CN104140780B - Conductive adhesive - Google Patents
Conductive adhesive Download PDFInfo
- Publication number
- CN104140780B CN104140780B CN201310406522.7A CN201310406522A CN104140780B CN 104140780 B CN104140780 B CN 104140780B CN 201310406522 A CN201310406522 A CN 201310406522A CN 104140780 B CN104140780 B CN 104140780B
- Authority
- CN
- China
- Prior art keywords
- epoxy resin
- electrically conductive
- conductive adhesive
- metal powder
- flake metal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000853 adhesive Substances 0.000 title claims abstract description 64
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 64
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 91
- 239000003822 epoxy resin Substances 0.000 claims abstract description 90
- 229910052751 metal Inorganic materials 0.000 claims abstract description 77
- 239000002184 metal Substances 0.000 claims abstract description 77
- 239000000843 powder Substances 0.000 claims abstract description 76
- 235000021122 unsaturated fatty acids Nutrition 0.000 claims abstract description 39
- 150000004670 unsaturated fatty acids Chemical class 0.000 claims abstract description 39
- 150000004671 saturated fatty acids Chemical class 0.000 claims abstract description 31
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims description 32
- 239000004593 Epoxy Substances 0.000 claims description 17
- 239000013008 thixotropic agent Substances 0.000 claims description 16
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 10
- 230000000996 additive effect Effects 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
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- 230000000052 comparative effect Effects 0.000 description 71
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- 238000000034 method Methods 0.000 description 8
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Abstract
The invention provides a conductive adhesive, which comprises 8 to 20 weight percent of epoxy resin, 10 to 25 weight percent of solvent, 0.5 to 5 weight percent of latent hardening accelerator, 3.5 to 35 weight percent of saturated fatty acid surface-treated flaky metal powder and 35 to 75 weight percent of unsaturated fatty acid surface-treated flaky metal powder.
Description
Technical field
The invention relates to a kind of electrically conductive composition, and relate to a kind of electrically conductive adhesive especially.
Background technology
Because the conductive resin containing metal-powders such as silver has good electroconductibility, so can be widely used in various e-machine part, in order to form conductor wirings.In recent years, above-mentioned conductor wirings is applied to the movable termination of mobil phone, game machine etc., the touch control screen panel etc. of PC, for example live width/the interval of conductor wirings is microminiaturized to 150 μm/150 μm, and for forming the requirement of the good fine pattern of tolerance range more very.
At present, in conventional process, usually carry out the making of conductor wirings through screen painting method.But screen painting presses by with sdueegee etc., and make conductive resin through the pattern printing on half tone on substrate.That is the screen painting genealogy of law according to by with pressings such as sdueegees, and makes half tone bend, and the method for being printed.Therefore, compared to the live width as target, carry out screen painting and the live width of print that obtains is usually comparatively large, make distribution and distribution closer to each other, and then produce the problem of contact or the edge part flushing of distribution, become the problem that boundary line does not understand etc.
In addition, the thixotropy index (thixotropicindex) of known conductive resin and printing characteristic low, therefore after carrying out screen painting, conductive resin has the shortcoming of drip immediately and cannot form the fine pattern with good accuracy.
Summary of the invention
The invention provides a kind of electrically conductive adhesive, it can be formed tolerance range is good, electroconductibility is high fine pattern.
Electrically conductive adhesive of the present invention, the potentiality hardening accelerator that the solvent that it comprises epoxy resin that content is 8wt% to 20wt%, content is 10wt% to 25wt%, content are 0.5wt% to 5wt%, content are the saturated fatty acid surface-treated flake metal powder of 3.5wt% to 35wt%, and content is the unsaturated fatty acids surface-treated flake metal powder of 35wt% to 75wt%.
In one embodiment of this invention, above-mentioned saturated fatty acid surface-treated flake metal powder and unsaturated fatty acids surface-treated flake metal powder comprise silver, copper or its alloy.
In one embodiment of this invention, the median size D50 of above-mentioned saturated fatty acid surface-treated flake metal powder and unsaturated fatty acids surface-treated flake metal powder is 0.5 μm to 20 μm, tap density is 1.1g/cm
3to 5.0g/cm
3and specific surface area is 0.5m
2/ g to 2.6m
2/ g.
In one embodiment of this invention, above-mentioned epoxy resin comprises solid epoxy resin, liquid-state epoxy resin or its combination.
In one embodiment of this invention, when combinationally using above-mentioned solid epoxy resin and liquid-state epoxy resin, the part by weight of solid epoxy resin and liquid-state epoxy resin is 9/1 to 1/9.
In one embodiment of this invention, the epoxy equivalent (weight) of above-mentioned solid epoxy resin is 1000g/eq to 20000g/eq.
In one embodiment of this invention, the weight average molecular weight of above-mentioned solid epoxy resin is 5000g/mol to 65000g/mol.
In one embodiment of this invention, the epoxy equivalent (weight) of above-mentioned liquid-state epoxy resin is 100g/eq to 1500g/eq.
In one embodiment of this invention, the weight average molecular weight of above-mentioned liquid-state epoxy resin is 100g/mol to 3000g/mol.
In one embodiment of this invention, the boiling point of above-mentioned solvent is 140 DEG C to 220 DEG C.
In one embodiment of this invention, more comprise additive, wherein relative to the weight of epoxy resin, the content of additive is 0.1wt% to 30wt%.
In one embodiment of this invention, above-mentioned additive comprises thixotropic agent, silane coupling agent, dispersion agent or its combination.
In one embodiment of this invention, with 100 parts by weight of above-mentioned epoxy resin, the content of silane coupling agent is 0.5 weight part to 25 weight part.
Based on above-mentioned, the electrically conductive adhesive that embodiments of the invention propose contains saturated fatty acid surface-treated flake metal powder and unsaturated fatty acids surface-treated flake metal powder, thus the printing characteristic of the electrically conductive adhesive that is improved, to be formed, there is the good fine pattern of tolerance range.
For above-mentioned feature and advantage of the present invention can be become apparent, special embodiment below elaborates.
Embodiment
Having good print characteristic to prepare, can form the good and meticulous pattern of tolerance range and having the electrically conductive adhesive of the advantages such as high conductivity, the present invention proposes a kind of electrically conductive adhesive, and it can reach above-mentioned advantage.In addition, electrically conductive adhesive proposed by the invention can be coated on substrate (such as ceramic substrate or glass substrate), to form conductive pattern.For example, in an electronic, described conductive pattern can be used as wire.Below especially exemplified by the example that embodiment can be implemented really according to this as the present invention.
The potentiality hardening accelerator that the solvent that the electrically conductive adhesive of the present embodiment comprises epoxy resin that content is 8wt% to 20wt%, content is 10wt% to 25wt%, content are 0.5wt% to 5wt%, content are the saturated fatty acid surface-treated flake metal powder of 3.5wt% to 35wt%, and content is the unsaturated fatty acids surface-treated flake metal powder of 35wt% to 75wt%.
Epoxy resin comprises solid epoxy resin, liquid-state epoxy resin or its combination.In the present invention, the term " solid-state " used and " liquid state " mean the state of epoxy resin under room temperature (25 DEG C).
Described solid epoxy resin can be solid-state or is the state close to solid under room temperature (25 DEG C), and can comprise one or more functional group.In addition, the epoxy equivalent (weight) of solid epoxy resin is such as 1000g/eq to 20000g/eq." epoxy equivalent (weight) " used herein means the grams (g/eq) of the resin containing epoxy group(ing) of 1 equivalent, and is the value that the method specified according to JISK7236 measures.The weight average molecular weight of solid epoxy resin is such as 5000g/mol to 65000g/mol.
Solid epoxy resin of the present invention comprises bisphenol epoxy, phenolic resin varnish, ortho-cresol novolac epoxy resins, polyfunctional epoxy resin, aminoepoxy resins, the epoxy resin containing heterocycle, the epoxy resin be substituted, naphthols epoxy resin and/or their derivative, is wherein preferably bisphenol epoxy.These solid epoxy resins can be used alone or can they the mixture of two or more use.
As solid epoxy resin, also various commercially available prod can be used.The example being suitable as the commercially available prod of solid epoxy resin comprises: bisphenol epoxy, such as YD-017H, YD-020, YD020-L, YD-014, YD-014ER, YD-013K, YD-019K, YD-019, YD-017R, YD-017, YD-012, YD-011H, YD-011S, YD-011, YDF-2004 and YDF-2001 (national capital chemistry limited-liability company); BE504H and BE509 (Changchun Artificial Resin Factory Co. Ltd.); JER4210, JER4250, JER4275 and JER1256 (Nippon Epoxy Resin Co., Ltd.); Phenolic resin varnish, such as EPIKOTE152 and EPIKOTE154 (three and synthesis limited-liability company); EPPN-201 (Japanese chemical drug limited-liability company); DN-483 (DOW Chemical limited-liability company) and YDPN-641, YDPN-638A80, YDPN-638, YDPN-637, YDPN-644 and YDPN-631 (national capital chemistry limited-liability company); Ortho-cresol novolac epoxy resins, such as YDCN-500-1P, YDCN-500-2P, YDCN-500-4P, YDCN-500-5P, YDCN-500-7P, YDCN-500-8P, YDCN-500-10P, YDCN-500-80P, YDCN-500-80PCA60, YDCN-500-80PBC60, YDCN-500-90P and YDCN-500-90PA75 (national capital chemistry limited-liability company); EOCN-102S, EOCN-103S, EOCN-104S, EOCN-1012, EOCN-1025 and EOCN-1027 (Japanese chemical drug limited-liability company); YDCN-701, YDCN-702, YDCN-703 and YDCN-704 (Dongdu changes into limited-liability company) and EPICLONN-665-EXP (large Japanese ink chemical industry limited-liability company); Bis-phenol novolac epoxy resins, such as KBPN-110, KBPN-120 and KBPN-115 (national capital chemistry limited-liability company); Polyfunctional epoxy resin, such as EPON1031S (three and synthesis limited-liability company); Araldite0163 (the different chemical company of Switzerland vapour Bart (Ciba company limited)); DENACOLEX-611, DENACOLEX-614, DENACOLEX-614B, DENACOLEX-622, DENACOLEX-512, DENACOLEX-521, DENACOLEX-421, DENACOLEX-411 and DENACOLEX-321 (length is rapids changes into limited-liability company) and EP-5200R, KD-1012, EP-5100R, KD-1011, KDT-4400A70, KDT-4400, YH-434L, YH-434 and YH-300 (national capital chemistry limited-liability company); Aminoepoxy resins, such as EPIKOTE604 (three and synthesis limited-liability company), YH-434 (Dongdu changes into limited-liability company), TETRAD-X and TETRAD-C (gas chemistry limited-liability company of Mitsubishi) and ELM-120 (Sumitomo Chemical limited-liability company); Containing the epoxy resin of heterocycle, such as PT-810 (vapour bar speciality chemical); The epoxy resin be substituted, such as ERL-4234, ERL-4299, ERL-4221 and ERL-4206 (UCC); And naphthols epoxy resin, such as EPICLONHP-4032, EPICLONHP-4032D, EPICLONHP-4700 and EPICLON4701 (large Japanese ink chemical industry limited-liability company).These solid epoxy resins can be used alone or can they the mixture of two or more use.
Described liquid-state epoxy resin is liquid epoxy resin under using room temperature (25 DEG C).In one embodiment, liquid-state epoxy resin can have about-70 to about 0 DEG C, compared with the fusing point (Tm) of Jia Yue-50 to about-10 DEG C.In addition, the epoxy equivalent (weight) of liquid-state epoxy resin is such as 100g/eq to 1500g/eq, is preferably 150g/eq to 800g/eq, and is more preferred from 150g/eq to 400g/eq.Specifically, when the epoxy equivalent (weight) of liquid-state epoxy resin is in above-mentioned scope, contribute to guaranteeing, after electrically conductive adhesive solidification of the present invention, good adhesion and high heat resistance can be had, and maintain the glass transformation temperature of electrically conductive adhesive simultaneously.
In addition, the weight average molecular weight (Mw) of liquid-state epoxy resin is such as 100g/mol to 3000g/mol.Specifically, when the weight average molecular weight of liquid-state epoxy resin is in above-mentioned scope, can contribute to guaranteeing to use electrically conductive adhesive of the present invention to have good mobility.
Liquid-state epoxy resin of the present invention can comprise bisphenol A epoxide resin, the epoxy resin of such as NPEL-127E and NPEL-128E (Nan Ya Plastics company) etc., bisphenol F epoxy resin, three or more functional epoxy resins, modified rubber, the epoxy resin of urethane modification, acrylic modified epoxy resin and/or photosensitive epoxy resin, be wherein preferably bisphenol A epoxide resin.These liquid-state epoxy resins can be used alone or can they the mixture of two or more use.
In order to obtain the electrically conductive adhesive of suitable viscosity, in one embodiment, can be used alone solid epoxy resin allocate its viscosity with solvent; In another embodiment, also may be combined with use solid epoxy resin, liquid-state epoxy resin and solvent.When combinationally using solid epoxy resin and liquid-state epoxy resin, the part by weight of solid epoxy resin and liquid-state epoxy resin is such as 9/1 to 1/9.
As solvent of the present invention, be preferably boiling point at 140 DEG C to any one high boiling solvent within the scope of 220 DEG C.Specifically, when the boiling point of solvent falls in above-mentioned scope, the problem causing printing characteristic or operability not good because volatilization causes the viscosity of electrically conductive adhesive suddenly to increase in impregnation/wire mark process can be avoided.
In one embodiment, preferred solvents comprises ketone solvent, ether solvents and acetate solvent.These solvents can be used alone, or capable of being combined two or more uses.The particular instance of ketone solvent can comprise pimelinketone.The particular instance of ether solvents can comprise ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol ether, ethylene glycol monobutyl ether, ethyleneglycol monophenylether, glycol dimethyl ether, ethylene glycol diethyl ether, ethylene glycol bisthioglycolate propyl ether, ethylene glycol dibutyl ether, ethylene diphenyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monopropyl ether, diethylene glycol monobutyl ether, diglycol monotertiary phenylate, diglyme, diethyl carbitol, glycol ether dipropyl ether, diethylene glycol dibutyl ether, glycol ether hexichol and propylene glycol monomethyl ether.The particular instance of acetate solvent comprises glycol-monoacetin, ethylene glycol monomethyl ether acetate, ethylene glycol monoethyl ether acetate, ethylene glycol ether acetic ester, ethylene glycol monomethyl ether acetate (2-BXA), ethyleneglycol monophenylether acetic ester, ethylene diacetate, diethylene glycol monomethyl acetic ester, carbiphene acetic ester (DGMEA), diethylene glycol monobutyl ehter acetic ester, diethylene glycol acetate, propylene glycol monomethyl ether acetate, and PGDA.
In addition, preferred solvents of the present invention is by least one selected in diglyme, ethylene glycol monobutyl ether, ethylene glycol monomethyl ether acetate, ethylene glycol monoethyl ether acetate, ethylene glycol monomethyl ether acetate (2-BXA), carbiphene acetic ester (DGMEA), propylene glycol monomethyl ether acetate, PGDA.
As potentiality hardening accelerator of the present invention, can be used under room temperature (25 DEG C) in insoluble solid-state in epoxy resin, and via the compound just had after heating for dissolving as hardening accelerator function.
In one embodiment, potentiality hardening accelerator is imidazolium compounds system potentiality hardening accelerator, the solid dispersing amine-epoxy adduct system potentiality hardening accelerator of solid under being included in normal temperature, the reaction product of such as amine compound and epoxy compounds, solid dispersing amine-urea adduct system potentiality hardening accelerator, the reaction product etc. of such as amine compound and isocyanate compound or urea compounds.
The example of imidazolium compounds system used in the present invention potentiality hardening accelerator comprises 2-heptadecyl imidazole, 2-phenyl-4, 5-hydroxymethyl-imidazole, 2-undecyl imidazole, 2 phenyl 4 methyl 5 hydroxy methylimidazole, glyoxal ethyline, 2-phenylimidazole, 2-phenyl-4-methylimidazole, 1-cyanoethyl-2-phenylimidazole, 1-1-cyanoethyl-2-methylimidazole-trimellitate, 1-cyanoethyl-2-phenylimidazole-trimellitate, N-(glyoxal ethyline quinoline-1-ethyl)-urea, N, N ' (glyoxal ethyline quinoline-(1)-ethyl)-adipyl diamide etc., but be not limited to this.
The example of the epoxy compounds in solid dispersing amine used in the present invention-epoxy adduct system potentiality hardening accelerator comprises the polyglycidyl ether that the multivalence phenol such as dihydroxyphenyl propane, Bisphenol F, pyrocatechol, Resorcinol or the polyvalent alcohol such as glycerol and polyoxyethylene glycol and Epicholorohydrin react gained; The hydroxycarboxylic acid of p-hydroxy Benzoic Acid, β-oxynaphthoic acid and Epicholorohydrin react the Racemic glycidol ether-ether of gained; The poly carboxylic acid of phthalic acid, terephthalic acid and Epicholorohydrin react the poly glycidyl ester of gained; 4,4 '-two aminodiphenylmethane and m-amino-phenol etc. and Epicholorohydrin react the glycidyl amine compound of gained; The multi-functional epoxy compounds of epoxidized phenol novolac resin, epoxidation cresylol novolac resin, epoxidized polyolefin etc.; And mono-functional's epoxy compounds etc. of butylglycidyl ether, phenyl glycidyl ether, glycidyl methacrylate etc., but not as limit.
In addition, as potentiality hardening accelerator of the present invention, also commercially available prod can be used, its particular instance comprises AMICUREPN-23 (AjinomotoCo., Inc.), AMICUREPN-H (AjinomotoCo., Inc.), NOVACUREHX-3742 (AsahiKaseiCo.), NOVACUREHX-3721 (AsahiKaseiCo.), FUJICUREFXE-1000 (FujiChemicalIndustryCo., Ltd), FUJICUREFXR-1030 (FujiChemicalIndustryCo., etc., but be not limited thereto Ltd).
Saturated fatty acid surface-treated flake metal powder of the present invention and unsaturated fatty acids surface-treated flake metal powder are such as silver, copper or its alloy, are wherein preferably silver.In the present invention, the size in the direction (such as thickness direction) that so-called " sheet " means among orthogonal three directions (being defined as length direction, width and thickness direction herein) be about other two directions (that is, length direction and width) size maximum value less than 1/2, be especially preferably 1/50 ~ 1/5.
In one embodiment, saturated fatty acid surface-treated flake metal powder and unsaturated fatty acids surface-treated flake metal powder can be the different surface treatment of the flake metal powder tool of same metal; In other embodiments, the flake metal powder of different metal kind can also be used respectively.
In one embodiment, saturated fatty acid such as: enanthic acid, sad, n-nonanoic acid, capric acid, undeeanoic acid, lauric acid, tridecyl acid, tetradecanoic acid, pentadecylic acid, palmitinic acid, margaric acid, stearic acid, nondecylic acid, arachic acid, docosanoic acid etc.In one embodiment, saturated fatty acid surface-treated flake metal powder is such as commercially available prod: LCP-267, KP-75, KP-84, LCP-1-19SFA, LCP-1-19SFS, LCP-1-19SM, LCP-1-19VS, LCP-1-19VSH, LCP-1-19VSS, LCP-1-36, LCP-120, LCP-270 and LCP-701 (AmesGoldsmith company) and SA-0201, SA-2831 and SA-0635 (Mei Taile science and technology) etc.
In one embodiment, unsaturated fatty acids such as: vinylformic acid, butenoic acid, methylacrylic acid, undecylenic acid, oleic acid, elaidic acid, cetoleic acid, brassidic acid, erucic acid, Sorbic Acid, linolenic acid, linolenic acid, arachidonic acid, nervonic acid etc.In one embodiment, unsaturated fatty acids surface-treated flake metal powder is such as commercially available prod: 12XJ, 22XJ, SFA-AB, SF-ABJ, SF-2J, SF-3, SF-3J, SF-4, SF-5, SF-5H, SF-6 and MBT-579 (AmesGoldsmith company) and AA-0014, AA-2043, AB-0022, AB-0222, AA-3462, AA-0023, AA-0909, AA-192N, AA-4703, AA-0005, AA-0707, AA-1831, AA-1832, AA-4091, AA-40736, AC-4048, AA-0981, AA-0101, AC2594, P629-3 and P629-4 (Mei Taile science and technology) etc.
In one embodiment, the tap density (TapDensity) of saturated fatty acid surface-treated flake metal powder and unsaturated fatty acids surface-treated flake metal powder is such as 1.1g/cm
3to 5.0g/cm
3and specific surface area (SurfaceArea) is such as 0.5m
2/ g to 2.6m
2/ g.In addition, the median size D50 of saturated fatty acid surface-treated flake metal powder and unsaturated fatty acids surface-treated flake metal powder is such as 0.5 μm to 50 μm, is preferably 0.5 μm to 20 μm.Herein so-called " median size (D50) ", be utilize BeckmanCoulter Inc. MultiSizer-3, carry out with Ku Ertefa the value measuring gained.In detail, D* representative is accumulated to the grain diameter of * %, represents a particle diameter (μm) for D50: D50, and it is that the summation being accumulated to this particle diameter from smallest particles accounts for overall 50%.Generally speaking, D50 general reference is median size.
Furthermore, when the median size D50 of saturated fatty acid surface-treated flake metal powder and unsaturated fatty acids surface-treated flake metal powder is lower than 0.5 μm, because described flake metal powder contact resistance to each other cannot be reduced, reduce causing the electroconductibility of formed conductive pattern.In addition, when the median size D50 of saturated fatty acid surface-treated flake metal powder and unsaturated fatty acids surface-treated flake metal powder is more than 50 μm, when carrying out screen painting, the problem that described flake metal powder blocks half tone mesh will be produced, this will cause print smudgy or produce broken string and wait and print bad phenomenon, and then affects tolerance range.
In addition, in the present embodiment, goodly saturated fatty acid surface-treated flake metal powder and unsaturated fatty acids surface-treated flake metal powder is combinationally used.When combinationally using saturated fatty acid surface-treated flake metal powder and unsaturated fatty acids surface-treated flake metal powder, the part by weight (saturated/unsaturated) of saturated fatty acid surface-treated flake metal powder and unsaturated fatty acids surface-treated flake metal powder is such as 1/2 to 1/9.
In addition, electrically conductive adhesive of the present invention more can comprise additive if desired, and wherein relative to the weight of epoxy resin, the content of additive is 0.1wt% to 30wt%.In the present embodiment, additive comprises thixotropic agent, silane coupling agent, dispersion agent or its combination.But the present invention is not limited with disclosed content.This area has usually to be known that the knowledgeable should be understood that and can add the additive with different function according to actual needs, such as flow agent, defoamer etc.
In one embodiment, in order to adjust shake-change property or the viscosity of electrically conductive adhesive, thixotropic agent can be added.In one embodiment, relative to the weight of epoxy resin, the content of thixotropic agent is such as 5wt% to 20wt%.
In addition, thixotropic agent can include the thixotropic agent of organic compounds or the thixotropic agent of mineral compound.As the thixotropic agent of organic compound, its particular instance comprises the salt of ethyl cellulose, hydroxypropylcellulose, acrylic resin, fatty acid amide wax, oxidic polyethylene, the amine salt of macromolecule polyester, straight-chain polyamine base acid amides and polymer acid polyester, the amide solution of poly carboxylic acid, alkylsulfonate, alkylallyl sulfonate, colloid system ester, vibrin, phenolic resin, melamine resin, epoxy resin, amido formate resin, polyimide resin and its composition.As the thixotropic agent of mineral compound, its particular instance comprises calcium stearate, Zinic stearas, aluminum stearate, aluminum oxide, zinc oxide, magnesium oxide, glass, diatomite, titanium oxide, zirconium white, silicon-dioxide, talcum, mica, feldspar, kaolinite (kaolin clay), pyrophyllite (alabaster clay), sericite, wilkinite, montmorillonite, vermiculite class (montmorillonite, beidellite, nontronite and saponite etc.), organobentonite and organic montmorillonite etc.
In addition, as thixotropic agent, also commercially available prod can be used.As the thixotropic agent of organic compound, the example of its commercially available prod comprises SELNY-HPC-H, HPC-M, HPC-L, HPC-SL and HPC-SSL (Japanese Cao Da limited-liability company); DIYANALBR series (Li Ang limited-liability company of Mitsubishi); Dispalone#6900-20X, Dispalone#4200, DispaloneKS-873N and Dispalone#1850 (nanmu originally changes into limited-liability company); BYK-E405 and BYK-E410 (BYKChemJapan company); PrimalRW-12W (Rhom & Haas company); And A-S-AT-20S, A-S-AT-350F, A-S-AD-10A and A-S-AD-160 (her rattan liquefaction limited-liability company) etc.As the thixotropic agent of mineral compound, the example of its commercially available prod comprises CrownClay, BagesClay#60, BagesClayKF and Optiwhite (Bai Shi Industries, Inc); KaolinJP-100, NNKaolinClay, STKaolinClay and Hardsil (earth house Kaolin Industries, Inc); ASP-072, SatentonPlus, TRANSLINK37 and HighdrasdelamiNCD (EnjelHard limited-liability company); SYKaolin, OSCLAY, HACLAY and MCHARDCLAY (Wan Wei Calicum limited-liability company); RusentiteSWN, RusentiteSAN, RusentiteSTN, RusentiteSEN and RusentiteSPN (Copchemical company); Aerosil300 (Degussa company); Smecton (Cunimina industrial); Bengel, BengelFW, SBen, SBen74, Oruganite and OruganiteT (Hojun limited-liability company); Fringe Gao Yin, Oluben, 250M, Benton34 and Benton38 (WilbaElis company); And Laponite, LaponiteRD and LaponiteRDS (Japanese Silica Industries, Inc) etc.
In one embodiment, in order to promote the tack of electrically conductive adhesive for substrate, can silane coupling agent be added, and with 100 parts by weight of epoxy resin, the content of silane coupling agent is such as preferably 0.5 weight part to 25 weight part, is more preferred from 2.5 weight part to 15 weight parts.Specifically, when with 100 parts by weight of epoxy resin, when the content of silane coupling agent is more than 0.5 weight part, electrically conductive adhesive can have preferably tack.When with 100 parts by weight of epoxy resin, when the content of silane coupling agent is below 25 weight parts, the balance between the non-exudative of electrically conductive adhesive and gluing reliability can be guaranteed.
In addition, silane coupling agent is better comprises trialkoxy silane compound or methyl dioxane TMOS compound, and its particular instance comprises γ-glycidyl-oxypropyl methyl dimethoxysilane, γ-glycidoxypropyl trimethoxy silane, γ-glycidyl-oxypropyl methyldiethoxysilane, γ-glycidyl-oxypropyl triethoxyl silane, γ-amine hydroxypropyl methyl dimethoxysilane, γ-amine propyl trimethoxy silicane, γ-amine hydroxypropyl methyl dimethoxysilane, γ-amine propyl trimethoxy silicane, N-amine ethyl-γ-imines hydroxypropyl methyl dimethoxysilane, N-amine ethyl-γ-imines propyl trimethoxy silicane, N-amine ethyl-γ-imines propyl trimethoxy silicane, N-phenyl-γ-amine propyl trimethoxy silicane, N-phenyl-γ-amine propyl-triethoxysilicane, N-phenyl-γ-amine hydroxypropyl methyl dimethoxysilane, N-phenyl-γ-amine hydroxypropyl methyl diethoxy silane, γ-hydrogen thiopropyl methyl dimethoxysilane, γ-amine propyl trimethoxy silicane, γ-hydrogen thiopropyl Trimethoxy silane, isocyanic ester hydroxypropyl methyl diethoxy silane, γ-isocyanic ester propyl-triethoxysilicanes etc., are wherein preferably γ-glycidyl-oxypropyl methyl dimethoxysilane, γ-glycidoxypropyl trimethoxy silane, γ-glycidyl-oxypropyl methyldiethoxysilane, γ-glycidyl-oxypropyl triethoxyl silane etc.The Commercial examples of silane coupling agent is such as KBM-403 (chemical industrial company of SHIN-ETSU HANTOTAI).
In one embodiment, in order to improve the dispersiveness of flake metal powder in electrically conductive adhesive, can dispersion agent be added, and with 100 parts by weight of epoxy resin, the content of dispersion agent is such as preferably 10 weight part to 30 weight parts, is more preferred from 15 weight part to 25 weight parts.Specifically, when with 100 parts by weight of epoxy resin, when the content of dispersion agent is more than 10 weight parts, flake metal powder can have preferably dispersed.But, when with 100 parts by weight of epoxy resin, when the content of dispersion agent is more than 30 weight parts, the viscosity performance of electrically conductive adhesive can be had influence on.
In one embodiment, can use the dispersion agent with amine value, it is such as commercially available prod: DisperBYK102, DisperBYK160, DisperBYK161, DisperBYK162, DisperBYK2163, DisperBYK2164, DisperBYK166, DisperBYK167, DisperBYK168, DisperBYK2000, DisperBYK2050, DisperBYK2150, DisperBYK2155, DisperBYKLPN6919, DisperBYKLPN21116, DisperBYKLPN21234, DisperBYK9075 and DisperBYK9077 (BYKChemie company); And EFKA4015, EFKA4020, EFKA4046, EFKA4047, EFKA4050, EFKA4055, EFKA4060, EFKA4080, EFKA4300, EFKA4330, EFKA4340, EFKA4400, EFKA4401, EFKA4402, EFKA4403 and EFKA4800 (BASF AG) etc.
The characteristic of the conductive pattern describing electrically conductive adhesive of the present invention in detail by embodiment below and use described electrically conductive adhesive to be formed.But the following example is also not used to limit the present invention.
The preparation of electrically conductive adhesive
Embodiment 1
Possessing in churned mechanically reaction unit, adding 7wt%NPEL-127E (liquid-state epoxy resin) and 2wt%BE504H (solid epoxy resin) and 9.99wt%DGMEA and 7.62wt%2-BXA.After NPEL-127E and BE504H dissolves homogenization, then add 1.41wt% potentiality hardening accelerator FXR-1030,14.4wt% saturated fatty acid surface-treated flake metal powder KP-75 (D50=9.7 μm, tap density=2g/cm
3, specific surface area=1.85m
2/ g) and 57.58wt% unsaturated fatty acids surface-treated flake metal powder AA-40736 (D50=2.9 μm, tap density=2g/cm
3, specific surface area=2.05m
2/ g).Then, after above-mentioned each material is stirred, then disperse equably with three roller machines.
Embodiment 2
Embodiment 2 with the difference of embodiment 1 is: while adding potentiality hardening accelerator FXR-1030, saturated fatty acid surface-treated flake metal powder KP-75 and unsaturated fatty acids surface-treated flake metal powder AA-40736, add dispersion agent DisperBYK2000, the detailed addition of its each component is as shown in table 1.In addition, the preparation method that embodiment 2 tool is identical with embodiment 1.
Embodiment 3
Embodiment 3 with the difference of embodiment 1 is: while adding potentiality hardening accelerator FXR-1030, saturated fatty acid surface-treated flake metal powder KP-75 and unsaturated fatty acids surface-treated flake metal powder AA-40736, add thixotropic agent Aerosil300, the detailed addition of its each component is as shown in table 1.In addition, the preparation method that embodiment 3 tool is identical with embodiment 1.
Embodiment 4
Embodiment 4 with the difference of embodiment 1 is: while adding NPEL-127E (liquid-state epoxy resin) and BE504H (solid epoxy resin) and DGMEA and 2-BXA, add silane coupling agent KBM-403, the detailed addition of its each component is as shown in table 1.In addition, the preparation method that embodiment 4 tool is identical with embodiment 1.
Embodiment 5
Embodiment 5 with the difference of embodiment 1 is: while adding potentiality hardening accelerator FXR-1030, saturated fatty acid surface-treated flake metal powder KP-75 and unsaturated fatty acids surface-treated flake metal powder AA-40736, add thixotropic agent BYK-E410, the detailed addition of its each component is as shown in table 1.In addition, the preparation method that embodiment 5 tool is identical with embodiment 1.
Embodiment 6
Embodiment 6 with the difference of embodiment 5 is: while adding NPEL-127E (liquid-state epoxy resin) and BE504H (solid epoxy resin) and DGMEA and 2-BAX, add silane coupling agent KBM-403, the detailed addition of its each component is as shown in table 1.In addition, the preparation method that embodiment 6 tool is identical with embodiment 5.
Comparative example 4 and comparative example 7
Comparative example 4 and comparative example 7 with the difference of embodiment 1 are: comparative example 4 and comparative example 7 are respectively and are used alone saturated fatty acid surface-treated flake metal powder KP-75 or unsaturated fatty acids surface-treated flake metal powder AA-40736, and comparative example 4 is as shown in table 2 with the detailed addition of the component out of the ordinary of comparative example 7.Specifically, comparative example 4 only adds saturated fatty acid surface-treated flake metal powder KP-75, and comparative example 7 only adds unsaturated fatty acids surface-treated flake metal powder AA-40736.In addition, comparative example 4 and comparative example 7 preparation method that all tool is identical with embodiment 1.
Comparative example 5, comparative example 6 and comparative example 8
Comparative example 5, comparative example 6 and comparative example 8 from the difference of comparative example 7 are: use unsaturated fatty acids surface-treated flake metal powder SF-2J (D50=1.5 μm, the tap density=4.2g/cm different with unsaturated fatty acids surface-treated flake metal powder AA-40736 respectively
3, specific surface area=1.35m
2/ g), MBT-579 (D50=2.8 μm, tap density=3g/cm
3, specific surface area=1.17m
2/ g) and AC-4048 (D50=2.1 μm, tap density=4.7g/cm
3, specific surface area=0.9m
2/ g), the detailed addition of the component out of the ordinary of comparative example 5, comparative example 6 and comparative example 8 is as shown in table 2.Specifically, use in comparative example 5 in unsaturated fatty acids surface-treated flake metal powder SF-2J, comparative example 6 and use unsaturated fatty acids surface-treated flake metal powder MBT-579, comparative example 8 then uses unsaturated fatty acids surface-treated flake metal powder AC-4048.In addition, comparative example 5, comparative example 6 and comparative example 8 preparation method that all tool is identical with comparative example 7.
Comparative example 3
Comparative example 3 with the difference of comparative example 7 is: while adding NPEL-127E (liquid-state epoxy resin) and BE504H (solid epoxy resin) and DGMEA and 2-BAX, add silane coupling agent KBM-403, and while adding potentiality hardening accelerator FXR-1030 and unsaturated fatty acids surface-treated flake metal powder AA-40736, add thixotropic agent Aerosi300 and BYK-E410, dispersion agent DisperBYK2000 and stiffening agent dicyanodiamide (DICY), the detailed addition of each component of comparative example 3 is as shown in table 2.In addition, the preparation method that comparative example 3 tool is identical with comparative example 7.
Comparative example 2
Comparative example 2 from the difference of comparative example 3 is: use unsaturated fatty acids surface-treated flake metal powder 12XJ (D50=1.6 μm, the tap density=4.1g/cm different with unsaturated fatty acids surface-treated flake metal powder AA-40736
3, specific surface area=1.17m
2/ g), the detailed addition of the component out of the ordinary of comparative example 2 is as shown in table 2.In addition, the preparation method that comparative example 2 tool is identical with comparative example 3.
Comparative example 1
Comparative example 1 with the difference of comparative example 2 is: use spherical silver powder AEP-1 (D50=1.1 μm, tap density=3.9g/cm
3, specific surface area=0.88m
2/ g), the detailed addition of the component out of the ordinary of comparative example 1 is as shown in table 2.In addition, the preparation method that comparative example 1 tool is identical with comparative example 2.
The making of conductive pattern
The electrically conductive adhesive of the electrically conductive adhesive of embodiment 1 to embodiment 6 and comparative example 1 to comparative example 8 is carried out screen painting, forms in the mode of screen painting the line pattern that the blocky of 8cm × 2cm, the line segment pattern of 300 μm × 8cm and live width/line-spacing are 100 μm/100 μm on the glass substrate.Then, glass coupon is inserted in the baking oven of 170 DEG C, dry 3 minutes and obtain conductive pattern.
Below, for cited various character respectively to the electrically conductive adhesive of embodiment 1 to embodiment 6 and the electrically conductive adhesive of comparative example 1 to comparative example 8, and blocky, line segment pattern or line pattern that the electrically conductive adhesive of the electrically conductive adhesive of embodiment 1 to embodiment 6 and comparative example 1 to comparative example 8 is formed carry out testing and assessing, and the result of each test is presented in table 3 and table 4.Hereinafter in detail the principle of these tests will be described.
The mensuration > of < viscosity
The viscosity (50rpm) of electrically conductive adhesive is with the CAP200+ of Brookfield under room temperature, measures when rotating speed is 50rpm.In table, numerical value is higher, and represent that electrically conductive adhesive is when carrying out screen painting, viscosity (now, viscosity is dynamic viscosity) is larger.
The viscosity (5.0rpm) of electrically conductive adhesive is with the CAP200+ of Brookfield under room temperature, measures when rotating speed is 5rpm.In table, numerical value is higher, and represent that electrically conductive adhesive is after screen painting, viscosity (now, viscosity is static viscosity) is larger, is namely more less likely to occur beach stream.In addition, in table, the numerical value of viscosity (5.0rpm) is greater than the numerical value of viscosity (50rpm).
In addition, in this article, thixotropy index is defined as viscosity (5.0rpm)/viscosity (50rpm).Usually, the preferably thixotropy index of electrically conductive adhesive is between 3.5 ~ 12, and numerical value gets over Gao Yuejia.In detail, when numerical value is higher, represent that viscosity is low when carrying out screen painting processing procedure, is easy to printing process, and viscosity height not easily beach stream after screen painting.
< pencil hardness >
Measurement of hardness is carried out to the blocky surface of 8cm × 2cm that above-mentioned drying obtains afterwards.Usually, the pencil hardness specification of the conductive pattern that electrically conductive adhesive is formed is preferably and is greater than more than H, is more preferred from and is more than or equal to more than 2H.
< sticking power >
The print surface 3 minutes of alcohol dampening test piece is dipped in cotton swab.Afterwards, under the pressure of 200g, reciprocal wiping 20 times, and then confirm that surface is with or without obviously coming off.
< hundred lattice tack test >
According to the method for JISK5600,8cm × 2cm blocky on the surface, cut out 100 grids of 10 lattice (square) × 10 lattice with cutting knife.Afterwards, 600 adhesive tape stickings 3M company manufactured on print surface, and then give peeling off rapidly, assess with residual grid number.If there is obscission to occur, then direct table on annotation NG.
< electroconductibility test >
Avometer is used to measure, as then carried out the calculating of volume specific resistance for conducting.If be shown as insulation, then direct table on annotation NG.
The calculating > of < volume specific resistance
25 DEG C, under humidity 50% environment, use LorestaAPMCP-T400 tester (Mitsubishi Chemical Ind's manufacture) to measure the sheet resistance value of above-mentioned 300 μm × 8cm line segment pattern.Then, volume specific resistance is calculated by measured sheet resistance value and thickness.Volume specific resistance (Ω cm)=(surface resistivity: Ω/cm
2) × (thickness: cm).
< printing characteristic >
Live width/the line-spacing formed in glass coupon by optical microscope inspection is the line pattern of 100 μm/100 μm, according to formed line pattern whether have burr, the bad problem of printing such as smudgy or with predetermined size whether close to the printing characteristic assessing electrically conductive adhesive.If present above-mentioned problem as bad in burr, the printing such as smudgy, then direct on table annotation NG.
As shown in Table 3, the electrically conductive adhesive of embodiments of the invention 1 to embodiment 6 all has good printing characteristic, and can form the high and conductive pattern that tolerance range is good of electroconductibility.In addition, the conductive pattern formed has more good surface hardness, tack and tack.On the contrary, as shown in Table 4, the electrically conductive adhesive of comparative example 1 to comparative example 8 then all cannot possess good printing characteristic simultaneously and form the conductive pattern of tool high conductivity.
Specifically, the electrically conductive adhesive of comparative example 1, because employing spherical silver powder, therefore cannot provide good electroconductibility, and viscosity (5.0rpm) is too low, causes easy beach stream after carrying out screen painting, the printing characteristic that thus tool is not good.In addition, be used alone the comparative example 2 of unsaturated fatty acids surface-treated flake metal powder, comparative example 3, comparative example 7 and comparative example 8 and also cannot provide good electroconductibility, wherein the volume specific resistance of comparative example 7 and comparative example 8 is too high, and this will cause circuit poorly conductive.
In addition, the electrically conductive adhesive printing characteristic that neither tool is good of the comparative example 4 of saturated fatty acid surface-treated flake metal powder or unsaturated fatty acids surface-treated flake metal powder, comparative example 5, comparative example 6 and comparative example 8 is used alone.What illustrate is, comparative example 4 has been used alone the larger saturated fatty acid surface-treated flake metal powder KP-75 of median size, thus good electroconductibility (namely lower volume specific resistance) is presented, but also therefore easily produce the clustering phenomena of metal powder Granular composite inequality, make line pattern present the bad result of the printings such as burr.
In addition, the electrically conductive adhesive of comparative example 1 to comparative example 8 all cannot form the conductive pattern with good adhesion, and the electrically conductive adhesive of comparative example 4 to comparative example 8 does not more have good tack.
In sum, the electrically conductive adhesive that above-described embodiment proposes contains saturated fatty acid surface-treated flake metal powder and unsaturated fatty acids surface-treated flake metal powder, thus make electrically conductive adhesive can have good printing characteristic, and the high and fine pattern that tolerance range is good of electroconductibility can be formed.In addition, the saturated fatty acid surface-treated flake metal powder in the electrically conductive adhesive that proposes of above-described embodiment and unsaturated fatty acids surface-treated flake metal powder combinationally use.
Although the present invention discloses as above with embodiment; so itself and be not used to limit the present invention; have in any art and usually know the knowledgeable; without departing from the spirit and scope of the present invention; when doing a little change and retouching, therefore protection scope of the present invention is when being as the criterion depending on the accompanying claim person of defining.
Claims (13)
1. an electrically conductive adhesive, is characterized in that, this electrically conductive adhesive comprises:
Epoxy resin, its content is 8wt% to 20wt%;
Solvent, its content is 10wt% to 25wt%;
Potentiality hardening accelerator, its content is 0.5wt% to 5wt%;
Saturated fatty acid surface-treated flake metal powder, its content is 3.5wt% to 35wt%; And
Unsaturated fatty acids surface-treated flake metal powder, its content is 35wt% to 75wt%,
Wherein, the median size D50 of this saturated fatty acid surface-treated flake metal powder and this unsaturated fatty acids surface-treated flake metal powder is 0.5 μm to 50 μm.
2. electrically conductive adhesive as claimed in claim 1, is characterized in that this saturated fatty acid surface-treated flake metal powder and this unsaturated fatty acids surface-treated flake metal powder comprise silver, copper or its alloy.
3. electrically conductive adhesive as claimed in claim 1, is characterized in that the median size D50 of this saturated fatty acid surface-treated flake metal powder and this unsaturated fatty acids surface-treated flake metal powder is 0.5 μm to 20 μm, tap density is 1.1g/cm
3to 5.0g/cm
3and specific surface area is 0.5m
2/ g to 2.6m
2/ g.
4. electrically conductive adhesive as claimed in claim 1, is characterized in that this epoxy resin comprises solid epoxy resin, liquid-state epoxy resin or its combination.
5. the electrically conductive adhesive as described in claim 4, it is characterized in that when combinationally using this solid epoxy resin and this liquid-state epoxy resin, the part by weight of this solid epoxy resin and this liquid-state epoxy resin is 9/1 to 1/9.
6. electrically conductive adhesive as claimed in claim 4, is characterized in that the epoxy equivalent (weight) of this solid epoxy resin is 1000g/eq to 20000g/eq.
7. electrically conductive adhesive as claimed in claim 4, is characterized in that the weight average molecular weight of this solid epoxy resin is 5000g/mol to 65000g/mol.
8. electrically conductive adhesive as claimed in claim 4, is characterized in that the epoxy equivalent (weight) of this liquid-state epoxy resin is 100g/eq to 1500g/eq.
9. electrically conductive adhesive as claimed in claim 4, is characterized in that the weight average molecular weight of this liquid-state epoxy resin is 100g/mol to 3000g/mol.
10. electrically conductive adhesive as claimed in claim 1, is characterized in that the boiling point of this solvent is 140 DEG C to 220 DEG C.
11. electrically conductive adhesives as claimed in claim 1, it is characterized in that, this electrically conductive adhesive also comprises additive, and wherein relative to the weight of this epoxy resin, the content of this additive is 0.1wt% to 30wt%.
12. electrically conductive adhesives as claimed in claim 11, is characterized in that this additive comprises thixotropic agent, silane coupling agent, dispersion agent or its combination.
13. electrically conductive adhesives as claimed in claim 12, is characterized in that 100 parts by weight with this epoxy resin, and the content of this silane coupling agent is 0.5 weight part to 25 weight part.
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| KR101725748B1 (en) * | 2014-09-30 | 2017-04-10 | 다츠다 덴센 가부시키가이샤 | Conductive coating material for shielding package of electronic parts and method for producing shield package using same |
| MY175446A (en) * | 2015-01-27 | 2020-06-29 | Teikoku Printing Inks Mfg Co Ltd | Ink composition for high-quality/high-definition screen printing, printed matter produced by the screen printing ink composition, and method for producing the printed matter |
| JP6431998B1 (en) * | 2018-03-20 | 2018-11-28 | タツタ電線株式会社 | Conductive adhesive layer |
| JP7332129B2 (en) * | 2019-02-27 | 2023-08-23 | ナミックス株式会社 | Conductive composition and conductive adhesive |
| CN109837050A (en) * | 2019-03-15 | 2019-06-04 | 苏州凡络新材料科技有限公司 | A kind of low temperature curing type conductive adhesive and preparation method thereof |
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| CN101288133A (en) * | 2005-09-29 | 2008-10-15 | 阿尔法科学株式会社 | Conductive powder and process for producing the same, conductive powder paste, and process for producing the conductive powder paste |
| CN102119427A (en) * | 2008-08-13 | 2011-07-06 | 住友电气工业株式会社 | Conductive adhesive and LED substrate using the same |
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| JP4242019B2 (en) * | 1999-09-01 | 2009-03-18 | 住友金属鉱山株式会社 | Conductive resin composition |
| JP5916633B2 (en) * | 2011-01-26 | 2016-05-11 | ナミックス株式会社 | Conductive paste and method for producing conductive film |
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| CN101288133A (en) * | 2005-09-29 | 2008-10-15 | 阿尔法科学株式会社 | Conductive powder and process for producing the same, conductive powder paste, and process for producing the conductive powder paste |
| CN102119427A (en) * | 2008-08-13 | 2011-07-06 | 住友电气工业株式会社 | Conductive adhesive and LED substrate using the same |
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Effective date of registration: 20201009 Address after: 104, building D, No.1, Yingfeng West Road, Rucheng Town, Ruyuan County, Shaoguan City, Guangdong Province Patentee after: Ruyuan Yao Autonomous County Weijin Pharmaceutical Co., Ltd Address before: Tainan City, Taiwan, China Patentee before: Chi Mei Industrial Co.,Ltd. |