CN101036199A - Conductive ink - Google Patents
Conductive ink Download PDFInfo
- Publication number
- CN101036199A CN101036199A CN 200580034046 CN200580034046A CN101036199A CN 101036199 A CN101036199 A CN 101036199A CN 200580034046 CN200580034046 CN 200580034046 CN 200580034046 A CN200580034046 A CN 200580034046A CN 101036199 A CN101036199 A CN 101036199A
- Authority
- CN
- China
- Prior art keywords
- conductive ink
- powder
- ink
- surface tension
- nickel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000843 powder Substances 0.000 claims abstract description 79
- 229910052751 metal Inorganic materials 0.000 claims abstract description 53
- 239000002184 metal Substances 0.000 claims abstract description 53
- 239000002904 solvent Substances 0.000 claims abstract description 34
- 239000007822 coupling agent Substances 0.000 claims abstract description 25
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 20
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 15
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 8
- 239000010936 titanium Substances 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 146
- 239000002245 particle Substances 0.000 claims description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 37
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 26
- 239000003607 modifier Substances 0.000 claims description 22
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 21
- 150000002148 esters Chemical class 0.000 claims description 19
- 239000011164 primary particle Substances 0.000 claims description 19
- 239000004411 aluminium Substances 0.000 claims description 18
- 239000002270 dispersing agent Substances 0.000 claims description 17
- 239000012744 reinforcing agent Substances 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 14
- 238000009835 boiling Methods 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 229920002125 Sokalan® Polymers 0.000 claims description 12
- 239000000908 ammonium hydroxide Substances 0.000 claims description 12
- 239000004584 polyacrylic acid Substances 0.000 claims description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 11
- 125000000962 organic group Chemical group 0.000 claims description 9
- 238000007747 plating Methods 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
- 150000001412 amines Chemical class 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 229930195734 saturated hydrocarbon Natural products 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 229910000906 Bronze Inorganic materials 0.000 claims description 3
- 239000010974 bronze Substances 0.000 claims description 3
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 3
- 239000000758 substrate Substances 0.000 abstract description 49
- 239000011521 glass Substances 0.000 abstract description 21
- 239000000126 substance Substances 0.000 abstract description 15
- 238000007641 inkjet printing Methods 0.000 abstract description 12
- 239000000203 mixture Substances 0.000 abstract description 12
- 230000015572 biosynthetic process Effects 0.000 abstract description 10
- 229910052759 nickel Inorganic materials 0.000 description 51
- 238000007639 printing Methods 0.000 description 47
- 238000000034 method Methods 0.000 description 40
- 239000002002 slurry Substances 0.000 description 29
- 238000004519 manufacturing process Methods 0.000 description 27
- 238000009826 distribution Methods 0.000 description 25
- -1 4-epoxycyclohexyl Chemical group 0.000 description 23
- 238000002156 mixing Methods 0.000 description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 18
- 238000004140 cleaning Methods 0.000 description 18
- 238000003756 stirring Methods 0.000 description 18
- 239000006185 dispersion Substances 0.000 description 16
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 12
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 12
- 238000011156 evaluation Methods 0.000 description 11
- IAGCDJZAYOZMCS-UHFFFAOYSA-N 2-hydroxypropanoic acid;titanium Chemical compound [Ti].CC(O)C(O)=O IAGCDJZAYOZMCS-UHFFFAOYSA-N 0.000 description 10
- 239000002253 acid Substances 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- 238000005245 sintering Methods 0.000 description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 8
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 8
- 239000000853 adhesive Substances 0.000 description 8
- 230000001070 adhesive effect Effects 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- 238000000576 coating method Methods 0.000 description 7
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 229910052709 silver Inorganic materials 0.000 description 7
- 239000004332 silver Substances 0.000 description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000006071 cream Substances 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N Propionic acid Chemical compound CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 4
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 4
- 229940043237 diethanolamine Drugs 0.000 description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- UODXCYZDMHPIJE-UHFFFAOYSA-N menthanol Chemical compound CC1CCC(C(C)(C)O)CC1 UODXCYZDMHPIJE-UHFFFAOYSA-N 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 4
- 239000011342 resin composition Substances 0.000 description 4
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 4
- IIYFAKIEWZDVMP-UHFFFAOYSA-N tridecane Chemical compound CCCCCCCCCCCCC IIYFAKIEWZDVMP-UHFFFAOYSA-N 0.000 description 4
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 4
- WVYWICLMDOOCFB-UHFFFAOYSA-N 4-methyl-2-pentanol Chemical compound CC(C)CC(C)O WVYWICLMDOOCFB-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 238000002309 gasification Methods 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 229920000058 polyacrylate Polymers 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- DUFCMRCMPHIFTR-UHFFFAOYSA-N 5-(dimethylsulfamoyl)-2-methylfuran-3-carboxylic acid Chemical compound CN(C)S(=O)(=O)C1=CC(C(O)=O)=C(C)O1 DUFCMRCMPHIFTR-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical group CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical group CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 2
- 235000011613 Pinus brutia Nutrition 0.000 description 2
- 241000018646 Pinus brutia Species 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- AOWPVIWVMWUSBD-RNFRBKRXSA-N [(3r)-3-hydroxybutyl] (3r)-3-hydroxybutanoate Chemical compound C[C@@H](O)CCOC(=O)C[C@@H](C)O AOWPVIWVMWUSBD-RNFRBKRXSA-N 0.000 description 2
- RPELOZWDWZQYDV-UHFFFAOYSA-N [Si]=O.[Ni] Chemical compound [Si]=O.[Ni] RPELOZWDWZQYDV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 2
- JNYUEHVKLOZOHU-UHFFFAOYSA-N diethoxy-[(2-methylpropan-2-yl)oxy]silane Chemical compound CC(C)(O[SiH](OCC)OCC)C JNYUEHVKLOZOHU-UHFFFAOYSA-N 0.000 description 2
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012776 electronic material Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002334 glycols Chemical class 0.000 description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000009766 low-temperature sintering Methods 0.000 description 2
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
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- SGNLDVYVSFANHW-UHFFFAOYSA-N pentane-2,4-dione;zirconium Chemical compound [Zr].CC(=O)CC(C)=O SGNLDVYVSFANHW-UHFFFAOYSA-N 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
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- 238000012360 testing method Methods 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N tetraisopropyl titanate Substances CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 2
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- LCZVSXRMYJUNFX-UHFFFAOYSA-N 2-[2-(2-hydroxypropoxy)propoxy]propan-1-ol Chemical compound CC(O)COC(C)COC(C)CO LCZVSXRMYJUNFX-UHFFFAOYSA-N 0.000 description 1
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- MQWCXKGKQLNYQG-UHFFFAOYSA-N 4-methylcyclohexan-1-ol Chemical compound CC1CCC(O)CC1 MQWCXKGKQLNYQG-UHFFFAOYSA-N 0.000 description 1
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- DRNPGEPMHMPIQU-UHFFFAOYSA-N O.[Ti].[Ti].CCCCO.CCCCO.CCCCO.CCCCO.CCCCO.CCCCO Chemical compound O.[Ti].[Ti].CCCCO.CCCCO.CCCCO.CCCCO.CCCCO.CCCCO DRNPGEPMHMPIQU-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
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- 229920002319 Poly(methyl acrylate) Polymers 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- NUKYRBMYNRDNTE-UHFFFAOYSA-N [Ag].[Si]=O Chemical compound [Ag].[Si]=O NUKYRBMYNRDNTE-UHFFFAOYSA-N 0.000 description 1
- ZJBSGROMUAGJPA-UHFFFAOYSA-N [Ni].[Ni].[Ni].[Ag] Chemical compound [Ni].[Ni].[Ni].[Ag] ZJBSGROMUAGJPA-UHFFFAOYSA-N 0.000 description 1
- GXSDJHNAWHTIGA-UHFFFAOYSA-M [O--].[Al+3].CCCCCCCC([O-])=O Chemical compound [O--].[Al+3].CCCCCCCC([O-])=O GXSDJHNAWHTIGA-UHFFFAOYSA-M 0.000 description 1
- IARREFARZQUSAH-UHFFFAOYSA-M [Zr+].CCCCCCCCCCCCCCCCCC([O-])=O Chemical compound [Zr+].CCCCCCCCCCCCCCCCCC([O-])=O IARREFARZQUSAH-UHFFFAOYSA-M 0.000 description 1
- BTKXSYWWRGMQHR-UHFFFAOYSA-N [amino(diethoxy)silyl]oxyethane Chemical compound CCO[Si](N)(OCC)OCC BTKXSYWWRGMQHR-UHFFFAOYSA-N 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- BHGPTGSAHKMFSZ-UHFFFAOYSA-M aluminum;octadecanoate;oxygen(2-) Chemical compound [O-2].[Al+3].CCCCCCCCCCCCCCCCCC([O-])=O BHGPTGSAHKMFSZ-UHFFFAOYSA-M 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- NDKBVBUGCNGSJJ-UHFFFAOYSA-M benzyltrimethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)CC1=CC=CC=C1 NDKBVBUGCNGSJJ-UHFFFAOYSA-M 0.000 description 1
- BMRWNKZVCUKKSR-UHFFFAOYSA-N butane-1,2-diol Chemical compound CCC(O)CO BMRWNKZVCUKKSR-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 1
- KQAHMVLQCSALSX-UHFFFAOYSA-N decyl(trimethoxy)silane Chemical compound CCCCCCCCCC[Si](OC)(OC)OC KQAHMVLQCSALSX-UHFFFAOYSA-N 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- WCOATMADISNSBV-UHFFFAOYSA-K diacetyloxyalumanyl acetate Chemical compound [Al+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WCOATMADISNSBV-UHFFFAOYSA-K 0.000 description 1
- GAURFLBIDLSLQU-UHFFFAOYSA-N diethoxy(methyl)silicon Chemical compound CCO[Si](C)OCC GAURFLBIDLSLQU-UHFFFAOYSA-N 0.000 description 1
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 1
- CZWLNMOIEMTDJY-UHFFFAOYSA-N hexyl(trimethoxy)silane Chemical compound CCCCCC[Si](OC)(OC)OC CZWLNMOIEMTDJY-UHFFFAOYSA-N 0.000 description 1
- 229940051250 hexylene glycol Drugs 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 125000003253 isopropoxy group Chemical group [H]C([H])([H])C([H])(O*)C([H])([H])[H] 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- ITNVWQNWHXEMNS-UHFFFAOYSA-N methanolate;titanium(4+) Chemical class [Ti+4].[O-]C.[O-]C.[O-]C.[O-]C ITNVWQNWHXEMNS-UHFFFAOYSA-N 0.000 description 1
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 description 1
- ZWRUINPWMLAQRD-UHFFFAOYSA-N n-Nonyl alcohol Natural products CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 description 1
- MWKFXSUHUHTGQN-UHFFFAOYSA-N n-decyl alcohol Natural products CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 229940055577 oleyl alcohol Drugs 0.000 description 1
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- ZCBSOTLLNBJIEK-UHFFFAOYSA-N silane titanium Chemical compound [SiH4].[Ti] ZCBSOTLLNBJIEK-UHFFFAOYSA-N 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000002345 surface coating layer Substances 0.000 description 1
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Substances [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- JRSJRHKJPOJTMS-MDZDMXLPSA-N trimethoxy-[(e)-2-phenylethenyl]silane Chemical compound CO[Si](OC)(OC)\C=C\C1=CC=CC=C1 JRSJRHKJPOJTMS-MDZDMXLPSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- HADKRTWCOYPCPH-UHFFFAOYSA-M trimethylphenylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C1=CC=CC=C1 HADKRTWCOYPCPH-UHFFFAOYSA-M 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Landscapes
- Conductive Materials (AREA)
Abstract
An object of the invention is to provide a conductive metal ink having an excellent adhesion to various kinds of substrates such as a glass substrate, and making it possible to form fine wiring or electrodes. Another object is to provide a conductive ink which can be used for ink jet printing system etc. For the purpose of achieving the objects, ''a conductive ink comprising a solvent, a metal powder, and an adhesion improver, which is characterized in that the adhesion improver is one or mixture selected from the group consisting of a silane coupling agent, a titanium coupling agent, a zirconium coupling agent, and an aluminum coupling agent.'' is adopted. Furthermore, a surface tension of the solvent is adjusted to be in the range of 15 mN/m to 50 mN/m with a surface tension adjustor to provide conductive ink suitable for ink jet printing system etc.Disclosed is a conductive metal ink which has excellent adhesion to various bases such as glass substrates and enables formation of fine wiring or electrodes. Also disclosed is a conductive ink which can be used in inkjet systems. Specifically disclosed is a conductive ink containing a solvent, a metal powder and an adhesion improver which is characterized in that the adhesion improver is composed of one or more substances selected from the group consisting of silane coupling agents, titanium coupling agents, zirconia coupling agents and aluminum coupling agents. By adjusting the surface tension of the solvent to be within the range from 15 mN/m to 50 mN/m using a surface tension regulator, the conductive ink is formed into an ink which can be suitably used in inkjet systems or the like.
Description
Technical field
The present invention relates to utilize the circuit formation method of conductive metal printing ink, more particularly, relate to can be at low temperatures at ceramic substrate, glass substrate, and be on the resin substrate etc. of representative with the polyimide substrate, form the metal ink and the manufacture method thereof of high-density metal distribution or electrode.Simultaneously, thus relate to and can describe circuitry shapes and make its curing on substrate, form the conductive ink of circuit by ink-jetting style etc.
Background technology
In the past, as the method that on various substrates, forms circuit pattern, just like utilizing lithoprinting photomechanical printing or etching method or method for printing screen described in patent documentation 1 or the patent documentation 2.As method in the past, the Copper Foil of etching and processing copper clad laminate makes it form the method for circuit pattern, or the mixing conductive paste that becomes cream (paste) shape of metal powder and solvent or resin directly formed the method for distribution or electrode pattern by silk screen printing on substrate surface, extensively popularize.As mentioned above, with metal powder be processed into cream (below, abbreviate conductive paste as) or printing ink (below, abbreviate conductive ink as), on substrate surface, directly form the method for circuit by the technology of the method for printing screen of migrating etc., the engraving method that forms circuit with the Copper Foil of etching and processing copper clad laminate is compared, and is few because of its operation, can reduce production costs significantly, extensively popularizes.
In addition, in recent years, to carry the electroconductive circuit pattern that information device or TV are the thin display inside of representative, densification year by year, the distribution width that not only begins one's study is the following zones of 40 μ m, and research forms the technology of circuit pattern on flexible resin substrate by low-temperature sintering.In the normally used circuit pattern that forms by silk screen printing, do not break and the live width of distribution shape excellence is about 100 μ m, still, in the zone below meticulousr zone, particularly live width are 40 μ m, then be difficult to form substantial distribution.In addition, as the technology that on various substrates, forms circuit pattern by low-temperature sintering, the existing silver-colored printing ink that contains Nano silver grain shown in patent documentation 3.
On the other hand, about the liquid cream (hereinafter referred to as conductive metal printing ink) that metal powder is mixed with a large amount of organic solvent and resinae, as utilizing point gum machine (dispenser) rubbing method or as the raw material of the formation very fine circuit pattern of patent documentation 4 described ink-jet printing technologies, various conductive metal printing ink has been proposed, but, owing to depend on the organic resin class with the adhesive strength of various substrates, therefore, in the operation of the use hydrogen when being generally used for forming low-resistance distribution or electrode or the reduction sintering of nitrogen, the gas that takes place owing to the decomposition of organic resin composition is easy to produce small crack, and make the bulk density step-down of distribution or electrode therefrom, consequently be difficult to form the low resistance circuit.
In addition, as the composition of conductive ink, water-based nickel slurry is disclosed in the patent documentation 5, and the conductive paste that contains this water-based nickel slurry and binding agent.Described water-based nickel slurry contains water, set has nickel particle powder, polyacrylic acid and its ester of insoluble inorganic oxide or its salt, and the ammonium hydroxide that replaces of organic group on the powder surface of each particulate nickel powder.This water-based nickel slurry, it is the water-based nickel slurry that the nickel particle powder of high concentration no longer condenses and stably disperses, though with the internal electrode of making laminated ceramic compacitor be representative, during by high temperature sintering calcining metal powder without any problem, but, in recent years on various substrates, forming under the low temperature in the purposes of circuit, owing to come down to zero with the adhesive strength of substrate, therefore exist the problem that can not form circuit.
In addition, when using ink-jet printing technology to form the very fine circuit pattern, because do not have the surface tension that is fit to printing, therefore in the time of will forming circuit by continuous printing, the easy plug nozzle of printing ink, and causing on the purpose printing position not the phenomenon of printing ink, therefore, be difficult in fact form circuit by industrial continuous printing.In addition, because do not contain the binding agent of giving with the adhesive strength of substrate, even temporarily can on substrate, print by printing process, owing to be essentially zero with the adhesive strength of substrate, therefore, calcine at the high temperature sintering that with the internal electrode of making laminated ceramic compacitor is representative beyond the purposes of metal powder etc., be difficult to form circuit in fact.
Patent documentation 1:JP spy opens flat 9-246688 communique
Patent documentation 2:JP spy opens flat 8-18190 communique
Patent documentation 3:JP spy opens the 2002-334618 communique
Patent documentation 4:JP spy opens the 2002-324966 communique
Patent documentation 5:JP spy opens the 2002-317201 communique
Summary of the invention
The problem that invention will solve
Be appreciated that as mentioned above, in order to form above-mentioned fine circuitry at low temperatures, studied the point gum machine rubbing method or the ink jet printing method that adopt conductive metal printing ink, still, to exist adhesive strength with various base materials low or can not get the problem of tack at all.Consequently can not be used in ink-jet method.
In conductive metal printing ink in the past, used the organic resin composition as the binding agent that is used to improve with the tack of base material, therefore printed circuit on the resin substrate of pottery, glass, polyimides etc., when the low temperature below 300 ℃ reduces sintering, the resinous principle that it contained produce to decompose and to gasify owing to the influence of being heated or be subjected to reducibility gas, consequently can not have the high adhesive strength with various base materials.
As mentioned above, require the tack of conductive ink and substrate excellent and can form meticulous distribution or electrode.Simultaneously, require this conductive ink for using ink discharge device and point gum machine device, more wish further to improve the tack of the circuit described etc. and substrate at the distribution of printing very fine on the substrate or electrode and the conductive ink that when forming circuit, can print continuously.
Solve the method for problem
Therefore, the result that the inventor concentrates one's attention on research if find to contain the conductive ink of solvent, metal powder, tack reinforcing agent, then can achieve the above object, thereby finish the present invention.
Basic composition is of conductive ink of the present invention contains solvent, metal powder, tack reinforcing agent, it is characterized in that above-mentioned tack reinforcing agent is selected from one or more in the group of being made up of silane coupling agent, titanium coupling agent, zirconium coupling agent, aluminium coupling agent.
In addition, by using surface tension modifier the surface tension of above-mentioned solvent is adjusted into the scope of 15mN/m～50mN/m, so that conductive ink becomes the conductive ink that is suitable for the ink-jet printer purposes.
In addition, preferred above-mentioned surface tension modifier is 100 ℃～300 ℃ alcohol, one or more surface tension modifier that combined in the group that glycol is formed for being selected from by the boiling point under the normal pressure.
Further, in the conductive ink of the present invention, preferred above-mentioned solvent is that being selected from by the boiling point under the normal pressure is in the group formed of water, alcohols, saturated hydrocarbons below 300 ℃ one or more.
In the conductive ink of the present invention, preferred above-mentioned metal powder is selected from nickel powder, silver powder, bronze, platinum powder, copper powder, palladium powder, and the primary particle diameter of this metal powder is below the 500nm.
In addition, consider the application of conductive ink of the present invention in ink-jet printer, the maximum particle diameter of the particle of the cohesion that contains in the preferred above-mentioned metal powder is below the 0.8 μ m.
In the conductive ink of the present invention, preferred above-mentioned metal powder is for being attached with the plating inorganic oxide nickel powder of insoluble inorganic oxide on this powder surface.
In the conductive ink of the present invention, the insoluble inorganic oxide of preferred above-mentioned plating inorganic oxide nickel powder is to contain the oxide that is selected from least a element in the group of being made up of silicon dioxide, aluminium oxide, zirconia and titanium oxide.
In the conductive ink of the present invention, preferably add to be selected from (a) polyacrylic acid, its ester or its salt as dispersant; (b) one or more materials that form that made up of any group in (a)～(c) of the ammonium hydroxide that replaces of organic group and the amines that (c) contains hydroxyl.
In addition, consider the application of conductive ink of the present invention in ink-jet printer, preferably its viscosity in the time of 25 ℃ is below the 60cP.
The effect of invention
Conductive ink of the present invention is the tack excellence with the various base materials that comprise glass substrate, and can form the conductive metal printing ink of meticulous distribution or electrode, and is also excellent for the tack of the circuit that forms with different elements etc.Therefore, form guard electrode or protection tunicle etc. on the circuit surface that forms applicable to the glass substrate that in the TFT panel, uses, ito transparent electrode surface, with silver paste of this conductive ink etc.In addition, conductive film of the present invention also is applicable to, adopts point gum machine coating method or ink jet printing mode to form in correct and the meticulous distribution or electrode.
Implement preferred plan of the present invention
Conductive ink of the present invention contains solvent, metal powder, tack reinforcing agent.In addition, the invention is characterized in, use one or more materials that made up that are selected from the group of being formed by silane coupling agent, titanium coupling agent, zirconium coupling agent, aluminium coupling agent as the tack reinforcing agent.
Here said tack reinforcing agent is meant and uses the material that is selected from the group of being made up of silane coupling agent, titanium coupling agent, zirconium coupling agent, aluminium coupling agent.At this moment, not only can only use a kind of composition of from above-mentioned group, selecting, also can use two or more combinations.That is, by containing multiple composition, the tack that may command is consistent with the substrate character of the formation of carrying out circuit etc.
Here said silane coupling agent, be preferably vinyl trichlorosilane, vinyltrimethoxy silane, vinyltriethoxysilane, 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane, the 3-glycidoxypropyltrime,hoxysilane, 3-glycidoxy propyl group methyldiethoxysilane, 3-glycidoxy propyl-triethoxysilicane, to the styryl trimethoxy silane, 3-methacryloxypropyl methyl dimethoxysilane, the 3-methacryloxypropyl trimethoxy silane, 3-methacryloxypropyl methyldiethoxysilane, 3-methacryloxypropyl triethoxysilane, 3-acryloxy propyl trimethoxy silicane, N-2 (amino-ethyl)-3-aminopropyl methyl dimethoxysilane, N-2 (amino-ethyl)-3-TSL 8330, N-2 (amino-ethyl)-3-aminopropyltriethoxywerene werene, the 3-TSL 8330, the amino triethoxysilane of 3-, 3-triethoxysilicane alkyl-N-(1,3-dimethyl-butylidene) propyl group amine, N-phenyl-3-TSL 8330, N-(Ethylbenzyl)-2-amino-ethyl-3-TSL 8330 hydrochloride, 3-urea groups propyl-triethoxysilicane, the 3-r-chloropropyl trimethoxyl silane, 3-sulfydryl propyl group methyl dimethoxysilane, 3-sulfydryl propyl trimethoxy silicane, two (tri-ethoxy silylpropyl) tetrasulfide, 3-isocyanates propyl-triethoxysilicane, tetramethoxy-silicane, tetraethoxysilane, methyltrimethoxy silane, methyl triethoxysilane, the dimethyl triethoxysilane, phenyl triethoxysilane, hexamethyldisilazane, the hexyl trimethoxy silane, silane coupling agent arbitrarily in the decyl trimethoxy silane.Wherein, from considering stable aspect the methyltrimethoxy silane of the performance that preferred use is played stably, methyl triethoxysilane, dimethyl triethoxysilane etc. with the tack of substrate.
Here said titanium coupling agent is preferably the coupling agent of silane titanium arbitrarily in tetra isopropyl titanate, tetra-n-butyl titanate esters, butyltitanate dimer, four (2-ethylhexyl) titanate esters, tetramethyl titanate esters, titanium acetylacetone, four titanium acetylacetones, titanium ethyl acetoacetic ester, titanium octane two greases, lactic acid titanium (チ Application ラ Network テ one ト), titanium triethanolamine compound, the poly-hydroxyl titanium stearate.Wherein, consider the preferred tetra isopropyl titanate that uses the performance of playing stably, tetra-n-butyl titanate esters, lactic acid titanium etc. from can be with the tack of substrate stable aspect.
Here said zirconium coupling agent is preferably the coupling agent of zirconium arbitrarily in n Propanoic acid zirconium (ジ Le コ ニ ウ system ノ Le マ Le プ ロ ピ レ one ト), n-butyric acie zirconium, tetrem acyl acetone zirconium, single acetyl acetone zirconium, bis-acetylacetonate zirconium, zirconium list ethyl acetoacetic ester, the two ethyl acetoacetic esters of zirconium acetylacetone,2,4-pentanedione, zirconium acetate, the monostearate zirconium.Wherein, from considering stable aspect the preferred two ethyl acetoacetic esters of n Propanoic acid zirconium, n-butyric acie zirconium, tetrem acyl acetone zirconium, single acetyl acetone zirconium, bis-acetylacetonate zirconium, zirconium list ethyl acetoacetic ester, zirconium acetylacetone,2,4-pentanedione, the zirconium acetate that uses the performance of playing stably with the tack of substrate.
Here said aluminium coupling agent is preferably the coupling agent of aluminium arbitrarily in aluminum isopropoxide, single aluminium-sec-butylate diisopropyl acid esters, secondary butyric acid aluminium, aluminium acetate, oacetic acid aluminium diisopropyl acid esters, aluminium three (ethyl acetoacetic ester), alkyl acetoacetate aluminium diisopropyl acid esters, aluminium single acetyl acetone two (ethyl acetoacetic ester), aluminium three (levulinic ketone ester), aluminium list isopropoxy list oleyl alcohol base ethyl acetoacetic ester, ring-type aluminium oxide isopropyl acid ester, ring-type aluminium oxide caprylate, the ring-type aluminium oxide stearate.Wherein, from considering stable aspect preferred oacetic acid aluminium diisopropyl acid esters, aluminium three (ethyl acetoacetic ester), alkyl acetoacetate aluminium diisopropyl acid esters, aluminium single acetyl acetone two (ethyl acetoacetic ester), the aluminium three (levulinic ketone ester) that use the performance of playing stably with the tack of substrate.
Next, solvent is described.Said solvent among the present invention can be extensive use of water, organic solvent etc., and have intermiscibility with above-mentioned tack reinforcing agent at least, as long as it can modulate the cream viscosity of regulation etc., is not particularly limited.Therefore, if limit, then for by the boiling point under the normal pressure being one or more materials that made up in the group formed of water, alcohols, saturated hydrocarbons below 300 ℃.
Here, be defined as " boiling point under the normal pressure is below 300 ℃ ", be because when boiling point surpasses 300 ℃ temperature province, in the reduction sintering circuit, cause the resin glue decomposition and vaporize the same with the conductive ink of organic resin composition with utilization as resin glue, at high temperature solvent produces gasification, thereby can not form fine and close electrode, consequently, can not bring into play high adhesive strength with various base materials.
When making water, be water, and do not comprise the water of the purity of running water etc. with purity of degree such as ion exchange water, distilled water as solvent.
Use pure time-like as solvent, the preferred use is selected from the 1-propyl alcohol, the 1-butanols, the 1-amylalcohol, the 1-hexanol, cyclohexanol, the 1-enanthol, the 1-octanol, 1 nonyl alcohol, the 1-decyl alcohol, epoxy prapanol, benzylalcohol, methyl cyclohexanol, 2-methyl-1-butene alcohol, 3-methyl-2-butanols, 4-methyl-2-amylalcohol, isopropyl alcohol, the 2-ethyl butanol, 2-Ethylhexyl Alcohol, sec-n-octyl alcohol, terpineol, dihydro-terpineol, 2-methyl cellosolve, cellosolvo, the 2-n-butoxy ethanol, the 2-phenoxetol, carbitol, ethyl carbitol, the normal-butyl carbitol, in the diacetone alcohol-kind or two or more compositions.Wherein, more preferably to use boiling point under the normal pressure be more than 80 ℃ and be difficult to gasify under the room temperature normal pressure 1-butanols, 1-octanol, terpineol, dihydro-terpineol, 2-methyl cellosolve, cellosolvo, 2-n-butoxy ethanol, diacetone alcohol.
When using saturated hydrocarbons as solvent, preferred one or more the composition that is selected from heptane, octane, nonane, decane, hendecane, dodecane, tridecane, the tetradecane, pentadecane, the hexadecane that uses.Wherein, more preferably use decane, hendecane, dodecane, tridecane, the tetradecane.This is because their boiling points under normal pressure are to be difficult to gasification thereby processing ease below 300 ℃ and under the room temperature that steam forces down.
Aforesaid conductive ink can be by the surface tension of using surface tension modifier to give optimum ink-jetting style.That is, be adjusted into the scope of 15mN/m～50mN/m, form circuit etc. with ink-jet method, point gum machine method easily by surface tension with conductive ink of the present invention.Therefore, the addition of surface tension modifier described later is, adds various auxiliary agents and makes the surface tension of conductive ink be adjusted into 15mN/m～50mN/m, preferably is adjusted into the amount of 20mN/m～40mN/m.If the surface tension of conductive ink exceeds above-mentioned scope, then produce and to spray conductive ink or promptly allow to from the nozzle ejection from inkjet nozzle also from dislocation of purpose printing position or the phenomenon that can not print continuously etc.Therefore, be suitable for using in the above-mentioned scope of ink-jet method, can use ink discharge device to form fine circuitry distribution etc. by the surface tension of conductive ink of the present invention is adjusted to.
When considering the surface tension of above-mentioned conductive ink, the problem of the combination of solvent and surface tension modifier is arranged.Solvent during therefore, at first to consideration reconciliation statement surface tension is described.Solvent when considering the adjustment form surface tension both can have only organic solvent also can contain water.When making water, can use the water of purity, not comprise the water of the purity of running water etc. with ion exchange water, distilled water etc. as solvent.
In addition, when mixing water and organic solvent etc. use in the solvent, be at least with above-mentioned water, dispersant, tack reinforcing agent and have intermiscibility, as long as and can modulate the ink viscosity of regulation, then there is no particular limitation.At this moment, when water is 100 weight portions, mix organic solvent about 3 weight portions～5000 weight portions etc., carefully adjust the viscosity of conductive ink, the dispersiveness of metal powder etc.Especially, require to consider and the combination of the metal powder kind used and select to use.Therefore, if limit this organic solvent etc., then for by the boiling point under the normal pressure being one or more materials that made up in the group formed of 100 ℃～300 ℃ water, alcohols, glycols.
Be defined herein to " boiling point under the normal pressure is 100 ℃～300 ℃ ", be because when boiling point surpasses 300 ℃ temperature province, in the reduction sintering circuit, cause the resin glue decomposition and vaporize the same with the conductive ink of organic resin composition with utilization as resin glue, at high temperature solvent produces gasification, thereby can not form fine and close electrode, consequently, can not bring into play high adhesive strength with various base materials.In addition, being set at more than 100 ℃, is because this temperature for more than the boiling point of water, can be selected the cause to the truly feasible heating-up temperature scope of the removal that must be included in the water in the solvent.
Use pure time-like as solvent, preferred one or more compositions that are selected from 1-butanols, 1-amylalcohol, epoxy prapanol, benzylalcohol, 3-methyl-2-butanols, 4-methyl-2-amylalcohol, 2-methyl cellosolve, cellosolvo, 2-n-butoxy ethanol, 2-phenoxetol, carbitol, ethyl carbitol, normal-butyl carbitol, the diacetone alcohol that use.Wherein, more preferably to use boiling point under the normal pressure be more than 100 ℃ and be difficult to gasify under the room temperature normal pressure 1-butanols, 1-amylalcohol, 2-methyl cellosolve, cellosolvo, 2-n-butoxy ethanol, 2-phenoxetol, diacetone alcohol.
When using glycols as solvent, the preferred use is selected from ethylene glycol, diethylene glycol, triethylene glycol, TEG, propylene glycol, trimethylene glycol, DPG, tripropylene glycol, 1,2-butanediol, 1,3-butanediol, 1, one or more compositions in 4-butanediol, pentamethylene glycol, the hexylene glycol.Wherein, more preferably use the viscosity under the normal temperature to be the ethylene glycol below the 100cp, diethylene glycol, propylene glycol, 1,4-butanediol, trimethylene glycol.If viscosity is too high, then be difficult to be adjusted to the viscosity that is fit to point gum machine method or ink ejecting method.
In addition, above-mentioned surface tension modifier uses surface tension to be the additive below the 40mN/m.When use has above-mentioned capillary surface tension modifier, the easiest surface tension that is adjusted into the printing ink that is suitable in ink discharge device, using, it is simple and easily that the viscosity adjustment that meets the ink discharge device design can become.Can form meticulous wiring circuit.Here said surface tension modifier, preferably uses by surface tension as the viscosity below the 40mN/m, under 25 ℃ as below the 100cp, also can be used as one or more materials that made up of selecting in the alcohol of solvent use, the group that glycol is formed.
In this surface tension modifier, as surface tension below the 40mN/m and the viscosity under 25 ℃ be alcohol below the 100cp, for example, can enumerate 1-butanols, 1-amylalcohol, 4-methyl-2-amylalcohol, cellosolvo, 2-n-butoxy ethanol, normal-butyl carbitol etc.Among the present invention,, preferably use 2-n-butoxy ethanol or 1-butanols in the above-mentioned surface tension modifier from keeping the long-term stay in grade shape aspect of conductive ink.
In the conductive ink of the present invention, the amount of the surface tension modifier of cooperation is set at the suitable capillary amount of adjusting conductive ink and gets final product, and there is no particular limitation.But, generally in conductive ink, be generally 1 weight %～50 weight %, be preferably 3 weight %～30 weight %.During the quantity not sufficient 1 weight % of surface tension modifier, can not the adjustment form surface tension.In addition, if the surface tension modifier addition is that 50 weight % are when above, add before and after the surface tension modifier, great changes will take place for the discrete form of the particle metal powder that contains in the conductive ink, consequently the particle metal powder begins cohesion, hindered the even dispersion of of paramount importance particle metal powder in the conductive ink, thereby can not use as conductive ink.
And, said here metal powder, there is no particular limitation to the powder characteristics of its particle diameter, dispersiveness etc., and that the powder shape comprises is spherical, sheet, have whole notion of the powder of surface coating layer.But conductive ink of the present invention mainly is to use as prerequisite in forming with the circuit at electronic material.Therefore, expect from the electronic material purposes, often selecting in the nickel powder of use, silver powder, bronze, platinum powder, copper powder, the palladium powder, and the primary particle diameter of its metal powder is below the 500nm.
Further, consider in ink-jetting style and use, thereby preferably its average primary particle diameter is below the 500nm.If the average grain diameter of primary particle surpasses 500nm, then conductive ink stops up inkjet nozzle extremely easily, is difficult to continuous printing.Even can print,, and can not become meticulous distribution as purpose also because the thickness of formed distribution or electrode is blocked up.
Furtherly, according to the degree that becomes more meticulous of the circuit that forms, the particle metal powder of suitably selecting to have suitable primary particle size gets final product.But from the notion of particle metal powder, usually at 3nm～500nm, preferably at 5nm～200nm, further preferred the selection in the scope of 10nm～150nm used.When the not enough 3nm of the average primary particle diameter of particle metal powder, can not establish its manufacture method at present, can not verify by testing.And on the other hand, when average primary particle diameter surpasses 500nm, then be difficult to form width as purpose and be distribution or electrode below the 40 μ m, and the thickness of distribution that forms or electrode is blocked up, and therefore improper.As tendency, the average primary particle diameter of the powder of particle metal powder is meticulous more, causes that the possibility of jamming of inkjet nozzle is low more, is suitable for the formation of fine circuitry more.Average primary particle diameter among the present invention is meant when using scanning electron-microscopic observation, and the particle diameter of minimum 200 powders that comprise in the field of view is by adding up the particle diameter that average above-mentioned particle diameter is obtained.
Though the average primary particle diameter of particle metal powder is little, can become the basis of so-called fine silt,, big even particulate also condenses between the powder in the conductive ink if the particle diameter of secondary structure body becomes, then still cause the obstruction of inkjet nozzle easily.Therefore, with in the conductive ink as the flocculated particle of the secondary structure body of particle metal powder, be controlled to be and do not cause that the size that inkjet nozzle stops up is necessary, this size has obtained affirmation in experiment, if promptly the maximum particle diameter of flocculated particle is adjusted into 0.8 μ m when following, then almost can prevents the obstruction of inkjet nozzle really.In addition, the confirmation method as this flocculated particle then uses laser particle size measure of spread device.
In addition, consider as conductive ink through the time when variation, sintering characteristic etc., can use the applying oxidn powder etc. that carried out adhering on surface-treated metal powder or the powder surface oxide of regulation with oleic acid or stearic acid etc., select to use as long as consider the characteristic that requirement possesses in the conductive ink.Wherein, consider in the conductive ink of the present invention and use nickel powder, thereby preferably on this powder surface, be attached with the plating inorganic oxide nickel powder of insoluble inorganic oxide.
In addition, in the insoluble inorganic oxide that on the powder surface of plating inorganic oxide nickel powder, adheres to, can use silicon dioxide, aluminium oxide, zirconia, titanium oxide, metatitanic acid palladium, calcium zirconate etc., wherein, the preferred use contained one or more the oxide of element that is selected from the group of being made up of silicon dioxide, aluminium oxide, zirconia and titanium oxide.Wherein, more preferred because silicon dioxide is easy to stable adhering on the powder surface of nickel powder especially.
When forming insoluble inorganic oxide layer on the powder surface of nickel powder, can adopt the whole bag of tricks.For example, can adopt by the insoluble inorganic oxide of nickel powder and powdery and medium (being similar to the material of zirconium oxide bead) are dropped in the mixing and blending machine and stir, in the method for the insoluble inorganic oxide of powder surface set of nickel powder.
In addition, as the method for on the powder surface of nickel powder, adhering to insoluble inorganic oxide, can adopt in water disperse nickel powder and insoluble inorganic oxide after, pass through dried, remove moisture, make the method for insoluble inorganic oxide in nickel powder powder surface attachment.At this moment, the average primary particle diameter of preferred insoluble inorganic oxide is preferably below 0.15 times for below 0.2 times of average primary particle diameter of the powder of formation nickel powder.The tack of the insoluble inorganic oxide powder on nickel powder powder surface, the more little tendency of adhering to more equably of the particle diameter with insoluble inorganic oxide powder.
When using the applying oxidn nickel powder among the present invention, the amount of the insoluble inorganic oxide that adheres on the nickel particle surface, when the weight of nickel during, be generally 0.05 weight %～10 weight %, be preferably 0.1 weight %～5 weight %, more preferably 0.5 weight %～2 weight % as 100 weight %.When the quantity not sufficient 0.05 weight % of insoluble inorganic oxide, can not get as the long lifetime that the conductive ink of oxides coating meaning is set.In addition, when the amount of insoluble inorganic oxide surpassed 10 weight %, the oxides coating thickening formed uneven coating on the powder surface, and the powder surface loses slickness, causes undesired viscosity.Above-mentioned more suitably scope, in industrial processes, can be more certain reach the above-mentioned meaning that higher limit and lower limit had.
As mentioned above,,, also can prevent from effectively to condense again, therefore can realize the long lifetime of conductive ink even conductive ink middle and high concentration ground contains nickel powder by using the applying oxidn nickel powder.
Further, in the conductive ink of the present invention, particularly in the nickel ink, preferably add dispersant as required.As this dispersant, the preferred interpolation is selected from (a) polyacrylic acid, its ester or its salt; (b) one or more materials that made up of arbitrary group in (a)～(c) of the ammonium hydroxide that replaces of organic group and the amines that (c) contains hydroxyl.
As (a) polyacrylic acid, its ester or its salt that use among the present invention, for example, can enumerate polyacrylic acid, polymethyl acrylate, Sodium Polyacrylate, ammonium polyacrylate, wherein, because ammonium polyacrylate coordination on the metallic surface is easy, simultaneously, the ammonium polyacrylate of coordination repels by electricity and the steric hindrance effect is suppressed at the cohesion of the metallic in the solvent, so be preferred.(a) can use the independent material that one or more are made up in the above-mentioned substance among the present invention.
Replace ammonium hydroxide as (b) organic group that uses among the present invention, for example, the alkyl that can enumerate Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, tetrabutylammonium hydroxide amine etc. replaces the alkyl substituting aromatic base replacement ammonium hydroxide of ammonium hydroxide, trimethylphenyl ammonium hydroxide, benzyltrimethylammonium hydroxide etc., wherein, because it is easy that alkyl replaces ammonium hydroxide coordination on metallic, simultaneously, electric repulsive force is high and preferred.(b) of the present invention can use the independent material that one or more are made up in the above-mentioned material.
The amines that contains hydroxyl as (c) that uses among the present invention, for example, can enumerate, alkanolamine, wherein, two alkanolamines of dimethanolamine, diethanol amine, dipropanolamine etc. and the wetability of metallic are excellent and preferred, in addition, since diethanol amine be easy to most to suppress metallic through the time cohesion, so more preferred.(c) among the present invention can use the independent material that one or more are made up in the above-mentioned substance.
Among the present invention,, prevent the cohesion again of the nickel powder powder in the printing ink by in electroconductive nickel printing ink, adding above-mentioned dispersant.The dispersant that uses among the present invention is at least a the getting final product in above-mentioned (a)～(c), wherein, and if with (a) and (c), nickel powder is more stably disperseed, so be preferred.
When having " polyacrylic acid, its ester or its salt " in the conductive ink of the present invention, metal powder with respect to 100 weight portions, the amount of " polyacrylic acid, its ester or its salt " is generally 0.05 weight portion～5 weight portions, be preferably 0.1 weight portion～2 weight portions, do not injure the tack of printing ink for base material this moment, and the longest-lived of printing ink.
When having " organic group replacement ammonium hydroxide " in the conductive ink of the present invention, metal powder with respect to 100 weight portions, the amount of " organic group replacement ammonium hydroxide " is generally 0.01 weight portion～5 weight portions, be preferably 0.05 weight portion～1 weight portion, do not injure the tack of printing ink for base material, the longest-lived of printing ink this moment.
When having " amines that contains hydroxyl " in the conductive ink of the present invention, nickel with respect to 100 weight portions, the amount of " amines that contains hydroxyl " is generally 0.5 weight portion～20 weight portions, be preferably 5 weight portions～15 weight portions, do not injure the tack of printing ink for base material, the longest-lived of printing ink this moment.
Use under the situation of combined dispersant in the conductive ink of the present invention, when having " polyacrylic acid, its ester or its salt " and " organic group replacement ammonium hydroxide ", " polyacrylic acid, its ester or its salt " with respect to 100 weight portions, the amount of " organic group replacement ammonium hydroxide " is generally 1 weight portion～30 weight portions, be preferably 5 weight portions～20 weight portions, do not injure the tack of printing ink for base material, the longest-lived of printing ink this moment.
Viscosity for conductive ink describes.The present invention becomes easier for the circuit formation that makes ink-jet method or point gum machine method etc., and the preferred viscosity of conductive ink under 25 ℃ is below the 60cp.Viscosity adjustment of the present invention is reached by the most suitably cooperating above-mentioned solvent, dispersant, applying oxidn metal powder.Not putting down in writing the lower limit of viscosity among the present invention, is because the conductive ink of each metal is used for circuit when forming employed place and purpose difference, desirable distribution, electrode size with and shape also different.If 25 ℃ viscosity surpasses 60cp, even then want to utilize ink-jet method or point gum machine method to form meticulous distribution or electrode, because the viscosity of conductive ink is higher than from more than the energy of nozzle ejection conductive ink, therefore, is difficult to stably spray from nozzle the drop of conductive ink.When 25 ℃ viscosity are 60cp when following, by test as can be known can enough ink-jet methods or the point gum machine method form meticulous distribution or electrode.
Below, show embodiment, but the present invention is not limited to this explanation.At first, in embodiment 1～4, put down in writing the embodiment of the tack that is mainly used in the conducting film of estimating base material and formation.
Embodiment 1
(nickel powder)
Among this embodiment, use the applying oxidn nickel powder as nickel powder.The manufacture method of this applying oxidn nickel powder, as follows.
Be to inject the 10L pure water in the container of 20L toward capacity, mixing speed with 200rpm stirs on one side, (Mitsu Mining ﹠ Smelting Co., Ltd makes slowly to add the 4000g nickel powder on one side, NN-100, the average grain diameter of primary particle is 100nm), stir after 20 minutes, (Nissan Chemical Ind Ltd makes toward the cataloid that wherein adds 200g, 20 weight %, ス ノ one テ Star Network ス 0, the average grain diameter of primary particle is 20nm), continue stirring and obtained dispersion liquid in 20 minutes.
Next, in order to make cataloid equably in the nickel powder of blending in this dispersion liquid, use emulsify at a high speed dispersion machine T.K.filmix (special machine chemical industry society make) to carry out continuous mixed processing, obtain the cataloid slurries of blending state in nickel equably.Next, using vacuum drier, is below the 50Torr in vacuum degree, and the temperature in the drying machine is dry these slurries 24 hours under 120 ℃ the condition, obtains the dried powder of set silicon dioxide on the particle surface of nickel powder.Next, use Henschel mixer (Henschel mixer) (manufacturings of Mitsui mine society) with this dried powder pulverizing after, use the screen cloth of 20 μ m to carry out gradation sizing and remove thick particle.Next, for the silicon dioxide that exists on the nickel particles surface of improving the powder by 20 μ m sieve and the tack on nickel particles surface, further use vacuum drier the vacuumize degree as 10Torr below, dry built-in temperature is a heat treated 24 hours under 150 ℃ the condition, obtain applying silicon oxide nickel powder (below, be called " nickel powder A ").This nickel powder A is for adhering to the nickel powder of silicon dioxide on the particle surface of nickel particle.
(dispersant)
Toward capacity the diethanol amine (Wako Pure Chemical Industries, Ltd.'s manufacturing) that adds 380g in the beaker of 1L, 44% polyacrylic acid ammonium salt solution (Wako Pure Chemical Industries, Ltd.'s manufacturing) 45.6g and 13.4g, 15% tetramethyl-ammonium solution (Wako Pure Chemical Industries, Ltd.'s manufacturing), the preparation dispersant with the stirring of electromagnetic type blender (below, be called dispersant A).
(preparation conductive ink)
Be to add the pure water of 0.7L in the container of 1L toward capacity as solvent, with the mixing speed of 200rpm stir on one side, slowly add the nickel powder A of 300g on one side, add the dispersant A of 40.3g then, stir and obtained slurries in 20 minutes.
Next, after use emulsify at a high speed dispersion machine T.K.filmix (Tokushu Kika Kogyo K.K's manufacturing) carries out continuous dispersion treatment to these slurries, add the 0.96L pure water and obtain the slurries that nickel concentration is 15 weight %.
Next, (advantec Toyo Co., Ltd. makes with flowing through cartridge type (cartridge) filter, MCP-JX-E10S, average pore size is that 1 μ m is following) mode remove the above particle of 1 μ m that contains in these slurries, and then in order to remove the particle more than the 0.8 μ m, filter with mixed cellulose ester type membrane filter A065A293C (advantec Toyo Co., Ltd. makes, and average pore size is 0.65 μ m), obtain filtrate (nickel slurry A).
(preparation conductive ink)
Starch the lactic acid titanium as the tack reinforcing agent (this pure pharmaceutical worker's industry manufacturing TC-315 of Co., Ltd. of pine) that adds 65.8g among the A toward nickel, stirred 30 minutes, obtain conductive ink (conductive ink A) with the mixing speed of 200rpm.
(electrode forms and estimates)
In length is on the square alkali-free glass substrate OA-10 (manufacturing of NEG society) of 4cm, uses the condition coating conductive ink A of spin coater with the rotating speed of 2000rpm.Next, be in hydrogen-helium gas mixture body environment of 2 capacity % at hydrogen content, under 300 ℃ the glass substrate after filming being reduced sintering 2 hours, on glass substrate, form the nickel electrode film.Observe the thickness of electrode of measuring by SEM and be about 1 μ m.Measure the ratio resistance of nickel electrode film, in addition with four point probe resistance measurement machine ロ レ ス GP (manufacturing of Mitsubishi Chemical society), according to JIS K 5600 5-6 sections, by the tack of crosscut (cross cut) method evaluation and glass substrate.The ratio resistance of measuring is 3.8 * 10
-3Ω cm, being evaluated as of tack classifies 0, has good tack.In addition, above-mentioned nickel electrode film is used ultrasonic waves for cleaning 10 minutes in water, use ultrasonic waves for cleaning 10 minutes then in acetone, the result does not observe peeling off of nickel electrode film fully.
(formation of fine electrode and evaluation)
Upward engage the nozzle that the internal diameter of spray nozzle front end is processed into 25 μ m at point gum machine apparatus for coating (manufacturing of Musashi engineering society), make the state that can be coated with conductive ink continuously.Use this device at square alkali-free glass substrate OA-10 (NEG society manufacturing) the last coating conductive ink A of length, form the nickel electrode film as 4cm.Next, be in hydrogen-helium gas mixture body environment of 2 capacity % at hydrogen content, under 300 ℃, this glass substrate is reduced sintering 2 hours, on glass substrate, form the nickel electrode film.Width with the electrode of measurement microscope is about 40 μ m.In addition, in water, use the resulting nickel electrode film of ultrasonic waves for cleaning 10 minutes, in acetone, after 10 minutes, when using microscopic examination, do not observe peeling off of nickel electrode film fully then with ultrasonic waves for cleaning.
Embodiment 2
Except that using aminosilane coupling agent KBE-903 (chemistry society of SHIN-ETSU HANTOTAI makes) replacement lactic acid titanium, other obtains conductive ink (conductive ink B) similarly to Example 1, uses spin coater to obtain the nickel electrode film.For the nickel electrode film, measure than resistance similarly to Example 1, estimate tack.Than resistance is 4.5 * 10
-3Ω cm, being evaluated as of tack classifies 0, has good tack.In addition, use the above-mentioned nickel electrode film of ultrasonic waves for cleaning 10 minutes in water, use ultrasonic waves for cleaning 10 minutes then in acetone, the result does not observe peeling off of nickel electrode film fully.Next, similarly to Example 1 by the point gum machine rubbing method, on glass substrate, form meticulous nickel electrode film.Width with the electrode of measurement microscope is about 40 μ m.In addition, in water, use the resulting nickel electrode film of ultrasonic waves for cleaning 10 minutes, in acetone, after 10 minutes, when using microscopic examination, do not observe peeling off of nickel electrode film fully then with ultrasonic waves for cleaning.
Embodiment 3
(Mitsu Mining ﹠ Smelting Co., Ltd makes except the substrate that will form the nickel electrode film changes glass substrate with the ITO film into, the ITO film thickness is 0.2 μ m) in addition, carry out operation similarly to Example 1, having the meticulous nickel electrode film of formation on the glass substrate of ITO film by the point gum machine rubbing method.Width with the electrode of measurement microscope is about 40 μ m.In addition, the nickel electrode film that obtains with ultrasonic waves for cleaning in water 10 minutes after 10 minutes, when using microscopic examination, does not observe peeling off of nickel electrode film with ultrasonic waves for cleaning then fully in acetone.
Embodiment 4
(Mitsu Mining ﹠ Smelting Co., Ltd makes except the substrate that will form the nickel electrode film changes copper clad laminate into, copper thickness is 35 μ m) in addition, carry out operation similarly to Example 1, on copper clad laminate, form meticulous nickel electrode film by the point gum machine rubbing method.Width with the electrode of measurement microscope is about 40 μ m.Resulting nickel electrode film is used ultrasonic waves for cleaning 10 minutes in water, in acetone, after 10 minutes, when using microscopic examination, do not observe peeling off of nickel electrode film fully then with ultrasonic waves for cleaning.
Below, record be that conductive ink is carried out the viscosity adjustment, use ink-jet printer to form circuit, and the embodiment 5～embodiment 7 that estimates.
Embodiment 5
(preparation of particle metal powder)
Among this embodiment, use plating inorganic oxide particle nickel powder as the particle metal powder.Below, the preparation of plating the inorganic oxide particle nickel powder is described.Be to inject the 10L pure water in the container of 20L toward capacity, mixing speed with 200rpm stirs on one side, (Mitsu Mining ﹠ Smelting Co., Ltd makes slowly to add the 4000g nickel powder on one side, NN-100, the average grain diameter of primary particle is 100nm), stir after 20 minutes, (Nissan Chemical Ind Ltd makes toward the cataloid that wherein adds 200g, 20 weight %, ス ノ one テ Star Network ス 0, the average grain diameter of primary particle is 20nm), continue stirring and obtained dispersion liquid in 20 minutes.
Next, in order to make cataloid equably in the nickel powder of blending in this dispersion liquid, use emulsify at a high speed dispersion machine T.K.filmix (special machine chemical industry society make) to carry out continuous mixed processing, obtain the cataloid slurries of blending state in nickel equably.Next, using vacuum drier, is below the 50Torr in vacuum degree, and the temperature in the drying machine is the dried of under 120 ℃ the condition these slurries being carried out 24 hours, obtains the dried powder of set silicon dioxide on the particle surface of nickel powder.Next, use Henschel mixer (Henschel mixer) (Mitsui Mining Co Ltd. BJ Offc's manufacturings) with this dried powder pulverizing after, use the screen cloth of 20 μ m to carry out gradation sizing and remove thick particle.Next, for the silicon dioxide that exists on the nickel particles surface of improving the powder by 20 μ m sieve and the tack on nickel particles surface, further use vacuum drier the vacuumize degree as 10Torr below, dry built-in temperature is a heat treated 24 hours under 150 ℃ the condition, obtain applying silicon oxide nickel powder (below, be called " nickel powder ").This nickel powder is for adhering to the nickel powder of silicon dioxide on the particle surface of nickel particle.
(dispersant)
Toward capacity the diethanol amine (Wako Pure Chemical Industries, Ltd.'s manufacturings) that adds 380g in the beaker of 1L, 44% polyacrylic acid ammonium salt solution (Wako Pure Chemical Industries, Ltd.'s manufacturings) 45.6g and 13.4g, 15% tetramethyl-ammonium solution (Wako Pure Chemical Industries, Ltd.'s manufacturings), usefulness electromagnetic type blender stirring and prepare dispersant.
(preparation water-based nickel slurry)
Be to add the pure water of 0.7L in the container of 1L toward capacity as solvent, with the mixing speed of 200rpm stir on one side, slowly add the above-mentioned nickel powder of 300g on one side, add the 40.3g dispersant again, stir and obtained slurries in 20 minutes.
Next, after use emulsify at a high speed dispersion machine T.K.filmix (Tokushu Kika Kogyo K.K's manufacturing) carries out continuous dispersion treatment to these slurries, add the 0.96L pure water and obtain the slurries that nickel concentration is 15 weight %.
Next, (advantec Toyo Co., Ltd. makes with flowing through cartridge type (cartridge) filter, MCP-JX-E10S, average pore size is that 1 μ m is following) mode remove the above particle of 1 μ m that contains in these slurries, and then, filter with mixed cellulose ester type membrane filter A065A293C (advantec Toyo Co., Ltd. makes, and average pore size is 0.65 μ m) in order to remove the particle more than the 0.8 μ m, obtain filtrate (below, be called " water-based nickel slurry ").
(preparation conductive ink)
In above-mentioned water-based nickel slurry, add 2-n-butoxy ethanol (Kanto Kagaku K. K. manufacturing of 188.9g with respect to filtrate as surface tension modifier, surface tension is 28.2mN/m), mixing speed with 200rpm stirred 30 minutes, add the lactic acid titanium (pine this pure pharmaceutical worker industry Co., Ltd. manufacturing TC-315) of 65.8g then as the tack reinforcing agent, stirred 30 minutes with the mixing speed of 200rpm again, obtain conductive ink (below, be called " conductive ink A ").(エ of Co., Ltd. one ア Application De デ イ society makes with the dynamic contact angle determinator, DCA-100W) surface tension of this conductive ink A of Ce Dinging is 32.5mN/m, (manufacturing of CBC マ テ リ ア Le ズ Co., Ltd., the viscosity during 25 ℃ of VM-100A) measuring is 10.8cP with vibrating type viscometer.
(evaluation of printing)
For conductive ink A, (Seiko Epson society makes to use commercially available ink-jet printer, PM-G700), go up to make Wiring pattern (circuit width and circuit be spaced apart 100 μ m, length is 2cm) at alkali-free glass substrate OA-10 (Nippon Electric Glass Co., Ltd), its result can not stop up inkjet nozzle and printing conductive printing ink A.And, can print continuously more than 50 times.Whether after printing 50 times continuously, stop up in order to confirm nozzle, implemented the printing of nozzle check pattern, its result does not find the obstruction of nozzle.In addition, during with observation by light microscope resulting wiring pattern, not observing dispersing of broken string or printing ink on Wiring pattern, is good Wiring pattern.
(evaluation of conductivity)
Next, be on the square glass substrate of 4cm in length with above-mentioned ink-jet printer, making length is the square whole film of 3cm, is in the mixed-gas environment of hydrogen-helium of 2 capacity % at hydrogen content, 300 ℃ of following heat treated 2 hours, obtains electrode film.The ratio resistance of measuring this electrode film with four point probe resistance measurement machine ロ レ ス GP (Mitsubishi chemical Co., Ltd's manufacturing) is 1.8 * 10
-3Ω cm.
(evaluation of tack)
Next, according to JIS K 5600 5-6 sections, estimate the tack of the electrode film and the glass substrate of above-mentioned making by crosscut (cross cut) method.The evaluation result of tack has good tack for classification 0.In addition, this electrode film is used ultrasonic waves for cleaning 10 minutes in water, use ultrasonic waves for cleaning 10 minutes then in acetone, its result does not observe peeling off of nickel electrode film fully.With above-mentioned performance evaluation result etc., be shown in Table 1 with other embodiment and comparative example.
Embodiment 6
Among this embodiment, except interpolation 89.5g replaces carrying out similarly to Example 5 beyond the 2-n-butoxy ethanol as the 1-butanols (Kanto Kagaku K. K. makes, and surface tension is 24.9mN/m) of surface tension modifier, obtain conductive ink (below, claim " conductive ink B ").The surface tension of this conductive ink B is 41.8mN/m, and the viscosity in the time of 25 ℃ is 10.5cP.
Below, carry out similarly to Example 5, when making Wiring pattern, can not stop up inkjet nozzle and printing conductive printing ink B.And can print continuously more than 50 times.
In addition, during with observation by light microscope resulting wiring pattern, not observing dispersing of broken string or printing ink on Wiring pattern, is good Wiring pattern.In addition, make electrode film similarly to Example 1, the ratio resistance of mensuration is 2.3 * 10
-2Ω cm.In addition, the tack result who estimates above-mentioned electrode film similarly to Example 5 has good tack for classification 0.In addition, this electrode film is used ultrasonic waves for cleaning 10 minutes in water, use ultrasonic waves for cleaning 10 minutes then in acetone, the result does not observe peeling off of electrode film fully.With above-mentioned performance evaluation result etc., be shown in Table 1 with other embodiment and comparative example.
Embodiment 7
Among this embodiment, use plating inorganic oxide particle silver powder as the particle metal powder.Below the preparation of plating inorganic oxide particle silver powder is described.Be to inject the 10L pure water in the container of 20L toward capacity, mixing speed with 200rpm stirs on one side, (Mitsu Mining ﹠ Smelting Co., Ltd makes slowly to add 4000g particulate silver powder on one side, the average primary particle diameter is 0.3 μ m), stir after 20 minutes, (Nissan Chemical Ind Ltd makes, ス ノ one テ Star Network ス 0 toward the cataloid that wherein adds 200g, 20 weight %, the average grain diameter of primary particle is 20nm), continue stirring and obtained dispersion liquid in 20 minutes.
Next,, use emulsify at a high speed dispersion machine T.K.filmix to carry out continuous mixed processing, obtain the cataloid slurries of blending state in particulate silver powder equably in order to make cataloid equably in the particulate silver powder of blending in this dispersion liquid.Next, use vacuum drier, the temperature in drying machine is 50 ℃, and vacuum degree is under the following condition of 50Torr these slurries to be carried out dried 24 hours, obtains the dried powder of set silicon dioxide on the particle surface of particulate silver powder.Next, use Henschel mixer (Mitsui Mining Co Ltd. BJ Offc's manufacturings) with this dried powder pulverizing after, use the screen cloth of 20 μ m to carry out gradation sizing and remove thick particle.Next, in order to improve the silicon dioxide that on the silver particles surface of the powder by 20 μ m sieve, exists and the tack on silver particles surface, further use vacuum drier, in vacuum degree is below the 10Torr, dry built-in temperature is a heat treated 24 hours under 70 ℃ the condition, obtain applying silicon oxide silver powder (below, be called " silver powder ").This silver powder is for adhering to the silver powder of silicon dioxide on the particle surface of silver-colored particulate.
Be to add the pure water of 0.7L in the container of 1L toward capacity as solvent, with the mixing speed of 200rpm stir on one side, slowly add the above-mentioned silver powder of 300g on one side, add the 40.3g dispersant again, stir and obtained slurries in 20 minutes.
Next, after use emulsify at a high speed dispersion machine T.K.filmix (Tokushu Kika Kogyo K.K's manufacturing) carries out continuous dispersion treatment to these slurries, add the 0.96L pure water and obtain the slurries that silver concentration is 15 weight %.
Next, remove the above particle of 1 μ m that contains in these slurries, obtain filtrate (below, be called " water-based silver slurry ") with similarly to Example 5 cartridge filter and mixed cellulose ester type membrane filter.
Then, in above-mentioned water-based silver slurry, add the 2-n-butoxy ethanol of 188.9g with respect to filtrate as surface tension modifier, mixing speed with 200rpm stirred 30 minutes, add the lactic acid titanium of 65.8g then as the tack reinforcing agent, stirred 30 minutes with the mixing speed of 200rpm then, obtain conductive ink (below, be called " conductive ink C ").The surface tension of this conductive ink C that measures is 34.8mN/m, and the viscosity in the time of 25 ℃ is 10.8cP.
Below make Wiring pattern similarly to Example 5, the result can not stop up inkjet nozzle and printing conductive printing ink C.And, can print continuously more than 50 times.
In addition, during with observation by light microscope resulting wiring pattern, not observing dispersing of broken string or printing ink on Wiring pattern, is good Wiring pattern.In addition, make electrode film similarly to Example 5, the ratio resistance of mensuration is 3.5 * 10
-4Ω cm.In addition, estimate the tack of above-mentioned electrode film similarly to Example 1, the evaluation result of tack has good tack for classification 0.In addition, this electrode film is used ultrasonic waves for cleaning 10 minutes in water, use ultrasonic waves for cleaning 10 minutes then in acetone, the result does not observe peeling off of electrode film fully.With above-mentioned performance evaluation result etc., be shown in Table 1 with other embodiment and comparative example.
Comparative example 1
Except omit adding the 2-n-butoxy ethanol, obtain conductive ink D (below, be called " conductive ink D ") similarly to Example 5.In addition, the surface tension of this conductive ink D is 53.1mN/m, and the viscosity in the time of 25 ℃ is 10.4cP.When making Wiring pattern similarly to Example 5, conductive ink D stops up inkjet nozzle after printing 5 times, can not print continuously.In addition, during with the observation by light microscope Wiring pattern, on Wiring pattern, observe broken string, can not obtain good Wiring pattern.
In addition, attempt to make similarly to Example 5 electrode film, but poor to the wetability of glass substrate, can not form electrode film.With above-mentioned performance evaluation result etc., be shown in Table 1 with other embodiment.
Table 1
| Embodiment 5 | Embodiment 6 | Embodiment 7 | Comparative example 1 | ||
| Metal powder | Nickel | Nickel | Silver | Nickel | |
| The tack reinforcing agent | The lactic acid titanium | The lactic acid titanium | The lactic acid titanium | The lactic acid titanium | |
| Surface tension modifier | The 2-n-butoxy ethanol | The 1-butanols | The 2-n-butoxy ethanol | Do not have | |
| Surface tension | mN/m | 32.5 | 41.8 | 34.8 | 53.1 |
| Viscosity | cP | 10.8 | 10.5 | 10.8 | 10.4 |
| The ink jet printing experiment | The obstruction of inkjet nozzle | Do not have | Do not have | Do not have | Have |
| The broken string of distribution | Do not have | Do not have | Do not have | Have | |
| The electrode film characteristic | The resistance value of electrode film | 1.8×10 -3 | 2.3×10 -2 | 3.5×10 -4 | Can not make electrode film |
| Tack (JIS K 5600) | Classification 0 | Classification 0 | Classification 0 | Can not make electrode film | |
Utilize possibility on the industry
Conductive ink of the present invention is excellent with the tack of various base materials, and can form the conductive metal printing ink of meticulous distribution or electrode. In addition, conductive ink of the present invention is applicable to using ink-jetting style or point gum machine mode, forming the conductive ink of the purposes of meticulous distribution or electrode at substrate. Even use ink-jetting style etc., this conductive metal printing ink is by using the additive of tack reinforcing agent etc., and is excellent with the tack of various base materials, and can form meticulous distribution or electrode. Therefore, can form circuit at glass substrate, or can use silver paste or the formed circuit of copper cream or use the transparency electrode etc. of ITO to form distribution, electrode or holding circuit or protection tunicle. Therefore, the manufacture process that can be used for liquid crystal display etc. As mentioned above, on market, also occur to use dispensing machine or ink discharge device printed with fine distribution or electrode, can guarantee the conductive ink with the tack of various substrates, thereby make conductive ink of the present invention obtain tremendous being widely used.
Claims (10)
1. conductive ink, it contains solvent, metal powder, tack reinforcing agent, it is characterized in that, and above-mentioned tack reinforcing agent is to be selected from the group of being made up of silane coupling agent, titanium coupling agent, zirconium coupling agent, aluminium coupling agent one or more.
2. conductive ink according to claim 1 is characterized in that, uses surface tension modifier that the surface tension of above-mentioned solvent is adjusted into 15mN/m～50mN/m.
3. conductive ink according to claim 2, wherein, above-mentioned surface tension modifier is 100 ℃～300 ℃ alcohol, one or more surface tension modifier that combined in the group that glycol is formed for being selected from by the boiling point under the normal pressure.
4. according to any described conductive ink in the claim 1～3, it is characterized in that above-mentioned solvent is that being selected from by the boiling point under the normal pressure is in the group formed of water, alcohols, saturated hydrocarbons below 300 ℃ one or more.
5. according to any described conductive ink in the claim 1～4, wherein, above-mentioned metal powder is selected from nickel powder, silver powder, bronze, platinum powder, copper powder, palladium powder, and the primary particle diameter of this metal powder is below the 500nm.
6. conductive ink according to claim 5, wherein, the maximum particle diameter of the aggregated particle that contains in the above-mentioned metal powder is below the 0.8 μ m.
7. according to any described conductive ink in the claim 1～6, wherein, above-mentioned metal powder is for being attached with the plating inorganic oxide nickel powder of insoluble inorganic oxide on its powder surface.
8. conductive ink according to claim 7 is characterized in that, above-mentioned insoluble inorganic oxide is to contain the oxide that is selected from least a element in the group of being made up of silicon dioxide, aluminium oxide, zirconia and titanium oxide.
9. according to any described conductive ink in the claim 1～9, wherein, interpolation will be selected from (a) polyacrylic acid, its ester or its salt as dispersant; (b) one or more materials that combined of any group in (a)～(c) of the ammonium hydroxide that replaces of organic group and the amines that (c) contains hydroxyl.
10. according to any described conductive ink in the claim 1～9, wherein, the viscosity of this conductive ink in the time of 25 ℃ is below the 60cP.
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| JP2004296987 | 2004-10-08 | ||
| JP296987/2004 | 2004-10-08 | ||
| JP303863/2004 | 2004-10-19 |
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| CN102666747A (en) * | 2009-08-26 | 2012-09-12 | Lg化学株式会社 | Conductive metal ink composition and method for forming a conductive pattern |
| CN101691458B (en) * | 2007-12-10 | 2013-02-13 | 精工爱普生株式会社 | Conductive pattern formation ink, method of forming conductive pattern, conductive pattern and wiring substrate |
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| CN105990075B (en) * | 2015-03-16 | 2018-06-01 | 阿尔卑斯电气株式会社 | Thermal Cutoffs ink, Thermal Cutoffs and its manufacturing method and heater |
| CN106653146A (en) * | 2015-11-04 | 2017-05-10 | 株式会社则武 | Electrically conductive paste and method for forming conductive film |
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