three-dimensional unilateral conduction glued membrane.
Background technology
In order to satisfy flat-panel monitor to thin; Gently; The requirement microminiaturized and the environmental friendliness direction develops; A kind of panel of current most advanced level of representing is connected material with driver circuits for integrated circuit---and three-dimensional unilateral conduction glued membrane (or claiming the undirectional conducting film, Anisotropic Conductive Film ACF) comes out in Japan.ACF is used to connect the panel of LCD of electronic calculator the earliest, and constantly development has been widely used in the every field that liquid crystal relates to along with the development of liquid crystal, also begins to be applied to the semi-conductor manufacturing thereafter and waits other industrial circle.
Three-dimensional unilateral conduction glued membrane be the micron order list with uniform particle diameter to disperse nickel plating (or gold) polymer microballoon be that conducting particles is dispersed in the conducting membrane material that forms in the resin, be characterized on thickness direction, conducting electricity, insulate on the in-plane.Mainly form by conducting particles, sticker.It is attached between IC chip and the substrate electrode between the two; Under moment pressurized, heated condition, adhesive cures connects conducting through conducting particles between the electrode; Simultaneously can avoid adjacent two inter-electrode short-circuits again, and only reach purpose in the Z-direction conducting.
Sticker mainly is made up of thermoplastic elastomer, thermosetting resin and solidifying agent.Thermoplastic elastomer is not generally participated in reaction, low-temperature heat fusing, bonding effect originally.Thermoplastic elastomer can be carboxy nitrile rubber, SBS, SIS, SERS etc., and the patent that relates to has JP08-55514, CN99103372, CN200410022028.1 etc.; Polyurethane elastomer, the patent that relates to has CN00114692.0, JP2001176326, JP01249881, CN200610068710 etc.; Polyvinyl acetal, the patent that relates to has CN01118419.1, JP2001064207 etc.; Polypropylene acid resin, the patent that relates to have JP5-339556, JP08-003529, US 5,162,087 etc.Thermosetting resin epoxy resin commonly used and radical polymerization resin.Wherein epoxy resin is to use maximum; Mainly contain bisphenol A epoxide resin, bisphenol F epoxy resin, novolac epoxy, phenoxy resin etc., the related patent U.S. Patent No. that relates to has JP9-25967, JP2001207133, CN200410222202.8, JP5-339556, JP08-111124, JP01-113480, CN03813056, CN00114692.0, spy to open flat 3-12607, JP2000-178511 etc.
Solidifying agent is the latent imidazole curing agent, like US5733954, JP611268721, CN01118419.1, JP59-227925, EP0193068, JP3-129607, JP09-165435.The radical polymerization resin has: propenoate (CN01130200.3, CN200710166043.7); Urethane acrylate (CN00114692.0); Epoxy acrylate (JP2001171033) amine modified bismaleimide resin (CN1242403A); Unsaturated polyamides resin (JP2001171033) etc.Solidifying agent adopts peroxide radical to cause.
Compare with traditional wiping solder, the ACF technology has following characteristic: (1) but have high-density, any multijunction interconnection capability of thin space batch processing; (2) but low temperature connect, can reduce fatigue damage and stress cracking Problem of Failure in the interconnection process, thereby be particularly suitable for the interconnection of thermo-responsive components and parts and the interconnection of non-solderable surface; (3) have higher flexibility and fatigue resistence, can connect with different substrates; (4) interconnection process is simple, and process step is few, can improve industrial capacity and reduce production costs; (5) not leaded and other toxic metal, and interconnection process need not to clean, and has eliminated environmental pollution.It not only overcome traditional tin lead welding connect in plumbous murder by poisoning influence to human body and environment, and make connection efficient more, accurate, conveniently and microminiaturized, be a kind of revolution of traditional mode of connection.Yet; Existing ACF solidification value higher (more than 180 ℃) usually occurs, solidifies not thoroughly in the hot-press solidifying use, and cure shrinkage is big, long-pending big, the defective such as tack is poor, sticking cutter, cohesive strength are low of expansion after the pressing; Make product qualified rate low, cost increases.
Summary of the invention
The object of the invention is to provide a kind of preparation method of three-dimensional unilateral conduction glued membrane; Solved solidification value higher (more than 180 ℃) when ACF prepares in the prior art, solidified not thoroughly, cure shrinkage is big, long-pending big, the problem such as tack is poor, sticking cutter, cohesive strength are low of expansion after the pressing.
In order to solve these problems of the prior art, technical scheme provided by the invention is:
A kind of preparation method of three-dimensional unilateral conduction glued membrane is characterized in that said method comprising the steps of:
(1) with active thermoplastic elastomer, epoxy resin, epoxide resin reactive diluent, oxidation inhibitor, thixotropic agent and silane coupling agent by predetermined proportion mixing after, join in the mixed solvent of methylcyclohexane and butanone, heated and stirred is dissolved into initial soln;
(2) add conducting particles and latent curing agent successively after the cooling of initial soln that step (1) is made, stir and process glue;
(3) be applied on the polyethylene terephthalate dicing film after the glue vacuum outgas that step (2) is made, film forming promptly obtains three-dimensional unilateral conduction glued membrane after oven dry.
Preferably, the composition of raw materials that adds in the said method is counted with the parts by weight of its component:
Active thermoplastic elastomer 4～10 parts by weight;
Conducting particles 3～4 parts by weight;
Liquid-state epoxy resin 2～10 parts by weight;
Silane coupling agent 0～1 parts by weight;
Epoxide resin reactive diluent 2～4 parts by weight;
Oxidation inhibitor 0～0.3 parts by weight;
Solid epoxy resin 8～22 parts by weight;
Thixotropic agent gas-phase silica 0～0.3 parts by weight;
Latent curing agent 6～8 parts by weight;
Methylcyclohexane/butanone 45～70 parts by weight.
Preferably, thermoplastic elastomer described in the said method by the rubber that contains unsaturated double-bond with to contain epoxide group acrylate monomer reaction synthetic.
Preferably, the rubber that contains unsaturated double-bond described in the said method is selected from viton and tree elastomer.
Preferably, containing the epoxide group acrylate monomer described in the said method is SY-Monomer G.
Preferably, liquid epoxies is selected E-51 for use described in the said method; Said epoxide resin reactive diluent selects 3 for use, 4-epoxycyclohexyl formic acid-3,4-epoxycyclohexyl methyl ester (CY179); Said solid epoxy is selected phenoxy resin for use, and its weight-average molecular weight is 70000.
Preferably, latent curing agent is selected from the glyoxal ethyline modified firming agent described in the said method.
Preferably, the glyoxal ethyline modified firming agent is by after glyoxal ethyline and the ratio reaction of epoxide resin reactive diluent according to 2: 1 amount in the said method, obtains by isophorone diisocyanate (IPDI) end-blocking is synthetic again.
Preferably, silane coupling agent described in the said method is selected from 3-(2,3 epoxies, third oxygen) propyl trimethoxy silicane (KH-560), and said oxidation inhibitor is selected from 2,2 '-methylene-bis (4-methyl-6-tert butyl phenol) (2246), and said thixotropic agent is a gas-phase silica.
The invention provides the preparation method of the three-dimensional unilateral conduction glued membrane of a kind of low-temperature curing (ACF).This glued membrane is processed glue by active thermoplastic elastomer, epoxy resin and reactive thinner thereof, oxidation inhibitor, thixotropic agent, coupling agent, latent curing agent, methylcyclohexanone/butanone mixed solvent; Be coated on the polyethylene terephthalate dicing film film forming after oven dry after the glue degassing.This three-dimensional unilateral conduction glued membrane (ACF) only has electroconductibility along its thickness direction (Z axle), and in-plane (XY axle) is non-conductive, can be applicable to photoelectric field.
The present invention aims to provide a kind of low-temperature curing; The preparation method of the three-dimensional unilateral conduction glued membrane of excellent combination property; Technical solution key of problem of the present invention is: 1, synthetic a kind of active thermoplastic elastomer that contains epoxide group; Make it can participate in reaction, thereby increase tack and stripping strength.2, synthetic latent curing agent increases package stability, and solidification value reduces.
In order to arrive the object of the invention; In the technical scheme of the present invention active thermoplastic elastomer by the rubber that contains unsaturated double-bond with contain the epoxide group acrylate monomer by a certain percentage under action of free radical initiator, synthetic more than 10 hours 70 ℃ ± 2 ℃ reactions.The described rubber that contains unsaturated double-bond can be viton and tree elastomer, the preferred few tree elastomer of impurity ion content.The described epoxide group acrylate monomer that contains is a SY-Monomer G.
In order to arrive the object of the invention, latent curing agent is the glyoxal ethyline modified firming agent in the technical scheme of the present invention.Its preparation method is: reacted down at 70 ℃ ± 2 ℃ according to the mol ratio of 2:1 by glyoxal ethyline and epoxide resin reactive diluent and synthesized in 3～5 hours; After being cooled to 60 ℃, add with the equimolar isophorone diisocyanate of epoxy resin (IPDI) 2 hours synthetic end-blockings of reaction under 70 ℃ ± 2 ℃ synthetic.
The preparation method of the three-dimensional unilateral conduction glued membrane of low-temperature curing therefore of the present invention may further comprise the steps:
At first, the active thermoplastic elastomer in the sticker and epoxy resin, epoxide resin reactive diluent, oxidation inhibitor, thixotropic agent and silane coupling agent are joined in the mixed solvent of methylcyclohexane and butanone the heated and stirred dissolving after mixing by a certain percentage.
After the cooling, add conducting particles and latent curing agent successively, stir and process glue.
With being applied to after the made glue vacuum outgas on polyethylene terephthalate (PET) dicing film, film forming after oven dry is cut, bundling, packing, cold storage.
The base stock formulation of using is following:
Active thermoplastic elastomer 4～10 parts by weight;
Ni/Au conducting particles 3～4 parts by weight;
Liquid-state epoxy resin 2～10 parts by weight;
Silane coupling agent KH560 0～1 parts by weight;
Epoxide resin reactive diluent 2～4 parts by weight;
Antioxidant 2246 0～0.3 parts by weight;
Solid epoxy resin 8～22 parts by weight;
Thixotropic agent gas-phase silica 0～0.3 parts by weight;
Latent curing agent 6～8 parts by weight;
Methylcyclohexane/butanone 45～70 parts by weight.
Described epoxy resin is the compsn of liquid epoxies, epoxide resin reactive diluent, solid epoxy.Described epoxy resin is that liquid epoxies is E-51, and epoxide resin reactive diluent is 3,4-epoxycyclohexyl formic acid-3, and 4-epoxycyclohexyl methyl ester (CY179), solid epoxy is phenoxy resin (M.w.70000).
Described silane coupling agent is 3-(2,3 epoxies, third an oxygen) propyl trimethoxy silicane (KH-560), oxidation inhibitor is 2,2 '-methylene-bis (4-methyl-6-tert butyl phenol), thixotropic agent is a gas-phase silica.The conducting particles that adds different-grain diameter is regulated the three-dimensional unilateral conduction glued membrane that coat-thickness can obtain plurality of specifications.
With respect to scheme of the prior art, advantage of the present invention is:
The prepared three-dimensional unilateral conduction glued membrane tack of the present invention is good; Solidification value lower (110-130 ℃); Set time is shorter, is 10-15 second; Stripping strength is higher, more than 9N/cm (90 degree are peeled off); Connect resistance initial value≤1.0 Ω, after 20 thermal shockings≤1.5 Ω; Insulation resistance
109 Ω; Shelf lives surpasses 35 days (under 40 ℃ of environment).
Embodiment
Below in conjunction with specific embodiment such scheme is further specified.Should be understood that these embodiment are used to the present invention is described and are not limited to limit scope of the present invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
The preparation of embodiment 1 three-dimensional unilateral conduction glued membrane
1, synthetic latent curing agent.
Take by weighing 164.2 gram glyoxal ethylines and 252.3 gram epoxide resin reactive diluent CY179 70 ℃ of following reactions 3-5 hour; When bottle internal reaction fluid viscosity no longer changes, stop heating, be cooled to 60 ℃; Add 222.3 gram isophorone diisocyanates; 72 ℃ of reactions of temperature control 2 hours are measured nco value content less than 0.5% stopped reaction, cooling discharge after adding 100g CY179 stirs.Synthetic latent curing agent deepfreeze.
2, composite reactive thermoplastic elastomer.
Take by weighing the 270g tree elastomer, 350g methylcyclohexane/butanone solvent, 180g SY-Monomer G, stirring heating dissolving.Add Diisopropyl azodicarboxylate 17g temperature control reaction 15 hours, measure double bond content less than 0.5% stopped reaction, discharging while hot.
3, take by weighing active thermoplastic elastomer 100g; Liquid-state epoxy resin E-5150g, phenoxy resin (M.w.70000) 80g, epoxide resin reactive diluent CY179 30g; Antioxidant 2246 1.5g; Thixotropic agent gas-phase silica 2g, silane coupling agent KH-560 5g, on small-sized three roller mixing rolls mixing three times basic glue.
4, get basic glue 45g and add methylcyclohexane/butanone 70 grams, in 40 ℃～50 ℃ following heating for dissolving.Reduce to the plating Ni/Au conducting particles that adds 4 gram particles footpath, 3 μ m after the room temperature, the back that stirs adds latent curing agent 10g, continues to stir to process glue.
5, with made glue through being applied to after the vacuum outgas on the PET dicing film, 115 ℃ of oven dry 3 minutes are cut, bundling, packing, 16 micron thick, 2 mm wides, 100 meters grow up to the three-dimensional unilateral conduction glued membrane of article.The cold storage of finished product.
The preparation of embodiment 2 three-dimensional unilateral conduction glued membranes
1, synthetic latent curing agent.
Synthesis step is similar to the 1st step among the embodiment 1.
2, composite reactive thermoplastic elastomer.
Take by weighing the 200g tree elastomer, 350g methylcyclohexane/butanone solvent, 250g SY-Monomer G, stirring heating dissolving.Add Diisopropyl azodicarboxylate 20g temperature control reaction 18 hours, measure double bond content less than 0.5% stopped reaction, discharging while hot.
3, take by weighing active thermoplastic elastomer 80g, liquid-state epoxy resin E-51 45g, phenoxy resin (M.w.70000) 75g; Epoxide resin reactive diluent CY179 35g, antioxidant 2246 1.2g; Silane coupling agent KH-560 4g, on small-sized three roller mixing rolls mixing three times basic glue.
4, get basic glue 50g and add methylcyclohexane/butanone 80 grams, in 40 ℃～50 ℃ following heating for dissolving.Reduce to the plating Ni/Au conducting particles that adds 6 gram particles footpath, 8 μ m after the room temperature, the back that stirs adds latent curing agent 14g, continues to stir to process glue.
5, with made glue through being applied to after the vacuum outgas on the PET dicing film, 115 ℃ of oven dry 3 minutes are cut, bundling, packing, 45 micron thick, 2 mm wides, 100 meters grow up to the three-dimensional unilateral conduction glued membrane of article.The cold storage of finished product.
Two kinds of conductive adhesive film Characteristics Detection results that the foregoing description obtains are following:
The fine and close homogeneous of outward appearance, pore-free, no adhesion; 1000 power microscopes are observed conducting particles and are reunited a number average less than 5; The dicing film stripping strength all≤0.02N/2.5mm; Interim working strength all>=the 1.0N/cm hot pressing temperature all≤130 ℃, solidified in≤15 seconds; Cohesive strength all>=9N/cm; Connect the resistance initial value all≤0.2 Ω, after 20 thermal shockings all≤0.2 Ω; Insulation resistance all>=7 * 10
9Ω; 40 ℃ of package stabilities all reach more than January.
Above-mentioned instance only is explanation technical conceive of the present invention and characteristics, and its purpose is to let the people who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalent transformations that spirit is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (9)
1. the preparation method of a three-dimensional unilateral conduction glued membrane is characterized in that said method comprising the steps of:
(1) with active thermoplastic elastomer, epoxy resin, epoxide resin reactive diluent, oxidation inhibitor, thixotropic agent and silane coupling agent by predetermined proportion mixing after, join in the mixed solvent of methylcyclohexane and butanone, heated and stirred is dissolved into initial soln;
(2) add conducting particles and latent curing agent successively after the cooling of initial soln that step (1) is made, stir and process glue;
(3) be applied on the polyethylene terephthalate dicing film after the glue vacuum outgas that step (2) is made, film forming promptly obtains three-dimensional unilateral conduction glued membrane after oven dry.
2. method according to claim 1 is characterized in that the composition of raw materials that adds in the said method counts with the parts by weight of its component:
Active thermoplastic elastomer 4～10 parts by weight;
Conducting particles 3～4 parts by weight;
Liquid-state epoxy resin 2～10 parts by weight;
Silane coupling agent 0～1 parts by weight;
Epoxide resin reactive diluent 2～4 parts by weight;
Oxidation inhibitor 0～0.3 parts by weight;
Solid epoxy resin 8～22 parts by weight;
Thixotropic agent 0～0.3 parts by weight;
Latent curing agent 6～8 parts by weight;
Methylcyclohexane/butanone 45～70 parts by weight.
3. method according to claim 1, it is characterized in that thermoplastic elastomer described in the said method by the rubber that contains unsaturated double-bond with to contain epoxide group acrylate monomer reaction synthetic.
4. method according to claim 3 is characterized in that the rubber that contains unsaturated double-bond described in the said method is selected from viton and tree elastomer.
5. method according to claim 3, it is characterized in that containing described in the said method epoxide group acrylate monomer is SY-Monomer G.
6. method according to claim 1 is characterized in that liquid epoxies is selected E-51 for use described in the said method; Said epoxide resin reactive diluent selects 3 for use, 4-epoxycyclohexyl formic acid-3,4-epoxycyclohexyl methyl ester (CY179); Said solid epoxy is selected phenoxy resin for use, and its weight-average molecular weight is 70000.
7. method according to claim 1 is characterized in that latent curing agent is selected from the glyoxal ethyline modified firming agent described in the said method.
8. method according to claim 7; It is characterized in that glyoxal ethyline modified firming agent in the said method is by after glyoxal ethyline and the ratio reaction of epoxide resin reactive diluent according to the amount of 2:1, obtains by isophorone diisocyanate (IPDI) end-blocking is synthetic again.
9. method according to claim 1; It is characterized in that silane coupling agent is selected from 3-(2 described in the said method; 3 epoxies, third oxygen) propyl trimethoxy silicane (KH-560); Said oxidation inhibitor is selected from 2,2 '-methylene-bis (4-methyl-6-tert butyl phenol), and said thixotropic agent is a gas-phase silica.
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| CN2012101200152A CN102719199A (en) | 2012-04-23 | 2012-04-23 | Preparation method of three-dimensional anisotropic conductive film |
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| CN2012101200152A CN102719199A (en) | 2012-04-23 | 2012-04-23 | Preparation method of three-dimensional anisotropic conductive film |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104479298A (en) * | 2014-12-29 | 2015-04-01 | 宁波大榭开发区综研化学有限公司 | Conductive resin composition and preparation method thereof |
| CN106010321A (en) * | 2016-08-10 | 2016-10-12 | 苏州赛伍应用技术有限公司 | Conductive adhesive film |
| CN110885655A (en) * | 2019-12-13 | 2020-03-17 | 苏州凡络新材料科技有限公司 | Surface insulation type electromagnetic shielding adhesive and preparation method thereof |
| CN110885512A (en) * | 2019-12-13 | 2020-03-17 | 陕西易莱德新材料科技有限公司 | Polyvinyl chloride elastomer conductive composite material and preparation method thereof |
| CN110982463A (en) * | 2019-10-30 | 2020-04-10 | 上海润势科技有限公司 | Conductive adhesive and solar cell |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104479298A (en) * | 2014-12-29 | 2015-04-01 | 宁波大榭开发区综研化学有限公司 | Conductive resin composition and preparation method thereof |
| CN106010321A (en) * | 2016-08-10 | 2016-10-12 | 苏州赛伍应用技术有限公司 | Conductive adhesive film |
| CN110982463A (en) * | 2019-10-30 | 2020-04-10 | 上海润势科技有限公司 | Conductive adhesive and solar cell |
| CN110885655A (en) * | 2019-12-13 | 2020-03-17 | 苏州凡络新材料科技有限公司 | Surface insulation type electromagnetic shielding adhesive and preparation method thereof |
| CN110885512A (en) * | 2019-12-13 | 2020-03-17 | 陕西易莱德新材料科技有限公司 | Polyvinyl chloride elastomer conductive composite material and preparation method thereof |
| CN110885655B (en) * | 2019-12-13 | 2021-09-03 | 苏州凡络新材料科技有限公司 | Surface insulation type electromagnetic shielding adhesive and preparation method thereof |
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Application publication date: 20121010 |