JP5526578B2 - Method for producing particle dispersion and method for producing oxide semiconductor particles, metal particles, and metalloid particles using the particle dispersion - Google Patents
Method for producing particle dispersion and method for producing oxide semiconductor particles, metal particles, and metalloid particles using the particle dispersion Download PDFInfo
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- JP5526578B2 JP5526578B2 JP2009089331A JP2009089331A JP5526578B2 JP 5526578 B2 JP5526578 B2 JP 5526578B2 JP 2009089331 A JP2009089331 A JP 2009089331A JP 2009089331 A JP2009089331 A JP 2009089331A JP 5526578 B2 JP5526578 B2 JP 5526578B2
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- Prior art keywords
- acid
- particle dispersion
- oxide
- particle
- fluorine
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- 239000002245 particle Substances 0.000 title claims description 353
- 239000006185 dispersion Substances 0.000 title claims description 266
- 238000004519 manufacturing process Methods 0.000 title claims description 35
- 239000004065 semiconductor Substances 0.000 title claims description 23
- 239000002923 metal particle Substances 0.000 title claims description 20
- 229910052752 metalloid Inorganic materials 0.000 title claims description 9
- 150000002738 metalloids Chemical class 0.000 title claims description 9
- 239000000203 mixture Substances 0.000 claims description 90
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 72
- 239000003638 chemical reducing agent Substances 0.000 claims description 41
- 239000011521 glass Substances 0.000 claims description 41
- 239000002904 solvent Substances 0.000 claims description 41
- 229910052751 metal Inorganic materials 0.000 claims description 40
- 239000002184 metal Substances 0.000 claims description 40
- 239000011787 zinc oxide Substances 0.000 claims description 36
- 229910052738 indium Inorganic materials 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 25
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 claims description 24
- 229910003437 indium oxide Inorganic materials 0.000 claims description 23
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 23
- 229910052718 tin Inorganic materials 0.000 claims description 21
- 150000001875 compounds Chemical class 0.000 claims description 18
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 18
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 18
- 229910001887 tin oxide Inorganic materials 0.000 claims description 18
- 150000002737 metalloid compounds Chemical class 0.000 claims description 17
- 229910052725 zinc Inorganic materials 0.000 claims description 17
- 239000011701 zinc Substances 0.000 claims description 17
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 16
- 239000011737 fluorine Substances 0.000 claims description 16
- 229910052731 fluorine Inorganic materials 0.000 claims description 16
- 150000002736 metal compounds Chemical class 0.000 claims description 15
- -1 methacryloyl group Chemical group 0.000 claims description 15
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 14
- 150000007524 organic acids Chemical class 0.000 claims description 13
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 12
- 229910052737 gold Inorganic materials 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 229910052709 silver Inorganic materials 0.000 claims description 12
- 229910052719 titanium Inorganic materials 0.000 claims description 12
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052787 antimony Inorganic materials 0.000 claims description 10
- 229910052733 gallium Inorganic materials 0.000 claims description 10
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 10
- 150000002902 organometallic compounds Chemical class 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- XDOFQFKRPWOURC-UHFFFAOYSA-N 16-methylheptadecanoic acid Chemical compound CC(C)CCCCCCCCCCCCCCC(O)=O XDOFQFKRPWOURC-UHFFFAOYSA-N 0.000 claims description 8
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 150000002739 metals Chemical class 0.000 claims description 8
- UTOPWMOLSKOLTQ-UHFFFAOYSA-N octacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O UTOPWMOLSKOLTQ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052763 palladium Inorganic materials 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 229910052707 ruthenium Inorganic materials 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 229910052702 rhenium Inorganic materials 0.000 claims description 7
- 229910052703 rhodium Inorganic materials 0.000 claims description 7
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 6
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 6
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical group CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 claims description 6
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 6
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 6
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 6
- 235000005985 organic acids Nutrition 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
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 4
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- WYSNBIRBWGEORT-UHFFFAOYSA-N [F].[Ce] Chemical compound [F].[Ce] WYSNBIRBWGEORT-UHFFFAOYSA-N 0.000 claims description 4
- COFWJARDGQSZLX-UHFFFAOYSA-N [F].[Sb] Chemical compound [F].[Sb] COFWJARDGQSZLX-UHFFFAOYSA-N 0.000 claims description 4
- YDUSRVDVRPPCFI-UHFFFAOYSA-N [F].[Zn] Chemical compound [F].[Zn] YDUSRVDVRPPCFI-UHFFFAOYSA-N 0.000 claims description 4
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 claims description 4
- 235000020661 alpha-linolenic acid Nutrition 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 4
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 claims description 4
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- ZULTVNRFZRQYKL-UHFFFAOYSA-M fluorotin Chemical compound [Sn]F ZULTVNRFZRQYKL-UHFFFAOYSA-M 0.000 claims description 4
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 claims description 4
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- 235000020778 linoleic acid Nutrition 0.000 claims description 4
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 claims description 4
- 229960004488 linolenic acid Drugs 0.000 claims description 4
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 4
- 235000021313 oleic acid Nutrition 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- SECPZKHBENQXJG-FPLPWBNLSA-N palmitoleic acid Chemical compound CCCCCC\C=C/CCCCCCCC(O)=O SECPZKHBENQXJG-FPLPWBNLSA-N 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- ZDPHROOEEOARMN-UHFFFAOYSA-N undecanoic acid Chemical compound CCCCCCCCCCC(O)=O ZDPHROOEEOARMN-UHFFFAOYSA-N 0.000 claims description 4
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 3
- 229940114072 12-hydroxystearic acid Drugs 0.000 claims description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 3
- 239000005639 Lauric acid Substances 0.000 claims description 3
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 3
- 235000021314 Palmitic acid Nutrition 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
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- MHVJRKBZMUDEEV-UHFFFAOYSA-N (-)-ent-pimara-8(14),15-dien-19-oic acid Natural products C1CCC(C(O)=O)(C)C2C1(C)C1CCC(C=C)(C)C=C1CC2 MHVJRKBZMUDEEV-UHFFFAOYSA-N 0.000 claims description 2
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- NJBCRXCAPCODGX-UHFFFAOYSA-N 2-methyl-n-(2-methylpropyl)propan-1-amine Chemical compound CC(C)CNCC(C)C NJBCRXCAPCODGX-UHFFFAOYSA-N 0.000 claims description 2
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 claims description 2
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- 229910052748 manganese Inorganic materials 0.000 claims description 2
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- YWFWDNVOPHGWMX-UHFFFAOYSA-N n,n-dimethyldodecan-1-amine Chemical compound CCCCCCCCCCCCN(C)C YWFWDNVOPHGWMX-UHFFFAOYSA-N 0.000 claims description 2
- NHLUVTZJQOJKCC-UHFFFAOYSA-N n,n-dimethylhexadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCN(C)C NHLUVTZJQOJKCC-UHFFFAOYSA-N 0.000 claims description 2
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- VHOCUJPBKOZGJD-UHFFFAOYSA-N triacontanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O VHOCUJPBKOZGJD-UHFFFAOYSA-N 0.000 description 2
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 2
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- PDDRDHDSORJGMY-UHFFFAOYSA-L 2-methylprop-2-enoate platinum(2+) Chemical compound C(C(=C)C)(=O)[O-].[Pt+2].C(C(=C)C)(=O)[O-] PDDRDHDSORJGMY-UHFFFAOYSA-L 0.000 description 1
- 241000282994 Cervidae Species 0.000 description 1
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- 238000002441 X-ray diffraction Methods 0.000 description 1
- FTCXIBLSBSTMBL-UHFFFAOYSA-N [Au].C(C)C(CN)CCCC Chemical compound [Au].C(C)C(CN)CCCC FTCXIBLSBSTMBL-UHFFFAOYSA-N 0.000 description 1
- AEHOPYFWRSVXFF-UHFFFAOYSA-N [Re].C(CCCCCCCCCCCCCCC)N Chemical compound [Re].C(CCCCCCCCCCCCCCC)N AEHOPYFWRSVXFF-UHFFFAOYSA-N 0.000 description 1
- GNWPDFRZOLWVOI-UHFFFAOYSA-N [Rh].C(CCCCCCCCCCCCC)N Chemical compound [Rh].C(CCCCCCCCCCCCC)N GNWPDFRZOLWVOI-UHFFFAOYSA-N 0.000 description 1
- ODTZBOLRIFTHID-UHFFFAOYSA-N [Sn].C(CCCCCCCCCCC)N Chemical compound [Sn].C(CCCCCCCCCCC)N ODTZBOLRIFTHID-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
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- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZABPGQXWKVZCMK-UHFFFAOYSA-L docosanoate;nickel(2+) Chemical compound [Ni+2].CCCCCCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCCCCCC([O-])=O ZABPGQXWKVZCMK-UHFFFAOYSA-L 0.000 description 1
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- MBLKROWJGMVCRJ-UHFFFAOYSA-N gold propane-1,2-diamine Chemical compound [Au].CC(N)CN MBLKROWJGMVCRJ-UHFFFAOYSA-N 0.000 description 1
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- FRVCGRDGKAINSV-UHFFFAOYSA-L iron(2+);octadecanoate Chemical compound [Fe+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O FRVCGRDGKAINSV-UHFFFAOYSA-L 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Conductive Materials (AREA)
Description
本発明は、酸化物半導体粒子が分散した粒子分散体を製造する方法と、この粒子分散体を乾燥して得られた粉末状の酸化物半導体粒子、金属粒子及び半金属粒子を製造する方法に関するものである。 The present invention relates to a method for producing a method for producing particles dispersion oxide semiconductor particles are dispersed, obtained by drying a particle dispersion of this powder of the oxide semiconductor particles, metal particles and metalloid particles It is about.
従来、1,4-グルコシド結合を有する化合物と金属化合物とを溶媒に溶解し、得られた溶液中の金属イオンを還元し、金属ナノ粒子とする金属ナノ粒子の製造方法（例えば、特許文献１参照。）が開示されている。この金属ナノ粒子の製造方法では、上記溶液を加熱し、その後還元剤を添加することにより、金属イオンを還元する。このように極めて簡便な方法により単分散かつ微細な金属ナノ粒子を製造できるようになっている。 Conventionally, a method for producing metal nanoparticles by dissolving a compound having a 1,4-glucoside bond and a metal compound in a solvent and reducing metal ions in the resulting solution to form metal nanoparticles (for example, Patent Document 1) Reference). In this method for producing metal nanoparticles, the metal ions are reduced by heating the solution and then adding a reducing agent. Thus, monodispersed and fine metal nanoparticles can be produced by a very simple method.
しかし、上記従来の特許文献１に示された金属ナノ粒子の製造方法では、還元反応が有機金属の自己分解に頼っているため、不均一に反応して凝集物が発生し易く、分散体を得ることが難しく、歩留まりが悪いという不具合があった。
本発明の目的は、極めて簡便に、導電性、分散性、分散安定性、透明性、沈降防止性等を付与若しくは改善することができる、粒子分散体の製造方法並びにこの粒子分散体を用いた酸化物半導体粒子、金属粒子及び半金属粒子の製造方法を提供することにある。
However, in the method for producing metal nanoparticles shown in the above-mentioned conventional Patent Document 1, since the reduction reaction relies on the self-decomposition of the organic metal, the reaction tends to occur non-uniformly and aggregates are easily generated. There was a problem that it was difficult to obtain and the yield was poor.
An object of the present invention is to use a method for producing a particle dispersion, which can impart or improve conductivity, dispersibility, dispersion stability, transparency, anti-settling property, and the like, as well as the particle dispersion. The object is to provide a method for producing oxide semiconductor particles, metal particles, and metalloid particles .
本発明の第１の観点は、図１に示すように、有機金属化合物及び有機半金属化合物からなる群より選ばれた１種又は２種以上と還元剤とを混合して混合物を調製する工程と、この混合物を所定の雰囲気中で４０〜３６０℃の温度に加熱した状態に１０分〜５．０時間保持して粒子分散体を得る工程とを含む粒子分散体の製造方法であって、粒子分散体は、溶媒で希釈してコロイド液の状態した場合に、密栓したガラス瓶に入れて４０℃に２週間保持した後の状態において沈殿せずにコロイド液の状態を保つ、粒子分散体の製造方法である。
この第１の観点の粒子分散体の製造方法では、上記混合物を所定の雰囲気中で加熱すると、混合物が化学的に反応しながら有機金属化合物中の金属若しくは金属酸化物又は有機半金属化合物中の半金属又は半金属酸化物が中心となって有機金属化合物又は有機半金属化合物が分解する。この有機金属化合物又は有機半金属化合物の分解により、結合の外れた金属、半金属又はそれらの酸化物生成体からなる粒子の表面に、同様に結合の外れた有機物又はその分解生成物が付くため、導電性、分散性、分散安定性、透明性、沈降防止性等の特性を有する膜として用いられる粒子分散体が得られる。
As shown in FIG. 1, the first aspect of the present invention is a step of preparing a mixture by mixing one or more selected from the group consisting of an organic metal compound and an organic metalloid compound and a reducing agent. And a step of obtaining the particle dispersion by maintaining the mixture in a predetermined atmosphere at a temperature of 40 to 360 ° C. for 10 minutes to 5.0 hours , particle dispersions, when diluted with a solvent to a state of colloid solution, keeping the state of the colloidal solution without precipitation in the state after the holding for 2 weeks put 40 ° C. in stoppered glass bottle, the particle dispersion It is a manufacturing method.
In the method for producing a particle dispersion according to the first aspect, when the mixture is heated in a predetermined atmosphere, the metal or metal oxide in the organometallic compound or the organic semimetal compound in the organometallic compound is reacted while the mixture chemically reacts. The organometallic compound or the organometalloid compound is decomposed mainly by the semimetal or the semimetal oxide. The decomposition of the organometallic compound or the organometalloid compound causes the dissociated organic substance or its decomposition product to be similarly attached to the surface of the particles made of the unbonded metal, semimetal or oxide product thereof. Thus, a particle dispersion used as a film having properties such as conductivity, dispersibility, dispersion stability, transparency, and anti-settling property can be obtained.
本発明の第１の観点の粒子分散体の製造方法では、有機金属化合物及び有機半金属化合物からなる群より選ばれた１種又は２種以上と還元剤とを混合して混合物を調製した後に、この混合物を所定の雰囲気中で４０〜３６０℃の温度に加熱した状態に１０分〜５．０時間保持することにより２週間以上沈殿せずにコロイド液の状態を保つ粒子分散体を得たので、極めて簡便に、導電性、分散性、分散安定性、透明性、沈降防止性等を付与若しくは改善した粒子分散体を得ることができる。 In the method for producing a particle dispersion according to the first aspect of the present invention, after preparing a mixture by mixing one or more selected from the group consisting of an organic metal compound and an organic metalloid compound and a reducing agent. The mixture was kept at a temperature of 40 to 360 ° C. in a predetermined atmosphere for 10 minutes to 5.0 hours to obtain a particle dispersion that maintained a colloidal liquid state without precipitation for more than 2 weeks . Therefore, a particle dispersion imparted or improved with conductivity, dispersibility, dispersion stability, transparency, anti-settling property, etc. can be obtained very simply.
次に本発明を実施するための形態を図面に基づいて説明する。
＜第１の実施の形態＞
図１に示すように、粒子分散体を製造するには、先ず有機金属化合物及び有機半金属化合物からなる群より選ばれた１種又は２種以上と還元剤とを混合して混合物を調製する。上記有機金属化合物に含まれる金属は、Ｃｕ，Ａｕ，Ａｇ，Ｐｔ，Ｐｄ，Ｒｕ，Ｒｈ，Ｒｅ，Ｏｓ，Ｉｒ，Ｓｃ，Ｙ，Ｔｉ，Ｚｒ，Ｖ，Ｎｂ，Ｔａ，Ｃｒ，Ｍｏ，Ｗ，Ｍｎ，Ｆｅ，Ｃｏ，Ｎｉ，Ｚｎ，Ｃｄ，Ａｌ，Ｇａ，Ｉｎ，Ｔｌ，Ｓｎ，Ｐｂ，Ｌａ，Ｃｅ，Ｎｄ，Ｓｍ，Ｅｕ，Ｇｄ，Ｔｂ，Ｅｒ，Ｔｍ及びＹｂからなる群より選ばれた１種又は２種以上の金属、好ましくはＣｕ，Ａｕ，Ａｇ，Ｐｔ，Ｐｄ，Ｒｕ，Ｒｈ，Ｒｅ，Ｔｉ，Ｆｅ，Ｃｏ，Ｎｉ，Ｚｎ，Ｉｎ及びＳｎからなる群より選ばれた１種又は２種以上の金属である。また上記有機半金属化合物に含まれる半金属は、Ｓｉ，Ｇｅ，Ｓｂ及びＢｉからなる群より選ばれた１種又は２種以上の半金属である。
Next, an embodiment for carrying out the present invention will be described with reference to the drawings.
<First Embodiment>
As shown in FIG. 1, in order to produce a particle dispersion, first, one or more selected from the group consisting of an organic metal compound and an organic metalloid compound is mixed with a reducing agent to prepare a mixture. . The metal contained in the organometallic compound is Cu, Au, Ag, Pt, Pd, Ru, Rh, Re, Os, Ir, Sc, Y, Ti, Zr, V, Nb, Ta, Cr, Mo, W, Selected from the group consisting of Mn, Fe, Co, Ni, Zn, Cd, Al, Ga, In, Tl, Sn, Pb, La, Ce, Nd, Sm, Eu, Gd, Tb, Er, Tm and Yb One or more metals, preferably one selected from the group consisting of Cu, Au, Ag, Pt, Pd, Ru, Rh, Re, Ti, Fe, Co, Ni, Zn, In and Sn Two or more metals. The metalloid contained in the organic metalloid compound is one or more metalloids selected from the group consisting of Si, Ge, Sb and Bi.
上記有機金属化合物又は有機半金属化合物の有機成分は、有機酸及びアミンからなる群より選ばれた１種又は２種以上の化合物であり、上記有機酸は、炭素数２〜２９、好ましくは炭素数３〜１８の炭素を含む化合物からなる群より選ばれた１種又は２種以上の化合物であることが好ましい。具体的には、上記有機酸は、リンゴ酸、クエン酸、フマル酸、マレイン酸、酒石酸、酢酸、プロピオン酸、酪酸、イソ酪酸、ビバル酸、吉草酸、イソ吉草酸、カプロン酸、２−エチル酪酸、カプリル酸、ペラルゴン酸、２−エチルヘキサン酸、カプリン酸、ウンデカン酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、イソステアリン酸、アラキン酸、ベヘン酸、リグノセリン酸、セロチン酸、モンタン酸、メリシン酸、リシノール酸、１２−ヒドロキシステアリン酸、ナフテン酸、アビエチン酸、デキストロピマル酸、パルミトレイン酸、オレイン酸、リノール酸及びリノレン酸からなる群より選ばれた１種又は２種以上の有機酸であることが好ましく、更にリンゴ酸、クエン酸、フマル酸、マレイン酸、２−エチルヘキサン酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、イソステアリン酸、１２−ヒドロキシステアリン酸、オレイン酸、リノール酸及びリノレン酸からなる群より選ばれた１種又は２種以上の有機酸であることが好ましい。有機酸は、光重合性化合物であることが好ましい。具体的には、光重合性化合物は、アクリロイル基、メタクリロイル基及びビニル基からなる群より選ばれた１種又は２種以上を含むことが好ましい。ここで、炭素数を２〜２９の範囲に限定したのは、炭素数が２未満は所望の有機酸を得ることができず、炭素数が２９を越える有機酸は見当たらず実質的に使用しないからである。 The organic component of the organic metal compound or organic metalloid compound is one or more compounds selected from the group consisting of organic acids and amines, and the organic acid has 2 to 29 carbon atoms, preferably carbon. It is preferable that it is 1 type, or 2 or more types of compounds chosen from the group which consists of a compound containing several 3-18 carbons. Specifically, the organic acid is malic acid, citric acid, fumaric acid, maleic acid, tartaric acid, acetic acid, propionic acid, butyric acid, isobutyric acid, vibalic acid, valeric acid, isovaleric acid, caproic acid, 2-ethyl. Butyric acid, caprylic acid, pelargonic acid, 2-ethylhexanoic acid, capric acid, undecanoic acid, lauric acid, myristic acid, palmitic acid, stearic acid, isostearic acid, arachidic acid, behenic acid, lignoceric acid, serotic acid, montanic acid, It is one or more organic acids selected from the group consisting of melissic acid, ricinoleic acid, 12-hydroxystearic acid, naphthenic acid, abietic acid, dextropimaric acid, palmitoleic acid, oleic acid, linoleic acid and linolenic acid. Preferably malic acid, citric acid, fumaric acid, maleic acid, 2-ethylhexane , Lauric acid, myristic acid, palmitic acid, stearic acid, isostearic acid, 12-hydroxystearic acid, oleic acid, linoleic acid and linolenic acid may be one or more organic acids preferable. The organic acid is preferably a photopolymerizable compound. Specifically, the photopolymerizable compound preferably contains one or more selected from the group consisting of an acryloyl group, a methacryloyl group, and a vinyl group. Here, the reason why the number of carbon atoms is limited to the range of 2 to 29 is that when the number of carbon atoms is less than 2, a desired organic acid cannot be obtained, and an organic acid having more than 29 carbon atoms is not found and is not substantially used. Because.
一方、アミンは、ジブチルアミン、ジイソブチルアミン、トリペンチルアミン、アリルアミン、シクロヘキシルアミン、ジシクロヘキシルアミン、プロピレンジアミン、ジエチレントリアミン、ドデシルアミン、１，３−ジメチル−ｎ−ブチルアミン、１−アミノウンデカン、１−アミノトリデカン、テトラデシルアミン、ヘキサデシルアミン、オクタデシルアミン、オレイルアミン、ジオレイルアミン、ドデシルジメチルアミン、テトラデシルジメチルアミン、ヘキサデシルジメチルアミン、オクタデシルジメチルアミン、モノエタノールアミン、ジエタノールアミン、トリエタノールアミン及び３−メトキシプロピルアミンからなる群より選ばれた１種又は２種以上であることが好ましく、更にジブチルアミン、ドデシルアミン、テトラデシルアミン、ヘキサデシルアミン、オクタデシルアミン、オレイルアミン、モノエタノールアミン、ジエタノールアミン、トリエタノールアミン及び３−メトキシプロピルアミンからなる群より選ばれた１種又は２種以上のアミンであることが好ましい。また還元剤は、ヒドラジン、水素化ホウ素塩、ジメチルアミンボラン、ギ酸、ギ酸塩及びジ亜燐酸塩からなる群より選ばれた１種又は２種以上であることが好ましい。 On the other hand, amines are dibutylamine, diisobutylamine, tripentylamine, allylamine, cyclohexylamine, dicyclohexylamine, propylenediamine, diethylenetriamine, dodecylamine, 1,3-dimethyl-n-butylamine, 1-aminoundecane, 1-aminotridecane. Decane, tetradecylamine, hexadecylamine, octadecylamine, oleylamine, dioleylamine, dodecyldimethylamine, tetradecyldimethylamine, hexadecyldimethylamine, octadecyldimethylamine, monoethanolamine, diethanolamine, triethanolamine and 3-methoxypropyl It is preferably one or more selected from the group consisting of amines, and further dibutylamine, dodecylamine, tetra Shiruamin, hexadecylamine, octadecylamine, oleylamine, monoethanolamine, diethanolamine, is preferably one or more amines selected from the group consisting of triethanolamine and 3-methoxypropylamine. The reducing agent is preferably one or more selected from the group consisting of hydrazine, borohydride, dimethylamine borane, formic acid, formate and diphosphite.
次に上記混合物を所定の雰囲気中で４０〜３６０℃、好ましくは５０〜３５０℃の温度に加熱した状態に１０分〜５．０時間、好ましくは２０分〜４．０時間保持する。混合物の加熱雰囲気は、不活性ガス雰囲気、還元性ガス雰囲気又は大気雰囲気であることが好ましい。ここで、混合物の加熱温度を４０〜３６０℃の範囲に限定したのは、４０℃未満では分散体の生成が不十分となり、３６０℃を越えると有機物の分解が著しくなり、安定した分散体が得られないからである。また混合物の加熱時間を１０分〜５．０時間の範囲に限定したのは、１０分間未満では分散体の生成が不十分となり、５．０時間を越えると粒子の成長に変化がなくなり、これ以上保持する必要がないからである。このような簡便な方法で粒子が分散した分散体を作製できる。 Next, the above mixture is maintained in a predetermined atmosphere at a temperature of 40 to 360 ° C., preferably 50 to 350 ° C., for 10 minutes to 5.0 hours, preferably 20 minutes to 4.0 hours. The heating atmosphere of the mixture is preferably an inert gas atmosphere, a reducing gas atmosphere or an air atmosphere. Here, the heating temperature of the mixture is limited to the range of 40 to 360 ° C. The reason is that the dispersion is insufficiently generated at less than 40 ° C., and the decomposition of the organic matter becomes remarkable when the temperature exceeds 360 ° C. It is because it cannot be obtained. Moreover, the heating time of the mixture was limited to the range of 10 minutes to 5.0 hours. If less than 10 minutes, the formation of the dispersion was insufficient, and if it exceeded 5.0 hours, there was no change in the particle growth. This is because it is not necessary to hold the above. A dispersion in which particles are dispersed can be produced by such a simple method.
上記方法により製造された粒子分散体としては、平均粒径０．００５〜１．０μｍ、好ましくは０．０１〜０．８μｍの酸化錫、酸化インジウム、酸化亜鉛、錫含有酸化インジウム（ＩＴＯ）、亜鉛含有酸化インジウム（ＩＺＯ）、アルミニウム含有酸化亜鉛（ＡＺＯ）、ガリウム含有酸化亜鉛（ＧＺＯ）、セリウム含有酸化亜鉛（ＣＺＯ）、ホウ素含有酸化亜鉛（ＢＺＯ）、アンチモン含有酸化錫（ＡＴＯ）、或いはリン含有酸化錫（ＰＴＯ）の酸化物半導体粒子を含む粒子分散体が挙げられる。また上記粒子分散体を乾燥して得られた酸化物半導体粒子としては、平均粒径０．００５〜１．０μｍ、好ましくは０．０１〜０．８μｍの酸化錫、酸化インジウム、酸化亜鉛、錫含有酸化インジウム（ＩＴＯ）、亜鉛含有酸化インジウム（ＩＺＯ）、アルミニウム含有酸化亜鉛（ＡＺＯ）、ガリウム含有酸化亜鉛（ＧＺＯ）、セリウム含有酸化亜鉛（ＣＺＯ）、ホウ素含有酸化亜鉛（ＢＺＯ）、アンチモン含有酸化錫（ＡＴＯ）、或いはリン含有酸化錫（ＰＴＯ）の酸化物半導体粒子が挙げられる。ここで、酸化物半導体粒子の平均粒径を０．００５〜１．０μｍの範囲に限定したのは、０．００５μｍ未満の粒子や１．０μｍを越える粒子がこの方法では得られないからである。なお、本発明で使用される酸化物半導体粒子などの平均粒径とは、レーザー回折／散乱式粒度分布測定装置（堀場製作所製 ＬＡ−９５０）にて測定し、粒子径基準を個数として演算した５０％平均粒子径（Ｄ50）をいう。このレーザー回折／散乱式粒度分布測定装置による個数基準平均粒径の値は、走査型電子顕微鏡（日立ハイテクノロジーズ製 Ｓ−４３００ＳＥ及びＳ−９００）により観察した画像において、任意の５０個の粒子について粒径を実測したときのその平均粒径とほぼ一致する。 As the particle dispersion produced by the above method, an average particle diameter of 0.005 to 1.0 μm, preferably 0.01 to 0.8 μm of tin oxide, indium oxide, zinc oxide, tin-containing indium oxide (ITO), Zinc-containing indium oxide (IZO), aluminum-containing zinc oxide (AZO), gallium-containing zinc oxide (GZO), cerium-containing zinc oxide (CZO), boron-containing zinc oxide (BZO), antimony-containing tin oxide (ATO), or phosphorus Examples thereof include a particle dispersion containing oxide semiconductor particles of tin oxide (PTO). The oxide semiconductor particles obtained by drying the particle dispersion are tin oxide, indium oxide, zinc oxide, tin having an average particle size of 0.005 to 1.0 μm, preferably 0.01 to 0.8 μm. Containing indium oxide (ITO), zinc containing indium oxide (IZO), aluminum containing zinc oxide (AZO), gallium containing zinc oxide (GZO), cerium containing zinc oxide (CZO), boron containing zinc oxide (BZO), antimony containing oxidation Examples thereof include oxide semiconductor particles of tin (ATO) or phosphorus-containing tin oxide (PTO). Here, the reason why the average particle size of the oxide semiconductor particles is limited to the range of 0.005 to 1.0 μm is that particles having a particle size of less than 0.005 μm or particles exceeding 1.0 μm cannot be obtained by this method. . The average particle size of the oxide semiconductor particles used in the present invention is measured with a laser diffraction / scattering particle size distribution measuring device (LA-950, manufactured by Horiba, Ltd.), and the particle size reference is calculated as the number. 50% average particle diameter (D 50 ). The number-based average particle diameter measured by the laser diffraction / scattering particle size distribution measuring apparatus is the value of any 50 particles in an image observed with a scanning electron microscope (S-4300SE and S-900 manufactured by Hitachi High-Technologies). It almost coincides with the average particle diameter when the particle diameter is actually measured.
＜第２の実施の形態＞
上記第１の実施の形態で調製された混合物に更にフッ化アンモニウムを添加することを除いて、第１の実施の形態と同様にして粒子が分散した分散体を作製する。この方法により製造された粒子分散体としては、平均粒径０．００５〜１．０μｍ、好ましくは０．０１〜０．８μｍのフッ素含有酸化錫（ＦＴＯ）、フッ素含有酸化インジウム（ＦＩＯ）、フッ素含有酸化亜鉛（ＦＺＯ）、フッ素錫含有酸化インジウム（ＦＩＴＯ）、フッ素亜鉛含有酸化インジウム（ＦＩＺＯ）、フッ素アルミニウム含有酸化亜鉛（ＦＡＺＯ）、フッ素ガリウム含有酸化亜鉛（ＦＧＺＯ）、フッ素セリウム含有酸化亜鉛（ＦＣＺＯ）、或いはフッ素アンチモン含有酸化錫（ＦＡＴＯ）の酸化物半導体粒子を含む粒子分散体が挙げられる。また上記粒子分散体を乾燥して得られた酸化物半導体粒子としては、平均粒径０．００５〜１．０μｍ、好ましくは０．０１〜０．８μｍのフッ素含有酸化錫（ＦＴＯ）、フッ素含有酸化インジウム（ＦＩＯ）、フッ素含有酸化亜鉛（ＦＺＯ）、フッ素錫含有酸化インジウム（ＦＩＴＯ）、フッ素亜鉛含有酸化インジウム（ＦＩＺＯ）、フッ素アルミニウム含有酸化亜鉛（ＦＡＺＯ）、フッ素ガリウム含有酸化亜鉛（ＦＧＺＯ）、フッ素セリウム含有酸化亜鉛（ＦＣＺＯ）、或いはフッ素アンチモン含有酸化錫（ＦＡＴＯ）の酸化物半導体粒子が挙げられる。ここで、酸化物半導体粒子の平均粒径を０．００５〜１．０μｍの範囲に限定したのは、０．００５μｍ未満の粒子や１．０μｍを越える粒子がこの方法では得られないからである。
<Second Embodiment>
A dispersion in which particles are dispersed is produced in the same manner as in the first embodiment except that ammonium fluoride is further added to the mixture prepared in the first embodiment. The particle dispersion produced by this method includes fluorine-containing tin oxide (FTO), fluorine-containing indium oxide (FIO), fluorine having an average particle diameter of 0.005 to 1.0 μm, preferably 0.01 to 0.8 μm. Containing zinc oxide (FZO), fluorine tin containing indium oxide (FITO), fluorine zinc containing indium oxide (FIZO), fluorine aluminum containing zinc oxide (FAZO), fluorine gallium containing zinc oxide (FGZO), fluorine cerium containing zinc oxide (FCZO) ), Or a particle dispersion including oxide semiconductor particles of fluorine antimony-containing tin oxide (FATO). The oxide semiconductor particles obtained by drying the particle dispersion are fluorine-containing tin oxide (FTO) having an average particle diameter of 0.005 to 1.0 μm, preferably 0.01 to 0.8 μm, fluorine-containing Indium oxide (FIO), fluorine-containing zinc oxide (FZO), fluorine tin-containing indium oxide (FITO), fluorine zinc-containing indium oxide (FIZO), fluorine aluminum-containing zinc oxide (FAZO), fluorine gallium-containing zinc oxide (FGZO), Examples thereof include oxide semiconductor particles of fluorine-cerium-containing zinc oxide (FCZO) or fluorine-antimony-containing tin oxide (FATO). Here, the reason why the average particle size of the oxide semiconductor particles is limited to the range of 0.005 to 1.0 μm is that particles having a particle size of less than 0.005 μm or particles exceeding 1.0 μm cannot be obtained by this method. .
なお、上記第１及び第２の実施の形態では、酸化物半導体粒子を含む粒子分散体を製造したが、平均粒径０．００５〜１．０μｍ、好ましくは０．０１〜０．８μｍのＣｕ，Ａｕ，Ａｇ，Ｐｔ，Ｐｄ，Ｒｕ，Ｒｈ，Ｒｅ，Ｆｅ，Ｃｏ，Ｎｉ，Ｚｎ，Ｉｎ及びＳｎからなる群より選ばれた１種又は２種以上の純金属粒子、混合金属粒子或いは合金粒子を含む粒子分散体であってもよい。また、上記第１及び第２の実施の形態では、粒子分散体を乾燥して酸化物半導体粒子を製造したが、上記純金属粒子、混合金属粒子或いは合金粒子を含む粒子分散体を乾燥して、平均粒径０．００５〜１．０μｍ、好ましくは０．０１〜０．８μｍのＣｕ，Ａｕ，Ａｇ，Ｐｔ，Ｐｄ，Ｒｕ，Ｒｈ，Ｒｅ，Ｆｅ，Ｃｏ，Ｎｉ，Ｚｎ，Ｉｎ及びＳｎからなる群より選ばれた１種又は２種以上の純金属、混合金属或いは合金からなる金属粒子であってもよい。ここで、金属粒子の平均粒径を０．００５〜１．０μｍの範囲に限定したのは、０．００５μｍ未満の粒子や１．０μｍを越える粒子がこの方法では得られないからである。
また、上記第１及び第２の実施の形態では、酸化物半導体粒子を含む粒子分散体を製造したが、平均粒径０．００５〜１．０μｍ、好ましくは０．０１〜０．８μｍのＳｂの半金属粒子を含む粒子分散体であってもよい。更に、上記第１及び第２の実施の形態では、粒子分散体を乾燥して酸化物半導体粒子を製造したが、上記Ｓｂの半金属粒子を含む粒子分散体を乾燥して、平均粒径０．００５〜１．０μｍ、好ましくは０．０１〜０．８μｍのＳｂからなる半金属粒子であってもよい。ここで、半金属粒子の平均粒径を０．００５〜１．０μｍの範囲に限定したのは、０．００５μｍ未満の粒子や１．０μｍを越える粒子がこの方法では得られないからである。
In the first and second embodiments, a particle dispersion containing oxide semiconductor particles is manufactured. However, Cu having an average particle diameter of 0.005 to 1.0 μm, preferably 0.01 to 0.8 μm. , Au, Ag, Pt, Pd, Ru, Rh, Re, Fe, Co, Ni, Zn, In and Sn, one or more types of pure metal particles, mixed metal particles or alloy particles A particle dispersion containing In the first and second embodiments, the particle dispersion is dried to produce oxide semiconductor particles. However, the particle dispersion containing the pure metal particles, mixed metal particles, or alloy particles is dried. From Cu, Au, Ag, Pt, Pd, Ru, Rh, Re, Fe, Co, Ni, Zn, In and Sn having an average particle size of 0.005 to 1.0 μm, preferably 0.01 to 0.8 μm Metal particles made of one or more kinds of pure metals, mixed metals or alloys selected from the group may be used. Here, the reason why the average particle diameter of the metal particles is limited to the range of 0.005 to 1.0 μm is that particles having a particle size of less than 0.005 μm or particles exceeding 1.0 μm cannot be obtained by this method.
Moreover, in the said 1st and 2nd embodiment, although the particle dispersion containing an oxide semiconductor particle was manufactured, average particle diameter 0.005-1.0 micrometer, Preferably it is Sb of 0.01-0.8 micrometer. A particle dispersion containing the metalloid particles may be used. Further, in the first and second embodiments, the particle dispersion was dried to produce oxide semiconductor particles, but the particle dispersion containing the Sb semimetal particles was dried to obtain an average particle size of 0. It may be a semi-metal particle composed of 0.005 to 1.0 μm, preferably 0.01 to 0.8 μm of Sb. Here, the reason why the average particle size of the semi-metal particles is limited to the range of 0.005 to 1.0 μm is that particles having a particle size of less than 0.005 μm or particles exceeding 1.0 μm cannot be obtained by this method.
次に本発明の実施例を比較例とともに詳しく説明する。
＜実施例１＞
先ずエチレンオキシド変性コハク酸メタクリレート（新中村化学社製のＮＫエステルＳＡ）を水酸化ナトリウムでけん化して石鹸を調製した。この石鹸を２つに分け、一方の石鹸に塩化インジウム溶液（アジア物性社製）を混合して撹拌することによりインジウムの金属石鹸を調製した。このインジウムの金属石鹸を十分に水で洗浄して濾過することにより脱塩した後に、この脱塩したインジウムの金属石鹸を８０℃の真空乾燥機に一晩入れて脱水することによりインジウム石鹸（炭素数：１０）を得た。一方、上記石鹸の他方に塩化錫溶液（アジア物性社製）を混合して撹拌することにより錫の金属石鹸を調製した。この錫の金属石鹸を十分に水で洗浄して濾過することにより脱塩した後に、この脱塩した錫の金属石鹸を８０℃の真空乾燥機に一晩入れて脱水することにより錫石鹸（炭素数：１０）を得た。なお、上記エチレンオキシド変性コハク酸メタクリレートの化学式（１）をここに示す。
Next, examples of the present invention will be described in detail together with comparative examples.
<Example 1>
First, a soap was prepared by saponifying ethylene oxide-modified succinic acid methacrylate (NK ester SA manufactured by Shin-Nakamura Chemical Co., Ltd.) with sodium hydroxide. This soap was divided into two, and an indium chloride solution (manufactured by Asian Physical Properties) was mixed with one soap and stirred to prepare an indium metal soap. The indium metal soap was sufficiently desalted by washing with water and filtered, and then the desalted indium metal soap was placed in a vacuum dryer at 80 ° C. overnight to dehydrate it, so that the indium soap (carbon Number: 10) was obtained. On the other hand, a tin metal soap was prepared by mixing and stirring a tin chloride solution (manufactured by Asia Physical Properties Co., Ltd.) with the other soap. The tin metal soap was sufficiently desalted by washing with water and filtered, and then the desalted tin metal soap was placed in a vacuum dryer at 80 ° C. overnight and dehydrated to obtain tin soap (carbon Number: 10) was obtained. The chemical formula (1) of the ethylene oxide-modified succinic acid methacrylate is shown here.
＜実施例２＞
先ず12-ヒドロキシステアリン酸インジウム（炭素数：１８）７．５ｇとステアリン酸錫（炭素数：１８）０．５ｇとを石英シリンダに入れ、還元剤としてヒドラジン・一水和物０．１ｇを添加し、更にフッ化アンモニウムを０．３ｇ添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを３００℃のオイルバスに入れるとともに、この石英シリンダ内に空気（鈴木商事館社製の一般空気ボンベに貯留された空気）を０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例２とした。
＜実施例３＞
先ずステアリン酸錫（炭素数：１８）７．５ｇを石英シリンダに入れ、還元剤としてジ亜燐酸アンモニウム０．１ｇを添加し、更にフッ化アンモニウムを０．３ｇ添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを３００℃のオイルバスに入れるとともに、この石英シリンダ内に空気（鈴木商事館社製の一般空気ボンベに貯留された空気）を０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例３とした。
<Example 2>
First, 7.5 g of indium 12-hydroxystearate (carbon number: 18) and 0.5 g of tin stearate (carbon number: 18) are put in a quartz cylinder, and 0.1 g of hydrazine monohydrate is added as a reducing agent. Further, 0.3 g of ammonium fluoride was added, and these were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the mixture is placed in an oil bath at 300 ° C., and air (air stored in a general air cylinder manufactured by Suzuki Shoji Co., Ltd.) is supplied into the quartz cylinder at a rate of 0.2 cc / min. Then, after holding for 1 hour, it was taken out from the oil bath and cooled to room temperature to obtain a dispersion. This particle dispersion was designated as Example 2.
<Example 3>
First, 7.5 g of tin stearate (carbon number: 18) was put in a quartz cylinder, 0.1 g of ammonium diphosphite was added as a reducing agent, and 0.3 g of ammonium fluoride was further added. Mixing was obtained in the state. Next, the quartz cylinder containing the mixture is placed in an oil bath at 300 ° C., and air (air stored in a general air cylinder manufactured by Suzuki Shoji Co., Ltd.) is supplied into the quartz cylinder at a rate of 0.2 cc / min. Then, after holding for 1 hour, it was taken out from the oil bath and cooled to room temperature to obtain a dispersion. This particle dispersion was designated as Example 3.
＜実施例４＞
先ずステアリン酸錫（炭素数：１８）７．５ｇを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加し、更にフッ化アンモニウムを０．３ｇ添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを２７５℃のオイルバスに入れるとともに、この石英シリンダ内に空気（鈴木商事館社製の一般空気ボンベに貯留された空気）を０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例４とした。
＜実施例５＞
先ずステアリン酸錫（炭素数：１８）７．５ｇとモンタン酸／2-アミノエタノールアンチモン錯体（炭素数：２９）０．８ｇとを石英シリンダに入れ、還元剤としてジ亜燐酸アンモニウム０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを２５０℃のオイルバスに入れるとともに、この石英シリンダ内に空気（鈴木商事館社製の一般空気ボンベに貯留された空気）を０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例５とした。
＜実施例６＞
先ずオレイン酸インジウム（炭素数：１８）７．５ｇとパルミチン酸亜鉛（炭素数：１６）０．７ｇとを石英シリンダに入れ、還元剤としてヒドラジン・一水和物０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを３１０℃のオイルバスに入れるとともに、この石英シリンダ内に空気（鈴木商事館社製の一般空気ボンベに貯留された空気）を０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例６とした。
<Example 4>
First, 7.5 g of tin stearate (carbon number: 18) was put in a quartz cylinder, 0.1 g of dimethylamine borane was added as a reducing agent, and 0.3 g of ammonium fluoride was further added. To obtain a mixture. Next, the quartz cylinder containing the mixture is put into an oil bath at 275 ° C., and air (air stored in a general air cylinder manufactured by Suzuki Shoji Co., Ltd.) is supplied into the quartz cylinder at a rate of 0.2 cc / min. Then, after holding for 1 hour, it was taken out from the oil bath and cooled to room temperature to obtain a dispersion. This particle dispersion was designated as Example 4.
<Example 5>
First, 7.5 g of tin stearate (carbon number: 18) and 0.8 g of montanic acid / 2-aminoethanol antimony complex (carbon number: 29) are put in a quartz cylinder, and 0.1 g of ammonium diphosphite is used as a reducing agent. After the addition, they were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the above mixture is put into a 250 ° C. oil bath, and air (air stored in a general air cylinder manufactured by Suzuki Shoji Co., Ltd.) is supplied into the quartz cylinder at a rate of 0.2 cc / min. Then, after holding for 1 hour, it was taken out from the oil bath and cooled to room temperature to obtain a dispersion. This particle dispersion was designated as Example 5.
<Example 6>
First, 7.5 g of indium oleate (carbon number: 18) and 0.7 g of zinc palmitate (carbon number: 16) were placed in a quartz cylinder, and 0.1 g of hydrazine monohydrate was added as a reducing agent. These were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the mixture is put into a 310 ° C. oil bath, and air (air stored in a general air cylinder manufactured by Suzuki Shoji Co., Ltd.) is supplied into the quartz cylinder at a rate of 0.2 cc / min. Then, after holding for 1 hour, it was taken out from the oil bath and cooled to room temperature to obtain a dispersion. This particle dispersion was designated as Example 6.
＜実施例７＞
先ずエチレンオキシド変性コハク酸メタクリレート（新中村化学社製のＮＫエステルＳＡ）を水酸化ナトリウムでけん化して石鹸を調製した後に、この石鹸に塩化インジウム溶液（アジア物性社製）を混合して撹拌することによりインジウムの金属石鹸を調製した。このインジウムの金属石鹸を十分に水で洗浄して濾過することにより脱塩した後に、この脱塩したインジウムの金属石鹸を８０℃の真空乾燥機に一晩入れて脱水することによりインジウム石鹸（炭素数：１０）を得た。一方、ω−カルボキシ−ポリカプロラクトンモノアクリレート（東亞合成社製のアロニックスＭ−５３００）を水酸化ナトリウムでけん化して石鹸を調製した後に、この石鹸に塩化亜鉛溶液を混合して撹拌することにより亜鉛の金属石鹸を調製した。この亜鉛の金属石鹸を十分に水で洗浄して濾過することにより脱塩した後に、この脱塩した亜鉛の金属石鹸を８０℃の真空乾燥機に一晩入れて脱水することにより亜鉛石鹸（炭素数：１５）を得た。なお、上記ω−カルボキシ−ポリカプロラクトンモノアクリレートの化学式（２）をここに示す。
<Example 7>
First, a soap is prepared by saponifying ethylene oxide-modified succinic acid methacrylate (NK ester SA manufactured by Shin-Nakamura Chemical Co., Ltd.) with sodium hydroxide, and then mixing and stirring the soap with an indium chloride solution (manufactured by Asian Physical Properties). Indium metal soap was prepared. The indium metal soap was sufficiently desalted by washing with water and filtered, and then the desalted indium metal soap was placed in a vacuum dryer at 80 ° C. overnight to dehydrate it, so that the indium soap (carbon Number: 10) was obtained. On the other hand, a soap was prepared by saponifying ω-carboxy-polycaprolactone monoacrylate (Aronix M-5300 manufactured by Toagosei Co., Ltd.) with sodium hydroxide, and then mixing the zinc chloride solution with this soap and stirring the zinc. A metal soap was prepared. The zinc metal soap was thoroughly washed with water and filtered for desalting, and then the desalted zinc metal soap was placed in a vacuum dryer at 80 ° C. overnight to dehydrate it to obtain zinc soap (carbon Number: 15) was obtained. The chemical formula (2) of the ω-carboxy-polycaprolactone monoacrylate is shown here.
＜実施例８＞
先ずβ−カルボキシルエチルアクリレート（ダイセル・ユーシービー社製のβ−ＣＥＡ）を水酸化ナトリウムでけん化して石鹸を調製した後に、この石鹸に塩化チタン溶液を混合して撹拌することによりチタンの金属石鹸を調製した。このチタンの金属石鹸を十分に水で洗浄して濾過することにより脱塩した後に、この脱塩したチタンの金属石鹸を８０℃の真空乾燥機に一晩入れて脱水することによりチタン石鹸を得た。なお、上記β−カルボキシルエチルアクリレートの化学式（３）をここに示す。
<Example 8>
First, β-carboxyethyl acrylate (β-CEA manufactured by Daicel UCB) was saponified with sodium hydroxide to prepare a soap, and then mixed with a titanium chloride solution and stirred to obtain a titanium metal soap. Was prepared. The titanium metal soap was sufficiently washed with water and filtered to desalinate, and the desalted titanium metal soap was placed in a vacuum dryer at 80 ° C. overnight to dehydrate it to obtain a titanium soap. It was. The chemical formula (3) of the β-carboxyethyl acrylate is shown here.
＜実施例９＞
先ずチタンカップリング剤（味の素社製のＫＲ４４、炭素数：３及び４）７．５ｇを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを３００℃のオイルバスに入れるとともに、この石英シリンダ内に空気（鈴木商事館社製の一般空気ボンベに貯留された空気）を０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例９とした。なお、上記チタンカップリング剤（味の素社製のＫＲ４４）の化学式（４）をここに示す。
<Example 9>
First, 7.5 g of titanium coupling agent (KR44, carbon number: 3 and 4 by Ajinomoto Co., Inc.) is put in a quartz cylinder, 0.1 g of dimethylamine borane is added as a reducing agent, and these are mixed in a non-uniform state. To obtain a mixture. Next, the quartz cylinder containing the mixture is placed in an oil bath at 300 ° C., and air (air stored in a general air cylinder manufactured by Suzuki Shoji Co., Ltd.) is supplied into the quartz cylinder at a rate of 0.2 cc / min. Then, after holding for 1 hour, it was taken out from the oil bath and cooled to room temperature to obtain a dispersion. This particle dispersion was referred to as Example 9. The chemical formula (4) of the titanium coupling agent (KR44 manufactured by Ajinomoto Co., Inc.) is shown here.
先ずチタンカップリング剤（味の素社製の９ＳＡ、炭素数：３及び１８）７．５ｇを石英シリンダに入れ、還元剤として水素化ホウ素ナトリウム０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを３５０℃のオイルバスに入れるとともに、この石英シリンダ内に空気（鈴木商事館社製の一般空気ボンベに貯留された空気）を０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例１０とした。なお、上記チタンカップリング剤（味の素社製の９ＳＡ）の化学式（５）をここに示す。
First, 7.5 g of titanium coupling agent (9SA manufactured by Ajinomoto Co., Inc., carbon number: 3 and 18) was put in a quartz cylinder, and 0.1 g of sodium borohydride was added as a reducing agent. Mix to obtain a mixture. Next, the quartz cylinder containing the mixture is placed in an oil bath at 350 ° C., and air (air stored in a general air cylinder manufactured by Suzuki Shoji Co., Ltd.) is supplied into the quartz cylinder at a rate of 0.2 cc / min. Then, after holding for 1 hour, it was taken out from the oil bath and cooled to room temperature to obtain a dispersion. This particle dispersion was designated as Example 10. The chemical formula (5) of the titanium coupling agent (9SA manufactured by Ajinomoto Co., Inc.) is shown here.
先ずアクリル酸銀（炭素数：４）７．５ｇを石英シリンダに入れ、還元剤として水素化ホウ素ナトリウム０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを６０℃のオイルバスに入れるとともに、この石英シリンダ内に硫化水素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例１１とした。
First, 7.5 g of silver acrylate (carbon number: 4) was put in a quartz cylinder, 0.1 g of sodium borohydride was added as a reducing agent, and these were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 60 ° C., and hydrogen sulfide gas is supplied into the quartz cylinder at a rate of 0.2 cc / min for 1 hour, and then taken out from the oil bath to room temperature. Cooled to obtain a dispersion. This particle dispersion was designated as Example 11.
＜比較例１＞
先ずオレイン酸インジウム（炭素数：１８）７．５ｇとステアリン酸錫（炭素数：１８）０．５ｇとを石英シリンダに入れ、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを２００℃のオイルバスに入れるとともに、この石英シリンダ内に空気（鈴木商事館社製の一般空気ボンベに貯留された空気）を０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を比較例１とした。
＜比較例２＞
先ずオレイン酸インジウム（炭素数：１８）７．５ｇとステアリン酸錫（炭素数：１８）０．５ｇとを石英シリンダに入れ、還元剤としてヒドラジン・一水和物０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを３７０℃のオイルバスに入れるとともに、この石英シリンダ内に空気（鈴木商事館社製の一般空気ボンベに貯留された空気）を０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を比較例２とした。
<Comparative Example 1>
First, 7.5 g of indium oleate (carbon number: 18) and 0.5 g of tin stearate (carbon number: 18) were put in a quartz cylinder and mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the mixture is placed in an oil bath at 200 ° C., and air (air stored in a general air cylinder manufactured by Suzuki Shoji Co., Ltd.) is supplied into the quartz cylinder at a rate of 0.2 cc / min. Then, after holding for 1 hour, it was taken out from the oil bath and cooled to room temperature to obtain a dispersion. This particle dispersion was designated as Comparative Example 1.
<Comparative example 2>
First, 7.5 g of indium oleate (carbon number: 18) and 0.5 g of tin stearate (carbon number: 18) were placed in a quartz cylinder, and 0.1 g of hydrazine monohydrate was added as a reducing agent. These were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 370 ° C., and air (air stored in a general air cylinder manufactured by Suzuki Shoji Co., Ltd.) is supplied into the quartz cylinder at a rate of 0.2 cc / min. Then, after holding for 1 hour, it was taken out from the oil bath and cooled to room temperature to obtain a dispersion. This particle dispersion was designated as Comparative Example 2.
＜比較例３＞
先ずオレイン酸インジウム（炭素数：１８）７．５ｇとステアリン酸錫（炭素数：１８）０．５ｇとを石英シリンダに入れ、還元剤としてヒドラジン・一水和物０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを３５℃のオイルバスに入れるとともに、この石英シリンダ内に空気（鈴木商事館社製の一般空気ボンベに貯留された空気）を０．２ｃｃ／分ずつ供給しながら１時間保持して分散体を得た。この粒子分散体を比較例３とした。
＜比較例４＞
先ずオレイン酸インジウム（炭素数：１８）７．５ｇとステアリン酸錫（炭素数：１８）０．５ｇとを石英シリンダに入れ、溶媒としてメチルカルビトール７．５ｇを加えた後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを２００℃のオイルバスに入れるとともに、この石英シリンダ内に空気（鈴木商事館社製の一般空気ボンベに貯留された空気）を０．２ｃｃ／分ずつ供給しながら１時間保持して分散体を得た。この粒子分散体を比較例４とした。
<Comparative Example 3>
First, 7.5 g of indium oleate (carbon number: 18) and 0.5 g of tin stearate (carbon number: 18) were placed in a quartz cylinder, and 0.1 g of hydrazine monohydrate was added as a reducing agent. These were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the mixture is placed in a 35 ° C. oil bath, and air (air stored in a general air cylinder manufactured by Suzuki Shoji Co., Ltd.) is supplied into the quartz cylinder at a rate of 0.2 cc / min. The dispersion was obtained by holding for 1 hour. This particle dispersion was designated as Comparative Example 3.
<Comparative Example 4>
First, 7.5 g of indium oleate (carbon number: 18) and 0.5 g of tin stearate (carbon number: 18) are put in a quartz cylinder, and after adding 7.5 g of methyl carbitol as a solvent, they are heterogeneous. Was mixed to obtain a mixture. Next, the quartz cylinder containing the mixture is placed in an oil bath at 200 ° C., and air (air stored in a general air cylinder manufactured by Suzuki Shoji Co., Ltd.) is supplied into the quartz cylinder at a rate of 0.2 cc / min. The dispersion was obtained by holding for 1 hour. This particle dispersion was designated as Comparative Example 4.
＜比較試験１及び評価＞
実施例１〜１１及び比較例１〜４の粒子分散体をアセトンで洗浄した後、真空雰囲気中に室温で２時間保持して金属又は半金属化合物粒子からなる乾燥粉末を作製し、Ｘ線回折法（ＸＲＤ法）により乾燥粉末を構成する化合物の同定を行ってその化合物のパターン（結晶構造）及び名称を特定し、また蛍光Ｘ線分光分析法（ＸＦＳ法）により上記乾燥粉末の元素分析を行い、更に透過電子顕微鏡（ＴＥＭ）により乾燥粉末の一次粒子の平均粒径を求めた。その結果を表１に示す。表１において、「ＨＤ」はヒドラジンであり、「Ｎａ／ＢＨ」は水素化ホウ素ナトリウムであり、「ＤＭＡＢ」はジメチルアミンボランであり、「Ａ／ＨＰＰ」はジ亜燐酸アンモニウムである。
<Comparative test 1 and evaluation>
After the particle dispersions of Examples 1 to 11 and Comparative Examples 1 to 4 were washed with acetone, the powders were held in a vacuum atmosphere at room temperature for 2 hours to produce dry powders composed of metal or metalloid compound particles. X-ray diffraction The compound constituting the dry powder is identified by the XRD method (XRD method), the pattern (crystal structure) and name of the compound is specified, and the elemental analysis of the dry powder is performed by X-ray fluorescence spectrometry (XFS method) Then, the average particle diameter of the primary particles of the dry powder was determined by a transmission electron microscope (TEM). The results are shown in Table 1. In Table 1, “HD” is hydrazine, “Na / BH” is sodium borohydride, “DMAB” is dimethylamine borane, and “A / HPP” is ammonium diphosphite.
＜実施例１２＞
実施例１の粒子分散体を2-イソプロポキシエタノール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を実施例１２とした。
＜実施例１３＞
実施例２の粒子分散体をメチルカルビトール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を実施例１３とした。
＜実施例１４＞
実施例３の粒子分散体をイソプロパノール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を実施例１４とした。
＜実施例１５＞
実施例４の粒子分散体をイソプロパノール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を実施例１５とした。
＜実施例１６＞
実施例５の粒子分散体をイソプロパノール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を実施例１６とした。
<Example 12>
After the particle dispersion of Example 1 was diluted with 2-isopropoxyethanol (solvent), it was washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 30% by weight. . This particle dispersion was designated as Example 12.
<Example 13>
After the particle dispersion of Example 2 was diluted with methyl carbitol (solvent), it was washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 30% by weight. This particle dispersion was designated as Example 13.
<Example 14>
The particle dispersion of Example 3 was diluted with isopropanol (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 30% by weight. This particle dispersion was designated as Example 14.
<Example 15>
The particle dispersion of Example 4 was diluted with isopropanol (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 30% by weight. This particle dispersion was designated as Example 15.
<Example 16>
The particle dispersion of Example 5 was diluted with isopropanol (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 30% by weight. This particle dispersion was designated as Example 16.
＜実施例１７＞
実施例６の粒子分散体をN-メチルピロリドン（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を実施例１７とした。
＜実施例１８＞
実施例８の粒子分散体をヘキサン（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を実施例１８とした。
＜実施例１９＞
実施例８の粒子分散体をプロピレングリコールモノメチルエーテルアセテート（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を実施例１９とした。
＜実施例２０＞
実施例９の粒子分散体をプロピレングリコールモノメチルエーテル（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を実施例２０とした。
＜実施例２１＞
実施例１０の粒子分散体をプロピレングリコールモノメチルエーテルアセテート（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を実施例２１とした。
＜実施例２２＞
実施例１１の粒子分散体をN-メチルピロリドン（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を実施例２２とした。
<Example 17>
After the particle dispersion of Example 6 was diluted with N-methylpyrrolidone (solvent), it was washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 30% by weight. This particle dispersion was designated as Example 17.
<Example 18>
The particle dispersion of Example 8 was diluted with hexane (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 30% by weight. This particle dispersion was designated as Example 18.
<Example 19>
After the particle dispersion of Example 8 was diluted with propylene glycol monomethyl ether acetate (solvent), it was washed and concentrated by ultrafiltration to prepare a particle dispersion so that the particle content was about 30% by weight. . This particle dispersion was designated as Example 19.
<Example 20>
After the particle dispersion of Example 9 was diluted with propylene glycol monomethyl ether (solvent), it was washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 30% by weight. This particle dispersion was designated as Example 20.
<Example 21>
After the particle dispersion of Example 10 was diluted with propylene glycol monomethyl ether acetate (solvent), it was washed and concentrated by ultrafiltration to prepare a particle dispersion so that the particle content was about 30% by weight. . This particle dispersion was designated as Example 21.
<Example 22>
The particle dispersion of Example 11 was diluted with N-methylpyrrolidone (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 30% by weight. This particle dispersion was designated as Example 22.
＜比較例５＞
比較例１の粒子分散体をメチルカルビトール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を比較例５とした。
＜比較例６＞
比較例２の粒子分散体をメチルカルビトール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約３０重量％となるように粒子分散体を調製した。この粒子分散体を比較例６とした。
<Comparative Example 5>
After the particle dispersion of Comparative Example 1 was diluted with methyl carbitol (solvent), it was washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 30% by weight. This particle dispersion was designated as Comparative Example 5.
<Comparative Example 6>
After the particle dispersion of Comparative Example 2 was diluted with methyl carbitol (solvent), it was washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 30% by weight. This particle dispersion was designated as Comparative Example 6.
＜比較試験２及び評価＞
実施例１２〜２２、比較例５及び６の約３０重量％に洗浄・濃縮した直後の粒子分散体の状態と、密栓したガラス瓶に入れて４０℃に２週間保持した後の状態を目視にて観察した。その結果を表２に示す。表２において、「ＨＤ」はヒドラジンであり、「Ｎａ／ＢＨ」は水素化ホウ素ナトリウムであり、「ＤＭＡＢ」はジメチルアミンボランであり、「Ａ／ＨＰＰ」はジ亜燐酸アンモニウムである。
<Comparative test 2 and evaluation>
The state of the particle dispersion immediately after washing and concentration to about 30% by weight of Examples 12 to 22 and Comparative Examples 5 and 6 and the state after being kept in a sealed glass bottle at 40 ° C. for 2 weeks are visually observed. Observed. The results are shown in Table 2. In Table 2, “HD” is hydrazine, “Na / BH” is sodium borohydride, “DMAB” is dimethylamine borane, and “A / HPP” is ammonium diphosphite.
＜実施例２３＞
先ずイソステアリン酸銅（炭素数：１８）０．７ｇを石英シリンダに入れ、還元剤としてヒドラジン・一水和物０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを１５０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例２３とした。
＜実施例２４＞
先ずカプロン酸銀（炭素数：６）０．７ｇを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを４５℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例２４とした。
<Example 23>
First, 0.7 g of copper isostearate (carbon number: 18) was put in a quartz cylinder, 0.1 g of hydrazine monohydrate was added as a reducing agent, and these were mixed in a non-uniform state to obtain a mixture. . Next, the quartz cylinder containing the above mixture is placed in an oil bath at 150 ° C. and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, and then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 23.
<Example 24>
First, 0.7 g of silver caproate (carbon number: 6) was put in a quartz cylinder, 0.1 g of dimethylamine borane was added as a reducing agent, and these were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 45 ° C. and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, and then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 24.
＜実施例２５＞
先ずオレイン酸銀（炭素数：１８）０．３５ｇと2-エチルヘキサン酸パラジウム（炭素数：８）０．３５ｇとを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを２００℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例２５とした。
＜実施例２６＞
先ず2-エチルヘキサン酸パラジウム（炭素数：８）０．７ｇを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを１５０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例２６とした。
<Example 25>
First, 0.35 g of silver oleate (carbon number: 18) and 0.35 g of palladium 2-ethylhexanoate (carbon number: 8) were placed in a quartz cylinder, and 0.1 g of dimethylamine borane was added as a reducing agent. These were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 200 ° C. and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, and then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 25.
<Example 26>
First, 0.7 g of palladium 2-ethylhexanoate (carbon number: 8) was put in a quartz cylinder, 0.1 g of dimethylamine borane was added as a reducing agent, and these were mixed in a non-uniform state to obtain a mixture. . Next, the quartz cylinder containing the above mixture is placed in an oil bath at 150 ° C. and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, and then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 26.
＜実施例２７＞
先ずカプロン酸／2-エチルヘキシルアミン金錯体（炭素数：６，８）０．７ｇを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを１５０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例２７とした。
＜実施例２８＞
先ずオレイン酸／プロピレンジアミン金錯体（炭素数：１８，３）０．６ｇとイソステアリン酸銅（炭素数：１８）０．１ｇとを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを１５０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例２８とした。
<Example 27>
First, 0.7 g of caproic acid / 2-ethylhexylamine gold complex (carbon number: 6, 8) was put in a quartz cylinder, 0.1 g of dimethylamine borane was added as a reducing agent, and these were mixed in a non-uniform state. To obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 150 ° C. and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, and then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 27.
<Example 28>
First, 0.6 g of oleic acid / propylenediamine gold complex (carbon number: 18,3) and 0.1 g of copper isostearate (carbon number: 18) are placed in a quartz cylinder, and 0.1 g of dimethylamine borane is added as a reducing agent. Then, they were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 150 ° C. and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, and then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 28.
＜実施例２９＞
先ずオレイルアミン白金錯体（炭素数：１８）０．７ｇを石英シリンダに入れ、還元剤としてジ亜燐酸アンモニウム０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを８０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例２９とした。
＜実施例３０＞
先ずビバル酸ルテニウム（炭素数：５）０．７ｇを石英シリンダに入れ、還元剤としてジ亜燐酸アンモニウム０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを４５℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例３０とした。
<Example 29>
First, 0.7 g of oleylamine platinum complex (carbon number: 18) was put in a quartz cylinder, 0.1 g of ammonium diphosphite was added as a reducing agent, and these were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 80 ° C., and nitrogen gas is supplied into the quartz cylinder at a rate of 0.2 cc / min for 1 hour, then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 29.
<Example 30>
First, 0.7 g of ruthenium vibalate (carbon number: 5) was put in a quartz cylinder, 0.1 g of ammonium diphosphite was added as a reducing agent, and these were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 45 ° C. and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, and then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 30.
＜実施例３１＞
先ずステアリン酸鉄（炭素数：１８）０．３ｇと酢酸コバルト（炭素数：２）０．１ｇとベヘン酸ニッケル（炭素数：２２）０．３ｇとを石英シリンダに入れ、還元剤としてヒドラジン・一水和物０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを３５０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例３１とした。
＜実施例３２＞
先ずリノール酸／テトラデシルアミンロジウム錯体（炭素数：１８，１４）０．７ｇを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを１３０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例３２とした。
<Example 31>
First, 0.3 g of iron stearate (carbon number: 18), 0.1 g of cobalt acetate (carbon number: 2) and 0.3 g of nickel behenate (carbon number: 22) were placed in a quartz cylinder, and hydrazine as a reducing agent. After adding 0.1 g of monohydrate, they were mixed in a heterogeneous state to obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 350 ° C. and held for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 31.
<Example 32>
First, 0.7 g of linoleic acid / tetradecylamine rhodium complex (carbon number: 18, 14) was put in a quartz cylinder, 0.1 g of dimethylamine borane was added as a reducing agent, and these were mixed in a non-uniform state. A mixture was obtained. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 130 ° C., and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was defined as Example 32.
＜実施例３３＞
先ずリノレン酸／ヘキサデシルアミンレニウム錯体（炭素数：１８，１６）０．７ｇを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを１８０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例３３とした。
＜実施例３４＞
先ずオレイン酸インジウム（炭素数：１８）０．６５ｇとドデシルアミン錫錯体（炭素数：１２）０．５ｇとを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを１３０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例３４とした。
<Example 33>
First, 0.7 g of linolenic acid / hexadecylamine rhenium complex (carbon number: 18, 16) is put in a quartz cylinder, 0.1 g of dimethylamine borane is added as a reducing agent, and these are mixed in a non-uniform state. A mixture was obtained. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 180 ° C. and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 33.
<Example 34>
First, 0.65 g of indium oleate (carbon number: 18) and 0.5 g of dodecylamine tin complex (carbon number: 12) are placed in a quartz cylinder, and 0.1 g of dimethylamine borane is added as a reducing agent. Mixing in a heterogeneous state gave a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 130 ° C., and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 34.
＜実施例３５＞
先ず12-ヒドロキシステアリン酸インジウム（炭素数：１８）０．６ｇとパルミチン酸亜鉛（炭素数：１６）０．１ｇとを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを１１０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例３５とした。
＜実施例３６＞
先ずアクリル酸銀（炭素数：４）０．７ｇを石英シリンダに入れ、還元剤としてヒドラジン・一水和物０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを６０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例３６とした。
<Example 35>
First, 0.6 g of indium 12-hydroxystearate (carbon number: 18) and 0.1 g of zinc palmitate (carbon number: 16) were placed in a quartz cylinder, and 0.1 g of dimethylamine borane was added as a reducing agent. These were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 110 ° C. and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 35.
<Example 36>
First, 0.7 g of silver acrylate (carbon number: 4) is put in a quartz cylinder, 0.1 g of hydrazine monohydrate is added as a reducing agent, and these are mixed in a non-uniform state to obtain a mixture. It was. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 60 ° C., and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 36.
＜実施例３７＞
先ずモンタン酸／2-アミノエタノールアンチモン錯体（炭素数：２９）０．３５ｇとアクリル酸パラジウム（炭素数：４）０．３５ｇとを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを６０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例３７とした。
＜実施例３８＞
実施例１のインジウム石鹸（炭素数：１０）０．６５ｇと実施例１の錫石鹸（炭素数：１０）０．５ｇとを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを１３０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例３８とした。
<Example 37>
First montanic acid / 2-aminoethanol antimony complexes (carbon number: 29) 0.35g of acrylic acid palladium (carbon number: 4) and 0.35g placed in a quartz cylinder, added dimethylamine borane 0.1g as a reducing agent Then, they were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 60 ° C., and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 37.
<Example 38>
0.65 g of indium soap (carbon number: 10) of Example 1 and 0.5 g of tin soap (carbon number: 10) of Example 1 were put in a quartz cylinder, and 0.1 g of dimethylamine borane was added as a reducing agent. Later, they were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 130 ° C., and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 38.
＜実施例３９＞
先ずエチレンオキシド変性コハク酸メタクリレート（新中村化学社製のＮＫエステルＳＡ）を水酸化ナトリウムでけん化して石鹸を調製した後に、この石鹸に塩化金溶液を混合して撹拌することにより金の金属石鹸を調製した。次いでこの金の金属石鹸を十分に水で洗浄して濾過することにより脱塩した後に、この脱塩した金の金属石鹸を８０℃の真空乾燥機に一晩入れて脱水することにより金石鹸（炭素数：１０）を得た。次にこの金石鹸０．７ｇを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。更に上記混合物の入った石英シリンダを１５０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例３９とした。
＜実施例４０＞
先ずメタクリル酸白金（炭素数：５）０．７ｇを石英シリンダに入れ、還元剤としてジ亜燐酸アンモニウム０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次に上記混合物の入った石英シリンダを１５０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を実施例４０とした。
<Example 39>
First, a soap was prepared by saponifying ethylene oxide-modified succinic acid methacrylate (NK ester SA, manufactured by Shin-Nakamura Chemical Co., Ltd.) with sodium hydroxide, and then mixing the gold chloride solution with the soap and stirring the gold metal soap. Prepared. Next, the gold metal soap was sufficiently washed with water and filtered for desalting, and then the desalted gold metal soap was placed in a vacuum dryer at 80 ° C. overnight to dehydrate it to dehydrate the gold soap ( Carbon number: 10) was obtained. Next, 0.7 g of this gold soap was placed in a quartz cylinder, 0.1 g of dimethylamine borane was added as a reducing agent, and these were mixed in a non-uniform state to obtain a mixture. Further, the quartz cylinder containing the above mixture is placed in an oil bath at 150 ° C. and kept for one hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, then taken out from the oil bath and cooled to room temperature. A dispersion was obtained. This particle dispersion was referred to as Example 39.
<Example 40>
First, 0.7 g of platinum methacrylate (carbon number: 5) was put in a quartz cylinder, 0.1 g of ammonium diphosphite was added as a reducing agent, and these were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder containing the above mixture is placed in an oil bath at 150 ° C. and kept for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, and then taken out from the oil bath and cooled to room temperature. To obtain a dispersion. This particle dispersion was designated as Example 40.
＜比較例７＞
先ずカプロン酸銀（炭素数：６）０．７ｇを石英シリンダに入れた。次にこの石英シリンダを４５℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を比較例７とした。
＜比較例８＞
先ずカプロン酸銀（炭素数：６）０．７ｇを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次にこの石英シリンダを３５℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を比較例８とした。
<Comparative Example 7>
First, 0.7 g of silver caproate (carbon number: 6) was put in a quartz cylinder. Next, the quartz cylinder is placed in an oil bath at 45 ° C. and held for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, and then taken out from the oil bath and cooled to room temperature. Got. This particle dispersion was designated as Comparative Example 7.
<Comparative Example 8>
First, 0.7 g of silver caproate (carbon number: 6) was put in a quartz cylinder, 0.1 g of dimethylamine borane was added as a reducing agent, and these were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder is placed in an oil bath at 35 ° C., and held for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, and then taken out from the oil bath and cooled to room temperature. Got. This particle dispersion was designated as Comparative Example 8.
＜比較例９＞
先ずカプロン酸銀（炭素数：６）０．７ｇを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次にこの石英シリンダを３７０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を比較例９とした。
＜比較例１０＞
先ずカプロン酸銀（炭素数：６）０．７ｇを石英シリンダに入れ、還元剤としてジメチルアミンボラン０．１ｇを添加し、更に溶媒としてトルエン０．７ｇを添加した後に、これらを不均一な状態で混合して混合物を得た。次にこの石英シリンダを１５０℃のオイルバスに入れるとともに、この石英シリンダ内に窒素ガスを０．２ｃｃ／分ずつ供給しながら１時間保持した後に、オイルバスから取出して室温まで冷却し、分散体を得た。この粒子分散体を比較例１０とした。
<Comparative Example 9>
First, 0.7 g of silver caproate (carbon number: 6) was put in a quartz cylinder, 0.1 g of dimethylamine borane was added as a reducing agent, and these were mixed in a non-uniform state to obtain a mixture. Next, the quartz cylinder is placed in an oil bath at 370 ° C. and held for 1 hour while supplying nitrogen gas into the quartz cylinder at a rate of 0.2 cc / min, and then taken out from the oil bath and cooled to room temperature. Got. This particle dispersion was designated as Comparative Example 9.
<Comparative Example 10>
First, 0.7 g of silver caproate (carbon number: 6) is put in a quartz cylinder, 0.1 g of dimethylamine borane is added as a reducing agent, and 0.7 g of toluene is further added as a solvent. To obtain a mixture. Next, the quartz cylinder is placed in a 150 ° C. oil bath, and nitrogen gas is supplied into the quartz cylinder at a rate of 0.2 cc / min for 1 hour, and then taken out from the oil bath and cooled to room temperature. Got. This particle dispersion was designated as Comparative Example 10.
＜比較試験３及び評価＞
実施例２３〜４０及び比較例７〜１０の粒子分散体をアセトンで洗浄した後、真空雰囲気中に室温で２時間保持して金属粒子からなる乾燥粉末を作製し、Ｘ線光電子スペクトル法（ＸＰＳ法）により乾燥粉末を構成する化合物の同定を行ってその化合物の酸化数を求め、またフィールドエミッション透過電子顕微鏡（ＦＥ−ＴＥＭ）により上記乾燥粉末の元素分析を行うとともに、乾燥粉末の一次粒子の平均粒径を求めた。その結果を表３及び表４に示す。表３及び表４において、「ＨＤ」はヒドラジンであり、「Ｎａ／ＢＨ」は水素化ホウ素ナトリウムであり、「ＤＭＡＢ」はジメチルアミンボランであり、「Ａ／ＨＰＰ」はジ亜燐酸アンモニウムである。
<Comparative test 3 and evaluation>
After the particle dispersions of Examples 23 to 40 and Comparative Examples 7 to 10 were washed with acetone, they were kept in a vacuum atmosphere at room temperature for 2 hours to produce dry powders composed of metal particles, and X-ray photoelectron spectroscopy (XPS) The compound constituting the dry powder is identified by the method) to determine the oxidation number of the compound, and elemental analysis of the dry powder is performed by a field emission transmission electron microscope (FE-TEM). The average particle size was determined. The results are shown in Tables 3 and 4. In Tables 3 and 4, “HD” is hydrazine, “Na / BH” is sodium borohydride, “DMAB” is dimethylamine borane, and “A / HPP” is ammonium diphosphite. .
＜実施例４１＞
実施例２３の粒子分散体をトルエン（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例４１とした。
＜実施例４２＞
実施例２４の粒子分散体をイソプロパノール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例４２とした。
＜実施例４３＞
実施例２５の粒子分散体を2-イソプロポキシエタノール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例４３とした。
＜実施例４４＞
実施例２６の粒子分散体をイソプロパノール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例４４とした。
＜実施例４５＞
実施例２７の粒子分散体をイソプロパノール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例４５とした。
<Example 41>
The particle dispersion of Example 23 was diluted with toluene (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was defined as Example 41.
<Example 42>
The particle dispersion of Example 24 was diluted with isopropanol (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 42.
<Example 43>
The particle dispersion of Example 25 was diluted with 2-isopropoxyethanol (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. . This particle dispersion was designated as Example 43.
<Example 44>
The particle dispersion of Example 26 was diluted with isopropanol (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 44.
<Example 45>
The particle dispersion of Example 27 was diluted with isopropanol (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was defined as Example 45.
＜実施例４６＞
実施例２８の粒子分散体をα−テルピネオール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例４６とした。
＜実施例４７＞
実施例２９の粒子分散体をα−テルピネオール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例４７とした。
＜実施例４８＞
実施例３０の粒子分散体を水（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例４８とした。
＜実施例４９＞
実施例３１の粒子分散体をプロピレングリコールモノメチルエーテル（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例４９とした。
＜実施例５０＞
実施例３２の粒子分散体をヘキサン（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例５０とした。
<Example 46>
The particle dispersion of Example 28 was diluted with α-terpineol (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 46.
<Example 47>
The particle dispersion of Example 29 was diluted with α-terpineol (solvent), and then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 47.
<Example 48>
The particle dispersion of Example 30 was diluted with water (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 48.
<Example 49>
The particle dispersion of Example 31 was diluted with propylene glycol monomethyl ether (solvent), and then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 49.
<Example 50>
After the particle dispersion of Example 32 was diluted with hexane (solvent), it was washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 50.
＜実施例５１＞
実施例３３の粒子分散体をメチルカルビトール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例５１とした。
＜実施例５２＞
実施例３４の粒子分散体をデカリン（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例５２とした。
＜実施例５３＞
実施例３５の粒子分散体をデカリン（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例５３とした。
＜実施例５４＞
実施例３６の粒子分散体をイソプロパノール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例５４とした。
＜実施例５５＞
実施例３７の粒子分散体をイソプロパノール（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例５５とした。
<Example 51>
The particle dispersion of Example 33 was diluted with methyl carbitol (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 51.
<Example 52>
The particle dispersion of Example 34 was diluted with decalin (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 52.
<Example 53>
The particle dispersion of Example 35 was diluted with decalin (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 53.
<Example 54>
The particle dispersion of Example 36 was diluted with isopropanol (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 54.
<Example 55>
The particle dispersion of Example 37 was diluted with isopropanol (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was defined as Example 55.
＜実施例５６＞
実施例３８の粒子分散体をテトラデカン（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例５６とした。
＜実施例５７＞
実施例３９の粒子分散体をヘキサン（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例５７とした。
＜実施例５８＞
実施例４０の粒子分散体をプロピレングリコールモノメチルエーテルアセテート（溶媒）で希釈した後に、限外濾過法により洗浄・濃縮して粒子の含有量が約４０重量％となるように粒子分散体を調製した。この粒子分散体を実施例５８とした。
＜比較例１１＞
比較例９の粒子分散体をイソプロパノール等の溶媒と混合した。この混合物を比較例１１とした。
<Example 56>
The particle dispersion of Example 38 was diluted with tetradecane (solvent), and then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 56.
<Example 57>
The particle dispersion of Example 39 was diluted with hexane (solvent), then washed and concentrated by an ultrafiltration method to prepare a particle dispersion so that the particle content was about 40% by weight. This particle dispersion was designated as Example 57.
<Example 58>
The particle dispersion of Example 40 was diluted with propylene glycol monomethyl ether acetate (solvent), then washed and concentrated by ultrafiltration to prepare a particle dispersion so that the particle content was about 40% by weight. . This particle dispersion was referred to as Example 58.
<Comparative Example 11>
The particle dispersion of Comparative Example 9 was mixed with a solvent such as isopropanol. This mixture was designated as Comparative Example 11.
＜比較試験４及び評価＞
実施例４１〜５８の粒子分散体と比較例１１の混合物の、約３０重量％に洗浄・濃縮した直後の粒子分散体の状態と、密栓したガラス瓶に入れて４０℃に２週間保持した後の状態を目視にて観察した。その結果を表５及び表６に示す。表５及び表６において、「ＨＤ」はヒドラジンであり、「Ｎａ／ＢＨ」は水素化ホウ素ナトリウムであり、「ＤＭＡＢ」はジメチルアミンボランであり、「Ａ／ＨＰＰ」はジ亜燐酸アンモニウムである。
<Comparative test 4 and evaluation>
The state of the particle dispersion immediately after being washed and concentrated to about 30% by weight of the mixture of the particle dispersions of Examples 41 to 58 and Comparative Example 11, and after being kept in a sealed glass bottle at 40 ° C. for 2 weeks The state was observed visually. The results are shown in Tables 5 and 6. In Tables 5 and 6, “HD” is hydrazine, “Na / BH” is sodium borohydride, “DMAB” is dimethylamine borane, and “A / HPP” is ammonium diphosphite. .
＜実施例５９＞
先ず実施例１２の粒子分散体（濃度約３０重量％のＩＴＯ粒子を分散した分散液）をエタノールで、ＩＴＯ粒子の含有量が４．０重量％となるように希釈し、この希釈した粒子分散体に光開始剤（チバ・スペシャリティー・ケミカルズ社製のイルガキュア５００）を０．１重量％溶かして粒子分散体を調製した。次いで洗浄済みのソーダガラス板（縦１００ｍｍ、横１００ｍｍ、厚さ２．８ｍｍ）を４０℃に保温し、このソーダガラス板をスピンコーターで１５０ｒｐｍの速度で回転させた状態で、上記希釈調製した粒子分散体を５ｃｃ滴下し、１２０秒間振り切って膜を作製した。
上記膜を上に向けたガラス板にステンレス製フォトマスク３１（図２）を載せた。このフォトマスク３１は、縦×横×厚さがそれぞれ１００ｍｍ×１００ｍｍ×１．０ｍｍの正方形状に形成され、幅×長さがそれぞれ２０ｍｍ×５０ｍｍの長方形の窓孔３１ａが１０ｍｍ間隔で３個形成される。次いでガラス板の上方から紫外線照射装置（１６０Ｗメタルハライドランプ：距離１０ｃｍ）により２５０ｍＪ／ｃｍ2の紫外線エネルギを照射した後、フォトマスクを取除いたガラス板をホットプレートに載せて大気中で１００℃に１０分間保持した。次にN,N-ジメチルホルムアミド１０重量％及びアセチルアセトン５重量％を相溶させたエタノール溶液で上記ガラス板をリンスすることにより、非光照射部の膜を溶かし、光照射の膜だけを残して、フォトマスクの長方形の窓孔と同一形状のパターニングされた膜を得た。更にこのガラス板を窒素ガス雰囲気中で２２０℃に３０分間保持して膜を焼成した後に室温まで冷却した。このガラス板を実施例５９とした。
<Example 59>
First, the particle dispersion of Example 12 (dispersion in which ITO particles having a concentration of about 30% by weight were dispersed) was diluted with ethanol so that the content of ITO particles became 4.0% by weight. A particle dispersion was prepared by dissolving 0.1% by weight of photoinitiator (Irgacure 500 manufactured by Ciba Specialty Chemicals) into the body. Next, the diluted soda glass plate (length 100 mm, width 100 mm, thickness 2.8 mm) is kept at 40 ° C., and this diluted and prepared particle is rotated with a spin coater at a speed of 150 rpm. 5 cc of the dispersion was dropped and shaken for 120 seconds to prepare a film.
A stainless steel photomask 31 (FIG. 2) was placed on a glass plate with the film facing upward. This
＜実施例６０＞
実施例１８の粒子分散体（濃度約３０重量％のＩＺＯ粒子を分散した分散液）を用いたことを除いて、実施例５９と同様の方法でガラス板を作製した。このガラス板を実施例６０とした。
<Example 60>
A glass plate was produced in the same manner as in Example 59, except that the particle dispersion of Example 18 (dispersion in which IZO particles having a concentration of about 30% by weight were dispersed) was used. This glass plate was referred to as Example 60.
＜比較試験５及び評価＞
実施例５９及び６０のガラス板の膜の厚さを走査型電子顕微鏡（ＳＥＭ）にて測定した。その結果、実施例５９の膜の厚さは２６０ｎｍと見積もられ、実施例６０の膜の厚さは３２０ｎｍと見積もられた。またこれらの膜の表面抵抗値を四探針法にて測定したところ、実施例５９の膜は４４６０Ω／□の導電性を示し、実施例６０の膜は４９００Ω／□の導電性を示した。更に実施例５９及び６０の膜の可視光透過率を分光光度計にて測定したところ、９８％及び９６％と高い透明性を示した。
<Comparative test 5 and evaluation>
The thickness of the glass plate of Examples 59 and 60 was measured with a scanning electron microscope (SEM). As a result, the film thickness of Example 59 was estimated to be 260 nm, and the film thickness of Example 60 was estimated to be 320 nm. Further, when the surface resistance values of these films were measured by a four-point probe method, the film of Example 59 showed a conductivity of 4460 Ω / □, and the film of Example 60 showed a conductivity of 4900 Ω / □. Further, when the visible light transmittance of the films of Examples 59 and 60 was measured with a spectrophotometer, it showed high transparency of 98% and 96%.
＜実施例６１＞
先ず実施例５４の粒子分散体（濃度約３０重量％のＡｇ粒子を分散した分散液）をイソプロパノールで、Ａｇ粒子の含有量が２０重量％となるように希釈し、この希釈した粒子分散体に光開始剤（チバ・スペシャリティー・ケミカルズ社製のイルガキュア５００）を０．５重量％溶かして粒子分散体を調製した。次いで洗浄済みのソーダガラス板（縦１００ｍｍ、横１００ｍｍ、厚さ２．８ｍｍ）を４０℃に保温し、このソーダガラス板をスピンコーターで１５０ｒｐｍの速度で回転させた状態で、上記希釈調製した粒子分散体を５ｃｃ滴下し、１２０秒間振り切って膜を作製した。
上記膜を上に向けたガラス板にステンレス製フォトマスクをそれぞれ載せた。このフォトマスクは、縦×横×厚さがそれぞれ１００ｍｍ×１００ｍｍ×１．０ｍｍの正方形状に形成され、幅×長さがそれぞれ２０ｍｍ×５０ｍｍの長方形の窓孔が１０ｍｍ間隔で３個形成される。次いでガラス板の上方から紫外線照射装置（１６０Ｗメタルハライドランプ：距離１０ｃｍ）により２５０ｍＪ／ｃｍ2の紫外線エネルギを照射した後、フォトマスクを取除いたガラス板をホットプレートに載せて大気中で１００℃に１０分間保持した。次にN,N-ジメチルホルムアミド１０重量％及びアセチルアセトン５重量％を相溶させたエタノール溶液で上記ガラス板をリンスすることにより、非光照射部の膜を溶かし、光照射の膜だけを残して、フォトマスクの長方形の窓孔と同一形状のパターニングされた膜を得た。更にこのガラス板を大気中で２００℃に３０分間保持して膜を焼成した後に室温まで冷却した。このガラス板を実施例６１とした。
＜実施例６２＞
実施例５５の粒子分散体（濃度約３０重量％のＡｇ粒子及びＰｄ粒子を分散した分散液）を用いたことを除いて実施例６１と同様にしてガラス板を作製した。このガラス板を実施例６２とした。
<Example 61>
First, the particle dispersion of Example 54 (dispersion in which Ag particles having a concentration of about 30% by weight were dispersed) was diluted with isopropanol so that the content of Ag particles was 20% by weight. A particle dispersion was prepared by dissolving 0.5% by weight of a photoinitiator (Irgacure 500 manufactured by Ciba Specialty Chemicals). Next, the diluted soda glass plate (length 100 mm, width 100 mm, thickness 2.8 mm) is kept at 40 ° C., and this diluted and prepared particle is rotated with a spin coater at a speed of 150 rpm. 5 cc of the dispersion was dropped and shaken for 120 seconds to prepare a film.
A stainless steel photomask was placed on each glass plate with the membrane facing upward. This photomask is formed in a square shape having a length × width × thickness of 100 mm × 100 mm × 1.0 mm, respectively, and three rectangular window holes each having a width × length of 20 mm × 50 mm are formed at intervals of 10 mm. . Next, after irradiating UV energy of 250 mJ / cm 2 from above the glass plate with an ultraviolet irradiation device (160 W metal halide lamp: distance 10 cm), the glass plate from which the photomask has been removed is placed on a hot plate and brought to 100 ° C. in the atmosphere. Hold for 10 minutes. Next, the glass plate is rinsed with an ethanol solution in which 10% by weight of N, N-dimethylformamide and 5% by weight of acetylacetone are mixed to dissolve the film of the non-light-irradiated portion, leaving only the light-irradiated film. A patterned film having the same shape as the rectangular window hole of the photomask was obtained. Further, this glass plate was kept at 200 ° C. for 30 minutes in the atmosphere to fire the film, and then cooled to room temperature. This glass plate was referred to as Example 61.
<Example 62>
A glass plate was produced in the same manner as in Example 61 except that the particle dispersion of Example 55 (dispersion in which Ag particles and Pd particles having a concentration of about 30% by weight were dispersed) was used. This glass plate was referred to as Example 62.
＜実施例６３＞
先ず実施例５６の粒子分散体（濃度約３０重量％のＩｎ粒子及びＳｎ粒子を分散した分散液）をヘキサンで、Ｉｎ粒子及びＳｎ粒子の含有量が１．０重量％となるように希釈し、この希釈した粒子分散体に光開始剤（チバ・スペシャリティー・ケミカルズ社製のイルガキュア５００）を０．０５重量％溶かして粒子分散体を調製した。次いで洗浄済みのアクリル板（縦１００ｍｍ、横１００ｍｍ、厚さ２．８ｍｍ）を４０℃に保温し、このアクリル板をスピンコーターで１５０ｒｐｍの速度で回転させた状態で、上記希釈調製した粒子分散体を５ｃｃ滴下し、１２０秒間振り切って膜を作製した。
上記膜に向けたアクリル板にステンレス製フォトマスクをそれぞれ載せた。このフォトマスクは、縦×横×厚さがそれぞれ１００ｍｍ×１００ｍｍ×１．０ｍｍの正方形状に形成され、幅×長さがそれぞれ２０ｍｍ×５０ｍｍの長方形の窓孔が１０ｍｍ間隔で３個形成される。次いでアクリル板の上方から紫外線照射装置（１６０Ｗメタルハライドランプ：距離１０ｃｍ）により２５０ｍＪ／ｃｍ2の紫外線エネルギを照射した後、フォトマスクを取除いたアクリル板をホットプレートに載せて大気中で１００℃に１０分間保持した。次にN,N-ジメチルホルムアミド１０重量％及びアセチルアセトン５重量％を相溶させたエタノール溶液で上記アクリル板をリンスすることにより、非光照射部の膜を溶かし、光照射の膜だけを残して、フォトマスクの長方形の窓孔と同一形状のパターニングされた膜を得た。更にこのアクリル板を窒素ガス雰囲気中で２００℃に３０分間保持し、大気中で２００℃に６０分間保持して、膜を焼成した後に室温まで冷却した。このアクリル板を実施例６３とした。
<Example 63>
First, the particle dispersion of Example 56 (dispersion in which In particles and Sn particles having a concentration of about 30 wt% were dispersed) was diluted with hexane so that the content of In particles and Sn particles was 1.0 wt%. Then, 0.05 wt% of a photoinitiator (Irgacure 500 manufactured by Ciba Specialty Chemicals) was dissolved in the diluted particle dispersion to prepare a particle dispersion. Next, the cleaned acrylic plate (100 mm long, 100 mm wide, 2.8 mm thick) is kept at 40 ° C. and the acrylic dispersion is rotated at a speed of 150 rpm with a spin coater, and the diluted particle dispersion prepared above. 5 cc was dropped and shaken for 120 seconds to prepare a film.
A stainless steel photomask was placed on each acrylic plate facing the film. This photomask is formed in a square shape having a length × width × thickness of 100 mm × 100 mm × 1.0 mm, respectively, and three rectangular window holes each having a width × length of 20 mm × 50 mm are formed at intervals of 10 mm. . Next, after irradiating ultraviolet energy of 250 mJ / cm 2 from above the acrylic plate with an ultraviolet irradiation device (160 W metal halide lamp: distance 10 cm), the acrylic plate with the photomask removed is placed on a hot plate and heated to 100 ° C. in the atmosphere. Hold for 10 minutes. Next, by rinsing the acrylic plate with an ethanol solution in which 10% by weight of N, N-dimethylformamide and 5% by weight of acetylacetone are mixed together, the non-light-irradiated part film is dissolved, leaving only the light-irradiated film. A patterned film having the same shape as the rectangular window hole of the photomask was obtained. Further, the acrylic plate was held at 200 ° C. for 30 minutes in a nitrogen gas atmosphere, and held at 200 ° C. for 60 minutes in the air, and the film was baked and then cooled to room temperature . The this acrylic plate were as in Example 63.
＜実施例６４＞
先ず実施例５７の粒子分散体（濃度約３０重量％のＡｕ粒子を分散した分散液）をヘキサンで、Ａｕ粒子の含有量が２０重量％となるように希釈し、この希釈した粒子分散体に光開始剤（チバ・スペシャリティー・ケミカルズ社製のイルガキュア５００）を０．５重量％溶かして粒子分散体を調製した。次いで洗浄済みのソーダガラス板（縦１００ｍｍ、横１００ｍｍ、厚さ２．８ｍｍ）を４０℃に保温し、このソーダガラス板をスピンコーターで１５０ｒｐｍの速度で回転させた状態で、上記希釈調製した粒子分散体を５ｃｃ滴下し、１２０秒間振り切って膜を作製した。
上記膜を上に向けたガラス板にステンレス製フォトマスクをそれぞれ載せた。このフォトマスクは、縦×横×厚さがそれぞれ１００ｍｍ×１００ｍｍ×１．０ｍｍの正方形状に形成され、幅×長さがそれぞれ２０ｍｍ×５０ｍｍの長方形の窓孔が１０ｍｍ間隔で３個形成される。次いでガラス板の上方から紫外線照射装置（１６０Ｗメタルハライドランプ：距離１０ｃｍ）により２５０ｍＪ／ｃｍ2の紫外線エネルギを照射した後、フォトマスクを取除いたガラス板をホットプレートに載せて大気中で１００℃に１０分間保持した。次にN,N-ジメチルホルムアミド１０重量％及びアセチルアセトン５重量％を相溶させたエタノール溶液で上記ガラス板をリンスすることにより、非光照射部の膜を溶かし、光照射の膜だけを残して、フォトマスクの長方形の窓孔と同一形状のパターニングされた膜を得た。更にこのガラス板を大気中で１５０℃に３０分間保持して膜を焼成した後に室温まで冷却した。このガラス板を実施例６４とした。
<Example 64>
First, the particle dispersion of Example 57 (dispersion in which Au particles having a concentration of about 30% by weight were dispersed) was diluted with hexane so that the content of Au particles was 20% by weight. A particle dispersion was prepared by dissolving 0.5% by weight of a photoinitiator (Irgacure 500 manufactured by Ciba Specialty Chemicals). Next, the diluted soda glass plate (length 100 mm, width 100 mm, thickness 2.8 mm) is kept at 40 ° C., and this diluted and prepared particle is rotated with a spin coater at a speed of 150 rpm. 5 cc of the dispersion was dropped and shaken for 120 seconds to prepare a film.
A stainless steel photomask was placed on each glass plate with the membrane facing upward. This photomask is formed in a square shape having a length × width × thickness of 100 mm × 100 mm × 1.0 mm, respectively, and three rectangular window holes each having a width × length of 20 mm × 50 mm are formed at intervals of 10 mm. . Next, after irradiating UV energy of 250 mJ / cm 2 from above the glass plate with an ultraviolet irradiation device (160 W metal halide lamp: distance 10 cm), the glass plate from which the photomask has been removed is placed on a hot plate and brought to 100 ° C. in the atmosphere. Hold for 10 minutes. Next, the glass plate is rinsed with an ethanol solution in which 10% by weight of N, N-dimethylformamide and 5% by weight of acetylacetone are mixed to dissolve the film of the non-light-irradiated portion, leaving only the light-irradiated film. A patterned film having the same shape as the rectangular window hole of the photomask was obtained. Further, this glass plate was kept at 150 ° C. in the air for 30 minutes to fire the film, and then cooled to room temperature. This glass plate was referred to as Example 64.
＜実施例６５＞
先ず実施例５８の粒子分散体（濃度約３０重量％のＰｔ粒子を分散した分散液）をプロピレングリコールモノメチルエーテルアセテートで、Ｐｔ粒子の含有量が２０重量％となるように希釈し、この希釈した粒子分散体に光開始剤（チバ・スペシャリティー・ケミカルズ社製のイルガキュア５００）を０．５重量％溶かして粒子分散体を調製した。次いで洗浄済みのソーダガラス板（縦１００ｍｍ、横１００ｍｍ、厚さ２．８ｍｍ）を４０℃に保温し、このソーダガラス板をスピンコーターで１５０ｒｐｍの速度で回転させた状態で、上記希釈調製した粒子分散体を５ｃｃ滴下し、１２０秒間振り切って膜を作製した。
上記膜を上に向けたガラス板にステンレス製フォトマスクをそれぞれ載せた。このフォトマスクは、縦×横×厚さがそれぞれ１００ｍｍ×１００ｍｍ×１．０ｍｍの正方形状に形成され、幅×長さがそれぞれ２０ｍｍ×５０ｍｍの長方形の窓孔が１０ｍｍ間隔で３個形成される。次いでガラス板の上方から紫外線照射装置（１６０Ｗメタルハライドランプ：距離１０ｃｍ）により２５０ｍＪ／ｃｍ2の紫外線エネルギを照射した後、フォトマスクを取除いたガラス板をホットプレートに載せて大気中で１００℃に１０分間保持した。次にN,N-ジメチルホルムアミド１０重量％及びアセチルアセトン５重量％を相溶させたエタノール溶液で上記ガラス板をリンスすることにより、非光照射部の膜を溶かし、光照射の膜だけを残して、フォトマスクの長方形の窓孔と同一形状のパターニングされた膜を得た。更にこのガラス板を大気中で１５０℃に３０分間保持して膜を焼成した後に室温まで冷却した。このガラス板を実施例６５とした。
<Example 65>
First, the particle dispersion of Example 58 (dispersion in which Pt particles having a concentration of about 30% by weight were dispersed) was diluted with propylene glycol monomethyl ether acetate so that the content of Pt particles was 20% by weight. A particle dispersion was prepared by dissolving 0.5 wt% of a photoinitiator (Irgacure 500 manufactured by Ciba Specialty Chemicals) into the particle dispersion. Next, the diluted soda glass plate (length 100 mm, width 100 mm, thickness 2.8 mm) is kept at 40 ° C., and this diluted and prepared particle is rotated with a spin coater at a speed of 150 rpm. 5 cc of the dispersion was dropped and shaken for 120 seconds to prepare a film.
A stainless steel photomask was placed on each glass plate with the membrane facing upward. This photomask is formed in a square shape having a length × width × thickness of 100 mm × 100 mm × 1.0 mm, respectively, and three rectangular window holes each having a width × length of 20 mm × 50 mm are formed at intervals of 10 mm. . Next, after irradiating UV energy of 250 mJ / cm 2 from above the glass plate with an ultraviolet irradiation device (160 W metal halide lamp: distance 10 cm), the glass plate from which the photomask has been removed is placed on a hot plate and brought to 100 ° C. in the atmosphere. Hold for 10 minutes. Next, the glass plate is rinsed with an ethanol solution in which 10% by weight of N, N-dimethylformamide and 5% by weight of acetylacetone are mixed to dissolve the film of the non-light-irradiated portion, leaving only the light-irradiated film. A patterned film having the same shape as the rectangular window hole of the photomask was obtained. Further, this glass plate was kept at 150 ° C. in the air for 30 minutes to fire the film, and then cooled to room temperature. This glass plate was referred to as Example 65.
＜比較試験６及び評価＞
実施例６１、６２、６４及び６５のガラス板の膜と実施例６３のアクリル板の膜の厚さと可視光透過率と体積抵抗率をそれぞれ測定した。上記膜の厚さは走査型電子顕微鏡（ＳＥＭ）にて測定し、透明膜の可視光透過率は分光光度計にて測定し、体積抵抗率は四探針法にて測定した。その結果を表７に示す。
<Comparative test 6 and evaluation>
The thickness, visible light transmittance, and volume resistivity of the glass plate films of Examples 61, 62, 64, and 65 and the acrylic plate film of Example 63 were measured. The thickness of the film was measured with a scanning electron microscope (SEM), the visible light transmittance of the transparent film was measured with a spectrophotometer, and the volume resistivity was measured with a four-probe method. The results are shown in Table 7.
１２ 混合物
１４ 粒子分散体
12
Claims (20)
前記混合物を所定の雰囲気中で４０〜３６０℃の温度に加熱した状態に１０分〜５．０時間保持して粒子分散体を得る工程と
を含む粒子分散体の製造方法であって、
前記粒子分散体は、溶媒で希釈してコロイド液の状態した場合に、密栓したガラス瓶に入れて４０℃に２週間保持した後の状態において沈殿せずにコロイド液の状態を保つ、粒子分散体の製造方法。 A step of preparing a mixture by mixing one or more selected from the group consisting of an organic metal compound and an organic metalloid compound and a reducing agent;
Maintaining the mixture in a predetermined atmosphere at a temperature of 40 to 360 ° C. for 10 minutes to 5.0 hours to obtain a particle dispersion;
A method for producing a particle dispersion comprising:
When the particle dispersion is diluted with a solvent to form a colloidal solution , the particle dispersion is kept in the state of the colloidal solution without being precipitated in a state after being placed in a sealed glass bottle and kept at 40 ° C. for 2 weeks. Manufacturing method.
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