CN111087941A - Transparent conductive adhesive composition and preparation and application thereof - Google Patents
Transparent conductive adhesive composition and preparation and application thereof Download PDFInfo
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- CN111087941A CN111087941A CN202010051014.1A CN202010051014A CN111087941A CN 111087941 A CN111087941 A CN 111087941A CN 202010051014 A CN202010051014 A CN 202010051014A CN 111087941 A CN111087941 A CN 111087941A
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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
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/02—Polymerisation in bulk
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/04—Polymerisation in solution
- C08F2/06—Organic solvent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F257/00—Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/02—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of acids, salts or anhydrides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
- C08F265/06—Polymerisation of acrylate or methacrylate esters on to polymers thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F273/00—Macromolecular compounds obtained by polymerising monomers on to polymers of sulfur-containing monomers as defined in group C08F28/00
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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
- 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
- C09J151/003—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 macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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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
- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/10—Presence of inorganic materials
- C09J2400/16—Metal
- C09J2400/163—Metal in the substrate
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- 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
- C09J2467/00—Presence of polyester
- C09J2467/005—Presence of polyester in the release coating
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a transparent acrylic conductive adhesive composition, a preparation method thereof and application thereof in a conductive adhesive tape, wherein the transparent acrylic conductive adhesive composition adopts a mode of adding an ionic conductive compound, converts traditional electronic conduction into ionic transmission conduction, can realize doping blending with matrix resin at a molecular level, does not have the problems of sedimentation, appearance and the like, improves the problems of poor conductivity, poor appearance and the like of a conductive adhesive in the prior art, and simultaneously realizes the performances of viscosity, conductivity, transparency, stability and the like.
Description
Technical Field
The invention relates to a transparent acrylic conductive adhesive composition, in particular to a transparent acrylic conductive adhesive composition, a preparation method thereof and application thereof in a conductive adhesive tape.
Background
The conductive adhesive is an adhesive with bonding and conductive properties, can be uniformly coated on a conductive base material, can realize connection of multiple materials, realizes XYZ omnidirectional conduction, and has excellent electromagnetic shielding property. As a conductive medium of an electronic element, the conductive adhesive is widely applied to design and production of quartz crystal resonators, semiconductor wafers, LED light-emitting diodes, PTC ceramic heating elements, filters, piezoelectric ceramics, circuit repair and the like, and meanwhile, the conductive adhesive is also applied to the fields of microelectronic packaging, printed circuit boards, conductive circuit bonding, electromagnetic shielding and the like.
The commercially available conductive adhesive is obtained by curing an organic polymer matrix and a conductive filler, and in addition, comprises a diluent, a dispersant, a curing agent and other auxiliary agents. Most of conductive adhesives in the current market are filler type conductive adhesives, the matrix is usually a thermosetting adhesive, such as epoxy resin, organic silicon resin, polyimide resin, phenolic resin, polyurethane, acrylic resin and the like, and the resins form a molecular skeleton structure after being cured, so that the mechanical property and the bonding property are provided for the conductive adhesives, and the conductive filler forms a conductive channel. The conductive filler is a main source of conductive performance of the conductive adhesive, and common conductive fillers comprise metal fillers, inorganic fillers, mixed fillers and the like. The metal filler is commonly gold powder, silver powder, copper powder, nickel powder and alloy powder, the inorganic filler is carbon black, carbon nano tubes, graphene and silver nano wires, and the mixed filler is a novel conductive filler which comprehensively uses the metal filler and the inorganic filler, such as silver plating on the surface of the carbon nano tubes, micron silver sheets, micron silver balls, acidified single-walled carbon nano tubes and the like.
A large amount of conductive metal filler substances are added in the existing conductive adhesive, and the density of the metal filler is higher than that of matrix resin, so that the adhesive surface is easy to settle and is not conductive locally; the metal filler is easy to agglomerate, thereby causing the problems of poor surface appearance such as black spots or particle spots on the surface of the rubber, and the like; if the prepared product needs to be added with a large amount of metal filler when used in a small area, the transparency of the conductive adhesive film is greatly reduced, and a series of problems in the process are caused.
In order to overcome the defects, the transparent conductive adhesive film with the special bonding function has a simple formula and low process realization difficulty, and has a plurality of potential applications in the fields of flexible electronic devices and soft functional materials.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a transparent conductive adhesive composition which is easy to dissolve in a common solvent by adding an ionic conductive compound, can realize doping and blending with matrix resin at a molecular level, does not have the problems of sedimentation, appearance and the like, and solves the problems of poor conductivity, poor appearance and the like of a conductive adhesive in the prior art.
According to the purpose, the invention provides a transparent conductive adhesive composition, which comprises the following components in parts by weight: (a) 100 parts of mixed monomers; (b) 5-6 parts of a cross-linking agent; (c) 1-10 parts of ionic conductive compound; (d) 1.0-2.0 parts of curing agent; (e) 20-50 parts of a solvent.
As a preferred embodiment of the present invention, the mixed monomer comprises: (I) 80-98 parts by weight of an acrylic monomer or an alkyl-substituted acrylic monomer having 1-10 carbon atoms; and (II) a monomer containing a crosslinking group, wherein the weight part of the monomer is 2-20.
Further, the acrylic monomer or alkyl substituted acrylic monomer with the carbon number of 1-10 is at least one of acrylic acid, methacrylic acid, methyl acrylate, ethyl acrylate, methyl methacrylate, ethyl methacrylate, n-propyl acrylate, isopropyl acrylate, butyl methacrylate, tert-butyl acrylate, n-propyl methacrylate, isopropyl methacrylate, tert-butyl methacrylate and acrylonitrile.
Further, the crosslinking group-containing monomer includes at least one of vinyl (meth) acrylate, epoxy acrylate, urethane acrylate, ethylene glycol diacrylate, ethylene glycol di (meth) acrylate, propylene glycol di (meth) acrylate, butylene glycol di (meth) acrylate, (neo) pentanediol di (meth) acrylate, pentaerythritol di (meth) acrylate, hexanediol diacrylate, and hexanediol di (meth) acrylate.
The acrylate monomer contains functional groups such as ester group, carboxyl group, hydroxyl group, epoxy group and the like, has strong polarity and good adhesive property to various surfaces. The soft monomer structures of ethyl acrylate, butyl acrylate and the like contain relatively long alkyl chain segments, and the glass transition temperature of the soft monomer structures is low (below-10 ℃), so that the adhesive composition can be endowed with good initial adhesion, flexibility and film-forming property; methyl methacrylate, acrylonitrile and other hard monomers containing methyl and carboxyl groups in their structures have high glass transition temperatures (about 100 ℃), and the addition of the hard monomers is intended to improve the hardness and cohesion of the resin. The crosslinking monomer usually contains functional groups, such as hydroxyl, carboxyl, alkenyl, amino, epoxy and the like, and the functional groups or crosslinking density points can be introduced into the molecular chain structure, so that the adhesive force, the solvent resistance, the temperature resistance and other properties of the adhesive are improved. The monomers are matched with each other, so that the conventional performances of the glue formula, such as heat resistance, weather resistance, oil resistance and the like, can be realized.
In a preferred embodiment of the present invention, the ionic conductive compound is at least one selected from the group consisting of sodium polyacrylate, sodium polymethacrylate, sodium polyvinylsulfonate, sodium polystyrenesulfonate, lithium bis (trifluoromethylsulfonimide) salt, lithium chloride, lithium tetrafluoroborate, and lithium hexafluorophosphate.
The above ionic conductive compound has high stability in air, and it uses ions as conductive carriers to achieve conduction through ion transport between polymer segments. The addition of the ionic conductive compound provides conductivity for the adhesive on one hand, and provides transparency (visible light transmittance is more than 98%), viscosity, elasticity and stability for the obtained conductive adhesive on the other hand, and the traditional conductive filler is difficult to achieve the performances at the same time.
In a preferred embodiment of the present invention, the crosslinking agent increases cohesive force of the adhesive by reacting carboxyl, hydroxyl, alkenyl, amino, epoxy, and the like in the structure thereof with alkenyl groups in the soft and hard monomers, and may be at least one of the following: at least one of polyethylene glycol diacrylate, butadiene, isoprene, octadiene, and octadecadiene, and it is particularly preferable to use polyethylene glycol diacrylate.
In a preferred embodiment of the present invention, the non-alcoholic solvent may be at least one of esters, aliphatic hydrocarbons, aromatic hydrocarbons, alicyclic hydrocarbons, and ketones, such as ethyl acetate, n-butyl acetate, n-hexane, n-heptane, toluene, benzene, cyclohexane, methylcyclohexane, methyl ethyl ketone, methyl isobutyl ketone, and the like, and may be used alone or in combination of two or more thereof. The selection of an alcohol solvent can cause solute precipitation due to compatibility problems.
In a preferred embodiment of the present invention, the curing agent is an isocyanate-based curing agent, and toluene diisocyanate and diphenylmethyl diisocyanate are particularly preferred.
The second purpose of the invention is to provide a preparation method of the transparent conductive adhesive composition.
In a preferred embodiment of the present invention, the production method includes a solution polymerization method and a bulk polymerization method. Particularly preferably prepared by a solution polymerization method, and the polymerization temperature is preferably 25-130 ℃.
Taking materials according to the following proportion: 80-98 parts of acrylic monomers or alkyl substituted acrylic monomers, 2-20 parts of monomers containing crosslinking groups, 1-10 parts of ionic conductive compounds, 1.0-2.0 parts of curing agents and 20-45 parts of non-alcohol solvents.
The preparation method comprises the following steps: adding the above substances in parts by weight into a reaction bottle in sequence except for a curing agent, wherein the total volume of reactants accounts for 1/3-2/3 of the total volume of the reaction bottle, mechanically stirring, heating the reaction bottle to enable the temperature of the reactants in the reaction bottle to be 50-60 ℃, dropwise adding a mixed solution of a solvent (5 parts) and the curing agent into the reaction bottle after a uniform and transparent solution is formed, and continuously heating to 70-80 ℃ after dropwise adding is finished, and stirring and reacting for 3-4 hours. And (3) when the temperature of the reaction system is reduced to room temperature (25-30 ℃), filtering and discharging the reaction liquid to obtain the transparent conductive adhesive composition.
The third purpose of the invention is to provide an application of the transparent conductive adhesive composition in a conductive adhesive tape, wherein the conductive adhesive tape comprises a substrate layer, transparent adhesive layers positioned on one side or two sides of the substrate layer, and a release film, wherein the adhesive layers are formed by coating the transparent conductive adhesive composition.
Compared with the prior art, the invention has the following beneficial effects.
(1) The ionic conductive compound is adopted to replace the traditional inorganic filler to realize the conduction mode, the traditional electronic conduction is converted into the ionic transmission conduction, and the performances of viscosity, conductivity, transparency, stability and the like are realized.
(2) According to the invention, a solution polymerization reaction system is adopted, monomers with different glass transition temperatures are blended, and the structure, molecular weight and distribution of a high molecular chain are adjusted through the amount of a cross-linking agent and a curing agent, so that transparent conductive adhesive compositions with different viscosities are obtained.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to the following embodiments, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1.
Adding butyl methacrylate (84 parts), methyl methacrylate (10 parts), vinyl acrylate (6 parts), lithium bis (trifluoromethylsulfonyl imide) (5 parts), polyethylene glycol diacrylate (5 parts) and toluene (40 parts) into a reaction bottle, uniformly mixing to form a uniform and transparent solution, heating the reaction bottle to 50-60 ℃, dissolving and diluting toluene diisocyanate (15 parts) with toluene (2 parts), dripping into the reaction bottle, continuously heating to 70-80 ℃, and stirring for reaction for 3-4 hours. And (3) when the temperature of the reaction system is reduced to room temperature (25-30 ℃), filtering and discharging the reaction liquid to obtain the transparent conductive adhesive composition.
The conductive adhesive composition is coated with a dry adhesive film of 25 mu m on a PET release film, is thermally cured at 110 ℃, is then transferred and coated on a copper foil substrate of 45 mu m, has a transparent adhesive layer, and shows the primary color of the copper foil after being bonded with the copper foil. The 180 DEG peel strength (SUS) was 1850 gf/in, the horizontal resistance was 155 m.OMEGA/sq, and the vertical resistance was 50 m.OMEGA/in2。
Example 2.
Simultaneously adding 80 parts of ethyl methacrylate, 13 parts of vinyl acrylate, 7 parts of methacrylic acid, 8 parts of lithium chloride, 2 parts of sodium polyacrylate, 5 parts of polyethylene glycol diacrylate and 40 parts of toluene into a reaction bottle, stirring to uniformly mix the materials to form a uniform and transparent solution, raising the temperature of the reaction bottle to 55 ℃, adding 2 parts of toluene solution of 12 parts of benzoyl peroxide, continuously raising the temperature to 80 ℃, and stirring for reaction for 5 hours. And (3) when the temperature of the reaction system is reduced to room temperature (25-30 ℃), filtering and discharging the reaction solution to obtain the transparent conductive adhesive composition.
The conductive adhesive composition is coated with a dry adhesive film of 15 micrometers on a PET release film, the PET release film is subjected to UV illumination (365 nm, 500W) for 10min and then is coated on a copper foil substrate of 45 micrometers in a transfer manner, the adhesive layer is transparent, and the original color of the copper foil is presented after the copper foil is attached. The 180 DEG peel strength (SUS) was 1000 gf/in, the horizontal resistance was 137 m.OMEGA/sq, and the vertical resistance was 57 m.OMEGA/in2。
Example 3.
Adding isopropyl methacrylate (86), (methyl) epoxy acrylate (8 parts), acrylonitrile (6 parts), lithium bis (trifluoromethylsulfonyl imide) (9 parts), sodium polystyrene sulfonate (1 part), polyethylene glycol diacrylate (5 parts) and toluene (45 parts) into a reaction bottle at the same time, stirring to uniformly mix the materials and form a uniform and transparent solution, raising the temperature of the reaction bottle to 60 ℃, adding a mixed solution of toluene diisocyanate (15 parts) and toluene (5 parts), and continuing to stir for reaction for 4 hours. And (3) when the temperature of the reaction system is reduced to room temperature (25-30 ℃), filtering and discharging the reaction solution to obtain the transparent conductive adhesive composition.
The conductive adhesive composition is directly coated with a 20-micron dry adhesive film on a 45-micron copper foil substrate, is put in a drying oven at 110 ℃ for curing for 3-5min, is taken out to be attached to a PET release film, and has a transparent adhesive layer, and the copper foil is attached to the PET release film to show the original color of the copper foil. The 180 DEG peel strength (SUS) was 1450 gf/in, the horizontal resistance was 133 m.OMEGA./sq, and the vertical resistance was 34 m.OMEGA./in2。
Example 4.
Adding 80 parts of n-propyl acrylate, 10 parts of propylene glycol di (meth) acrylate, 10 parts of methyl acrylate, 6 parts of lithium tetrafluoroborate, 6 parts of polyethylene glycol diacrylate and 40 parts of toluene into a reaction bottle at the same time, stirring to uniformly mix the materials to form a uniform and transparent solution, heating the temperature of the reaction bottle to 60 ℃, adding a mixed solution of 15 parts of toluene diisocyanate and 5 parts of toluene, continuously stirring for reaction for 4 hours, cooling the temperature of a reaction system to room temperature (25-30 ℃), and filtering and discharging the reaction solution to obtain the transparent conductive adhesive composition.
The conductive adhesive composition is coated with a dry adhesive film of 25 micrometers on two PET release films in a scraping way, the dry adhesive film is thermally cured at 110 ℃, the dry adhesive film is coated on two sides of a copper foil base material of 45 micrometers in a transferring way, the adhesive layer is transparent, and the original color of the copper foil is presented after the copper foil is attached. The 180 DEG peel strength (SUS) was found to be 1790 gf/in on one side, 2000gf/in on one side, 106 and 135 m.OMEGA/sq in horizontal resistance and 38 m.OMEGA/in vertical resistance, respectively2。
Example 5.
Adding butyl acrylate (85 parts), urethane acrylate (15 parts), lithium bis (trifluoromethylsulfonyl imide) (8 parts), sodium polyvinyl sulfonate (2 parts), polyethylene glycol diacrylate (5 parts) and toluene (35 parts) into a reaction bottle at the same time, stirring to uniformly mix the materials and form a uniform and transparent solution, raising the temperature of the reaction bottle to 60 ℃, adding a toluene (5 parts) solution of toluene diisocyanate (15 parts), and continuing to stir for reaction for 4 hours. And (3) when the temperature of the reaction system is reduced to room temperature (25-30 ℃), filtering and discharging the reaction solution to obtain the transparent conductive adhesive composition.
The conductive adhesive composition is coated with a dry adhesive film of 20 mu m on a PET release film in a scraping way, is thermally cured at 110 ℃, is then coated on a conductive cloth substrate of 30 mu m in a transferring way, has a transparent adhesive layer, and shows the original color of the copper foil after being attached with the copper foil. The 180 DEG peel strength (SUS) was 2110gf/in, the horizontal resistance was 112 m.OMEGA./sq, and the vertical resistance was 36 m.OMEGA./in2。
Example 6.
Adding 81 parts of n-propyl methacrylate, 10 parts of ethylene glycol diacrylate, 9 parts of ethyl acrylate, 9 parts of lithium hexafluorophosphate, 5 parts of polyethylene glycol diacrylate and 40 parts of toluene into a reaction bottle at the same time, stirring to uniformly mix the materials to form a uniform and transparent solution, raising the temperature of the reaction bottle to 60 ℃, adding a mixed solution of 15 parts of toluene diisocyanate and 4 parts of toluene, and continuing to stir for reaction for 4 hours. And (3) when the temperature of the reaction system is reduced to room temperature (25-30 ℃), filtering and discharging the reaction solution to obtain the transparent conductive adhesive composition.
The conductive adhesive composition is coated with a dry adhesive film of 15 micrometers on a PET release film in a blade mode, the PET release film is subjected to UV (365 nm, 500W) illumination for 10min and then is coated on a conductive cloth substrate of 30 micrometers in a transfer mode, the adhesive layer is transparent, and the conductive cloth is attached to the conductive cloth to form primary-color gray color of the conductive cloth. The 180 DEG peel strength (SUS) was 1500 gf/in, the horizontal resistance was 121 m.OMEGA/sq, and the vertical resistance was 62 m.OMEGA/in2。
Example 7.
Adding tert-butyl methacrylate (83 parts), butanediol di (meth) acrylate (10 parts), acrylic acid (7 parts), lithium bis (trifluoromethylsulfonyl imide) (7 parts), sodium polymethacrylate (3 parts), polyethylene glycol diacrylate (5 parts) and toluene (40 parts) into a reaction bottle at the same time, stirring to uniformly mix the materials and form a uniform and transparent solution, heating the reaction bottle to 60 ℃, adding a toluene (4 parts) solution of toluene diisocyanate (15 parts), and continuing to stir for reaction for 4 hours. And (3) when the temperature of the reaction system is reduced to room temperature (25-30 ℃), filtering and discharging the reaction solution to obtain the transparent conductive adhesive composition.
The conductive adhesive composition is directly coated with a 20-micron dry adhesive film on a 30-micron conductive cloth substrate, is put in a drying oven at 110 ℃ for curing for 3-5min, is taken out to be attached to a PET release film, and has a transparent adhesive layer, and the conductive cloth is attached to be in grey primary color. The 180 DEG peel strength (SUS) was 1850 gf/in, the horizontal resistance was 133 m.OMEGA/sq, and the vertical resistance was 34 m.OMEGA/in2。
Example 8.
Adding methyl acrylate (85 parts), ethylene glycol di (meth) acrylate (5 parts), tert-butyl acrylate (10 parts), lithium bis (trifluoromethylsulfonyl imide) (7 parts), sodium polyacrylate (3 parts), polyethylene glycol diacrylate (6 parts) and toluene (35 parts) into a reaction bottle at the same time, stirring to uniformly mix the materials and form a uniform and transparent solution, raising the temperature of the reaction bottle to 60 ℃, adding a toluene (5 parts) solution of toluene diisocyanate (15 parts), and continuing to stir for reaction for 4 hours. And (3) when the temperature of the reaction system is reduced to room temperature (25-30 ℃), filtering and discharging the reaction solution to obtain the transparent conductive adhesive composition.
The conductive adhesive composition is coated with a dry adhesive film of 25 mu m on two PET release films in a scraping way, is thermally cured at 110 ℃, is coated on two sides of a conductive cloth base material of 30 mu m in a transferring way, has a transparent adhesive layer, and presents the primary color gray of the conductive cloth after being attached with the conductive cloth. The 180 DEG peel strength (SUS) was measured to be 2280gf/in for one side, 1860gf/in for one side, 97 and 114m omega/sq for horizontal resistance, and 41 m omega/in for vertical resistance2。
Comparative example.
Adding 85 parts of methyl acrylate, 5 parts of ethylene glycol di (meth) acrylate, 10 parts of tert-butyl acrylate, 10 parts of conductive nickel powder, 6 parts of polyethylene glycol diacrylate and 35 parts of toluene into a reaction bottle at the same time, stirring to uniformly mix the materials to form a uniform gray solution, heating the temperature of the reaction bottle to 60 ℃, adding 5 parts of toluene diisocyanate (15 parts) solution, and continuing to stir for reaction for 4 hours. And (3) when the temperature of the reaction system is reduced to room temperature (25-30 ℃), filtering and discharging the reaction solution to obtain the transparent conductive adhesive composition.
The conductive adhesive composition is coated with a dry adhesive film of 25 mu m on two PET release films in a scraping way, is thermally cured at 110 ℃, and is then coated to two sides of a conductive cloth substrate of 30 mu m in a transferring way. Because the nickel powder is dispersed in the glue system, the nickel powder is distributed on the glue surface in a black spot shape after being cured, and the transparency of the glue layer is reduced (less than 90 percent). The grey color of the conductive cloth still appears after the conductive cloth is attached.
The scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution of the present invention and the inventive concept within the technical scope of the present invention.
Claims (10)
1. A transparent conductive adhesive composition is characterized in that: the transparent conductive adhesive composition does not contain a solid conductive filler and consists of the following components in parts by weight:
100 parts of mixed monomers;
5-6 parts of a cross-linking agent;
1-10 parts of ionic conductive compound;
1.0-2.0 parts of curing agent;
20-50 parts of a non-alcohol solvent;
the ionic conductive compound is at least one of sodium polyacrylate, sodium polymethacrylate, sodium polyvinyl sulfonate, sodium polystyrene sulfonate, lithium bis (trifluoromethyl sulfimide), lithium chloride, lithium tetrafluoroborate and lithium hexafluorophosphate.
2. The transparent conductive adhesive composition of claim 1, wherein: the mixed monomer comprises
(I) 80-98 parts by weight of an acrylic monomer or an alkyl-substituted acrylic monomer having 1-10 carbon atoms; and
(II) a monomer containing a crosslinking group, wherein the weight part is 2-20.
3. The transparent conductive adhesive composition of claim 2, wherein: the acrylic monomer or alkyl substituted acrylic monomer with the carbon atom number of 1-10 is at least one of acrylic acid, methacrylic acid, methyl acrylate, ethyl acrylate, methyl methacrylate, ethyl methacrylate, n-propyl acrylate, isopropyl acrylate, butyl methacrylate, tert-butyl acrylate, n-propyl methacrylate, isopropyl methacrylate, tert-butyl methacrylate and acrylonitrile.
4. The transparent conductive adhesive composition of claim 2, wherein: the crosslinking group-containing monomer includes at least one of vinyl (meth) acrylate, epoxy acrylate, urethane acrylate, ethylene glycol diacrylate, ethylene glycol di (meth) acrylate, propylene glycol di (meth) acrylate, butylene glycol di (meth) acrylate, (neo) pentanediol di (meth) acrylate, pentaerythritol di (meth) acrylate, hexanediol diacrylate, and hexanediol di (meth) acrylate.
5. The transparent conductive adhesive composition of claim 1, wherein: the cross-linking agent is at least one of polyethylene glycol diacrylate, butadiene, isoprene, octadiene and octadecadiene.
6. The transparent conductive adhesive composition of claim 1, wherein: the curing agent is isocyanate curing agent.
7. The transparent conductive adhesive composition of claim 1, wherein: the curing agent is toluene diisocyanate or diphenyl methyl diisocyanate.
8. The transparent conductive adhesive composition of claim 1, wherein: the non-alcohol solvent is at least one of esters, aliphatic hydrocarbons, aromatic hydrocarbons, alicyclic hydrocarbons and ketones.
9. The transparent conductive adhesive composition according to any one of claims 1 to 8, wherein: the preparation method adopts a solution polymerization method and a bulk polymerization method.
10. Use of the transparent conductive adhesive composition according to any one of claims 1 to 8 in a conductive tape.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010051014.1A CN111087941A (en) | 2020-01-17 | 2020-01-17 | Transparent conductive adhesive composition and preparation and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114106708A (en) * | 2020-08-31 | 2022-03-01 | 南北兄弟药业投资有限公司 | Transparent conductive adhesive composition, transparent conductive film and preparation method thereof |
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| CN1884415A (en) * | 2005-06-24 | 2006-12-27 | 东洋油墨制造株式会社 | Antistatic acroleic acid binding agent |
| CN104342072A (en) * | 2013-07-23 | 2015-02-11 | 藤森工业株式会社 | Adhesive composition, adhesive film and surface protection film |
| CN108690535A (en) * | 2017-04-07 | 2018-10-23 | 藤森工业株式会社 | Adhesion agent composition and adhesive film |
| JP2019196501A (en) * | 2019-08-09 | 2019-11-14 | 藤森工業株式会社 | Surface protective film |
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| CN1884415A (en) * | 2005-06-24 | 2006-12-27 | 东洋油墨制造株式会社 | Antistatic acroleic acid binding agent |
| CN104342072A (en) * | 2013-07-23 | 2015-02-11 | 藤森工业株式会社 | Adhesive composition, adhesive film and surface protection film |
| CN108690535A (en) * | 2017-04-07 | 2018-10-23 | 藤森工业株式会社 | Adhesion agent composition and adhesive film |
| JP2019196501A (en) * | 2019-08-09 | 2019-11-14 | 藤森工業株式会社 | Surface protective film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114106708A (en) * | 2020-08-31 | 2022-03-01 | 南北兄弟药业投资有限公司 | Transparent conductive adhesive composition, transparent conductive film and preparation method thereof |
| CN114106708B (en) * | 2020-08-31 | 2023-07-21 | 南北兄弟药业投资有限公司 | Transparent conductive adhesive composition, transparent conductive film and preparation method thereof |
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