CN104541333A - Conductive material, connection structure and method for producing connection structure - Google Patents
Conductive material, connection structure and method for producing connection structure Download PDFInfo
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- CN104541333A CN104541333A CN201380042626.2A CN201380042626A CN104541333A CN 104541333 A CN104541333 A CN 104541333A CN 201380042626 A CN201380042626 A CN 201380042626A CN 104541333 A CN104541333 A CN 104541333A
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- electric conducting
- conducting material
- substrate
- electroconductive particle
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- 229920002799 BoPET Polymers 0.000 description 1
- NGMNTLCQDNNBNT-UHFFFAOYSA-N C(C=C)(=O)OC.C(CS)(=O)OCCOC(CS)=O Chemical compound C(C=C)(=O)OC.C(CS)(=O)OCCOC(CS)=O NGMNTLCQDNNBNT-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- PDQAZBWRQCGBEV-UHFFFAOYSA-N Ethylenethiourea Chemical compound S=C1NCCN1 PDQAZBWRQCGBEV-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- 239000004696 Poly ether ether ketone Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- DBHQYYNDKZDVTN-UHFFFAOYSA-N [4-(4-methylphenyl)sulfanylphenyl]-phenylmethanone Chemical compound C1=CC(C)=CC=C1SC1=CC=C(C(=O)C=2C=CC=CC=2)C=C1 DBHQYYNDKZDVTN-UHFFFAOYSA-N 0.000 description 1
- UUQQGGWZVKUCBD-UHFFFAOYSA-N [4-(hydroxymethyl)-2-phenyl-1h-imidazol-5-yl]methanol Chemical class N1C(CO)=C(CO)N=C1C1=CC=CC=C1 UUQQGGWZVKUCBD-UHFFFAOYSA-N 0.000 description 1
- 0 [B-]C(C)(C)c1c(*)c(*)c(*C(C)CC)c(*)c1* Chemical compound [B-]C(C)(C)c1c(*)c(*)c(*C(C)CC)c(*)c1* 0.000 description 1
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000004840 adhesive resin Substances 0.000 description 1
- 229920006223 adhesive resin Polymers 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 125000005370 alkoxysilyl group Chemical group 0.000 description 1
- 125000005037 alkyl phenyl group Chemical group 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- DHXJFECNLYYCDM-UHFFFAOYSA-N benzyl(dimethyl)sulfanium Chemical compound C[S+](C)CC1=CC=CC=C1 DHXJFECNLYYCDM-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 125000001246 bromo group Chemical group Br* 0.000 description 1
- OCKPCBLVNKHBMX-UHFFFAOYSA-N butylbenzene Chemical group CCCCC1=CC=CC=C1 OCKPCBLVNKHBMX-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 description 1
- 229910000020 calcium bicarbonate Inorganic materials 0.000 description 1
- 235000012241 calcium silicate Nutrition 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 150000001244 carboxylic acid anhydrides Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 125000005578 chrysene group Chemical group 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- 150000003983 crown ethers Chemical class 0.000 description 1
- IOJUPLGTWVMSFF-UHFFFAOYSA-N cyclobenzothiazole Natural products C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000012933 diacyl peroxide Substances 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- IAZPIYCBYSLQIY-UHFFFAOYSA-N dimethyl(3-phenylprop-2-enyl)sulfanium Chemical compound C[S+](C)CC=CC1=CC=CC=C1 IAZPIYCBYSLQIY-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- HJYKVGWOAOLIKY-UHFFFAOYSA-N methyl 2-methylidenenonanoate Chemical compound CCCCCCCC(=C)C(=O)OC HJYKVGWOAOLIKY-UHFFFAOYSA-N 0.000 description 1
- UNBDCVXGGDKSCP-UHFFFAOYSA-N methyl 2-methylidenetetradecanoate Chemical compound CCCCCCCCCCCCC(=C)C(=O)OC UNBDCVXGGDKSCP-UHFFFAOYSA-N 0.000 description 1
- QPJVMBTYPHYUOC-UHFFFAOYSA-N methyl benzoate Chemical class COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- RIWRFSMVIUAEBX-UHFFFAOYSA-N n-methyl-1-phenylmethanamine Chemical compound CNCC1=CC=CC=C1 RIWRFSMVIUAEBX-UHFFFAOYSA-N 0.000 description 1
- NVSYANRBXPURRQ-UHFFFAOYSA-N naphthalen-1-ylmethanamine Chemical compound C1=CC=C2C(CN)=CC=CC2=C1 NVSYANRBXPURRQ-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- SLIUAWYAILUBJU-UHFFFAOYSA-N pentacene Chemical compound C1=CC=CC2=CC3=CC4=CC5=CC=CC=C5C=C4C=C3C=C21 SLIUAWYAILUBJU-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 1
- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 description 1
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical group C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920005644 polyethylene terephthalate glycol copolymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- QTECDUFMBMSHKR-UHFFFAOYSA-N prop-2-enyl prop-2-enoate Chemical compound C=CCOC(=O)C=C QTECDUFMBMSHKR-UHFFFAOYSA-N 0.000 description 1
- 125000005581 pyrene group Chemical group 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 150000003440 styrenes Chemical class 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- ATZHWSYYKQKSSY-UHFFFAOYSA-N tetradecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCOC(=O)C(C)=C ATZHWSYYKQKSSY-UHFFFAOYSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000005591 trimellitate group Chemical group 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- KRLHYNPADOCLAJ-UHFFFAOYSA-N undecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCOC(=O)C(C)=C KRLHYNPADOCLAJ-UHFFFAOYSA-N 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/66—Additives characterised by particle size
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/12—Light sources with substantially two-dimensional radiating surfaces
- H05B33/26—Light sources with substantially two-dimensional radiating surfaces characterised by the composition or arrangement of the conductive material used as an electrode
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/80—Constructional details
- H10K59/82—Interconnections, e.g. terminals
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/50—Forming devices by joining two substrates together, e.g. lamination techniques
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/60—Forming conductive regions or layers, e.g. electrodes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K2102/00—Constructional details relating to the organic devices covered by this subclass
- H10K2102/301—Details of OLEDs
- H10K2102/331—Nanoparticles used in non-emissive layers, e.g. in packaging layer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Conductive Materials (AREA)
- Electroluminescent Light Sources (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Manufacturing Of Electrical Connectors (AREA)
Abstract
Provided is a conductive material which forms a connection part that is not susceptible to voids in cases where electrodes of members to be connected are electrically connected with each other, and which is capable of increasing the connection reliability after connection. A conductive material of the present invention is heated and cured at a temperature of 120 DEG C or less for use without being heated to a temperature more than 120 DEG C. Each conductive particle (11) comprises a base particle (12) and a conductive layer (13) that is arranged on the surface of the base particle (12). The compressive modulus at 20% compressive deformation at 100 DEG C of the conductive particle (11) is from 500 N/mm2 to 2,000 N/mm2 (inclusive). The compression recovery rate at 100 DEG C of the conductive particle (11) is from 3% to 30% (inclusive).
Description
Technical field
The present invention relates to a kind of electric conducting material containing multiple electroconductive particle.More specifically, the present invention relates to the electric conducting material be electrically connected between a kind of electrode that such as may be used for various connecting object parts such as flexible printing substrate, glass substrate, glass epoxy substrate, semiconductor chip and organic electro-luminescent display unit substrates, particularly can be preferred for the electric conducting material be electrically connected between the electrode to organic electro-luminescent display unit substrate.In addition, the present invention relates to a kind of use and have the connection structural bodies of above-mentioned electric conducting material and the manufacture method of connection structural bodies.
Background technology
Pulpous state or membranaceous electric conducting material are widely known by the people.With regard to this electric conducting material, in adhesive resin etc., be dispersed with multiple electroconductive particle.In addition, the electric conducting material containing electroconductive particle is sometimes for the interelectrode connection of organic electroluminescent (following, to be sometimes recited as organic EL) display element.
Above-mentioned organic EL display element has the structure inserting the laminated body of organic light emitting material between mutually corresponding pair of electrodes.By simultaneously to above-mentioned organic light emitting material from an electrode injection electronics, and from another electrode injection hole, in above-mentioned organic light emitting material, electronics and hole combine and luminous.Because above-mentioned organic EL display element carries out self-luminous, therefore, compared with needing the liquid crystal display cells etc. of backlight, have visual good, can slimming and the advantage that can drive with DC low-voltage.
As an example of above-mentioned organic EL display element, in Fig. 9-A of following patent documentation 1, disclose a kind of organic EL element, wherein, the organic electrode of EL substrate possessing organic EL element is undertaken bonding with the electrode of hermetic sealing substrate by adhesive portion.Recording in the embodiment of above-mentioned patent documentation 1: in order to form above-mentioned adhesive portion, using the Thermocurable epoxies bonding agent containing anisotropic conductive particle.
In addition, in order to obtain various connection structural bodies, above-mentioned electric conducting material also uses in the connection (COF (Chi Pon Film)) of the connection of such as flexible printing substrate and glass substrate (FOG (Film on Glass)), semiconductor chip and flexible printing substrate, semiconductor chip and the connection (COG (Chip on Glass)) of glass substrate and the connection (FOB (Film on Board)) of flexible printing substrate and glass epoxy substrate etc.
When being such as electrically connected with the electrode of glass substrate the electrode of semiconductor chip by above-mentioned electric conducting material, the electric conducting material of configuration containing electroconductive particle on the glass substrate.Then, stacked semiconductor chips, carries out heating and pressurizeing.Thus, electric conducting material is solidified, and is electrically connected between electrode via electroconductive particle, obtain connection structural bodies.
Routine as of the electric conducting material that may be used for connection structural bodies as above, in following patent documentation 2, disclose a kind of anisotropic conductive material, it contains alicyclic epoxy resin, glycols, the styrene analog thermoplastic elastomer with epoxy radicals, UV active type cationic polymerization catalyst and electroconductive particle.
In addition, in following patent documentation 3, disclose cationically polymerizable organic material composition, it has coordinated guanidine compound, thiazole compound, benzothiazole compound, thiazole carboxylic acid's compounds, sulfenamide compound, thiourea, ethylene thiourea, glyoxaline compound, benzimidazoles compound or alkyl phenyl thio-ether type compounds as stabilizer in the composition containing cationic polymerization catalyst and cationically polymerizable organic material.It should be noted that, this cationically polymerizable organic material composition is not containing electroconductive particle.
Prior art document
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 2009-117214 publication
Patent documentation 2: Japanese Unexamined Patent Publication 11-060899 publication
Patent documentation 3: Japanese Unexamined Patent Publication 8-283320 publication
Summary of the invention
The problem that invention will solve
Use the Thermocurable epoxies bonding agent containing, for example the anisotropic conductive particle recorded in patent documentation 1, and when carrying out bonding to the above-mentioned electrode of organic EL substrate with the electrode of above-mentioned hermetic sealing substrate by adhesive portion, in order to make electrode contact fully with anisotropic conductive particle, anisotropic conductive particle is compressed.But sometimes in the solidification of bonding agent, anisotropic conductive particle easily reverts to original shape, due to the bounce of anisotropic conductive particle, interelectrode interval expands, and produces space in above-mentioned adhesive portion.In addition, after bonding, organic EL substrate and hermetic sealing substrate can not be firmly bonding by above-mentioned adhesive portion sometimes.
When obtaining various connection structural bodies using the electric conducting material of record in as patent documentation 2,3, connecting object parts can not be firmly bonding by the solidfied material of electric conducting material sometimes.In the such electric conducting material particularly recorded in patent documentation 2,3, during curing temperature step-down, be difficult to improve cementability fully.
In addition, when the existing anisotropic conductive material containing, for example the cationic polymerization catalyst recorded in patent documentation 2 is taken care of for a long time, curability changes sometimes.That is, storage stability is low sometimes for the existing anisotropic conductive material containing cationic polymerization catalyst.
In addition, with regard to the existing anisotropic conductive material containing cationic polymerization catalyst, the conductive part that there is electroconductive particle easily produces the problem of corrosion.Therefore, interelectrode conducting reliability step-down sometimes.
The object of the invention is to, a kind of electric conducting material is provided and uses and have the connection structural bodies of this electric conducting material and the manufacture method of connection structural bodies, described electric conducting material is electrically connected between by the electrode of connecting object parts, not easily produce space at the connecting portion formed by electric conducting material, and the connection reliability after connection can be improved.
The object of restriction of the present invention is, a kind of electric conducting material is provided and uses and have the connection structural bodies of this electric conducting material and the manufacture method of connection structural bodies, although described electric conducting material uses cation propellant, but excellent storage stability, when being electrically connected between by electrode, interelectrode conducting reliability can be improved.
For the technical scheme of dealing with problems
According to the aspect of broadness of the present invention, a kind of electric conducting material is provided, be heated the temperature of less than 120 DEG C but not the temperature more than 120 DEG C makes it solidify rear use, described electric conducting material contains curability composition and electroconductive particle, described electroconductive particle has substrate particle and is arranged at the conductive layer on described substrate particle surface, and modulus of elasticity in comperssion when described electroconductive particle has carried out 20% compression at 100 DEG C is 500N/mm
2above and 2000N/mm
2below, the compression recovery of described electroconductive particle at 100 DEG C is more than 3% and less than 30%.
Electric conducting material of the present invention is preferred for the electrical connection of electrode in organic electro-luminescent display unit.
Electric conducting material of the present invention is preferred for the electrical connection between the electrode of the organic electroluminescent substrate having electro-luminescence element and the electrode of hermetic sealing substrate.
In a certain particular aspects of electric conducting material of the present invention, this electric conducting material is also containing inorganic filler.
In a certain particular aspects of electric conducting material of the present invention, this electric conducting material is also containing inorganic filler and organic filler.
In a certain particular aspects of electric conducting material of the present invention, described curability composition contains curability compound and cation propellant.
In a certain particular aspects of electric conducting material of the present invention, described electric conducting material is also containing amines, and described amines is the primary amine with aromatic ring, and described curability composition contains curability compound and cation propellant.
In a certain particular aspects of electric conducting material of the present invention, described curability compound to contain at 23 DEG C for liquid epoxy compounds and is the epoxy compounds of solid at 23 DEG C.
According to the aspect of broadness of the present invention, provide a kind of connection structural bodies, it has:
1st connecting object parts, the 2nd connecting object parts, described 1st, the 2nd connecting object parts are carried out the connecting portion that is electrically connected, described connecting portion is by being heated to the temperature of less than 120 DEG C but not the temperature more than 120 DEG C make it be solidified to form by above-mentioned electric conducting material.
In a certain particular aspects of connection structural bodies of the present invention, the connecting object parts of the described 1st have the 1st electrode on surface, described 2nd connecting object parts have the 2nd electrode on surface, described 1st electrode and described 2nd electrode are electrically connected by described electroconductive particle.
In a certain particular aspects of connection structural bodies of the present invention, described 1st, the 2nd connecting object parts are organic electro-luminescent display unit substrate.
In a certain particular aspects of connection structural bodies of the present invention, described 1st connecting object parts and described 2nd connecting object parts are the organic electroluminescent substrate and the hermetic sealing substrate that have electro-luminescence element.
According to the aspect of broadness of the present invention, provide a kind of manufacture method of connection structural bodies, it is the manufacture method of above-mentioned connection structural bodies, and the method comprises:
The operation of conductive material layer is set by described electric conducting material on the surface of described 1st connecting object parts;
At described conductive material layer, the operation of described 2nd connecting object parts is set with the surface of described 1st connecting object component side opposite side; Be heated to the temperature of less than 120 DEG C but not the temperature more than 120 DEG C, described conductive material layer is solidified, formed and make described 1st, the 2nd connecting object parts realize the operation of the connecting portion of electrical connection.
In a certain particular aspects of the manufacture method of connection structural bodies of the present invention, described connection structural bodies is organic electro-luminescent display unit, wherein, described 1st connecting object parts are the 1st substrates as organic electro-luminescent display unit substrate, described 2nd connecting object parts are the 2nd substrates as organic electro-luminescent display unit substrate, and the manufacture method of described connection structural bodies comprises: the surface of described the 1st substrate as organic electro-luminescent display unit substrate is arranged the operation of conductive material layer by described electric conducting material; At described conductive material layer, the operation of described the 2nd substrate as organic electro-luminescent display unit substrate is set with the surface of described 1st substrate-side opposite side; Light is irradiated to described conductive material layer, and described conductive material layer is heated to the temperature of less than 120 DEG C, make described conductive material layer generation photocuring and hot curing, formed and make described 1st, the 2nd substrate realize the operation of the connecting portion of electrical connection
The effect of invention
Electric conducting material of the present invention contains curability composition and electroconductive particle, and modulus of elasticity in comperssion when above-mentioned electroconductive particle being carried out at 100 DEG C 20% compression is 500N/mm
2above and 2000N/mm
2below, compression recovery at 100 DEG C of above-mentioned electroconductive particle is more than 3% and less than 30%, therefore, above-mentioned electric conducting material is heated to the temperature of less than 120 DEG C but not the temperature more than 120 DEG C makes it solidify, and when making to be electrically connected between electrode by electroconductive particle contained in electric conducting material, not easily can produce space at the connecting portion formed by electric conducting material.Further, the connection reliability after connection can be improved.
Accompanying drawing explanation
Fig. 1 is the front cross-sectional view schematically showing the connection structural bodies using the electric conducting material having one embodiment of the present invention to relate to.
Fig. 2 (a) ~ (c) is the front cross-sectional view for illustration of the electric conducting material using one embodiment of the present invention to relate to obtains to each operation of connection structural bodies.
Fig. 3 is the profile of the example representing electroconductive particle.
Symbol description
1 ... connection structural bodies
2 ... 1st connecting object parts
2a ... 1st electrode
3 ... connecting portion
3A ... conductive material layer
3B ... the conductive material layer of B-stage
4 ... 2nd connecting object parts
4a ... 2nd electrode
11 ... electroconductive particle
12 ... substrate particle
13 ... conductive layer
Embodiment
Below, the present invention is described in detail.
Electric conducting material of the present invention is heated to the temperature of less than 120 DEG C but not the temperature more than 120 DEG C makes it solidify rear use.Electric conducting material of the present invention contains curability composition and electroconductive particle.Modulus of elasticity in comperssion (following, to be sometimes recited as 20%K value) when above-mentioned electroconductive particle having been carried out at 100 DEG C 20% compression is 500N/mm
2above and 2000N/mm
2below.The compression recovery of above-mentioned electroconductive particle at 100 DEG C is more than 3% and less than 30%.
Electric conducting material of the present invention is by having above-mentioned formation, be heated to the temperature of less than 120 DEG C but not the temperature more than 120 DEG C makes above-mentioned electric conducting material solidify, and when can make to be electrically connected between the electrode of connecting object parts by electroconductive particle contained in above-mentioned electric conducting material, not easily produce space at the connecting portion formed by electric conducting material.Such as, specifically, in order to make the electrode of organic electroluminescent (organic EL) display element be electrically connected, when use has electric conducting material of the present invention, the repulsive force having carried out the electroconductive particle of compression less becomes large, and therefore, space not easily produces.Not easily produce the result in space, interelectrode contact resistance step-down.In addition, because the contact area of electrode and electroconductive particle increases, interelectrode contact resistance also step-down.And then, above-mentioned connecting object parts can be made firmly bonding by above-mentioned connecting portion.Therefore, the conducting reliability in organic EL display element and connection reliability can be improved.
At the value of the 20%K value of above-mentioned electroconductive particle and the compression recovery of above-mentioned electroconductive particle is set as 100 DEG C, be because: the temperature that electric conducting material of the present invention is heated to less than 120 DEG C makes it solidify and use, preferably be heated to more than 60 DEG C and the temperature of less than 120 DEG C makes it solidify and use, the temperature being preferably heated to less than 100 DEG C further makes it solidify and use.When above-mentioned 20%K value at 100 DEG C is below more than above-mentioned lower limit and the above-mentioned upper limit, suitably compression is there is when above-mentioned electric conducting material carries out hot curing at inter-electrode conductive particle, the contact area of electrode and electroconductive particle increases, and the bounce that the electroconductive particle of compression causes diminishes.When above-mentioned 20%K value is below more than above-mentioned lower limit and the above-mentioned upper limit, go far towards suppress the generation in space and contribute to reducing interelectrode contact resistance.When above-mentioned compression recovery is below more than above-mentioned lower limit and the above-mentioned upper limit, also go far towards suppress the generation in space and contribute to reducing interelectrode contact resistance.And then, when above-mentioned compression recovery is below more than above-mentioned lower limit and the above-mentioned upper limit, go far towards to make above-mentioned connecting object parts more firmly bonding with above-mentioned connecting portion.
Further, electric conducting material of the present invention is preferably also containing inorganic filler.By the use of inorganic filler, the moisture-proof of solidfied material is improved.
Further, electric conducting material of the present invention is more preferably also containing inorganic filler and organic filler.In existing electric conducting material, in solidification, the viscosity of electric conducting material is too low sometimes, and electric conducting material exceedingly flows.Therefore, sometimes can not configure electric conducting material in specific region, further, be electrically connected via multiple electroconductive particle between the adjacent electrode that sometimes can not be connected.On the other hand, when above-mentioned electric conducting material contain curability composition, inorganic filler, organic filler and electroconductive particle, be heated the temperature of less than 120 DEG C but not the temperature more than 120 DEG C makes it solidify time, the electric conducting material be configured on connecting object parts is difficult to flow significantly, the connecting portion formed and electroconductive particle precision can be configured at specific region well by electric conducting material.And then, can suppress being electrically connected via multiple electroconductive particle between the adjacent electrode that can not be connected.Thus, the conducting reliability of the connection structural bodies obtained can be improved.And then the solidfied material of electric conducting material is not easily exceedingly spreading wetting on the surface of connecting object parts, more not easily can produce space in the connection structural bodies obtained.
In addition, when above-mentioned electric conducting material contain curability composition, inorganic filler, organic filler and electroconductive particle, when being heated the temperature of less than 120 DEG C but not the temperature more than 120 DEG C makes it solidify, the pollution that the connecting portion formed by electric conducting material causes effectively can be suppressed.Specifically, such as, when using above-mentioned electric conducting material to make the electrode of organic electroluminescent (organic EL) display element be electrically connected, in the solidification of electric conducting material, the viscosity of electric conducting material can not be too low, therefore, above-mentioned connecting portion can be configured at the position of specifying.And then the solidfied material of electric conducting material is not easily exceedingly spreading wetting on the surface of connecting object parts, more not easily produces space in the connection structural bodies obtained.Therefore, effectively can improve the conducting reliability of the connection structural bodies in organic EL display element, not easily produce the malfunction of organic EL display element.
In addition, when above-mentioned electric conducting material contain curability composition, inorganic filler, organic filler and electroconductive particle, the moisture-proof of solidfied material is further improved.
From the view point of further suppressing the generation in space, further reducing interelectrode contact resistance, the above-mentioned 20%K value of above-mentioned electroconductive particle at 100 DEG C is preferably 700N/mm
2above, 1000N/mm is more preferably
2above, 1650N/mm is preferably
2below, 1500N/mm is more preferably
2below.
Above-mentioned modulus of elasticity in comperssion (20%K value) can measure as follows.
Use micro-compression tester, with the sub-end face of level and smooth pressure of cylinder (diameter 50 μm, Buddha's warrior attendant are made of stones), at 100 DEG C, under the condition of compression speed 2.6mN/ second and maximum testing load 10gf, electroconductive particle is compressed.Measure loading value (N) now and compression displacement (mm).Can by the measured value obtained, utilize following formula to obtain above-mentioned modulus of elasticity in comperssion.As above-mentioned micro-compression tester, such as FISCHER Inc. " FISCHER SCOPE H-100 " etc. can be used.
K value (N/mm
2)=(3/2
1/2) FS
-3/2r
-1/2
F: the loading value (N) during 20% compression occurs electroconductive particle
S: compression displacement (mm) during 20% compression occurs electroconductive particle
R: the radius (mm) of electroconductive particle
Above-mentioned modulus of elasticity in comperssion generally and represent the hardness of electroconductive particle quantitatively.By the use of above-mentioned modulus of elasticity in comperssion, the hardness of electroconductive particle quantitatively and uniquely can be represented.
From the view point of further suppressing the generation in space, further improving the cementability of connecting portion generation and further reduce interelectrode contact resistance, the compression recovery of above-mentioned electroconductive particle at 100 DEG C is preferably more than 5%, be more preferably more than 8%, be preferably less than 20%, be more preferably less than 17%.
Above-mentioned compression recovery can measure as follows.
Sample bench scatters electroconductive particle.To the electroconductive particle that 1 is scattered, use micro-compression tester, at 100 DEG C, the center position along electroconductive particle gives load (reversion loading value), to electroconductive particle, 30% compression occurs.Thereafter carry out except lotus, until initially use loading value (0.40mN).Can loading-compression displacement between test period, obtain compression recovery by following formula.It should be noted that, load speed is set to 0.33mN/ second.As above-mentioned micro-compression tester, use such as FISCHER Inc. " FISCHERSCOPE H-100 " etc.
Compression recovery (%)=[(L1-L2)/L1] × 100
L1: be shifted to the compression reaching reversion loading value by initial loading value when applying load
L2: be shifted to the lotus that removes reaching initial loading value by reversion loading value during release load
As the method making electric conducting material solidify of the present invention, can enumerate: the method that electric conducting material is heated; After irradiating light to electric conducting material, to the method that electric conducting material heats; And after electric conduction of heating material, electric conducting material is irradiated to the method for light.In addition, the speed of photocuring and the different situation of the speed of hot curing inferior, illumination can be carried out simultaneously penetrate and heat.Wherein, after preferably irradiating light to electric conducting material, to the method that electric conducting material heats.By combinationally using of photocuring and hot curing, electric conducting material can be made to solidify at short notice.And by combinationally using of photocuring and hot curing, even if carry out the heating of low temperature, curability also further becomes good.When making electric conducting material of the present invention solidify, at least heat.Namely, electric conducting material of the present invention is thermally cured and uses.
Above-mentioned electric conducting material contains curing agent as above-mentioned curability composition.Above-mentioned electric conducting material preferably contains cation propellant as above-mentioned curing agent.Above-mentioned curability composition is preferably containing curability compound and cation propellant.The discoveries such as the present inventor: by using cation propellant, compared with the situation of the thermal curing agents employed beyond cation propellant (imidazolium compounds etc.), can effectively improve conducting reliability.
Further, electric conducting material of the present invention contains amines, and above-mentioned amines is the primary amine with aromatic ring, and above-mentioned curability composition is preferably containing curability compound and cation propellant.Between existing electric conducting material containing cation propellant is long-term during keeping, curability changes sometimes.That is, with regard to the existing electric conducting material containing cation propellant, storage stability is low sometimes.In addition, with regard to the existing electric conducting material containing cation propellant, there is the problem of the corrosion of the conductive part easily producing electroconductive particle.Therefore, interelectrode conducting reliability step-down sometimes.On the other hand, curability compound, cation propellant, amines and electroconductive particle is contained at above-mentioned electric conducting material, and above-mentioned amines is when being the primary amine with aromatic ring, although use cation propellant, but the storage stability of electric conducting material can be improved, when being electrically connected between to electrode, effectively can improve interelectrode conducting reliability.
Curability compound, cation propellant, amines and electroconductive particle is contained at above-mentioned electric conducting material, and above-mentioned amines is when being the primary amine with aromatic ring, particularly by using above-mentioned cation propellant and the primary amine with above-mentioned aromatic ring, although use cation propellant, the storage stability of electric conducting material becomes quite high.With regard to electric conducting material of the present invention, even if keeping between long-term, curability also not easily changes.Its result, the cementability of the connecting object parts bonding by electric conducting material further raises.And, with regard to above-mentioned electric conducting material, although use cation propellant, when being electrically connected between to electrode, interelectrode conducting reliability can be improved.
In addition, the discoveries such as the present inventor: by using the primary amine with above-mentioned aromatic ring, with use compared with the amines without aromatic ring or the situation using the amines beyond primary amine, in the electric conducting material containing cation propellant, the storage stability of electric conducting material and interelectrode conducting reliability can be improved.
Above-mentioned curability compound can for the curability compound (Thermocurable compound or light and Thermocurable compound) that can be solidified by heating, also can for being penetrated by illumination and the curability compound (photocurable compound or light and Thermocurable compound) that can solidify.Curability compound that above-mentioned curability compound can solidify preferably by heating (Thermocurable compound or light and Thermocurable compound).
Above-mentioned electric conducting material is the electric conducting material that can be solidified by heating, as above-mentioned curability compound, and can containing the curability compound (Thermocurable compound or light and Thermocurable compound) that can be solidified by heating.Should the curability compound that can be solidified by heating can for penetrate by illumination the curability compound (Thermocurable compound) do not solidified, also can be the curability compound (light and Thermocurable compound) penetrated by illumination and can solidify both heating.
In addition, above-mentioned electric conducting material is the electric conducting material penetrated and heat both by illumination and can solidify, as above-mentioned curability compound, the curability compound (photocurable compound or light and Thermocurable compound) that preferably also can solidify containing being penetrated by illumination.In this situation, make electric conducting material semi-solid preparation (B-stage) being penetrated by illumination, make the mobility of electric conducting material reduce after, electric conducting material can be solidified by heating.So-called semi-solid preparation instigates electric conducting material to be cured, but do not make electric conducting material solidify completely.Penetrate above by illumination and the curability compound that can solidify can for by heating the curability compound (photocurable compound) do not solidified, also can for being penetrated by illumination and heat both and the curability compound (light and Thermocurable compound) that can solidify.
The above-mentioned cation propellant that can use in electric conducting material of the present invention can for producing cationic cation propellant (hot cation propellant or light and hot cation propellant) by heating, also can produce cationic smooth cation propellant (light cation propellant or light and hot cation propellant) for being penetrated by illumination.Above-mentioned cation propellant produces cationic cation propellant (hot cation propellant or light and hot cation propellant) preferably by heating.Preferably by the effect of above-mentioned cation propellant, make above-mentioned electric conducting material generation hot curing.Also by the effect of above-mentioned cation propellant, above-mentioned electric conducting material generation photocuring can be made, and by the effect of above-mentioned cation propellant, make above-mentioned electric conducting material generation hot curing.
Electric conducting material of the present invention can contain trigger for optical solidification.Electric conducting material of the present invention preferably contains optical free radical propellant as above-mentioned trigger for optical solidification.
Above-mentioned electric conducting material preferably contains Thermocurable compound, contains photocurable compound or light and Thermocurable compound as above-mentioned curability compound further.Above-mentioned electric conducting material preferably containing Thermocurable compound and photocurable compound as above-mentioned curability compound.
Below, the details of each composition being preferred for electric conducting material of the present invention is described.
(curability compound)
Curability compound contained in above-mentioned electric conducting material is not particularly limited.As above-mentioned curability compound, existing known curability compound can be used.Above-mentioned curability compound can be used singly or in combination of two or more.
Above-mentioned curability compound is preferably containing the curability compound with epoxy radicals.The curability compound with epoxy radicals is epoxy compounds.The above-mentioned curability compound with epoxy radicals can be used singly or in combination of two or more.
The above-mentioned curability compound with epoxy radicals preferably has aromatic ring.As above-mentioned aromatic ring, can enumerate: phenyl ring, naphthalene nucleus, anthracene nucleus, phenanthrene ring, aphthacene ring,
(chrysene) ring, triphen pushing out ring, butylbenzene ring, pyrene ring, pentacene Huan, Pi Huan are Ji perylene ring etc.Wherein, above-mentioned aromatic ring is preferably phenyl ring, naphthalene nucleus or anthracene nucleus, is more preferably phenyl ring or naphthalene nucleus, more preferably naphthalene nucleus.Because naphthalene nucleus has planar structure, therefore, can it be further made to solidify rapidly.
From the view point of the curability improving above-mentioned electric conducting material, in the entirety 100 % by weight of above-mentioned curability compound, the above-mentioned content with the curability compound of epoxy radicals is preferably more than 10 % by weight, is more preferably more than 20 % by weight, less than 100 % by weight.The total amount of above-mentioned curability compound can for having the curability compound of above-mentioned epoxy radicals.When combinationally using the curability compound and other curability compound different from the curability compound with this epoxy radicals with above-mentioned epoxy radicals, in the entirety 100 % by weight of above-mentioned curability compound, the above-mentioned content with the curability compound of epoxy radicals is preferably less than 99 % by weight, be more preferably less than 95 % by weight, more preferably less than 90 % by weight, be particularly preferably less than 80 % by weight.
Above-mentioned curability compound, preferably containing be the epoxy compounds of liquid at 23 DEG C, preferably containing the epoxy compounds being solid at 23 DEG C, preferably to contain at 23 DEG C for the epoxy compounds of liquid and is both epoxy compoundss of solid at 23 DEG C.
As above-mentioned epoxy compounds, can enumerate: the hydride etc. of bisphenol A type epoxy compound, bisphenol F type epoxy compound, bisphenol E-type epoxy compounds and bisphenol S type epoxy compound and these epoxy compoundss.Wherein, further be improved from the viewpoint of the curability of electric conducting material, the glass transition temperature of solidfied material is further improved and moisture-proof further reduces and then can obtain the further excellent solidfied material of thermal endurance, uv-resistance and cementability, above-mentioned be that the epoxy compounds of liquid is preferably bisphenol A type epoxy compound, bisphenol F type epoxy compound, hydrogenated bisphenol A type epoxy compounds or A Hydrogenated Bisphenol A F type epoxy compounds at 23 DEG C.
The weight average molecular weight of the above-mentioned epoxy compounds for liquid at 23 DEG C is preferably more than 150, is more preferably more than 200, is preferably less than 1200, is more preferably less than 1000.When above-mentioned weight average molecular weight is more than above-mentioned lower limit, the glass transition temperature of solidfied material further raises, and the moisture-proof of solidfied material is further improved.When above-mentioned weight average molecular weight is below the above-mentioned upper limit, the screening characteristics of electric conducting material and curability further become good.
In the entirety 100 % by weight of above-mentioned curability compound, the content of the above-mentioned epoxy compounds for liquid at 23 DEG C is preferably more than 30 % by weight, is more preferably more than 40 % by weight, is preferably less than 90 % by weight, is more preferably less than 80 % by weight.When the content of the epoxy compounds of aforesaid liquid is more than above-mentioned lower limit, the screening characteristics of electric conducting material is further improved.When the content of the epoxy compounds of aforesaid liquid is below the above-mentioned upper limit, the screening characteristics of electric conducting material is further improved, and the moisture-proof of solidfied material further raises.
As above-mentioned be the epoxy compounds of solid at 23 DEG C, can enumerate such as: the hydride etc. of bisphenol A type epoxy compound, bisphenol F type epoxy compound, bisphenol E-type epoxy compounds, bisphenol S type epoxy compound and these epoxy compoundss.Wherein, further be improved from the curability of electric conducting material, the glass transition temperature of solidfied material further raises and moisture-proof further reduces, and then the consideration of thermal endurance, uv-resistance and aspect excellent in adhesion, the above-mentioned epoxy compounds for liquid at 23 DEG C is preferably bisphenol A type epoxy compound, bisphenol F type epoxy compound, hydrogenated bisphenol A type epoxy compounds or A Hydrogenated Bisphenol A F type epoxy compounds.
The weight average molecular weight of the above-mentioned epoxy compounds for solid at 23 DEG C is preferably more than 200, is more preferably more than 250, is preferably less than 5000, is more preferably less than 4500.When above-mentioned weight average molecular weight is more than above-mentioned lower limit, moisture-proof and the cementability of solidfied material are further improved.When above-mentioned weight average molecular weight is below the above-mentioned upper limit, the curability of electric conducting material further becomes good, the softening point of above-mentioned electric conducting material becomes suitable, and the compatibility of the epoxy compounds of aforesaid liquid shape and the epoxy compounds of above-mentioned solid is further improved.
Above-mentioned weight average molecular weight is with the value of the polystyrene basis utilizing gel permeation chromatography (GPC) to measure.The post used in mensuration as above-mentioned weight average molecular weight can be enumerated such as: Showa electrician Inc. " ShodexLF-804 " etc.
In the entirety 100 % by weight of above-mentioned curability compound, the content of the above-mentioned epoxy compounds for solid at 23 DEG C is preferably more than 10 % by weight, is more preferably more than 15 % by weight, is preferably less than 40 % by weight, is more preferably less than 35 % by weight.When the content of the epoxy compounds of above-mentioned solid is more than above-mentioned lower limit, the moisture-proof of solidfied material is further improved.When the content of the epoxy compounds of above-mentioned solid is below the above-mentioned upper limit, the screening characteristics of electric conducting material is further improved.
In addition, above-mentioned curability compound is preferably containing cycloaliphatic epoxy.This cycloaliphatic epoxy is preferably the epoxy compounds of aforesaid liquid, is preferably the epoxy compounds of above-mentioned solid, is more preferably the epoxy compounds of aforesaid liquid and both epoxy compoundss of above-mentioned solid.The weight average molecular weight of above-mentioned cycloaliphatic epoxy is preferably more than 100, is more preferably more than 150, is preferably less than 1000, is more preferably less than 800.By the use of cycloaliphatic epoxy, or be the use of cycloaliphatic epoxy of below more than above-mentioned lower limit and the above-mentioned upper limit by weight average molecular weight, the curability of electric conducting material further becomes good.When the weight average molecular weight of above-mentioned cycloaliphatic epoxy is more than above-mentioned lower limit, the volatility not easily producing cycloaliphatic epoxy reduces, and produces the problem of gas.When the weight average molecular weight of above-mentioned cycloaliphatic epoxy is below the above-mentioned upper limit, the viscosity of electric conducting material becomes suitable.The screening characteristics of electric conducting material is further improved.
As the commercially available product of above-mentioned alicyclic epoxy resin, can enumerate: CELLOXIDE2021P, CELLOXIDE2081P, CELLOXIDE2000, CELLOXIDE2083, CELLOXIDE2085 and CELLOXIDE3000 (being Daicel company to manufacture) etc.Wherein, low from the viewpoint of viscosity, curability is excellent, preferred CELLOXIDE2021P.
In the entirety 100 % by weight of above-mentioned curability compound, the content of above-mentioned cycloaliphatic epoxy is preferably more than 5 % by weight, is preferably less than 30 % by weight, is more preferably less than 25 % by weight.When the content of above-mentioned cycloaliphatic epoxy is more than above-mentioned lower limit, the curability of electric conducting material is further improved.When the content of above-mentioned cycloaliphatic epoxy is below the above-mentioned upper limit, the screening characteristics of electric conducting material is further improved.
In addition, above-mentioned curability compound is preferably containing phenol novolak-type epoxy compound.
Above-mentioned curability compound can further containing other curability compound different from the curability compound with epoxy radicals.As this other curability compound, can enumerate: there are the curability compound of unsaturated double-bond, phenol cured compound, amino curability compound, curable unsaturated polyester compound, urethane cures compound, silicone cure compound and polyimide curing compound etc.Other curability compound above-mentioned can be used singly or in combination of two or more.
From the view point of easily to regulate and control the solidification of above-mentioned electric conducting material or interelectrode conducting reliability is further improved, above-mentioned curability compound is preferably containing the curability compound with unsaturated double-bond.From the view point of easily to regulate and control the solidification of above-mentioned electric conducting material or interelectrode conducting reliability is further improved, the curability compound with above-mentioned unsaturated double-bond preferably has the curability compound of (methyl) acryloyl group.By using the curability compound with above-mentioned (methyl) acryloyl group; easily in the electric conducting material entirety (comprising the part of direct irradiation light and the part of not direct irradiation light) of having carried out B-stage, curing degree is regulated to preferred scope, or interelectrode conducting reliability is further improved.
From easily regulating and controlling the curing degree of the conductive material layer carrying out B-stage; and the viewpoint that interelectrode conducting reliability is further improved is set out, the curability compound with above-mentioned (methyl) acryloyl group preferably has 1 or 2 (methyl) acryloyl groups.
As the curability compound with above-mentioned (methyl) acryloyl group, can enumerate: not there is epoxy radicals and there is the curability compound of (methyl) acryloyl group and there is epoxy radicals and there is the curability compound of (methyl) acryloyl group.
As the above-mentioned curability compound with (methyl) acryloyl group, (methyl) acrylic acid is preferably used react with the compound with hydroxyl and epoxy (methyl) acrylate that the ester compounds, (methyl) acrylic acid and the epoxy compounds that obtain react and obtain or (methyl) acrylic acid derivative of making isocyanates and having a hydroxyl react and obtain (methyl) propenoic methyl carbamate etc.Above-mentioned " (methyl) acryloyl group " represents acryloyl group and methacryl.Above-mentioned " (methyl) acrylic " represents acrylic and methylpropenyl.Above-mentioned " (methyl) acrylate " represents acrylate and methacrylate.
Above-mentioned curability compound is preferably containing epoxy (methyl) acrylate.Above-mentioned epoxy (methyl) acrylate is make the whole epoxy radicals in epoxy compounds and (methyl) acrylic acid react the compound formed.
As the commercially available product of above-mentioned epoxy (methyl) acrylate, can enumerate: EBECRYL860, EBECRYL3200, EBECRYL3201, EBECRYL3412, EBECRYL3600, EBECRYL3700, EBECRYL3701, EBECRYL3702, EBECRYL3703, EBECRYL3800, EBECRYL6040 and EBECRYLRDX63182 (being Daicel-Allnex company to manufacture), EA-1010, EA-1020, EA-5323, EA-5520, EA-CHD and EMA-1020 (being chemical industrial company of Xin Zhong village to manufacture), EpoxyesterM-600A, Epoxyester 40EM, Epoxyester 70PA, Epoxyester 200PA, Epoxyester 80MFA, Epoxyester 3002M, Epoxyester 3002A, Epoxyester 1600A, Epoxyester 3000M, Epoxyester 3000A, Epoxyester 200EA and Epoxyester 400EA (being chemistry Inc. of common prosperity company to make), and Denacol Acrylate DA-141, Denacol Acrylate DA-314 and Denacol AcrylateDA-911 (being Nagase ChemteX company to manufacture) etc.
The ester compounds that above-mentioned (methyl) acrylic acid reacts with the compound with hydroxyl and obtains is not particularly limited.As this ester compounds, the ester compounds of simple function, the ester compounds of 2 officials' energy and 3 officials can all can use by ester compounds above.
There is above-mentioned epoxy radicals and the curability compound with (methyl) acryloyl group is transformed to (methyl) acryloyl group and the curability compound obtained preferably by the epoxy radicals of a part for the compound by having more than 2 epoxy radicals.This curability compound is part (methyl) Acrylated Epoxy compound.
Above-mentioned curability compound is preferably containing having the compound of more than 2 epoxy radicals and (methyl) acrylic acid reactant.This reactant conventionally reacts to obtain with (methyl) acrylic acid by making the compound with more than 2 epoxy radicals in the presence of a catalyst.20% of preferred epoxy radicals is (methyl) acryloyl group with up conversion (conversion ratio).Conversion ratio is more preferably more than 30%, is preferably less than 80%, is more preferably less than 70%.Most preferably more than 40%, less than 60% of epoxy radicals be transformed to (methyl) acryloyl group.
As above-mentioned part (methyl) Acrylated Epoxy compound, can enumerate: biphenol type epoxy part (methyl) acrylate, cresol novolak type epoxy part (methyl) acrylate, carboxylic acid anhydride modified epoxy moieties (methyl) acrylate and phenol novolak-type epoxy part (methyl) acrylate etc.
As above-mentioned curability compound, a part of epoxy radicals of the phenoxy resin with more than 2 epoxy radicals can be used to be transformed to the modification phenoxy resin of (methyl) acryloyl group.That is, the modification phenoxy resin with epoxy radicals and (methyl) acryloyl group can be used.
In addition, above-mentioned curability compound can be cross-linked compound, also can be non-crosslinked compound.
As the concrete example of above-mentioned cross-linked compound, can enumerate such as: 1, 4-butanediol two (methyl) acrylate, 1, 6-hexylene glycol two (methyl) acrylate, 1, 9-nonanediol two (methyl) acrylate, (gathering) ethylene glycol bisthioglycolate (methyl) acrylate, (gathering) propylene glycol two (methyl) acrylate, neopentyl glycol two (methyl) acrylate, pentaerythrite two (methyl) acrylate, glycerol methacrylate acrylate, pentaerythrite three (methyl) acrylate, trimethylol-propane trimethacrylate, (methyl) allyl acrylate, (methyl) vinyl acrylate, divinylbenzene, polyester (methyl) acrylate and (methyl) propenoic methyl carbamate etc.
As the concrete example of above-mentioned non-crosslinked compound, can enumerate: (methyl) ethyl acrylate, (methyl) n-propyl, (methyl) isopropyl acrylate, (methyl) n-butyl acrylate, (methyl) isobutyl acrylate, (methyl) tert-butyl acrylate, (methyl) amyl acrylate, (methyl) Hexyl 2-propenoate, (methyl) heptylacrylate, (methyl) 2-EHA, (methyl) n-octyl, (methyl) Isooctyl acrylate monomer, (methyl) acrylic acid ester in the ninth of the ten Heavenly Stems, (methyl) decyl acrylate, (methyl) acrylic acid undecyl ester, (methyl) dodecylacrylate, (methyl) tridecyl acrylate and (methyl) acrylic acid myristyl ester etc.
When combinationally using Thermocurable compound and photocurable compound, the mix proportion of photocurable compound and Thermocurable compound suitably adjusts according to the kind of photocurable compound and Thermocurable compound.Above-mentioned electric conducting material is preferably that 1:99 ~ 90:10 contains photocurable compound and Thermocurable compound with mass ratio range, more preferably contains with 5:95 ~ 60:40, preferably further contains with 10:90 ~ 40:60.
(curing agent)
Above-mentioned electric conducting material contains curing agent.This curing agent contains thermal curing agents, can contain trigger for optical solidification further.This curing agent contains cation propellant.As this cation propellant, existing known cation propellant can be used.In addition, in the present invention, cation propellant not only as making the light cation propellant of electric conducting material photocuring use, preferably as making the hot cation propellant of electric conducting material at least hot curing use.And then, in the present invention, cation propellant not only as making the light cation propellant of electric conducting material photocuring use, more preferably as making the hot cation propellant of electric conducting material hot curing use.Above-mentioned cation propellant can be used singly or in combination of two or more.
As above-mentioned cation propellant, preferably use salt compounded of iodine and sulfonium salt.Such as, as the commercially available product of above-mentioned cation propellant, can enumerate: Adekaoptomer SP-150, the Adekaoptomer SP-170 etc. of San-Aid SI-45L, San-AidSI-60L, San-Aid SI-80L, San-Aid SI-100L, San-Aid SI-110L, San-Aid SI-150L and ADEKA Inc. that three new chemical companies manufacture.
As the anionicsite of preferred cation propellant, can enumerate: PF
6, BF
4and B (C
6f
5)
4.
In addition, as other concrete example of above-mentioned cation propellant, can enumerate: 2-cyclobutenyl dimethyl sulfonium four (pentafluorophenyl group) borate, 2-cyclobutenyl dimethyl sulfonium tetrafluoroborate, 2-cyclobutenyl dimethyl sulfonium hexafluorophosphate, 2-cyclobutenyl tetramethylene sulfonium four (pentafluorophenyl group) borate, 2-cyclobutenyl tetramethylene sulfonium tetrafluoroborate, 2-cyclobutenyl tetramethylene sulfonium hexafluorophosphate, 3-methyl-2-butene base dimethyl sulfonium four (pentafluorophenyl group) borate, 3-methyl-2-butene base dimethyl sulfonium tetrafluoroborate, 3-methyl-2-butene base dimethyl sulfonium hexafluorophosphate, 3-methyl-2-butene base tetramethylene sulfonium four (pentafluorophenyl group) borate, 3-methyl-2-butene base tetramethylene sulfonium tetrafluoroborate, 3-methyl-2-butene base tetramethylene sulfonium hexafluorophosphate, 4-hydroxy phenyl cinnamyl methyl sulfonium four (pentafluorophenyl group) borate, 4-hydroxy phenyl cinnamyl methyl sulfonium tetrafluoroborate, 4-hydroxy phenyl cinnamyl methyl sulfonium hexafluorophosphate, Alpha-Naphthyl methyltetramethylene sulfonium four (pentafluorophenyl group) borate, Alpha-Naphthyl methyltetramethylene sulfonium tetrafluoroborate, Alpha-Naphthyl methyltetramethylene sulfonium hexafluorophosphate, cinnamyl dimethyl sulfonium four (pentafluorophenyl group) borate, cinnamyl dimethyl sulfonium tetrafluoroborate, cinnamyl dimethyl sulfonium hexafluorophosphate, cinnamyl tetramethylene sulfonium four (pentafluorophenyl group) borate, cinnamyl tetramethylene sulfonium tetrafluoroborate, cinnamyl tetramethylene sulfonium hexafluorophosphate, Biphenylmethyl dimethyl sulfonium four (pentafluorophenyl group) borate, Biphenylmethyl dimethyl sulfonium tetrafluoroborate, Biphenylmethyl dimethyl sulfonium hexafluorophosphate, Biphenylmethyl tetramethylene sulfonium four (pentafluorophenyl group) borate, Biphenylmethyl tetramethylene sulfonium tetrafluoroborate, Biphenylmethyl tetramethylene sulfonium hexafluorophosphate, phenyl methyl dimethyl sulfonium four (pentafluorophenyl group) borate, phenyl methyl dimethyl sulfonium tetrafluoroborate, phenyl methyl dimethyl sulfonium hexafluorophosphate, phenyl methyl tetramethylene sulfonium four (pentafluorophenyl group) borate, phenyl methyl tetramethylene sulfonium tetrafluoroborate, phenyl methyl tetramethylene sulfonium hexafluorophosphate, fluorenyl methyl dimethyl sulfonium four (pentafluorophenyl group) borate, fluorenyl methyl dimethyl sulfonium tetrafluoroborate, fluorenyl methyl dimethyl sulfonium hexafluorophosphate, fluorenyl methyl tetramethylene sulfonium four (pentafluorophenyl group) borate, fluorenyl methyl tetramethylene sulfonium tetrafluoroborate, and fluorenyl methyl tetramethylene sulfonium hexafluorophosphate etc.
Above-mentioned cation propellant is released inorganic acid ion preferably by heating or is released the organic acid ion containing boron atom by heating.Above-mentioned cation propellant releases the composition of inorganic acid ion preferably by heating, also releases the composition of the organic acid ion containing boron atom preferably by heating.
The cation propellant of being released inorganic acid ion by heating preferably has SbF
6-or PF
6as the compound of anionicsite.Above-mentioned cation propellant preferably has SbF
6-as the compound of anionicsite, also preferably there is PF
6-as the compound of anionicsite.
The anionicsite of above-mentioned cation propellant preferably uses B (C
6x
5)
4-represent.The cation propellant of releasing the organic acid ion containing boron atom preferably has the compound of the anionicsite shown in following formula (1).
[chemical formula 1]
In above-mentioned formula (1), X represents halogen atom.The preferred chlorine atom of X in above-mentioned formula (1), bromine atoms or fluorine atom, be more preferably fluorine atom.
The anionicsite of above-mentioned cation propellant preferably uses B (C
6f
5)
4-represent.The cation propellant that above-mentioned releasing contains the organic acid ion of boron atom more preferably has the compound of the anionicsite shown in following formula (1A).
[chemical formula 2]
In addition, the kind of above-mentioned cation propellant can be that ionic light produces acid type, also can produce acid type for nonionic light.Above-mentioned cation propellant is preferably antimony complex, has salt or the salt shown in following formula (2) that 6 fluoridize phosphonium ion.
[chemical formula 3]
In above-mentioned formula (2), n represents the integer of 1 ~ 12, and m represents the integer of 1 ~ 5, Rf represent alkyl all or part of hydrogen atom is substituted by the fluoroalkyl of fluorine atom.
Above-mentioned antimony complex is not particularly limited, and is preferably sulfonium salt.As the sulfonium salt of above-mentioned antimony complex, can enumerate: tetraphenyl (diphenylsulfide-4,4 '-two base) two sulfonium two (antimony hexafluoride), four (4-methoxyphenyls) [diphenylsulfide-4,4 '-two base] two sulfonium two (antimony hexafluoride), diphenyl (4-phenylthiophenyl) sulfonium antimony hexafluoride and two (4-methoxyphenyl) [4-phenylthiophenyl] sulfonium antimony hexafluoride etc.
As the commercially available product of above-mentioned antimony complex, can enumerate such as: Adekaoptomer SP170 (manufacture of ADEKA company) etc.
As above-mentioned, there is the commercially available product that 6 fluoridize the salt of phosphonium ion, can enumerate such as: WPI-113 (manufacturing with light pure pharmaceutical worker's industry company) and CPI-100P (manufacture of san-apro company) etc.
The content of above-mentioned cation propellant is not particularly limited.Relative to above-mentioned curability compound 100 weight portion, the content of above-mentioned cation propellant is preferably more than 0.01 weight portion, be more preferably more than 0.05 weight portion, more preferably more than 5 weight portions, be particularly preferably more than 10 weight portions, be preferably below 40 weight portions, be more preferably below 30 weight portions, more preferably below 20 weight portions.When being below more than above-mentioned lower limit and the above-mentioned upper limit relative to the content of above-mentioned curability compound above-mentioned cation propellant, electric conducting material solidifies fully.
Relative to curability compound 100 weight portion that can solidify above by heating, the content of above-mentioned cation propellant is preferably more than 0.01 weight portion, be more preferably more than 0.05 weight portion, more preferably more than 5 weight portions, be particularly preferably more than 10 weight portions, be preferably below 40 weight portions, be more preferably below 30 weight portions, more preferably below 20 weight portions.When being below more than above-mentioned lower limit and the above-mentioned upper limit relative to the content of the above-mentioned cation propellant of the curability compound that can solidify above by heating, electric conducting material is hot curing fully.
From the view point of further improving the connection reliability of connection structural bodies under high humidity such as interelectrode conducting reliability and organic EL display element, above-mentioned electric conducting material is preferably containing both above-mentioned cation propellant and hot radical propellant.Above-mentioned hot radical propellant is not particularly limited.As above-mentioned hot radical propellant, existing known hot radical propellant can be used.Above-mentioned hot radical propellant can be used singly or in combination of two or more.At this, " hot radical propellant " refers to the compound generating free radical kind by heating.
As above-mentioned hot radical propellant, be not particularly limited, can azo-compound and peroxide etc. be enumerated.As above-mentioned peroxide, can enumerate: diacyl peroxide compound, peroxyester compound, peroxide compound, peroxy dicarbonate compound, peroxy ketal compound, dialkyl peroxide compound and ketone peroxide compound etc.
As other example of above-mentioned thermal curing agents, can enumerate: the addition product etc. of hydrazide compound, imidazolium compounds, acid anhydrides, dicyandiamide, guanidine compound, modified aliphatic polyamines, amines and epoxy compounds.
As above-mentioned hydrazide compound, be not particularly limited, can enumerate such as: two [Hydrazinocarbonyl ethyl-5-isopropyl hydantoins] (1,3-PVC ス [ヒ De ラ ジ ノ カ Le ボ Application エ チ ル ー 5-イ ソ プ ロ ピ Le ヒ ダ Application ト イ Application]) of 1,3-etc.
As above-mentioned imidazolium compounds, be not particularly limited, can enumerate such as: 1-cyano ethyl-2-phenylimidazole, N-[2-(2-methyl isophthalic acid-imidazole radicals) ethyl] urea, 2,4-diaminourea-6-[2 '-methylimidazolyl-(1 ')]-ethyl-s-triazine, N, N '-bis-(2-methyl isophthalic acid-imidazolylethyl) urea, N, N '-(2-methyl isophthalic acid-imidazolylethyl)-adipamide, 2-phenyl-4-methyl-5-hydroxymethylimidazole and 2-phenyl-4,5-bishydroxymethyl imidazoles etc.
As above-mentioned acid anhydrides, be not particularly limited, such as tetrabydrophthalic anhydride and ethylene glycol-bis-(dehydration trimellitates) etc. can be enumerated.
The content of above-mentioned thermal curing agents is not particularly limited.Relative to curability compound 100 weight portion that can solidify above by heating in above-mentioned curability compound, the content of above-mentioned thermal curing agents is preferably more than 0.01 weight portion, be more preferably more than 0.05 weight portion, more preferably more than 5 weight portions, be particularly preferably more than 10 weight portions, be preferably below 40 weight portions, be more preferably below 30 weight portions, more preferably below 20 weight portions.When the content of above-mentioned thermal curing agents is below more than above-mentioned lower limit and the above-mentioned upper limit, electric conducting material hot curing fully can be made.With regard to the content of above-mentioned thermal curing agents, when above-mentioned thermal curing agents is only hot cation propellant, represent the content of cation propellant, when above-mentioned thermal curing agents comprise cation propellant and other thermal curing agents (hot radical propellant etc.) both, represent the total content of cation propellant and other thermal curing agents.
When above-mentioned curing agent contains hot radical propellant, relative to curability compound 100 weight portion that can solidify above by heating in above-mentioned curability compound, the content of above-mentioned hot radical propellant is preferably more than 0.01 weight portion, be more preferably more than 0.05 weight portion, be preferably below 10 weight portions, be more preferably below 5 weight portions.When the content of above-mentioned hot radical propellant is below more than above-mentioned lower limit and the above-mentioned upper limit, electric conducting material hot curing fully can be made.
Above-mentioned electric conducting material can containing trigger for optical solidification as above-mentioned curing agent.Containing above-mentioned light cation propellant (light cation propellant or light and hot cation propellant) in trigger for optical solidification.Above-mentioned trigger for optical solidification is not particularly limited.As above-mentioned trigger for optical solidification, existing known trigger for optical solidification can be used.From the view point of the connection reliability further improving the connection structural bodies such as interelectrode conducting reliability and organic EL display element, above-mentioned electric conducting material is preferably containing optical free radical propellant.Above-mentioned trigger for optical solidification can be used singly or in combination of two or more.
As other trigger for optical solidification beyond above-mentioned cation propellant; be not particularly limited, can enumerate: acetophenone trigger for optical solidification (acetophenone optical free radical propellant), benzophenone trigger for optical solidification (benzophenone optical free radical propellant), thioxanthones, ketal trigger for optical solidification (ketal optical free radical propellant), halogenation ketone, acylphosphine oxide and acyl phosphonate etc.
The content of above-mentioned trigger for optical solidification is not particularly limited.Relative to penetrating above by illumination and curability compound 100 weight portion that can solidify in above-mentioned curability compound, the content of above-mentioned trigger for optical solidification is preferably more than 0.1 weight portion, be more preferably more than 0.2 weight portion, be preferably below 2 weight portions, be more preferably below 1 weight portion.When the content of above-mentioned trigger for optical solidification is below more than above-mentioned lower limit and the above-mentioned upper limit, electric conducting material suitably photocuring can be made.By irradiating light to electric conducting material and carrying out B-stage, the flowing of electric conducting material can be suppressed.The content of above-mentioned trigger for optical solidification, when above-mentioned trigger for optical solidification is only cation propellant, represents the content of cation propellant; And when above-mentioned trigger for optical solidification contains cation propellant and other both trigger for optical solidification, represent the total content of cation propellant and other trigger for optical solidification.
(inorganic filler)
Above-mentioned electric conducting material is preferably containing inorganic filler.The reduction that this inorganic filler has electric conducting material is solidifying medium viscosity suppresses, and further improves the effect of the moisture-proof of solidfied material.Above-mentioned inorganic filler can be used singly or in combination of two or more.
The average grain diameter of above-mentioned inorganic filler is preferably more than 0.1 μm, is more preferably more than 0.2 μm, is preferably less than 2 μm, is more preferably less than 1.5 μm.Above-mentioned average grain diameter is that the inorganic filler below more than above-mentioned lower limit and the above-mentioned upper limit makes the moisture-proof of solidfied material further improve.When the average grain diameter of above-mentioned inorganic filler is below the above-mentioned upper limit, in solidfied material, more not easily produce space.It should be noted that, the average grain diameter of above-mentioned inorganic filler is volume average particle size.Above-mentioned average grain diameter can use the mensuration such as laser diffraction/diffuse transmission type particle size distribution analyzer.
As above-mentioned inorganic filler, can enumerate: talcum, asbestos, silicon dioxide, montmorillonite, bentonite, calcium carbonate, magnesium carbonate, aluminium oxide, imvite, diatomite, magnesium oxide, titanium oxide, magnesium hydroxide, aluminium hydroxide, bead, barium sulfate, gypsum, calcium silicates and sericite atlapulgite etc.Wherein, in order to adhesive improves and moisture-proof is improved, preferably talc.
Above-mentioned inorganic filler is preferably tabular.The average surplus ratio of above-mentioned inorganic filler is more than 1, is preferably more than 1.5, is more preferably more than 2, is preferably less than 10, is more preferably less than 5.The average surplus of above-mentioned inorganic filler, than when being below the above-mentioned upper limit, is difficult to insert inorganic filler, its result, interelectrode contact resistance further step-down between electrode and electroconductive particle.Further, also can carry out orientation well to inorganic filler, its result with low pressure, the thickness of the connecting portion formed by electroconductive particle further becomes even.Above-mentioned average surplus is than the mean value of minor axis of major diameter/inorganic filler referring to inorganic filler.
The content of above-mentioned inorganic filler is not particularly limited.Relative to above-mentioned curability compound 100 weight portion, the content of above-mentioned inorganic filler is preferably more than 1 weight portion, is more preferably more than 2 weight portions, is preferably below 30 weight portions, is more preferably below 28 weight portions.When the content of above-mentioned inorganic filler is more than above-mentioned lower limit, in solidfied material, more not easily produce space.When the content of above-mentioned inorganic filler is below the above-mentioned upper limit, the screening characteristics of electric conducting material is further improved.
(organic filler)
Above-mentioned electric conducting material is preferably containing organic filler.This organic filler works as gelating agent.Above-mentioned organic filler is swelling in electric conducting material at normal temperatures, and the viscosity of electric conducting material is suitably improved.Further, above-mentioned organic filler has the effect suppressing viscosity to reduce in the solidification of electric conducting material.In addition, by combinationally using above-mentioned organic filler and inorganic filler, even if adhesive substrates under a reduced-pressure atmosphere, also not easily in solidfied material, produce space significantly.Above-mentioned organic filler can be used singly or in combination of two or more.
Above-mentioned organic filler is more preferably the core shell particles having core He be configured at the shell on the surface of this core.Above-mentioned core is preferably formed by the 1st (methyl) acrylic resin.It should be noted that, (methyl) acrylic resin refers to (methyl) acrylate to be the general name of the resin of main component, also containing acrylic rubber etc. in (methyl) acrylic resin.Above-mentioned shell is preferably formed by the 2nd acrylic resin.The glass transition temperature of above-mentioned 1st (methyl) acrylic resin is preferably less than 23 DEG C.Preferably the glass transition temperature of above-mentioned 2nd (methyl) acrylic resin is higher than the glass transition temperature of above-mentioned 1st (methyl) acrylic resin.The glass transition temperature of above-mentioned 2nd (methyl) acrylic resin is preferably more than 23 DEG C.
Above-mentioned organic filler is more preferably the core shell particles having core He be configured at the shell on the surface of this core.Above-mentioned core is preferably formed by the 1st (methyl) acrylic resin.Above-mentioned shell is preferably formed by the 2nd acrylic resin.Preferably the glass transition temperature of above-mentioned 2nd (methyl) acrylic resin is higher than the glass transition temperature of above-mentioned 1st (methyl) acrylic resin.
As the commercially available product of above-mentioned organic filler, can enumerate such as: rayon Inc. of Mitsubishi " METABLENE W-5500, METABLENE W-450A " and GANZ change into core shell acrylate copolymer particulate " F-351 " etc. of Inc..
The average grain diameter of above-mentioned organic filler is preferably more than 0.05 μm, is more preferably more than 0.1 μm, more preferably more than 0.2 μm, is preferably less than 1 μm, is more preferably less than 0.9 μm.It should be noted that, the average grain diameter of above-mentioned organic filler is volume average particle size.Above-mentioned average grain diameter can use the mensuration such as laser diffraction/diffuse transmission type particle size distribution analyzer.
The content of above-mentioned organic filler is not particularly limited.Relative to above-mentioned curability compound 100 weight portion, the content of above-mentioned organic filler is preferably more than 1 weight portion, is more preferably more than 5 weight portions, is preferably below 30 weight portions, is more preferably below 20 weight portions.When the content of above-mentioned organic filler is more than above-mentioned lower limit, the viscosity of electric conducting material becomes suitable, not easily in solidfied material, produces space significantly.When the content of above-mentioned organic filler is below the above-mentioned upper limit, the screening characteristics of electric conducting material is further improved.
(amines)
Above-mentioned electric conducting material is preferably containing amines.Above-mentioned amines preferably has the primary amine of aromatic ring.The primary amine with this specific aromatic ring is used to go far towards the storage stability of the electric conducting material improved containing cation propellant.Above-mentioned amines can be used singly or in combination of two or more.
As the aromatic ring in above-mentioned primary amine, the aromatic ring that the aromatic ring as above-mentioned curability compound is enumerated can be enumerated.Wherein, preferred phenyl ring.
As the above-mentioned concrete example with the primary amine of aromatic ring, can enumerate: benzylamine, α, alpha-alpha-dimethyl benzylamine, aniline, 2-naphthylamines, 1-naphthyl methylamine, 2-aminobphenyl and 4-aminobphenyl etc.
Cation propellant in above-mentioned electric conducting material and the above-mentioned content with the primary amine of aromatic ring preferably count 99.9:0.1 ~ 97:3 with weight ratio (cation propellant: primary amine), are more preferably 99.5:0.5 ~ 98:2.
When the above-mentioned content with the primary amine of aromatic ring is in above-mentioned preferred scope, storage stability and the interelectrode conducting reliability of electric conducting material are further stablized.
(electroconductive particle)
As long as above-mentioned electroconductive particle has conductive part on the surface of conductivity.This conductive part is preferably conductive layer.In Fig. 3, as represented an example of electroconductive particle with profile, the conductive layer 13 that electroconductive particle 11 can possess substrate particle 12 and be configured on substrate particle 12 surface.The entirety of electroconductive particle can be the metallic of conductive part.Wherein, from the view point of reducing costs or improving the flexibility of electroconductive particle and improve interelectrode conducting reliability, preferred electroconductive particle has substrate particle and is configured at the conductive layer on substrate particle surface.
As above-mentioned substrate particle, can enumerate: resin particle, inorganic particulate, organic inorganic hybridization particle and metallic etc. except metallic.The substrate particle of above-mentioned substrate particle preferably except metallic, is preferably resin particle, inorganic particulate except metallic or organic inorganic hybridization particle.Above-mentioned substrate particle can for possessing core and the core shell particles being configured at the shell on wicking surface.Above-mentioned core can be organic core, and above-mentioned shell can be inorganic shell.
The resin particle that above-mentioned substrate particle is preferably formed by resin.When connecting between use electroconductive particle is to electrode, crimp after electroconductive particle being configured between electrode, electroconductive particle is compressed.When substrate particle is resin particle, when carrying out above-mentioned crimping, electroconductive particle is easily out of shape, and the contact area of electroconductive particle and electrode increases.Therefore, interelectrode conducting reliability further raises.
As the resin for the formation of above-mentioned resin particle, can enumerate such as: vistanex, acrylic resin, phenolic resin, melmac, benzene guanamine resin, carbamide resin, epoxy resin, unsaturated polyester resin, saturated polyester resin, PETG, polysulfones, polyphenylene oxide, polyacetals, polyimides, polyamidoimide, polyether-ether-ketone, polyether sulfone, divinyl benzene polymers and divinylbenzene analog copolymer etc.As above-mentioned divinylbenzene analog copolymer etc., divinyl benzene styrene copolymer and divinylbenzene-(methyl) acrylate copolymer etc. can be enumerated.Owing to easily regulating and controlling in preferred scope by the hardness of above-mentioned resin particle, therefore, the resin for the formation of above-mentioned resin particle preferably makes the one kind or two or more polymerizable monomer with ethylenically unsaturated group be polymerized and the polymer of formation.
As the inorganic matter for the formation of above-mentioned inorganic particulate, silicon dioxide and carbon black etc. can be enumerated.As above-mentioned organic inorganic hybridization particle, the organic inorganic hybridization particle etc. such as formed by the alkoxysilyl polymer be cross-linked and acrylic resin can be enumerated.
When above-mentioned substrate particle is metallic, as the metal for the formation of this metallic, silver, copper, nickel, silicon, gold and titanium etc. can be enumerated.
Metal for the formation of above-mentioned conductive part is not particularly limited.Further, when the entirety of electroconductive particle is the metallic of conductive part, the metal for the formation of this metallic is not particularly limited.As this metal, can enumerate such as: gold, silver, palladium, copper, platinum, zinc, iron, tin, lead, aluminium, cobalt, indium, nickel, chromium, titanium, antimony, bismuth, thallium, germanium, cadmium, silicon and their alloy etc.In addition, as above-mentioned metal, tin-doped indium oxide (ITO) and solder etc. can be enumerated.Wherein, interelectrode contact resistance further step-down, therefore, the alloy preferably containing tin, nickel, palladium, copper or gold, preferred nickel or palladium.
Above-mentioned conductive layer can be formed by 1 layer.Conductive layer can be formed by multilayer.That is, conductive layer can have the laminated construction of more than 2 layers.When conductive layer is formed by multilayer, outermost layer is preferably layer gold, nickel dam, palladium layers, layers of copper or contains the alloy-layer of tin and silver, is more preferably layer gold.When outermost layer is above-mentioned preferred conductive layer, interelectrode contact resistance further step-down.In addition, when outermost layer is layer gold, corrosion resistance is further improved.
The method forming conductive layer on the surface of above-mentioned substrate particle is not particularly limited.As forming the method for conductive layer, can enumerate such as: utilize the method for electroless plating, utilize electric plating method, utilize the method for physical vapor deposition and by the method etc. on the surface of metal dust or the slurry coated substrate particle containing metal dust and adhesive.Wherein, the formation of conductive layer is easy, therefore, preferably utilizes the method for electroless plating.As the above-mentioned method utilizing physical vapor deposition, the methods such as vacuum evaporation, ion plating and ion sputtering can be enumerated.
The average grain diameter of above-mentioned electroconductive particle is preferably more than 0.5 μm, is more preferably more than 1 μm, is preferably less than 500 μm, be more preferably less than 100 μm, be further preferably less than 80 μm, more preferably less than 70 μm, be particularly preferably less than 50 μm, most preferably be less than 20 μm.When the average grain diameter of electroconductive particle is below more than above-mentioned lower limit and the above-mentioned upper limit, when connecting between use electroconductive particle is to electrode, increase the contact area of electroconductive particle and electrode fully, and be difficult to the electroconductive particle forming cohesion when forming conductive layer.In addition, the interelectrode interval connected via electroconductive particle can not be excessive, and conductive layer is difficult to from substrate particle sur-face peeling.
" average grain diameter " of above-mentioned electroconductive particle represents number average bead diameter.The average grain diameter of electroconductive particle by observing arbitrary electroconductive particle 50 with electron microscope or light microscope, and calculates mean value and obtains.
The thickness of above-mentioned conductive layer is preferably more than 0.005 μm, is more preferably more than 0.01 μm, is preferably less than 10 μm, is more preferably less than 1 μm, more preferably less than 0.3 μm.When the thickness of conductive layer is below more than above-mentioned lower limit and the above-mentioned upper limit, can obtain sufficient conductivity, and electroconductive particle can not be really up to the mark, when carrying out interelectrode connection, electroconductive particle is out of shape fully.
When above-mentioned conductive layer is formed by multilayer, the layer gold thickness when thickness of outermost conductive layer, particularly outermost layer are layer gold is preferably more than 0.001 μm, is more preferably more than 0.01 μm, is preferably less than 0.5 μm, is more preferably less than 0.1 μm.When the thickness of above-mentioned outermost conductive layer is below more than above-mentioned lower limit and the above-mentioned upper limit, what produced by outermost conductive layer coatedly becomes even, and corrosion resistance raises fully, and interelectrode contact resistance step-down fully.In addition, the thickness of layer gold when above-mentioned outermost layer is layer gold is thinner, and cost is lower.
The thickness of above-mentioned conductive layer can measure by using the section of such as transmission electron microscope (TEM) to electroconductive particle or electroconductive particle to observe.
From the contact area increasing electrode and electroconductive particle, and the viewpoint further improving interelectrode conducting reliability is set out, above-mentioned electroconductive particle preferably has resin particle and is configured at the conductive layer (the 1st conductive layer) on the surface of this resin particle.
Insulation processing can be carried out by Ins. ulative material, solder flux etc. such as insulating barrier or insulating properties particles in the surface of the conductive part in above-mentioned electroconductive particle.Heat when preferred Ins. ulative material and solder flux etc. are by connecting occurs to soften, flow and got rid of by connecting portion.Thus, interelectrode short circuit can be suppressed.
The content of above-mentioned electroconductive particle is not particularly limited.In above-mentioned electric conducting material 100 % by weight, the content of above-mentioned electroconductive particle is preferably more than 0.1 % by weight, is more preferably more than 0.5 % by weight, more preferably more than 1 % by weight, be preferably less than 40 % by weight, be more preferably less than 30 % by weight, more preferably less than 19 % by weight.When the content of above-mentioned electroconductive particle is below more than above-mentioned lower limit and the above-mentioned upper limit, easily can configure electroconductive particle between the upper and lower electrode that should connect.Further, be difficult to via multiple electroconductive particle between the adjacent electrode that can not connect and be electrically connected.That is, adjacent interelectrode short circuit can further be prevented.
In above-mentioned electric conducting material, the content of above-mentioned electroconductive particle is preferably more than 0.1 relative to the ratio of the content of above-mentioned inorganic filler, is more preferably more than 1, is preferably less than 20, is more preferably less than 10.When above-mentioned ratio is below more than above-mentioned lower limit and the above-mentioned upper limit, can the moisture-proof of uniform solidification thing and interelectrode both contact resistances, can further become good.
(other composition)
Above-mentioned electric conducting material is preferably containing sensitizer.Benzophenone derivates shown in the preferred following formula of this sensitizer (11).Above-mentioned sensitizer has following effect: the polymerization initiation efficiency produced by above-mentioned cation propellant is improved further, and suitably promotes the curing reaction of electric conducting material.
[chemical formula 4]
In above-mentioned formula (11), R1 and R2 represents the substituting group that hydrogen atom, the substituting group shown in following formula (11a) or following formula (11b) represent respectively.Above-mentioned R1 can be identical with above-mentioned R2, also can be different.
[chemical formula 5]
[chemical formula 6]
In above-mentioned formula (11a) and above-mentioned formula (11b), R3 represent the alkoxyl of the alkyl of hydrogen atom, carbon number 1 ~ 20, carbon number 1 ~ 20, halogen atom, hydroxyl, carboxyl or, the alkyl-carboxylic acid ester group of carbon number 1 ~ 20.Abovementioned alkyl can be straight chain, also can be side chain.
As the benzophenone derivates shown in above-mentioned formula (11); can enumerate: benzophenone, 2; 4-dichloro benzophenone, o-benzoyl yl benzoic acid methyl esters, 4,4 '-bis-(dimethylamino) benzophenone and 4-benzoyl-4 '-methyldiphenyl sulfide etc.
The content of above-mentioned sensitizer is not particularly limited.Relative to above-mentioned curability compound 100 weight portion, the content of above-mentioned sensitizer, preferably more than 0.05 weight portion, is more preferably more than 0.1 weight portion, is preferably below 3 weight portions, is more preferably below 1 weight portion.When the content of above-mentioned sensitizer is more than above-mentioned lower limit, effect of enhanced sensitivity can be obtained fully.When the content of above-mentioned sensitizer is below the above-mentioned upper limit, light absorption becomes suitable, and light is easily passed to the deep of conductive material layer.
Preferred above-mentioned electric conducting material contains silane coupler.Above-mentioned silane coupler makes the cementability produced by the solidfied material of electric conducting material improve.
As above-mentioned silane coupler, can enumerate: gamma-amino propyl trimethoxy silicane, γ mercaptopropyitrimethoxy silane, γ-glycidoxypropyltrime,hoxysilane and γ-isocyanates propyl trimethoxy silicane etc.
The content of above-mentioned silane coupler is not particularly limited.Relative to above-mentioned curability compound 100 weight portion, the content of above-mentioned silane coupler is preferably more than 0.1 weight portion, is more preferably more than 0.5 weight portion, is preferably below 10 weight portions, is more preferably below 5 weight portions.When the content of above-mentioned silane coupler is more than above-mentioned lower limit, effectively can obtain the raising effect of cementability.When the content of above-mentioned silane coupler is below the above-mentioned upper limit, remaining silane coupler not easily oozes out.
Above-mentioned electric conducting material can contain cure retarder.By using above-mentioned cure retarder, the useful life of electric conducting material extends.
As above-mentioned cure retarder, be not particularly limited, can polyether compound etc. be enumerated.As above-mentioned polyether compound, be not particularly limited, can enumerate: polyethylene glycol, polypropylene glycol, tetramethylene glycol and crown compound etc.Wherein, preferred crown compound.
Above-mentioned crown compound is not particularly limited, and can enumerate: 12-crown-4,15-hat-5,18-hat-6,24-hat-8 and the compound etc. shown in following formula (12).
[chemical formula 7]
In above-mentioned formula (12), R1 ~ R12 represent respectively hydrogen atom or carbon number 1 ~ 20 replacement or without substituted alkyl.But, the alkyl of at least 1 expression carbon number 1 ~ 20 in R1 ~ R12.Above-mentioned replacement or the functional group of more than 1 that can be selected from without substituted alkyl in the alkyl-carboxylic acid ester group of the alkoxyl of carbon number 1 ~ 20, halogen atom, hydroxyl, carboxyl and carbon number 1 ~ 20 replace, and, adjacent Rn and Rn+1 (wherein, n represents the even number of 1 ~ 12) can form cyclic alkyl skeleton jointly.The alkoxyl of above-mentioned carbon number 1 ~ 20 can be straight chain, also can be side chain.
In compound shown in above-mentioned formula (12), preferably there is the compound of at least 1 cyclohexyl.Due to the existence of above-mentioned cyclohexyl, the skeleton of crown ether is stablized, and inhibition is improved.
As there is cyclohexyl and the compound represented by above-mentioned formula (12), specifically, the compound that following formula (12A) represents can be enumerated.
[chemical formula 8]
The compound that above-mentioned chemical formula (12A) represents becomes on the position of line symmetry at the line of the central authorities being preced with-6-ether molecule with respect to 18-and has 2 cyclohexyl.Therefore, the skeleton of 18-hat-6-ether molecule does not produce distortion etc., and carryover effects raises.
The content of above-mentioned cure retarder is not particularly limited.Relative to above-mentioned curability compound 100 weight portion, the content of above-mentioned cure retarder is preferably more than 0.05 weight portion, is more preferably more than 0.1 weight portion, is preferably below 5 weight portions, is more preferably below 3 weight portions.When the content of above-mentioned cure retarder is more than above-mentioned lower limit, carryover effects can be obtained fully.When the content of above-mentioned cure retarder is below the above-mentioned upper limit, not easily produce degassed when making electric conducting material solidify.
In order to improve the durability such as element electrode, above-mentioned electric conducting material can containing the compound or ion exchanger with the acid reaction produced in solidfied material.
As the above-mentioned compound of acid reaction with producing, the carbonate of material, such as alkali metal or the alkaline-earth metal neutralized with acid or bicarbonate etc. can be enumerated.As the concrete example of the compound of the above-mentioned acid reaction with producing, can enumerate: calcium carbonate, calcium bicarbonate, sodium carbonate, sodium acid carbonate etc.
As above-mentioned ion exchanger, any one in cation exchange, anion exchange and two ion-exchange types can be used.Particularly preferably can the cation exchange of adsorbing chlorinated thing ion or two ion-exchange types.
Above-mentioned electric conducting material can contain solvent.By the use of this solvent, the viscosity of electric conducting material easily can be adjusted.As above-mentioned solvent, can enumerate such as: ethyl acetate, methyl cellosolve, toluene, acetone, methyl ethyl ketone, cyclohexane, n-hexane, oxolane and Anaesthetie Ether etc.
Above-mentioned electric conducting material can contain the known various additives such as reinforcing agent, softening agent, plasticizer, ultra-violet absorber and antioxidant as required.
(other details of electric conducting material)
The method manufacturing above-mentioned electric conducting material is not particularly limited, and can enumerate the method such as using the mixers such as homogenous disperse device, homogeneous mixer, universal mixer, planetary-type mixer, kneader, 3 rollers, mix curability composition, electroconductive particle and other composition as required.
Preferred above-mentioned electric conducting material is anisotropic conductive material.Preferred above-mentioned electric conducting material is the electric conducting material for being electrically connected electrode.Above-mentioned electric conducting material is pulpous state or membranaceous electric conducting material, the electric conducting material of preferred pulpous state.The electric conducting material of pulpous state is electrocondution slurry.Membranaceous electric conducting material is conducting film.When electric conducting material is conducting film, lamination can carried out containing on the conducting film of this electroconductive particle to the film not containing electroconductive particle.
From the view point of the heat deterioration suppressing connecting object parts, electric conducting material of the present invention is preferably heated to the temperature of less than 120 DEG C but not the temperature more than 120 DEG C makes it solidify rear use, and is preferably heated the temperature of less than 100 DEG C but not the temperature more than 100 DEG C makes it solidify rear use.In organic electroluminescent device substrate, when being heated to the temperature more than 120 DEG C, heat deterioration sometimes quite becomes problem.
From the view point of further improve electric conducting material storage stability, further improve interelectrode conducting reliability, the pH of above-mentioned electric conducting material at 25 DEG C is preferably more than 4, be more preferably more than 5, more preferably more than 6, be preferably less than 10, be more preferably less than 9, more preferably less than 8.
Electric conducting material of the present invention is electrocondution slurry, preferably coats the electrocondution slurry on connecting object parts with the state of pulpous state.
The viscosity of above-mentioned electrocondution slurry at 25 DEG C is preferably more than 20Pas, is more preferably more than 100Pas, is preferably below 700Pas, is more preferably below 300Pas.When above-mentioned viscosity is more than above-mentioned lower limit, the precipitation of the electroconductive particle in electrocondution slurry can be suppressed.When above-mentioned viscosity is below the above-mentioned upper limit, the dispersiveness of electroconductive particle is further improved.If the above-mentioned viscosity of the above-mentioned electrocondution slurry before coating is in above-mentioned scope, then after applying conductive slurry, further can suppresses the flowing of the electrocondution slurry before solidifying, and then more not easily produce space on the connecting object parts of the 1st.It should be noted that, also comprise liquid in pulpous state.
In addition, electric conducting material of the present invention is preferred for the electrical connection of the electrode in organic EL display element.Electric conducting material of the present invention is more preferably for the interelectrode electrical connection of organic EL display element substrate.As above-mentioned organic EL display element substrate, the organic EL substrate and hermetic sealing substrate etc. that possess organic EL element can be enumerated.Above-mentioned hermetic sealing substrate is the substrate for sealing organic el element.Electric conducting material of the present invention is more preferably for the electrical connection of the organic electrode of EL substrate and the electrode of hermetic sealing substrate that possess organic EL element.
Electric conducting material of the present invention can use in order to bonding various connecting object parts.Above-mentioned electric conducting material be in order to obtain making the 1st connecting object parts, the 2nd connecting object parts electrical connection connection structural bodies and preferably use.Above-mentioned electric conducting material is to obtain the connection structural bodies that makes to be electrically connected between the electrode of the 1st connecting object parts, the 2nd connecting object parts and more preferably using.
In Fig. 1, schematically show an example of the connection structural bodies using the electric conducting material having an embodiment of the invention to relate to by front cross-sectional view.
Connection structural bodies 1 shown in Fig. 1 possesses: the 1st connecting object parts 2, the 2nd connecting object parts 4, the connecting portion 3 that the 1st connecting object parts 2 are electrically connected with the 2nd connecting object parts 4.Connecting portion 3 is solidification nitride layer, is by making the electric conducting material containing electroconductive particle 11 be solidified to form.
1st connecting object parts 2 surface (above) on there is multiple 1st electrode 2a.2nd connecting object parts 4 surface (below) on there is multiple 2nd electrode 4a.1st electrode 2a and the 2nd electrode 4a is electrically connected by one or more electroconductive particles 11.Therefore, the 1st connecting object parts 2 are electrically connected by electroconductive particle 11 with the 2nd connecting object parts 4.
Connection between the 1st electrode 2a and the 2nd electrode 4a usually make the 1st connecting object parts 2 and the 2nd connecting object parts 4 across electric conducting material superimposed make the 1st electrode 2a and the 2nd electrode 4a opposite each other after, undertaken by pressurization when making electric conducting material solidify.By pressurization, generally speaking, electroconductive particle 11 is compressed.
1st connecting object parts, the 2nd connecting object parts are not particularly limited.As the 1st connecting object parts, the 2nd connecting object parts, specifically, can enumerate: the electronic units etc. such as circuit substrate such as the electronic units such as semiconductor chip, capacitor and diode and printed base plate, flexible printing substrate, glass epoxy substrate and glass substrate.Above-mentioned electric conducting material is preferably the electric conducting material for the connection of electronic unit.
The manufacture method of connection structural bodies of the present invention preferably includes following operation: the operation being configured conductive material layer on the surface of above-mentioned 1st connecting object parts by above-mentioned electric conducting material; In the operation of the above-mentioned 2nd connecting object parts of surface configuration of the above-mentioned 1st connecting object component side opposition side with above-mentioned conductive material layer; Make above-mentioned conductive material layer hot curing, form the operation of connecting portion making the 1st connecting object parts, the 2nd connecting object parts electrical connection.Now, above-mentioned connecting portion is heated to the temperature of less than 120 DEG C but not the temperature more than 120 DEG C, and above-mentioned conductive material layer is solidified to form.Above-mentioned conductive material layer is more preferably heated to the temperature of less than 100 DEG C but not the temperature more than 100 DEG C make its hot curing.
In addition, the connection structural bodies 1 shown in Fig. 1 such as can obtain through the state shown in Fig. 2 (a) ~ (c) as follows.
As shown in Fig. 2 (a), prepare surface (above) on there are the 1st connecting object parts 2 of the 1st electrode 2a.Then, on the surface of the 1st connecting object parts 2, the electric conducting material of configuration containing multiple electroconductive particle 11, the surface of the 1st connecting object parts 2 forms conductive material layer 3A.Now, preferably on the 1st electrode 2a, one or more electroconductive particles 11 are configured.
Then, by irradiating light to conductive material layer 3A, the solidification of conductive material layer 3A is carried out.In Fig. 2 (a) ~ (c), light is irradiated to conductive material layer 3A, the solidification of conductive material layer 3A is carried out, B-stage is carried out to conductive material layer 3A.That is, as shown in Fig. 2 (b), the conductive material layer 3B of B-stage is formed on the surface of the 1st connecting object parts 2.By carrying out B-stage, the 1st connecting object parts 2 and the conductive material layer 3B temporary bond having carried out B-stage.The conductive material layer 3B having carried out B-stage is the semi-solid preparation thing being in semi-cured state.The conductive material layer 3B having carried out B-stage does not solidify completely, can carry out hot curing further.But, also can irradiate light to conductive material layer 3A or conductive material layer 3A be heated, and B-stage not carried out to conductive material layer 3A, make conductive material layer 3A disposal solidifying.Preferably conductive material layer 3A is heated, make conductive material layer 3A hot curing.
In order to effectively carry out the solidification of conductive material layer 3A, photo-irradiation intensity when preferably irradiating light is 0.1 ~ 8000mW/cm
2scope in.Accumulative light quantity is preferably 0.1 ~ 20000J/cm
2.The light source used when irradiating light is not particularly limited.As this light source, can enumerate such as to have at below wavelength 420nm and fully send out light source etc. photodistributed.In addition, as the concrete example of light source, can enumerate such as: Cooper-Hewitt lamp, middle medium pressure mercury lamp, high-pressure mercury-vapor lamp, extra-high-pressure mercury vapour lamp, chemical lamp, backlight, microwave-excitation mercury vapor lamp, metal halide lamp and LED etc.
Then, as shown in Fig. 2 (c), on the surface contrary with the 1st connecting object parts 2 side of the conductive material layer 3B having carried out B-stage, lamination is carried out to the 2nd connecting object parts 4.Connecting object parts 4 to the 2nd carry out lamination, make the 2nd electrode 4a on the 1st electrode 2a on the 1st connecting object parts 2 surface and the 2nd connecting object parts 4 surface opposed.
Further, when carrying out the lamination of the 2nd connecting object parts 4, by heating the conductive material layer 3B having carried out B-stage, the conductive material layer 3B having carried out B-stage being solidified further, forming connecting portion 3.But, before the lamination carrying out the 2nd connecting object parts 4, can the conductive material layer 3B having carried out B-stage be heated.Further, after the lamination having carried out the 2nd connecting object parts 4, the conductive material layer 3B of B-stage can be heated.
By heating make conductive material layer 3A or carried out B-stage conductive material layer 3B solidify time heating-up temperature be preferably more than 50 DEG C, be more preferably more than 80 DEG C, be further preferably more than 100 DEG C, less than 120 DEG C, be more preferably less than 110 DEG C.When electric conducting material of the present invention is used for the electrical connection of electrode in organic EL display element, the heating-up temperature when conductive material layer 3B making above-mentioned conductive material layer 3A or carried out B-stage solidifies is less than 120 DEG C, is more preferably less than 100 DEG C.
Preferably pressurize when making the conductive material layer 3B having carried out B-stage solidify.By pressurization, utilize the 1st electrode 2a and the 2nd electrode 4a compression conductive particle 11, the contact area of the 1st electrode 2a, the 2nd electrode 4a and electroconductive particle 11 can be increased thus.Therefore, conducting reliability can be improved.Further, by compression conductive particle 11, even if the distance of the 1st electrode 2a and the 2nd electrode 4a expands, the particle diameter of electroconductive particle 11 also increases to follow this expansion.
By making the conductive material layer 3B having carried out B-stage solidify, the 1st connecting object parts 2 are connected across connecting portion 3 with the 2nd connecting object parts 4.In addition, the 1st electrode 2a is electrically connected via electroconductive particle 11 with the 2nd electrode 4a.As mentioned above, the connection structural bodies 1 that the use shown in Fig. 1 has electric conducting material can be obtained.At this, combinationally use photocuring and hot curing, therefore, can electric conducting material be made at short notice to solidify.
Electric conducting material of the present invention may be used for the connection (FOG (Film on Glass)) of such as flexible printing substrate and glass substrate, the connection (COF (Chip onFilm)) of semiconductor chip and flexible printing substrate, semiconductor chip and the connection (COG (Chip on Glass)) of glass substrate or the connection (FOB (Film on Board)) etc. of flexible printing substrate and glass epoxy substrate.Wherein, above-mentioned electric conducting material is suitable for FOG purposes or COG purposes, in COG purposes more preferably.Electric conducting material of the present invention preferably for the electric conducting material of flexible printing substrate and the connection of glass substrate or the connection of semiconductor chip and glass substrate, more preferably for the electric conducting material of the connection of flexible printing substrate and glass substrate.
In connection structural bodies of the present invention, above-mentioned 2nd connecting object parts and above-mentioned 1st connecting object parts are preferably flexible printing substrate and glass substrate, or semiconductor chip and glass substrate, are more preferably flexible printing substrate and glass substrate.
In addition, connection structural bodies of the present invention is preferably organic EL display element.Electrode in above-mentioned organic EL display element can be electrically connected by electroconductive particle contained in above-mentioned electric conducting material.
In addition, above-mentioned 1st connecting object parts, the 2nd connecting object parts are preferably organic EL display element substrate respectively.Above-mentioned 1st connecting object parts, the 2nd connecting object parts are preferably the 1st substrate, the 2nd substrate as organic EL display element substrate.Above-mentioned 1st connecting object parts and above-mentioned 2nd connecting object parts preferably possess organic EL substrate and the hermetic sealing substrate of organic EL element.Now, above-mentioned 1st connecting object parts are above-mentioned organic EL substrate, and above-mentioned 2nd connecting object parts can be above-mentioned hermetic sealing substrate, above-mentioned 1st connecting object parts are above-mentioned hermetic sealing substrate, and above-mentioned 2nd connecting object parts can be above-mentioned organic EL substrate.Above-mentioned connection structural bodies is preferably organic EL display element.
Electrode width (the 1st electrode width and the 2nd electrode width) is preferably more than 5 μm, is more preferably more than 10 μm, is preferably less than 500 μm, is more preferably less than 300 μm.Width between electrode (between the 1st electrode between width and the 2nd electrode width) is preferably more than 3 μm, is more preferably more than 10 μm, is preferably less than 500 μm, is more preferably less than 300 μm.In addition, the L/S (line/interval) as width between electrode width/electrode is preferably 5 μm/more than 5 μm, is more preferably 10 μm/more than 10 μm, is preferably 500 μm/less than 500 μm, is more preferably 300 μm/less than 300 μm.
Below, enumerate embodiment and comparative example, the present invention is described particularly.The present invention is not limited to following embodiment.
(embodiment 1)
(1) preparation of electric conducting material:
At bisphenol A modified epoxy resin (DIC Inc. " EPICLON EXA-4850-150 ") 40 weight portions, SI-60L (Sanaid of three new chemical companies) 3 weight portions as cation propellant are added in bisphenol F epoxy resin (DIC Inc. " EXA-835LV ") 40 weight portions and phenol novolacs (Mitsubishi Chemical Ind's system " 1032H60 ") 20 weight portions, as silicon dioxide (East Asia Synesis Company system " HPS-0500 " of the average grain diameter 0.5 μm of inorganic filler, surplus is than 1.2) 10 weight portions, electroconductive particle A (the 20%K value at 100 DEG C: 1400N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 15%) 4 weight portions, use planetary stirring machine to stir 5 minutes with 2000rPm, obtain electrocondution slurry thus.
It should be noted that, the electroconductive particle A used and electroconductive particle B described later, electroconductive particle C, electroconductive particle D, electroconductive particle E, electroconductive particle F, electroconductive particle G, electroconductive particle I, electroconductive particle L, electroconductive particle W, electroconductive particle X, electroconductive particle Y, electroconductive particle Z are to have and form nickel plating layer on the surfaces of divinylbenzene resin particle, and on the surface of this nickel plating layer the electroconductive particle of the conductive layer that golden plating layer is formed.In addition, the electroconductive particle H of use has on the surface of resin particle, to form nickel plating layer and the electroconductive particle forming the conductive layer of palladium plating layer on the surface of this nickel plating layer.Electroconductive particle J is the electroconductive particle only forming nickel plating layer on the surface of resin particle.Electroconductive particle K forms nickel plating layer and on the surface of this nickel plating layer, forms palladium plating layer, the further electroconductive particle of the bossed projection of tool on the outer surface of above-mentioned conductive layer on the surface of resin particle.20%K value and compression recovery are undertaken changing by the composition of p-divinyl benzene resin particle and the thickness of conductive layer and are adjusted.
(2) making of organic EL display element:
That prepare to possess organic EL element and be formed with organic EL substrate (the 1st substrate, the 1st connecting object parts) that L/S is 500 μm/500 μm, length is the Mo/Al/Mo electrode pattern of 20mm above.In addition, prepare to be formed with the hermetic sealing substrate (the 2nd substrate, the 2nd connecting object parts) that L/S is 500 μm/500 μm, length is the Mo/Al/Mo electrode pattern of 20mm below.
Use disperser to become width 2mm the electrocondution slurry just made, the mode of thickness 50 μm is coated on above-mentioned 1st substrate, form the conductive paste bed of material.Then, the conductive paste bed of material make electrode opposite each other above-mentioned 2nd substrate joining.Use laminating apparatus, this laminated body is applied to the pressure of 0.3MPa, at 100 DEG C, make the conductive paste bed of material solidify 30 minutes, obtain organic EL display element.
(embodiment 2)
The heating-up temperature of the conductive paste bed of material is changed to 120 DEG C by 100 DEG C, in addition, operates similarly to Example 1, obtain organic EL display element.
(embodiment 3)
Electroconductive particle A is changed to electroconductive particle B (the 20%K value at 100 DEG C: 520N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 10%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 4)
Electroconductive particle A is changed to electroconductive particle C (the 20%K value at 100 DEG C: 1980N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 18%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 5)
Electroconductive particle A is changed to electroconductive particle D (the 20%K value at 100 DEG C: 1100N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 3%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 6)
Electroconductive particle A is changed to electroconductive particle E (the 20%K value at 100 DEG C: 1700N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 30%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 7)
Inorganic filler is changed to the talcum (Japanese talc Inc. " D-800 ", average surplus are than 2) of average grain diameter 0.8 μm, in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 8)
Bisphenol F epoxy resin (DIC Inc. " EXA-835LV ") is changed to bis-phenol E (printec Inc. " EPOX-MKR1710 "), in addition, operates similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 9)
SI-60L (Sanaid of three new chemical companies) is changed to the CXC-1612 (the K-PURE CXC of K-PURE Inc.) as cation propellant, in addition, operates similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 10)
Mismatch the SI-60L as cation propellant, and coordinate thermal curing agents (imidazolium compounds, four countries change into industrial group's system " 2P-4MZ ") 15 weight portions, in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 11)
Except mismatching inorganic filler, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 12)
SI-60L (Sanaid of three new chemical companies) is changed to the CPI-210S (san-apro Inc.) as cation propellant, in addition, operates similarly to Example 1, obtain electrocondution slurry.
Prepare the 1st substrate, the 2nd substrate similarly to Example 1.Use disperser to be coated on by electrocondution slurry on above-mentioned 1st substrate, after forming the conductive paste bed of material, become 3000mW/cm with photo-irradiation intensity
2mode irradiate the ultraviolet 3 seconds of 365nm, make conductive paste bed of material semi-solid preparation by photopolymerization, carry out B-stage.Then, the conductive paste bed of material make electrode opposite each other above-mentioned 2nd substrate joining.Use laminating apparatus, this laminated body is applied to the pressure of 0.3MPa, at 100 DEG C, make the conductive paste bed of material solidify 30 minutes, obtain organic EL display element.
(embodiment 13)
Electroconductive particle A is changed to electroconductive particle F (the 20%K value at 100 DEG C: 580N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 5%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 14)
Electroconductive particle A is changed to electroconductive particle G (the 20%K value at 100 DEG C: 1680N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 25%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 15)
Electroconductive particle A is changed to electroconductive particle H (the 20%K value at 100 DEG C: 1520N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 15%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 16)
Electroconductive particle A is changed to electroconductive particle J (the 20%K value at 100 DEG C: 1480N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 15%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 17)
Electroconductive particle A is changed to electroconductive particle K (the 20%K value at 100 DEG C: 1580N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 15%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 18)
Electroconductive particle A is changed to electroconductive particle L (the 20%K value at 100 DEG C: 1380N/mm of average grain diameter 20 μm
2, compression recovery at 100 DEG C: 13%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(embodiment 19)
(1) making of conducting film:
Add phenoxy resin (Phenoxy Associatese Inc. " PKHH ") 30 weight portions, naphthalene type epoxy resin (DIC Inc. " HP4032D ") 20 weight portions, liquid epoxy resin (Mitsubishi Chemical Ind's system " EP-828 ") 20 weight portions, as imidazole curing agent (E-Materials Inc. of Asahi Chemical Industry " NOVACURE3941HP ") 30 weight portions of curing agent, silane coupler (eastern beautiful DOW CORNING silicone Inc. " SH6040 ") 1 weight portion, silicon dioxide (East Asia Synesis Company system " HPS-0500 " that average grain diameter is 0.5 μm, surplus is than 1.2) the electroconductive particle A4 weight portion of 10 weight portions and average grain diameter 30 μm, adding toluene makes solid be divided into 50 % by weight, obtain resin combination.
The resin combination obtained being coated in one side has carried out in the PET film of thickness 50 μm of demoulding process, by the heated-air drying 5 minutes of 80 DEG C, and making conducting film.The thickness of the conducting film obtained is 50 μm.The conducting film obtained is cut into the size of width 2mm.
(2) making of organic EL display element:
With disperser, electrocondution slurry is coated on above-mentioned 1st substrate, and the technique forming the conductive paste bed of material is changed to attaching conducting film and forms the technique of conductive film layer, in addition, operate similarly to Example 1, obtain organic EL display element.
(comparative example 1)
Electroconductive particle A is changed to electroconductive particle W (the 20%K value at 100 DEG C: 350N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 5%), in addition, operate similarly to Example 1, obtain organic EL display element.
(comparative example 2)
Electroconductive particle A is changed to electroconductive particle X (the 20%K value at 100 DEG C: 3670N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 95%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(comparative example 3)
Electroconductive particle A is changed to electroconductive particle Y (the 20%K value at 100 DEG C: 600N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 1.5%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(comparative example 4)
Electroconductive particle A is changed to electroconductive particle Z (the 20%K value at 100 DEG C: 1800N/mm of average grain diameter 30 μm
2, compression recovery at 100 DEG C: 40%), in addition, operate similarly to Example 1, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 1, obtain organic EL display element.
(evaluation of embodiment 1 ~ 19 and comparative example 1 ~ 4)
(1) modulus of elasticity in comperssion (20%K value) at 100 DEG C of electroconductive particle
Micro-compression tester (FISCHER Inc. " FISCHERSCOPE H-100 ") is used to measure the modulus of elasticity in comperssion (20%K value) at 100 DEG C of the electroconductive particle used.
(2) compression recovery at 100 DEG C of electroconductive particle
Compression recovery when using micro-compression tester (FISCHER Inc. " FISCHERSCOPE H-100 ") to carry out 30% compression to the electroconductive particle used at 100 DEG C measures.
(3) presence or absence in space
In the organic EL display element obtained, observe and whether produce space at the connecting portion of conductive material layer solidification.The presence or absence in space is judged according to following benchmark.
[having void-free determinating reference]
Zero: there is no space
△: although there is space, not large than width between electrode width and electrode space
×: there is the space larger than width between electrode width or electrode
(4) moisture-proof
To become the mode of thickness 100 μm, by baker formula (ベ ー カ ー formula) electrocondution slurry obtained is coated on temperature-constant plate by applicator (manufacture of tester industry companies).Thereafter, with regard to embodiment 1 ~ 11,13 ~ 18 and comparative example 1 ~ 4, heat 30 minutes at 100 DEG C, with regard to embodiment 12, become 3000mW/cm with photo-irradiation intensity
2mode irradiate the ultraviolet of 365nm after 3 seconds, at 100 DEG C heat 30 minutes, obtain film.With regard to embodiment 19, lamination is carried out to 2 conducting films and makes total thickness become 100 μm, after being configured on temperature-constant plate, heating 30 minutes at 100 DEG C, obtain film.According to JIS Z0208,60 DEG C, expose 24 hours under the condition of 90%RH, the moisture permeability of the film obtained is measured.
It should be noted that, above-mentioned moisture permeability, as JIS Z0208, is generally and carries out method for measuring in moisture vapor transmission cup, but the PERMATRANW3/33 of Mocon Inc. of the U.S. also can be used to measure.
By the measured value of moisture permeability, judge moisture-proof according to following benchmark.
[determinating reference of moisture-proof]
00: moisture permeability is 25g/m
2below
Zero: moisture permeability is more than 25g/m
2, and be 50g/m
2below
△: moisture permeability is more than 50g/m
2, and be 100g/m
2below
×: moisture permeability is more than 100g/m
2
(5) contact resistance (conducting reliability)
4 terminal methods are utilized to measure the upper and lower interelectrode contact resistance of the organic EL display element obtained respectively.Calculate the mean value of the contact resistance at 100 places.It should be noted that, can by the relation of voltage=electric current × resistance, by measuring voltage when making certain current flowing and obtaining contact resistance.According to following benchmark, the interelectrode contact resistance in the organic EL display element obtained is judged.
[determinating reference of contact resistance]
00: lower than 3 Ω
Zero: 3 more than Ω and lower than 4 Ω
△: 4 more than Ω and lower than 5 Ω
△ △: 5 more than Ω and lower than 10 Ω
×: 10 more than Ω
(6) connection reliability
By the organic EL display element that obtains 85 DEG C, place 500 hours under the condition of 85%RH after, utilize 4 terminal methods to measure upper and lower interelectrode contact resistance respectively.Calculate the mean value of the contact resistance at 100 places.By the interelectrode contact resistance of transferring in hot and humid condition in the organic EL display element of postpone, according to following benchmark, connection reliability is judged.
[determinating reference of connection reliability]
00: lower than 3 Ω
Zero: lower than 5 Ω
△: 5 more than Ω and lower than 10 Ω
×: 10 more than Ω
Show the result in following table 1.
[table 1]
(embodiment 20)
(1) preparation of electric conducting material:
At bisphenol A modified epoxy resin (DIC Inc. " EPICLON EXA-4850-150 ") 40 weight portions, and SI-60L (Sanaid of three new chemical companies) 3 weight portions added in bisphenol F epoxy resin (DIC Inc. " EXA-835LV ") 30 weight portions as cation propellant, as epoxy acrylate (Daicel Allnex Inc. " EBECRYL3702 ") 20 weight portions of photocurable compound, as acylphosphine oxide compounds (ciba Japan Inc. " DAROCUR TPO ") 1 weight portion of trigger for optical solidification, as silica 10 weight portion of the average grain diameter 0.25 μm of filler and the electroconductive particle A (electroconductive particle used in embodiment 1 of average grain diameter 30 μm, 20%K value at 100 DEG C: 1400N/mm
2, compression recovery at 100 DEG C: 15%) 4 weight portions, use planetary stirring machine to stir 5 minutes with 2000rPm, obtain electrocondution slurry thus.
(2) making of organic EL display element:
Prepare possess organic EL element, be formed with above organic EL substrate (the 1st substrate, the 1st connecting object parts) that L/S is 500 μm/500 μm, length is the Mo/Al/Mo electrode pattern of 20mm.In addition, prepare to be formed with the hermetic sealing substrate (the 2nd substrate, the 2nd connecting object parts) that L/S is 500 μm/500 μm, length is the Mo/Al/Mo electrode pattern of 20mm below.
Use disperser by the electrocondution slurry just made to become width 2mm, the mode of thickness 50 μm is coated on above-mentioned 1st substrate, forms the conductive paste bed of material.Then, the conductive paste bed of material make electrode opposite each other above-mentioned 2nd substrate joining.3000mW/cm is become with photo-irradiation intensity
2mode irradiate the ultraviolet 3 seconds of 365nm, make conductive paste bed of material semi-solid preparation by photopolymerization, carry out B-stage.Use laminating apparatus, this laminated body is applied to the pressure of 0.3MPa, at 100 DEG C, make the conductive paste bed of material solidify 30 minutes, obtain organic EL display element.
(embodiment 21)
The heating-up temperature of the conductive paste bed of material is changed to 120 DEG C by 100 DEG C, in addition, operates similarly to Example 20, obtain organic EL display element.
(embodiment 22)
Before above-mentioned 2nd substrate of lamination, carry out illumination penetrate, above-mentioned 2nd substrate of lamination rapidly after illumination is penetrated, in addition, operates similarly to Example 20, obtains organic EL display element.
(embodiment 23)
The kind of Thermocurable compound is changed to phenol novolak type epoxy resin (DIC Inc. " EPICLONN-770 ") by bisphenol A modified epoxy resin (DIC Inc. " EPICLONEXA-4850-150 "), in addition, operate similarly to Example 20, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 20, obtain organic EL display element.
(embodiment 24)
The kind of cation propellant is changed to CXC-1612 (the K-Pure CXC of K-Pure Inc.) by SI-60L (Sanaid of three new chemical companies), in addition, operates similarly to Example 20, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 20, obtain organic EL display element.
(embodiment 25)
Do not add the SI-60L as cation propellant and add thermal curing agents (imidazolium compounds, four countries change into industrial group's system " 2P-4MZ ") 15 weight portions, in addition, operating similarly to Example 20, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 20, obtain organic EL display element.
(embodiment 26)
Electroconductive particle A is changed to electroconductive particle I (the 20%K value at 100 DEG C: 1400N/mm of average grain diameter 60 μm
2, compression recovery at 100 DEG C: 15%), in addition, operate similarly to Example 20, obtain electrocondution slurry.In addition, the electrode of above-mentioned 1st substrate is changed to L/S is 500 μm/500 μm, the Mo/Al/Mo electrode pattern of length 20mm, the electrode of hermetic sealing substrate (the 2nd substrate) is changed to L/S is 500 μm/500 μm, the ITO electrode pattern of length 20mm, use disperser by the electrocondution slurry just made to become width 1.5mm, the mode of thickness 120 μm is coated on above-mentioned 1st substrate, in addition, operate similarly to Example 20, obtain organic EL display element.
(embodiment 20 ~ 26 evaluation)
In embodiment 20 ~ 26, to assessment item (1) ~ (6) of embodiment 1 ~ 19 and comparative example 1 ~ 4, operate in the same manner as embodiment 1 ~ 19 and comparative example 1 ~ 4, implementation evaluation.
It should be noted that, in the evaluation of above-mentioned (4) moisture-proof, with baker formula applicator (manufacture of tester industry companies), the electrocondution slurry obtained is coated on temperature-constant plate in the mode becoming thickness 100 μm.Thereafter, 3000mW/cm is become with photo-irradiation intensity
2mode irradiate the ultraviolet of 365nm after 3 seconds, at 100 DEG C heat 30 minutes, obtain film.According to JISZ 0208,60 DEG C, expose 24 hours under the condition of 90%RH, the moisture permeability of the film obtained is measured.
Show the result in following table 2.
[table 2]
(embodiment 27)
(1) preparation of electric conducting material:
At bisphenol A modified epoxy resin (DIC Inc. " EPICLON EXA-4850-150 ") 40 weight portions, and SI-60L (Sanaid of three new chemical companies) 3 weight portions added in bisphenol F epoxy resin (DIC Inc. " EXA-835LV ") 30 weight portions as cation propellant, as epoxy acrylate (Daicel Allnex Inc. " EBECRYL3702 ") 20 weight portions of photocurable compound, as acylphosphine oxide compounds (ciba Japan Inc. " DAROCUR TPO ") 1 weight portion of trigger for optical solidification, as silica 10 weight portion of the average grain diameter 0.25 μm of filler, electroconductive particle A (the electroconductive particle used in embodiment 1 of benzylamine 0.05 weight portion and average grain diameter 30 μm, 20%K value at 100 DEG C: 1400N/mm
2, compression recovery at 100 DEG C: 15%) 4 weight portions, use planetary stirring machine, stir 5 minutes, obtain electrocondution slurry thus with 2000rPm.
(2) making of organic EL display element:
Prepare possess organic EL element, be formed with above organic EL substrate (the 1st substrate, the 1st connecting object parts) that L/S is 500 μm/500 μm, length is the Mo/Al/Mo electrode pattern of 20mm.In addition, prepare to be formed with the hermetic sealing substrate (the 2nd substrate, the 2nd connecting object parts) that L/S is 500 μm/500 μm, length is the Mo/Al/Mo electrode pattern of 20mm below.
Use disperser by the electrocondution slurry just made to become width 2mm, the mode of thickness 50 μm is coated on above-mentioned 1st substrate, forms the conductive paste bed of material.Then, on the conductive paste bed of material, make electrode opposite each other above-mentioned 2nd substrate joining.3000mW/cm is become with photo-irradiation intensity
2mode irradiate the ultraviolet 3 seconds of 365nm, make conductive paste bed of material semi-solid preparation by photopolymerization, carry out B-stage.Use this laminated body, and use laminating apparatus, apply the pressure of 0.3MPa, at 100 DEG C, make the conductive paste bed of material solidify 30 minutes, obtain organic EL display element (connection structural bodies X).
In addition, electrocondution slurry is placed 72 hours in shading plastic containers at 30 DEG C.Except the electrocondution slurry just made, be used at 30 DEG C and placed the electrocondution slurry after 72 hours, in addition, operate in the same manner as connection structural bodies X, obtain organic EL display element (connection structural bodies Y).
(embodiment 28)
The addition of benzylamine is changed to 0.09 weight portion by 0.05 weight portion, in addition, operates similarly to Example 27, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 27, obtain connection structural bodies X, Y.
(embodiment 29)
The addition of benzylamine is changed to 0.003 weight portion by 0.05 weight portion, in addition, operates similarly to Example 27, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 27, obtain connection structural bodies X, Y.
(embodiment 30)
The kind of above-mentioned amines is changed to α by benzylamine, alpha-alpha-dimethyl benzylamine, in addition, operate similarly to Example 27, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 27, obtain connection structural bodies X, Y.
(embodiment 31)
The kind of Thermocurable compound is changed to bis-phenol E (printec Inc. " EPOX-MK R1710 ") by bisphenol F epoxy resin (DIC Inc. " EXA-835LV "), in addition, operate similarly to Example 27, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 27, obtain connection structural bodies X, Y.
(embodiment 32)
The kind of cation propellant is changed to CXC-1612 (the K-PURE CXC of K-PURE Inc.) by SI-60L (Sanaid of three new chemical companies), in addition, operates similarly to Example 27, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 27, obtain connection structural bodies X, Y.
(embodiment 33)
Except not adding except benzylamine, operating similarly to Example 27, obtaining electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 27, obtain connection structural bodies X, Y.
(embodiment 34)
The kind of above-mentioned amines is changed to N-methylbenzylamine (having the secondary amine of aromatic ring) by benzylamine, in addition, operates similarly to Example 27, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 27, obtain connection structural bodies X, Y.
(embodiment 35)
The kind of above-mentioned amines is changed to n-hexyl amine (having the primary amine of aliphat skeleton) by above-mentioned benzylamine, in addition, operates similarly to Example 27, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 27, obtain connection structural bodies X, Y.
(embodiment 36)
Do not add the SI-60L as cation propellant and add thermal curing agents (imidazolium compounds, four countries change into industrial group's system " 2P-4MZ ") 15 weight portions, in addition, operating similarly to Example 27, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 27, obtain connection structural bodies X, Y.
(embodiment 37)
Do not add the SI-60L as cation propellant and add thermal curing agents (imidazolium compounds, four countries change into industrial group's system " 2P-4MZ ") 15 weight portions, and do not add benzylamine, in addition, operate similarly to Example 27, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate similarly to Example 27, obtain connection structural bodies X, Y.
(evaluation of embodiment 27 ~ 37)
In embodiment 27 ~ 37, to assessment item (1) ~ (6) of embodiment 1 ~ 19 and comparative example 1 ~ 4, operate in the same manner as embodiment 1 ~ 19 and comparative example 1 ~ 4, implementation evaluation.And then, in embodiment 27 ~ 37, to following assessment item (7) ~ (9), also implementation evaluation.
It should be noted that, in the evaluation of above-mentioned (4) moisture-proof, make its thickness become 100 μm by the electrocondution slurry baker formula applicator obtained (manufacture of tester industry companies) coating temperature-constant plate.Then, 3000mW/cm is become with photo-irradiation intensity
2mode irradiate the ultraviolet of 365nm after 3 seconds, at 100 DEG C heat 30 minutes, obtain film.According to JIS Z0208,60 DEG C, expose 24 hours under the condition of 90%RH, measure the moisture permeability of the film obtained.
(7) pH of electric conducting material
Measure the pH of electrocondution slurry at 25 DEG C just made.PH is judged according to following benchmark.
[determinating reference of pH]
A:pH is more than 6 and is less than 8
B:pH is more than 4 and lower than 6 or more than 8 and less than 10
C:pH is lower than 4 or more than 10
(8) storage stability (curability)
Prepare the electrocondution slurry just made, electrocondution slurry is placed 72 hours in shading plastic containers at 30 DEG C.After making making, the electrocondution slurry of (before placement) and the electrocondution slurry after placing utilize oven for solidifying 1 hour at 100 DEG C, obtain solidfied material (diameter 10mm, thickness 1mm).
Utilize sclerometer (D type), according to following benchmark, judged the curability of electrocondution slurry by the hardness D2 of the hardness D1 of solidfied material of electrocondution slurry and the solidfied material of the electrocondution slurry after placing that just make (before placement).
[determinating reference of storage stability (curability)]
Zero: hardness D2 and the ratio of hardness D1 be more than 0.9
△: hardness D2 and the ratio of hardness D1 be more than 0.8 and lower than 0.9
△ △: hardness D2 and the ratio of hardness D1 be more than 0.6 and lower than 0.8
×: the ratio of hardness D2 and hardness D1 is lower than 0.6
(9) storage stability (viscosity)
Prepare the electrocondution slurry just made, electrocondution slurry is placed 72 hours at 30 DEG C.Judge according to the storage stability of following benchmark by viscosities il 2 pairs of electrocondution slurries of the viscosities il 1 of electrocondution slurry and the electrocondution slurry after placing that just make (before placement).It should be noted that, above-mentioned viscosities il 1 and η 2 are the value using E type viscosimeter (TOKI SANGYO CO.LTD Inc. " VISCOMETERTV-22 ", cone rotor: No.7), measure gained under the condition of 2.5rPm and 25 DEG C.
[determinating reference of storage stability (viscosity)]
00: the ratio of viscosities il 2 and viscosities il 1 is lower than 1.2
Zero: viscosities il 2 and the ratio of viscosities il 1 are more than 1.2 and lower than 1.4
△: viscosities il 2 and the ratio of viscosities il 1 are more than 1.4 and lower than 1.6
△ △: viscosities il 2 and the ratio of viscosities il 1 are more than 1.6 and lower than 2.0
×: viscosities il 2 is more than 2.0 with the ratio of viscosities il 1
Show the result in following table 3.
[table 3]
(embodiment 38)
(1) preparation of electric conducting material:
Multifunctional type epoxy resin (Mitsubishi Chemical Ind's system " 1032H60 ") 50 weight portions of solid at 23 DEG C, and SI-60L (Sanaid of three new chemical companies) 3 weight portions added in liquid bisphenol F epoxy resin (DIC Inc. " EXA-835LV ") 50 weight portions at 23 DEG C as cation propellant, as core-shell-type acrylic rubber particle (the rayon Inc. of Mitsubishi " METABLENE W-5500 " of organic filler, average grain diameter 0.4 μm) 10 weight portions, as silicon dioxide (average grain diameter 0.25 μm) 10 weight portions of inorganic filler and the electroconductive particle A (electroconductive particle used in embodiment 1 of average grain diameter 30 μm, 20%K value at 100 DEG C: 1400N/mm
2, compression recovery at 100 DEG C: 15%) 4 weight portions, use planetary stirring machine, stir 5 minutes, obtain electrocondution slurry thus with 2000rPm.
(2) making of organic EL display element:
Prepare possess organic EL element, above be formed with organic EL substrate (the 1st substrate, the 1st connecting object parts) that L/S is 250 μm/250 μm, length is the Mo/Al/Mo electrode pattern of 20mm.In addition, prepare to be formed with the hermetic sealing substrate (the 2nd substrate, the 2nd connecting object parts) that L/S is 250 μm/250 μm, length is the Mo/Al/Mo electrode pattern of 20mm below.
Use disperser to become width 2mm the electrocondution slurry just made, the mode of thickness 50 μm is coated on above-mentioned 1st substrate, form the conductive paste bed of material.Then, the conductive paste bed of material make electrode opposite each other above-mentioned 2nd substrate joining.Use laminating apparatus, this laminated body is applied to the pressure of 0.2MPa, at 100 DEG C, make the conductive paste bed of material solidify 30 minutes, obtain organic EL display element.
(embodiment 39)
The heating-up temperature of the conductive paste bed of material is changed to 120 DEG C by 100 DEG C, in addition, operates in the same manner as embodiment 38, obtain organic EL display element.
(embodiment 40)
Organic filler is changed to core shell structure particulate (GANZ changes into Inc. " F351 ", average grain diameter 0.3 μm), in addition, operate in the same manner as embodiment 38, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate in the same manner as embodiment 38, obtain organic EL display element.
(embodiment 41)
Inorganic filler is changed to talcum (Japanese talc Inc. " D-800 ", average grain diameter 0.8 μm), in addition, operate in the same manner as embodiment 38, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate in the same manner as embodiment 38, obtain organic EL display element.
(embodiment 42)
Bisphenol F epoxy resin (DIC Inc. " EXA-835LV ") 50 weight portions are changed to bis-phenol E epoxy resin (printec Inc. " EPOX-MKR1710 ") 50 weight portions liquid at 23 DEG C, in addition, operate in the same manner as embodiment 38, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate in the same manner as embodiment 38, obtain organic EL display element.
(embodiment 43)
The kind of cation propellant is changed to CXC-1612 (K-Pure Inc. " K-Pure CXC ") by SI-60L (Sanaid of three new chemical companies), in addition, operates in the same manner as embodiment 38, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate in the same manner as embodiment 38, obtain organic EL display element.
(embodiment 44)
Do not add the SI-60L as cation propellant and add thermal curing agents (imidazolium compounds, four countries change into industrial group's system " 2P-4MZ ") 15 weight portions, in addition, operating in the same manner as embodiment 38, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate in the same manner as embodiment 38, obtain organic EL display element.
(embodiment 45)
Except mismatching organic filler and inorganic filler, operate in the same manner as embodiment 38, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate in the same manner as embodiment 38, obtain organic EL display element.
(embodiment 46)
Except mismatching organic filler, operate in the same manner as embodiment 38, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate in the same manner as embodiment 38, obtain organic EL display element.
(embodiment 47)
Except mismatching inorganic filler, operate in the same manner as embodiment 38, obtain electrocondution slurry.Use the electrocondution slurry obtained, operate in the same manner as embodiment 38, obtain organic EL display element.
(evaluation of embodiment 38 ~ 47)
In embodiment 38 ~ 47, to assessment item (1) ~ (6) of embodiment 1 ~ 19 and comparative example 1 ~ 4, operate in the same manner as embodiment 1 ~ 19 and comparative example 1 ~ 4, implementation evaluation.And then, in embodiment 38 ~ 47, to following assessment item (10), also implementation evaluation.
It should be noted that, in the evaluation of above-mentioned (4) moisture-proof, with baker formula applicator (manufacture of tester industry companies) electrocondution slurry obtained is coated on temperature-constant plate and makes its thickness become 100 μm.Then, heat 30 minutes at 100 DEG C, obtain film.According to JIS Z0208,60 DEG C, expose 24 hours under the condition of 90%RH, the moisture permeability of the film obtained is measured.
(10) lowest melt viscosity in the solidification of electric conducting material
Use rotary rheometer (STRESSTECH, REOLOGICA Inc.), by value minimum for the complex viscosity between gap 500um, frequency 1Hz, deflection 1rad, programming rate 10 DEG C/min, mensuration temperature range 30 DEG C ~ 120 DEG C is set to lowest melt viscosity, the lowest melt viscosity in the solidification of electric conducting material is evaluated.According to following benchmark, the viscosity in the solidification of electric conducting material is judged.
[lowest melt viscosity in the solidification of electric conducting material]
Zero: lowest melt viscosity is more than 2Pas and is below 10Pas
△: lowest melt viscosity is more than 0.4Pas and lower than 2Pas or more than 10Pas and for below 50Pas
×: lowest melt viscosity is lower than 0.4Pas or more than 50Pas
Show the result in following table 4.
[table 4]
Claims (14)
1. an electric conducting material, is heated the temperature of less than 120 DEG C but not the temperature more than 120 DEG C makes it solidify rear use, and described electric conducting material contains curability composition and electroconductive particle,
Described electroconductive particle has substrate particle and is arranged at the conductive layer on described substrate particle surface,
Modulus of elasticity in comperssion when described electroconductive particle has carried out 20% compression at 100 DEG C is 500N/mm
2above and 2000N/mm
2below,
The compression recovery of described electroconductive particle at 100 DEG C is more than 3% and less than 30%.
2. electric conducting material as claimed in claim 1, it is for the electrical connection of electrode in organic electro-luminescent display unit.
3. electric conducting material as claimed in claim 1 or 2, it is for having the electrical connection between the electrode of the organic electroluminescent substrate of electro-luminescence element and the electrode of hermetic sealing substrate.
4. the electric conducting material according to any one of claims 1 to 3, it is also containing inorganic filler.
5. the electric conducting material according to any one of claims 1 to 3, it is also containing inorganic filler and organic filler.
6. the electric conducting material according to any one of Claims 1 to 5, wherein, described curability composition contains curability compound and cation propellant.
7. the electric conducting material according to any one of Claims 1 to 5, it is also containing amines,
Described amines is the primary amine with aromatic ring,
Described curability composition contains curability compound and cation propellant.
8. the electric conducting material according to any one of claim 1 ~ 7, wherein,
Described curability compound to contain at 23 DEG C for liquid epoxy compounds and is the epoxy compounds of solid at 23 DEG C.
9. a connection structural bodies, it has:
1st connecting object parts, the 2nd connecting object parts, described 1st, the 2nd connecting object parts are carried out the connecting portion that is electrically connected,
Described connecting portion is by being heated to the temperature of less than 120 DEG C but not the temperature more than 120 DEG C make it be solidified to form by the electric conducting material according to any one of claim 1 ~ 8.
10. connection structural bodies as claimed in claim 9, wherein,
The connecting object parts of the described 1st have the 1st electrode on surface,
Described 2nd connecting object parts have the 2nd electrode on surface,
Described 1st electrode and described 2nd electrode are electrically connected by described electroconductive particle.
11. connection structural bodies as described in claim 9 or 10, wherein,
Described 1st, the 2nd connecting object parts are organic electro-luminescent display unit substrate.
12. connection structural bodies according to any one of claim 9 ~ 11, wherein,
Described 1st connecting object parts and described 2nd connecting object parts are the organic electroluminescent substrate and the hermetic sealing substrate that have electro-luminescence element.
The manufacture method of 13. 1 kinds of connection structural bodies, the manufacture method of its connection structural bodies according to any one of claim 9 ~ 11, the method comprises:
The operation of conductive material layer is set by described electric conducting material on the surface of described 1st connecting object parts;
At described conductive material layer, the operation of described 2nd connecting object parts is set with the surface of described 1st connecting object component side opposite side;
Be heated to the temperature of less than 120 DEG C but not the temperature more than 120 DEG C, described conductive material layer is solidified, formed and make described 1st, the 2nd connecting object parts realize the operation of the connecting portion of electrical connection.
The manufacture method of 14. connection structural bodies as claimed in claim 13, this connection structural bodies is organic electro-luminescent display unit, wherein,
Described 1st connecting object parts are the 1st substrates as organic electro-luminescent display unit substrate,
Described 2nd connecting object parts are the 2nd substrates as organic electro-luminescent display unit substrate,
The method comprises:
The operation of conductive material layer is set by described electric conducting material on the surface of described the 1st substrate as organic electro-luminescent display unit substrate;
At described conductive material layer, the operation of described the 2nd substrate as organic electro-luminescent display unit substrate is set with the surface of described 1st substrate-side opposite side;
Light is irradiated to described conductive material layer, and described conductive material layer is heated to the temperature of less than 120 DEG C, make described conductive material layer generation photocuring and hot curing, formed and make described 1st, the 2nd substrate realize the operation of the connecting portion of electrical connection.
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JP2012267379 | 2012-12-06 | ||
PCT/JP2013/082822 WO2014088095A1 (en) | 2012-12-06 | 2013-12-06 | Conductive material, connection structure and method for producing connection structure |
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KR (1) | KR20150092077A (en) |
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JPWO2014088095A1 (en) | 2017-01-05 |
JP6364191B2 (en) | 2018-07-25 |
WO2014088095A1 (en) | 2014-06-12 |
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