JP6530512B2 - 金属ナノ粒子の分散物 - Google Patents
金属ナノ粒子の分散物 Download PDFInfo
- Publication number
- JP6530512B2 JP6530512B2 JP2017561270A JP2017561270A JP6530512B2 JP 6530512 B2 JP6530512 B2 JP 6530512B2 JP 2017561270 A JP2017561270 A JP 2017561270A JP 2017561270 A JP2017561270 A JP 2017561270A JP 6530512 B2 JP6530512 B2 JP 6530512B2
- Authority
- JP
- Japan
- Prior art keywords
- dispersion
- metal nanoparticles
- weight
- acid
- vinylidene chloride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000006185 dispersion Substances 0.000 title claims description 91
- 239000002082 metal nanoparticle Substances 0.000 title claims description 81
- 229910052751 metal Inorganic materials 0.000 claims description 43
- 239000002184 metal Substances 0.000 claims description 43
- 229920001577 copolymer Polymers 0.000 claims description 39
- 150000001875 compounds Chemical class 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 25
- -1 alkyl methacrylate Chemical compound 0.000 claims description 24
- 229920000728 polyester Polymers 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 22
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 claims description 20
- 229920000642 polymer Polymers 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 20
- 239000011230 binding agent Substances 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- 239000000178 monomer Substances 0.000 claims description 13
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 12
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical group ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims description 12
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 10
- 230000002378 acidificating effect Effects 0.000 claims description 9
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 8
- 230000002708 enhancing effect Effects 0.000 claims description 8
- 125000005250 alkyl acrylate group Chemical group 0.000 claims description 7
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 6
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 5
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 5
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 5
- 239000011976 maleic acid Substances 0.000 claims description 5
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- OFNISBHGPNMTMS-UHFFFAOYSA-N 3-methylideneoxolane-2,5-dione Chemical compound C=C1CC(=O)OC1=O OFNISBHGPNMTMS-UHFFFAOYSA-N 0.000 claims description 2
- GYCMBHHDWRMZGG-UHFFFAOYSA-N Methylacrylonitrile Chemical compound CC(=C)C#N GYCMBHHDWRMZGG-UHFFFAOYSA-N 0.000 claims description 2
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims description 2
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 claims description 2
- 150000007522 mineralic acids Chemical class 0.000 claims description 2
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 42
- 239000000976 ink Substances 0.000 description 37
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 34
- 229910052709 silver Inorganic materials 0.000 description 34
- 239000004332 silver Substances 0.000 description 34
- 238000000576 coating method Methods 0.000 description 28
- 238000007639 printing Methods 0.000 description 27
- 239000011248 coating agent Substances 0.000 description 24
- 239000002270 dispersing agent Substances 0.000 description 20
- 239000012530 fluid Substances 0.000 description 19
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 16
- 239000004094 surface-active agent Substances 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 14
- 238000001723 curing Methods 0.000 description 12
- 239000000203 mixture Substances 0.000 description 12
- 125000004432 carbon atom Chemical group C* 0.000 description 11
- 239000002105 nanoparticle Substances 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 125000003118 aryl group Chemical group 0.000 description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 229920000139 polyethylene terephthalate Polymers 0.000 description 9
- 239000005020 polyethylene terephthalate Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 8
- 125000000217 alkyl group Chemical group 0.000 description 8
- 125000004429 atom Chemical group 0.000 description 8
- 229920005862 polyol Polymers 0.000 description 8
- 150000003077 polyols Chemical class 0.000 description 8
- 230000000087 stabilizing effect Effects 0.000 description 8
- 239000000654 additive Substances 0.000 description 7
- 238000009835 boiling Methods 0.000 description 7
- 125000001072 heteroaryl group Chemical group 0.000 description 7
- 239000003960 organic solvent Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 125000000547 substituted alkyl group Chemical group 0.000 description 6
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 5
- 239000000443 aerosol Substances 0.000 description 5
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 5
- 239000002612 dispersion medium Substances 0.000 description 5
- 238000000265 homogenisation Methods 0.000 description 5
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 5
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 5
- 150000002576 ketones Chemical group 0.000 description 5
- LAVARTIQQDZFNT-UHFFFAOYSA-N 1-(1-methoxypropan-2-yloxy)propan-2-yl acetate Chemical compound COCC(C)OCC(C)OC(C)=O LAVARTIQQDZFNT-UHFFFAOYSA-N 0.000 description 4
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 4
- ZPVFWPFBNIEHGJ-UHFFFAOYSA-N 2-octanone Chemical compound CCCCCCC(C)=O ZPVFWPFBNIEHGJ-UHFFFAOYSA-N 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical group N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical group CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 4
- 125000003342 alkenyl group Chemical group 0.000 description 4
- 125000002877 alkyl aryl group Chemical group 0.000 description 4
- 125000003710 aryl alkyl group Chemical group 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 150000002148 esters Chemical group 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- 125000000623 heterocyclic group Chemical group 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 238000007641 inkjet printing Methods 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 210000002381 plasma Anatomy 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 238000007650 screen-printing Methods 0.000 description 4
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000000080 wetting agent Substances 0.000 description 4
- 125000004169 (C1-C6) alkyl group Chemical group 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 125000002373 5 membered heterocyclic group Chemical group 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 150000001299 aldehydes Chemical group 0.000 description 3
- 125000000304 alkynyl group Chemical group 0.000 description 3
- 150000001408 amides Chemical group 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 3
- 125000005842 heteroatom Chemical group 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 125000001624 naphthyl group Chemical group 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
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- 230000008569 process Effects 0.000 description 3
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- 239000000126 substance Substances 0.000 description 3
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 3
- 150000003568 thioethers Chemical group 0.000 description 3
- CBECDWUDYQOTSW-UHFFFAOYSA-N 2-ethylbut-3-enal Chemical compound CCC(C=C)C=O CBECDWUDYQOTSW-UHFFFAOYSA-N 0.000 description 2
- GASMGDMKGYYAHY-UHFFFAOYSA-N 2-methylidenehexanamide Chemical compound CCCCC(=C)C(N)=O GASMGDMKGYYAHY-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
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical group CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical group [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 239000001361 adipic acid Substances 0.000 description 2
- 235000011037 adipic acid Nutrition 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
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- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 150000002009 diols Chemical class 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
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- 239000010931 gold Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
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- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 2
- 125000002883 imidazolyl group Chemical group 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 125000000842 isoxazolyl group Chemical group 0.000 description 2
- 125000005647 linker group Chemical group 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 125000002950 monocyclic group Chemical group 0.000 description 2
- YRVUCYWJQFRCOB-UHFFFAOYSA-N n-butylprop-2-enamide Chemical compound CCCCNC(=O)C=C YRVUCYWJQFRCOB-UHFFFAOYSA-N 0.000 description 2
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- JTHNLKXLWOXOQK-UHFFFAOYSA-N n-propyl vinyl ketone Natural products CCCC(=O)C=C JTHNLKXLWOXOQK-UHFFFAOYSA-N 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- 238000007645 offset printing Methods 0.000 description 2
- WCPAKWJPBJAGKN-UHFFFAOYSA-N oxadiazole Chemical compound C1=CON=N1 WCPAKWJPBJAGKN-UHFFFAOYSA-N 0.000 description 2
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- 239000001301 oxygen Substances 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000004417 polycarbonate Substances 0.000 description 2
- 229920000515 polycarbonate Polymers 0.000 description 2
- 125000003367 polycyclic group Chemical group 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
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- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 239000005033 polyvinylidene chloride Substances 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 125000000714 pyrimidinyl group Chemical group 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41F—PRINTING MACHINES OR PRESSES
- B41F17/00—Printing apparatus or machines of special types or for particular purposes, not otherwise provided for
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/16—Solid spheres
- C08K7/18—Solid spheres inorganic
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
-
- 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
- C09D11/00—Inks
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Description
& Co.KGaA,Weinheimにより編纂された´Approaches to the synthesis and Characterization of Spherical and Anisotropic Silver Nanomaterials(球形および異方性銀ナノ材料の合成法および特徴付け)´,Metallic Nanomaterial Vol.1.,中に開示された通りの、いわゆるポリオール合成によるか、ポリオール合成法の派生法(a derivative)によるか、または様々な還元剤の存在下における金属塩の現位置(in−situ)還元による。このような方法は例えば、特許文献1〜17に開示されている(特許文献1〜17参照)。
ーティング液中に存在するすべての成分と相容性のポリマー鎖をもつ。
of powder)および(c)付着性増強添加剤(adhesion promoting additive)、の混合物を含む、支持体上への付着のための導電インク組成物を開示している(特許文献24参照)。付着性増強添加剤はポリビニリデンクロリド、ポリビニルクロリド、ポリエチレンビニルクロリド、ポリエステル、それらのコポリマーから選択されるポリマーまたは第一ジアミンであることができる。
それをもって、様々な支持体に対して改善された付着性をもつ高度に導電性の被膜またはパターンを得ることができる、安定な金属ナノ粒子の分散物を提供することが本発明の目的である。この目的は、請求項1に規定される金属ナノ粒子の分散物により実現される。
定義
本明細書に使用される用語のポリマーサポート(support)および箔(foil)は、1枚以上の接着層(adhesion layers)、例えば下塗り層(subbing layers)を伴うことができる自立性の(self−supporting)ポリマー基材のシートを意味する。サポートおよび箔は通常、押し出し成形(extrusion)により製造される。
構造が炭素のみでできている同素環式基(homocyclic group)である。別記されない限り、置換もしくは未置換複素環式基は好適には酸素原子、窒素原子、硫黄原子、セレン原子またはそれらの組み合わせ物から選択される1、2、3もしくは4個のヘテロ原子により置換された、好適には5員もしくは6員環である。
本発明に従う金属ナノ粒子の分散物は金属ナノ粒子、結合剤および液体キャリアを含み、その結合剤が、結合剤の総重量に基づいて90重量%以下のビニリデンクロリドを含むビニリデンクロリド・コポリマーであることを特徴とする。
金属ナノ粒子の分散物は、結合剤として、結合剤の総合重量に基づいて90重量%以下のビニリデンクロリドを含むビニリデンクロリド・コポリマーを含む。ビニリデンクロリドの量が結合剤の総重量に基づいて90重量%を超える時は、結合剤の結晶化度(crystallinity)が高くなり過ぎ、液体キャリア中の低い溶解度をもたらす。更なるモノマーとのビニリデンクロリドの共重合が、コポリマーを、より非晶質にさせ、従って、液体キャリア中に、更に可溶性にさせる。
クリロニトリル、メタクリロニトリル、マレイン酸、無水マレイン酸、イタコン酸、無水イタコン酸およびクロトン酸よりなる群から選択される更なるモノマーを含む。
に従うモノマーのようなマレイン酸または無水マレイン酸の誘導体もまた、ビニリデンクロリド・コポリマーの更なるモノマーとして使用することができる。
もよいアルキル基,または1〜5個の炭素原子を含む、場合により置換されていてもよいアルケニル基を表わし
Lは1〜5個の炭素原子を含むアルキレン基、5までのエチレングリコール単位を含むポリエチレングリコール、または5までのプロピレングリコール単位を含むポリプロピレングリコールよりなる群から選択される結合基(linking group)を表わす]
に従うモノマーのようなコハク酸または無水コハク酸の誘導体もまた、ビニリデンクロリド・コポリマーの更なるモノマーとして使用することができる。
ある時は、付着性の改善を認めることができない。
本発明の金属ナノ粒子の分散物は金属ナノ粒子を含む。
金属ナノ粒子の分散物は液体キャリアを含む。
金属ナノ粒子の分散物は好適には界面活性剤を含む。様々な界面活性剤を使用することができる。しかし、Disperbyk 2151、Disperbyk 2025およびDiserbyk 2155よりなる群から選択される界面活性剤の金属ナノ粒子の分散物への添加が、特にITO(インジウム錫酸化物)支持体(substrates)上への分散物の付着性の更なる改善をもたらすことが確認された。特に優れた結果はDisperbyk 2151を使用して得られる。
付着性増強化合物の添加は様々な支持体に対する付着性を更に改善することができることが確認された。
の実質的に改善された付着性を特徴として示すことが確認された。
(a)2000〜10,000の分子量(Mn)、20〜75のヒドロキシル価(hydroxyl number)および15〜25の酸価(acid value)をもつポリエステル、ここで該ポリエステルは
(i)ジオールとトリオールの混合物を含むポリオール成分、
(ii)アルファ−、ベータ−エチレン状不飽和ポリカルボン酸を含む多酸(polyacid)成分:
の縮合物である、並びに
(b)リン酸(phosphorus acid)、
の反応生成物である。
本発明に従う金属ナノ粒子の分散物は式VII、VIII、IXまたはX、
Qは置換もしくは未置換の5もしくは6員の複素環式芳香環を形成するために必要な原子を表わし、
Mはプロトン、一価のカチオン基、アルキル基、ヘテロアルキル基およびアシル基よりなる群から選択され、
R9およびR10は水素、置換もしくは未置換アルキル基、置換もしくは未置換アルケニル基、置換もしくは未置換アルキニル基、置換もしくは未置換アルカリール基、置換もしくは未置換アラルキル基、置換もしくは未置換アリールもしくはヘテロアリール基、ヒドロキシル基、チオエーテル、エーテル、エステル、アミド、アミン、ハロゲン、ケトンおよびアルデヒドよりなる群から独立して選択され、
R9およびR10は5〜7員環を形成するために必要な原子を表わすことができ、
R11〜R13は水素、置換もしくは未置換アルキル基、置換もしくは未置換アルケニル基、置換もしくは未置換アルキニル基、置換もしくは未置換アルカリール基、置換もしくは未置換アラルキル基、置換もしくは未置換アリールもしくはヘテロアリール基、ヒドロキシル基、チオール、チオエーテル、スルホン、スルホキシド、エーテル、エステル、アミド、アミン、ハロゲン、ケトン、アルデヒド、ニトリルおよびニトロ基よりなる群から独立して選択され、
R12およびR13は5〜7員環を形成するために必要な原子を表わすことができる]に従う分散物安定化合物(DSC)を含むことができる。
−1H−テトラゾール−1−イル−アセタミド、5−ヘプチル−2−メルカプト−1,3,4−オキサジアゾール、1−フェニル−5−メルカプトテトラゾール、5−メチル−1,2,4−トリアゾロ−(1,5−a)プリミジン(primidine)−7−オールおよびS−[5−[(エトキシカルボニル)アミノ]−1,3,4−チアジアゾール−2−イル]O−エチルチオカーボネートよりなる群から選択される。
金属ナノ粒子の分散物はポリマーの分散剤を含むことができる。
コーティングまたは印刷特性を最適化するために、そして更に、それがそのために使用される適用に応じて、前記の金属ナノ粒子の分散物に、還元剤、湿潤剤(wetting)/均展材(levelling agents)、除湿剤(dewetting agent)、レオロジー修飾剤、接着剤(adhesion agents)、粘性付与剤、保湿剤(humectants)、噴射剤、硬化剤、殺生物剤(biocides)または抗酸化剤のような添加剤を添加することができる。
ることができる化合物を金属ナノ粒子の分散物に添加することは好都合かも知れない。このような金属ナノ粒子の分散物から形成される層またはパターンの、より高い導電率および/またはより低い硬化温度が認められた。
に従う化合物を含む金属ナノ粒子の分散物を使用する時にも得ることができる。
本発明に従う金属ナノ粒子の分散物の調製は典型的には、撹拌、高剪断混合、超音速処理またはそれらの組み合わせのような均質化法(homogenization technique)を使用することによる、金属ナノ粒子への、液体キャリア、ビニリデンコポリマーおよび場合により使用される添加剤の、添加を含む。
は好適には、25℃において、90s-1の剪断速度で測定されて、10〜200mPa.s間、より好適には25〜150mPa.s間、最も好適には50〜100mPa.s間の粘度を有する。
金属ナノ粒子の分散物から印刷または塗布される薄層またはパターンは、従来の金属の印刷液またはコーティング液を使用して得られるものに比較して、より低い焼結温度において導電性にされることができる。従って、本発明の金属の印刷液またはコーティング液から製造される導電薄層またはパターンは、例えばPETのような、高温における熱処理に耐えることができない柔軟なサポート(supports)上に塗布または印刷されることができる。
野で周知である。例えば、このような下塗り層の調製は、米国特許第3649336号および英国特許第1441591号明細書に開示されている。
層またはパターンがサポート上に適用された後に、硬化工程(curing step)とも呼ばれる焼結工程(sintering step)が実施される。この焼結工程
期間中に、溶媒は蒸発し、金属の粒子は一緒に焼結する。金属の粒子間に一旦、連続的な浸透性(percolating)網目が形成されると、層またはパターンが導電性になる。従来の焼結は典型的には、熱を適用することにより実施される。焼結温度および時間は、使用されるサポートおよび金属層またはパターンの組成に左右される。金属層を硬化するための焼結工程は250℃未満、好適には200℃未満、より好適には180℃未満、最も好適には160℃未満の温度で実施することができる。
本発明に従う金属ナノ粒子はあらゆる知られた調製法により調製されることができる。
以下の実施例中に使用されたすべての材料は、別記されない限りALDRICH CHEMICAL Co.(ベルギー)およびACROS(ベルギー)のような、標準製造元から容易に入手可能であった。使用された水は脱イオン水であった。
銀被膜の導電率
銀被膜の表面抵抗(SER)は、四点の同一線上(collinear)プローブを使用して測定した。表面またはシート抵抗は以下の式:
SER=(π/ln2)*(V/I)
[式中、
SERはΩ/□で表される層の表面抵抗である;
πはほぼ3.14に等しい数学の定数である;
ln2はほぼ0.693に等しい、値2の自然対数に等しい数学の定数である;
Vは四点プローブ測定装置の電圧計により測定される電圧である;
Iは四点プローブ測定装置により測定されるソース電流である]
により計算された。
を使用して、銀のバルクの導電性の百分率として導電率を計算することにより決定した。
異なる支持体上への銀被膜の付着性を、ASTM D3359に従うテープ試験により評価した。
評価は 0(非常に良好な付着性)から5(非常に低い付着性)までの採点をもたらす。
78.0gの酸化銀を275.0gのペンタン酸および401.0gの2−ピロリドンを含む1lの反応器に、撹拌しながら緩徐に添加した。混合物の温度は25℃に維持された。
銀インクSI−01〜SI−05を、透明溶液が得られるまで、撹拌しながら、表1の銀以外の成分と一緒に混合することにより調製した。次に銀ナノ粒子の分散物NPD−01を透明溶液に添加し、次に高剪断均質化を実施した。
銀インクSI−06〜SI−24を、透明溶液が得られるまで、撹拌しながら、表3の銀以外の成分と一緒に混合することにより調製した。次に銀ナノ粒子の分散物NPD−01を透明溶液に添加し、次に高剪断均質化を実施した。
Claims (9)
- 金属ナノ粒子、結合剤および液体キャリアと、付着性増強化合物として、酸性ポリエステルとを含み、結合剤が、結合剤の総重量に基づいて90重量%以下のビニリデンクロリドを含むビニリデンクロリド・コポリマーであることを特徴とする、金属ナノ粒子の分散物。
- ビニリデンクロリド・コポリマーが、ビニルクロリド、アルキルアクリレート、アルキ
ルメタクリレート、ビニルエーテル、ビニルアセテート、ビニルアルコール、アクリロニトリル、メタクリロニトリル、マレイン酸、無水マレイン酸、イタコン酸、無水イタコン酸およびクロトン酸よりなる群から選択される更なるモノマーを含む、請求項1記載の金属ナノ粒子の分散物。 - ビニリデンクロリド・コポリマーが、ビニルクロリド、アクリロニトリル、無水マレイン酸、アルキルアクリレートおよびアルキルメタクリレートよりなる群から選択される更なるモノマーを含む、請求項1記載の金属ナノ粒子の分散物。
- ビニリデンクロリド・コポリマーが、40〜90重量%のビニリデンクロリド、0.5〜50重量%のビニルクロリドおよび0.5〜5重量%のアクリロニトリルを含む、請求項1記載の金属ナノ粒子の分散物。
- ビニリデンクロリド・コポリマーの量が分散物の総量に対して0.25〜5.0重量%である、請求項1記載の金属ナノ粒子の分散物。
- 酸性ポリエステルの量が分散物の総量に対して0.01〜10.0重量%である、請求項1記載の金属ナノ粒子の分散物。
- 分散物の総重量に対して0.01〜0.1重量%の無機酸、または、金属ナノ粒子の分散物から形成される金属層またはパターンの硬化期間中にそのような酸を生成することができる化合物を更に含む、請求項1記載の金属ナノ粒子の分散物。
- 支持体(substrate)上に、請求項1に規定されるような金属ナノ粒子の分散物を適用する工程と、それに続く焼結工程とを含む、金属層またはパターンを調製する方法。
- 支持体が、紙の支持体、ガラスの支持体、プライマー層を伴うもしくは伴わないポリマーの支持体、または、ポリマーサポートもしくはガラスサポート上のITO層である、請求項8記載の方法。
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EP15169396.7A EP3099145B1 (en) | 2015-05-27 | 2015-05-27 | Method of preparing a silver layer or pattern comprising a step of applying a silver nanoparticle dispersion |
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PCT/EP2016/061750 WO2016189015A1 (en) | 2015-05-27 | 2016-05-25 | A metallic nanoparticle dispersion |
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