CN101698784B - Pressure sensitive conductive adhesive composition and preparation method thereof - Google Patents
Pressure sensitive conductive adhesive composition and preparation method thereof Download PDFInfo
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- CN101698784B CN101698784B CN2009100938478A CN200910093847A CN101698784B CN 101698784 B CN101698784 B CN 101698784B CN 2009100938478 A CN2009100938478 A CN 2009100938478A CN 200910093847 A CN200910093847 A CN 200910093847A CN 101698784 B CN101698784 B CN 101698784B
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Abstract
The invention discloses a pressure sensitive conductive adhesive composite and a preparation method thereof, belonging to the adhesive field. The composite comprises pressure sensitive adhesive and metal conductive particles, wherein, the metal conductive particles account for 30-80% of the total weight of the pressure sensitive adhesive; the pressure sensitive adhesive comprises the following components in percentage by weight: 30-50% of crylic acid soft monomer, 5-20% of crylic acid hard monomer, 0.5-2.5% of functional monomer containing carboxyl, 0.5-2.5% of cross linking monomer containing carboxyl, 40-60% of non alcohols solvent, 0.2-2.0% of oil soluble initiator and 0.01-0.2% of mercaptan chain transfer agent. The preparation method comprises the following steps: firstly preparing pressure sensitive adhesive, adding metal conductive particles into the prepared pressure sensitive adhesive to obtain the composite. In the invention, the pure crylic acid system is adopted to be matched with the high-low glass state temperature monomer to adjust the distribution of proper molecular weight and molecular weight to obtain the pressure sensitive adhesive with high initial viscidity and high hold viscidity and low-impedance composite adhesive.
Description
Technical field
The invention belongs to the polymer binder technical field, particularly relate to a kind of pressure sensitive conductive adhesive composite and preparation method thereof.
Background technology
The exploitation of domestic conductive resin is along with the exploitation of conducting polymer just launches, but base material mainly concentrates on epoxy, polyester and rubber structure, and it is less relatively to conduct electricity the exploitation of pressure sensitive adhesive in the vinylformic acid system.Patent CN1158745A provides a kind of conductive resin, but what adopt is the vinylformic acid system, and in the selection of electro-conductive material, adopts alkali-metal salt to do the inorganic conductive particle, big limitations the electroconductibility of system, restricted this tackiness agent in wider use.
Summary of the invention
The embodiment of the invention provides a kind of pressure sensitive conductive adhesive composite and preparation method thereof, can make high just gluing with height and hold compound conductive adhesive sticking, that resistance value is lower than 20ohmn/SQ inch.
The present invention realizes through following technical proposals:
The embodiment of the invention provides a kind of pressure sensitive conductive adhesive composite; This pressure sensitive conductive adhesive composite is made up of pressure sensitive adhesive and metal conductive particles; Metal conductive particles accounts for 30～80% of pressure sensitive adhesive gross weight, and wherein pressure sensitive adhesive is made up of each component of following weight percent:
Acrylic acid or the like soft monomer 30～50%, acrylic acid or the like hard monomer 5～20%, contain carboxyl class function monomer 0.5～2.5%, hydroxyl class cross-linking monomer 0.5～2.5, non-alcoholic solvent 40～60%, oil-soluble initiator 0.2～2.0% and mercaptan type chain transfer agent 0.01～0.2%.
The embodiment of the invention also provides a kind of preparation method of pressure sensitive conductive adhesive composite, comprising:
Get each raw material by following mass percent: acrylic acid or the like soft monomer 30～50%, acrylic acid or the like hard monomer 5～20%, contain carboxyl class function monomer 0.5～2.5%, hydroxyl class cross-linking monomer 0.5～2.5, non-alcoholic solvent 40～60%, oil-soluble initiator 0.2～2.0% and mercaptan type chain transfer agent 0.01～0.2%;
With the non-alcoholic solvent that accounts for non-alcoholic solvent gross weight 2/3, account for acrylic acid or the like soft monomer, acrylic acid or the like hard monomer, contain the monomer mixture of the monomer mixture gross weight 1/3 of carboxyl class function monomer and hydroxyl class cross-linking monomer, the oil-soluble initiator that accounts for oil-soluble initiator gross weight 1/3 adds reaction kettle; Temperature of reaction kettle is risen to 75～78 ℃; Reaction 1～1.5h; With remaining acrylic acid or the like soft monomer, acrylic acid or the like hard monomer, contain the mixed solution of carboxyl class function monomer, hydroxyl class cross-linking monomer, non-alcoholic solvent, oil-soluble initiator; In 3～4h, drip in the reaction system that gets in the reaction kettle; Insulation adds the mercaptan type chain transfer agent cooling at 70 ℃～80 ℃ slaking 3～4h;
When the temperature of question response system is reduced to below 50 ℃, with the conducting particles that accounts for said reaction system weight 30～80% under agitation, evenly splash in the reaction system; After treating that conducting particles adds; Behind dispersed with stirring 1～2h, filter discharging, promptly obtain pressure sensitive conductive adhesive composite of the present invention.
Effect of the present invention and advantage: adopt the pure acrylic acid system in the embodiment of the invention; Utilize the monomeric collocation of high low Tg; Regulate suitable molecular weight and MWD; Obtain high just sticking height and hold sticking pressure sensitive adhesive system, adopt excellent inorganic conductive particle of electroconductibility and the collocation of pressure-sensitive resin, make the composite adhesive that resistance value is lower than 20ohmn/SQ inch.
Embodiment
Below in conjunction with specific embodiment the present invention is described further.
Embodiment 1
Present embodiment 1 provides a kind of pressure sensitive conductive adhesive composite that has than low impedance value; It is a kind of conduction pressure sensitive adhesive of forming by pressure sensitive adhesive and metal conductive particles; Metal conductive particles accounts for 30～80% of pressure sensitive adhesive gross weight; Wherein, the composition of pressure sensitive adhesive (percentage composition meter by weight) is as follows:
Acrylic acid or the like soft monomer 30～50%, acrylic acid or the like hard monomer 5～20%, contain carboxyl class function monomer 0.5～2.5%, hydroxyl class cross-linking monomer 0.5～2.5, non-alcoholic solvent 40～60%, oil-soluble initiator 0.2～2.0%, mercaptan type chain transfer agent 0.01～0.2%.
Acrylic acid or the like soft monomer in the above-mentioned pressure sensitive conductive adhesive composite comprises: any in ethyl propenoate, Bing Xisuandingzhi, NSC 20956, EHA, the Isooctyl acrylate monomer or any several kinds compsn.
The acrylic acid or the like hard monomer comprises: any in methyl acrylate, vinyl acetate between to for plastic, TEB 3K, the vinyl cyanide etc. or any several kinds compsn.
Containing carboxyl class function monomer comprises: any in vinylformic acid, the methylacrylic acid or two kinds of mixing.
Hydroxyl class cross-linking monomer comprises: Hydroxyethyl acrylate, Propylene glycol monoacrylate, Rocryl 400, any in the Rocryl 410 or any several kinds compsn.
Non-alcoholic solvent comprises: any in ETHYLE ACETATE, toluene, the YLENE etc. or any several kinds mixture.
Oil-soluble initiator comprises: any in azo-initiator and the superoxide or any several kinds compsn.
Mercaptan type chain transfer agent mainly is meant lauryl mercaptan.
Metal conductive particles in the above-mentioned pressure sensitive conductive adhesive composite comprises: one or more in conduction silver powder, copper powder, aluminium powder, nickel powder, silver-plated copper powder, silvered aluminum powder, the milled fibre, it accounts for 30～80% of weight resin deal.
The preparation method of above-mentioned pressure sensitive conductive adhesive composite comprises the steps:
With the non-alcoholic solvent that accounts for non-alcoholic solvent gross weight 2/3, account for acrylic acid or the like soft monomer, acrylic acid or the like hard monomer, contain the monomer mixture of the monomer mixture gross weight 1/3 of carboxyl class function monomer and hydroxyl class cross-linking monomer, the oil-soluble initiator that accounts for oil-soluble initiator gross weight 1/3 adds reaction kettle; Temperature of reaction kettle is risen to 75～78 ℃; Reaction 1～1.5h; With remaining acrylic acid or the like soft monomer, acrylic acid or the like hard monomer, contain the mixed solution of carboxyl class function monomer, hydroxyl class cross-linking monomer, non-alcoholic solvent, oil-soluble initiator; In 3～4h, drip in the reaction system that gets in the reaction kettle; Insulation adds the mercaptan type chain transfer agent cooling at 70 ℃～80 ℃ slaking 3～4h;
When the temperature of question response system (being pressure sensitive adhesive) is reduced to below 50 ℃; With the conducting particles that accounts for said reaction system weight 30～80% under high-speed stirring; Evenly splash in the reaction system when splashing into (so that reach better dispersion effect), treat that conducting particles adds after, behind the dispersed with stirring 1h; Filter discharging, promptly obtain pressure sensitive conductive adhesive composite of the present invention.
Adopt the pure acrylic acid system in the present embodiment; Utilize the monomeric collocation of high low Tg; Regulate suitable molecular weight and MWD; Obtain high just sticking height and hold sticking pressure sensitive adhesive system, adopt excellent inorganic conductive particle of electroconductibility and the collocation of pressure-sensitive resin, make the composite adhesive that resistance value is lower than 20ohmn/SQ inch.
Adopt the pure acrylic acid system in the present embodiment; Utilize the monomeric collocation of high low Tg; Regulate suitable molecular weight and MWD; Obtain high just sticking height and hold sticking pressure sensitive adhesive system, adopt excellent inorganic conductive particle of electroconductibility and the collocation of pressure-sensitive resin, make the composite adhesive that resistance value is lower than 20ohmn/SQ inch.
Embodiment 2
The embodiment of the invention provides a kind of pressure sensitive conductive adhesive composite that has than low impedance value, and this pressure sensitive conductive adhesive composite mainly is made up of pressure sensitive adhesive and metal conductive particles, and wherein the composition of pressure sensitive adhesive and weight percentage are following:
Pressure-sensitive resin raw material weight
Isooctyl acrylate monomer (EHA) 220kg
Ethyl propenoate (EA) 150kg
TEB 3K (MMA) 130kg
Vinylformic acid (AA) 10kg
Hydroxyethyl acrylate (HEA) 15kg
Propylene glycol monoacrylate (HPA) 5kg
Lucidol (BPO) 9kg
ETHYLE ACETATE 320kg
Toluene 140kg
Dodecyl Mercaptan 11kg
The conducting particles raw material weight
Copper powder 150kg
Silver-plated copper powder 50kg
The preparation method of above-mentioned pressure sensitive conductive adhesive composite comprises the steps:
Non-alcoholic solvent (mixture of ETHYLE ACETATE and toluene) 308kg and monomer mixture (being comprised: 177kg and 3Kg Lucidol (BPO) the adding reaction kettle mixture of Isooctyl acrylate monomer (EHA), ethyl propenoate (EA), TEB 3K (MMA), vinylformic acid (AA), Hydroxyethyl acrylate (HEA) and Propylene glycol monoacrylate (HPA)); Temperature of reaction kettle is risen to 75～78 ℃; Reaction 1～1.5h; Whole residual monomers mixtures (comprising: Isooctyl acrylate monomer (EHA), ethyl propenoate (EA), TEB 3K (MMA), vinylformic acid (AA), Hydroxyethyl acrylate (HEA) and Propylene glycol monoacrylate (HPA)) are mixed the mixed solution that the back forms with ETHYLE ACETATE, toluene, Lucidol (BPO); In 3～4h, drip and get into reaction system; Insulation adds the cooling of chain-transfer agent Dodecyl Mercaptan at 80 ℃ of left and right sides slaking 3～4h;
When the temperature of question response system (pressure sensitive adhesive that promptly makes) is reduced to below 50 ℃; Under high-speed stirring, evenly slowly join in the reaction system conducting particles (copper powder and silver-plated copper powder); After treating that conducting particles adds; After high-speed stirring is disperseed 1h, filter discharging, promptly get pressure sensitive conductive adhesive composite.
Adopt the pure acrylic acid system in the present embodiment; Utilize the monomeric collocation of high low Tg; Regulate suitable molecular weight and MWD; Obtain high just sticking height and hold sticking pressure sensitive adhesive system, adopt excellent inorganic conductive particle of electroconductibility and the collocation of pressure-sensitive resin, make the composite adhesive that resistance value is lower than 20ohmn/SQ inch.
Embodiment 3
The embodiment of the invention three provides a kind of pressure sensitive conductive adhesive composite that has than low impedance value, and this pressure sensitive conductive adhesive composite mainly is made up of pressure sensitive adhesive and metal conductive particles, and wherein the composition of pressure sensitive adhesive and weight percentage are following:
Raw material weight
Bing Xisuandingzhi 380kg
Methyl acrylate 70kg
TEB 3K 50kg
Vinylformic acid 10kg
Methylacrylic acid 5kg
Hydroxyethyl acrylate 20kg
Lucidol 10kg
ETHYLE ACETATE 204kg
Toluene 250kg
Dodecyl Mercaptan 1kg
The conducting particles raw material weight
Silvered aluminum powder 70kg
Milled fibre 180kg
The preparation method of above-mentioned pressure sensitive conductive adhesive composite is following:
, comprise the steps:
Non-alcoholic solvent (mixture of ETHYLE ACETATE and toluene) 300kg and monomer mixture (being comprised: 182kg and 3.3Kg Lucidol (BPO) the adding reaction kettle mixture of Isooctyl acrylate monomer (EHA), ethyl propenoate (EA), TEB 3K (MMA), vinylformic acid (AA), Hydroxyethyl acrylate (HEA) and Propylene glycol monoacrylate (HPA)); Temperature of reaction kettle is risen to 75～78 ℃; Reaction 1～1.5h; Mixed solution with whole residual monomers (comprising: Isooctyl acrylate monomer (EHA), ethyl propenoate (EA), TEB 3K (MMA), vinylformic acid (AA), Hydroxyethyl acrylate (HEA) and Propylene glycol monoacrylate (HPA)), ETHYLE ACETATE, toluene, Lucidol (BPO); In 3～4h, drip the entering system; Insulation adds the chain-transfer agent cooling at 80 ℃ of left and right sides slaking 3～4h;
When the temperature of question response system (being the pressure sensitive adhesive that makes) is reduced to below 50 ℃; Under high-speed stirring, evenly slowly join in the reaction system conducting particles (silvered aluminum powder and milled fibre); After treating that conducting particles adds; Behind the dispersed with stirring 2h, filter discharging, promptly get pressure sensitive conductive adhesive composite.
Above-mentioned each embodiment is made pressure sensitive conductive adhesive composite detect, detected result is following:
| Test item | Embodiment 2 | Embodiment 3 |
| Resistance value (ohmn/SQ inch) | 0.9 | 7.1 |
| Stripping strength (N/15mm) | 8.3 | 11.6 |
In sum; In the embodiment of the invention be that solvent adopts solution polymerization process to synthesize the polyacrylate composition of high-peeling strength and pressure-sensitive property with ETHYLE ACETATE, interpolation accounting for weight resin part 5～20% Gum Rosins when reaction finishes, and adopts high speed dispersion then; The conducting particles of weight resin deal 30～80% is dispersed in the pressure-sensitive adhesive system processes pressure sensitive conductive adhesive composite; This pressure sensitive conductive adhesive composite has the initial viscosity height, and it is good to hold viscosity, pressure-sensitive low advantage.
The above; Be merely the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, any technician who is familiar with the present technique field is in the technical scope that the present invention discloses; The variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (6)
1. pressure sensitive conductive adhesive composite; It is characterized in that; This pressure sensitive conductive adhesive composite is made up of pressure sensitive adhesive and metal conductive particles, and metal conductive particles accounts for 30～80% of pressure sensitive adhesive gross weight, and wherein pressure sensitive adhesive is made up of each component of following weight percent:
Acrylic acid or the like soft monomer 30～50%, acrylic acid or the like hard monomer 5～20%, contain carboxyl class function monomer 0.5～2.5%, hydroxyl class cross-linking monomer 0.5～2.5%, non-alcoholic solvent 40～60%, oil-soluble initiator 0.2～2.0% and mercaptan type chain transfer agent 0.01～0.2%;
Said acrylic acid or the like soft monomer is: any in ethyl propenoate, Bing Xisuandingzhi, NSC 20956, EHA, the Isooctyl acrylate monomer or any several kinds mixture;
Said acrylic acid or the like hard monomer is: any in methyl acrylate, vinyl acetate between to for plastic, TEB 3K, the vinyl cyanide or any several kinds mixture;
The said carboxyl class function monomer that contains is: any in vinylformic acid, the methylacrylic acid or any two kinds mixture;
Said hydroxyl class cross-linking monomer is: Hydroxyethyl acrylate, Propylene glycol monoacrylate, Rocryl 400, any one in the Rocryl 410 or any several kinds compsn.
2. pressure sensitive conductive adhesive composite as claimed in claim 1 is characterized in that, the non-alcoholic solvent in the said pressure sensitive adhesive comprises:
In ETHYLE ACETATE, toluene, the YLENE any or any several kinds mixture.
3. pressure sensitive conductive adhesive composite as claimed in claim 1 is characterized in that, the oil-soluble initiator in the said pressure sensitive adhesive comprises:
The mixture of any in azo class and the superoxide or two kinds.
4. pressure sensitive conductive adhesive composite as claimed in claim 1 is characterized in that, the mercaptan type chain transfer agent in the said pressure sensitive adhesive is a lauryl mercaptan.
5. pressure sensitive conductive adhesive composite as claimed in claim 1 is characterized in that, said metal conductive particles comprises: any in conduction silver powder, copper powder, aluminium powder, nickel powder, silver-plated copper powder, the silvered aluminum powder or any several kinds.
6. the preparation method of one kind pressure sensitive conductive adhesive composite is characterized in that, comprising:
Get each raw material by following mass percent: acrylic acid or the like soft monomer 30～50%, acrylic acid or the like hard monomer 5～20%, contain carboxyl class function monomer 0.5～2.5%, hydroxyl class cross-linking monomer 0.5～2.5%, non-alcoholic solvent 40～60%, oil-soluble initiator 0.2～2.0% and mercaptan type chain transfer agent 0.01～0.2%;
Wherein, said acrylic acid or the like soft monomer is: any in ethyl propenoate, Bing Xisuandingzhi, NSC 20956, EHA, the Isooctyl acrylate monomer or any several kinds mixture;
Said acrylic acid or the like hard monomer is: any in methyl acrylate, vinyl acetate between to for plastic, TEB 3K, the vinyl cyanide or any several kinds mixture;
The said carboxyl class function monomer that contains is: any in vinylformic acid, the methylacrylic acid or any two kinds mixture;
Said hydroxyl class cross-linking monomer is: Hydroxyethyl acrylate, Propylene glycol monoacrylate, Rocryl 400, any one in the Rocryl 410 or any several kinds compsn;
With the non-alcoholic solvent that accounts for non-alcoholic solvent gross weight 2/3, account for acrylic acid or the like soft monomer, acrylic acid or the like hard monomer, contain the monomer mixture of the monomer mixture gross weight 1/3 of carboxyl class function monomer and hydroxyl class cross-linking monomer, the oil-soluble initiator that accounts for oil-soluble initiator gross weight 1/3 adds reaction kettle; Temperature of reaction kettle is risen to 75～78 ℃; Reaction 1～1.5h; With remaining acrylic acid or the like soft monomer, acrylic acid or the like hard monomer, contain the mixed solution of carboxyl class function monomer, hydroxyl class cross-linking monomer, non-alcoholic solvent, oil-soluble initiator; In 3～4h, drip in the reaction system that gets in the reaction kettle; Insulation adds the mercaptan type chain transfer agent cooling at 70 ℃～80 ℃ slaking 3～4h;
When the temperature of question response system is reduced to below 50 ℃, with the conducting particles that accounts for said reaction system weight 30～80% under agitation, evenly splash in the reaction system; After treating that conducting particles adds; Behind dispersed with stirring 1～2h, filter discharging, promptly obtain pressure sensitive conductive adhesive composite.
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| CN101857786A (en) * | 2010-05-26 | 2010-10-13 | 北京高盟新材料股份有限公司 | Pressure-sensitive adhesive and preparation method thereof |
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| CN102477269A (en) * | 2010-11-26 | 2012-05-30 | 上海恩意材料科技有限公司 | Conductive adhesive composition |
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| CN106065299B (en) * | 2016-07-26 | 2017-11-10 | 刘睿璇 | A kind of preparation method of conductive pressure sensitive adhesive |
| CN108659747A (en) * | 2018-04-16 | 2018-10-16 | 湖州科博信息科技有限公司 | A kind of pressure sensitive conductive adhesive and preparation method thereof |
| EP3877479A4 (en) | 2018-11-08 | 2022-06-08 | Avery Dennison Corporation | Yellowing resistant psa |
| CN111394007A (en) * | 2020-04-30 | 2020-07-10 | 张家港保税区汇英聚福材料科技合伙企业(有限合伙) | High-conductivity adhesive tape |
| CN111500215B (en) * | 2020-04-30 | 2021-11-26 | 张家港保税区汇英聚福材料科技合伙企业(有限合伙) | Pressure-sensitive conductive adhesive and preparation method thereof |
| CN112300712A (en) * | 2020-11-18 | 2021-02-02 | 江苏皇冠新材料科技有限公司 | Ultraviolet curing adhesive and ultraviolet curing protective film |
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