JP2010196120A - 金属微粒子の製造方法、金属微粒子分散液ならびに焼結体 - Google Patents
金属微粒子の製造方法、金属微粒子分散液ならびに焼結体 Download PDFInfo
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- JP2010196120A JP2010196120A JP2009042862A JP2009042862A JP2010196120A JP 2010196120 A JP2010196120 A JP 2010196120A JP 2009042862 A JP2009042862 A JP 2009042862A JP 2009042862 A JP2009042862 A JP 2009042862A JP 2010196120 A JP2010196120 A JP 2010196120A
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- 239000010419 fine particle Substances 0.000 title claims abstract description 57
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 53
- 239000002184 metal Substances 0.000 title claims abstract description 53
- 239000006185 dispersion Substances 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title abstract description 18
- 239000002798 polar solvent Substances 0.000 claims abstract description 15
- 150000002344 gold compounds Chemical class 0.000 claims abstract description 8
- 230000003993 interaction Effects 0.000 claims abstract description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 16
- 239000010931 gold Substances 0.000 claims description 16
- 229910052737 gold Inorganic materials 0.000 claims description 16
- 150000003839 salts Chemical class 0.000 claims description 11
- 238000005245 sintering Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 12
- 239000012954 diazonium Substances 0.000 abstract description 11
- 150000001989 diazonium salts Chemical class 0.000 abstract description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 6
- 229910052717 sulfur Inorganic materials 0.000 abstract description 6
- 239000011593 sulfur Substances 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 239000002253 acid Substances 0.000 description 12
- -1 phosphino groups Chemical group 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000000862 absorption spectrum Methods 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000003223 protective agent Substances 0.000 description 4
- 238000001953 recrystallisation Methods 0.000 description 4
- 239000012279 sodium borohydride Substances 0.000 description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 description 4
- 235000010288 sodium nitrite Nutrition 0.000 description 4
- CKBBJIAJAWFJEZ-UHFFFAOYSA-M 2,4,6-trichlorobenzenediazonium;chloride Chemical compound [Cl-].ClC1=CC(Cl)=C([N+]#N)C(Cl)=C1 CKBBJIAJAWFJEZ-UHFFFAOYSA-M 0.000 description 3
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical class B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 3
- 239000007810 chemical reaction solvent Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 229940125904 compound 1 Drugs 0.000 description 2
- 229940125782 compound 2 Drugs 0.000 description 2
- 229940126214 compound 3 Drugs 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- VYFOAVADNIHPTR-UHFFFAOYSA-N isatoic anhydride Chemical compound NC1=CC=CC=C1CO VYFOAVADNIHPTR-UHFFFAOYSA-N 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- SDKPSXWGRWWLKR-UHFFFAOYSA-M sodium;9,10-dioxoanthracene-1-sulfonate Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)[O-] SDKPSXWGRWWLKR-UHFFFAOYSA-M 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 125000003396 thiol group Chemical class [H]S* 0.000 description 2
- OJZQOQNSUZLSMV-UHFFFAOYSA-N (3-aminophenyl)methanol Chemical compound NC1=CC=CC(CO)=C1 OJZQOQNSUZLSMV-UHFFFAOYSA-N 0.000 description 1
- QXHDYMUPPXAMPQ-UHFFFAOYSA-N 2-(4-aminophenyl)ethanol Chemical compound NC1=CC=C(CCO)C=C1 QXHDYMUPPXAMPQ-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000012448 Lithium borohydride Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
- 235000005811 Viola adunca Nutrition 0.000 description 1
- 240000009038 Viola odorata Species 0.000 description 1
- 235000013487 Viola odorata Nutrition 0.000 description 1
- 235000002254 Viola papilionacea Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 125000005036 alkoxyphenyl group Chemical group 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- JBANFLSTOJPTFW-UHFFFAOYSA-N azane;boron Chemical compound [B].N JBANFLSTOJPTFW-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 229910000085 borane Inorganic materials 0.000 description 1
- WVMHLYQJPRXKLC-UHFFFAOYSA-N borane;n,n-dimethylmethanamine Chemical compound B.CN(C)C WVMHLYQJPRXKLC-UHFFFAOYSA-N 0.000 description 1
- MOOAHMCRPCTRLV-UHFFFAOYSA-N boron sodium Chemical compound [B].[Na] MOOAHMCRPCTRLV-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-O diazynium Chemical group [NH+]#N IJGRMHOSHXDMSA-UHFFFAOYSA-O 0.000 description 1
- ZOCHARZZJNPSEU-UHFFFAOYSA-N diboron Chemical compound B#B ZOCHARZZJNPSEU-UHFFFAOYSA-N 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- IZLAVFWQHMDDGK-UHFFFAOYSA-N gold(1+);cyanide Chemical compound [Au+].N#[C-] IZLAVFWQHMDDGK-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002366 halogen compounds Chemical class 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- GKYQBMNOFTZZSX-UHFFFAOYSA-K n-ethylethanamine;trichlorogold Chemical compound Cl[Au](Cl)Cl.CCNCC GKYQBMNOFTZZSX-UHFFFAOYSA-K 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 125000000914 phenoxymethylpenicillanyl group Chemical group CC1(S[C@H]2N([C@H]1C(=O)*)C([C@H]2NC(COC2=CC=CC=C2)=O)=O)C 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000007261 regionalization Effects 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- BEOOHQFXGBMRKU-UHFFFAOYSA-N sodium cyanoborohydride Chemical compound [Na+].[B-]C#N BEOOHQFXGBMRKU-UHFFFAOYSA-N 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 1
- 229940071240 tetrachloroaurate Drugs 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Conductive Materials (AREA)
- Non-Insulated Conductors (AREA)
Abstract
Description
<参考例1>
下記式で表される化合物1を合成した。
赤外線吸収スペクトル 2278cm-1:N≡N+伸縮振動、3329cm-1:O−H伸縮振動、768cm-1:C−H面外変角振動
<参考例2>
下記式で表される化合物2を合成した。
赤外線吸収スペクトル 2274cm-1:N≡N+伸縮振動、3377cm-1:O−H伸縮振動、797cm-1:C−H面外変角振動
<参考例3>
下記式で表される化合物3を合成した。
赤外線吸収スペクトル 2262cm-1:N≡N+伸縮振動、3431cm-1:O−H伸縮振動、824cm-1:C−H面外変角振動
<実施例1>
テトラクロロ金(III)酸(0.1030g、0.2501mmol)をイオン交換水(25g)に溶解させ、N2を15分間フローし、脱気した。N2雰囲気下、化合物1(0.0555g、0.2501mmol)を加え、1分間攪拌させた後、イオン交換水7.5gで溶解させた水素化ホウ素ナトリウム(0.0095g、0.2511mmol)を室温下、2時間で滴下した。滴下後、2時間熟成し、黒紫色分散液が得られた。得られた分散液を遠心分離、水洗等で精製し、金含有量29.67ppmの黒紫色分散液が得られた。
紫外−可視吸収スペクトル 560nm
<実施例2>
テトラクロロ金(III)酸(0.1997g、0.4849mmol)をイオン交換水(45g)に溶解させ、N2を15分間フローし、脱気した。N2雰囲気下、化合物2(0.1076g、0.4848mmol)を加え、1分間攪拌させた後、イオン交換水15gで溶解させた水素化ホウ素ナトリウム(0.0183g、0.4837mmol)を室温下、2時間で滴下した。滴下後、2時間熟成し、青紫色分散液が得られた。得られた分散液を遠心分離、水洗等で精製し、金含有量785ppmの黒紫色分散液が得られた。
紫外−可視吸収スペクトル 578nm
<実施例3>
テトラクロロ金(III)酸(0.1545g、0.3751mmol)をイオン交換水(37.5g)に溶解させ、N2を15分間フローし、脱気した。N2雰囲気下、化合物3(0.0885g、0.3750mmol)を加え、1分間攪拌させた後、イオン交換水11.3gで溶解させた水素化ホウ素ナトリウム(0.0142g、0.3753mmol)を室温下、2時間で滴下した。滴下後、2時間熟成し、黒紫色分散液が得られた。得られた分散液を遠心分離、水洗等で精製し、金含有量704ppmの黒紫色分散液が得られた。
紫外−可視吸収スペクトル 583nm
なお、実施例1〜3の金微粒子について赤外線吸収スペクトルを測定した結果、ジアゾニウム基由来の吸収ピークが消失し、3645cm-1、3210cm-1付近にO−H伸縮振動、770〜860 cm-1の範囲に芳香環のC−H面外変角振動が認められた。
<実施例4>
実施例3で得られた分散液を4%に濃縮し、アルミナ基板に塗布した。空気雰囲気下、150℃または200℃で1時間焼結した結果、金属光沢のある膜が得られ、導電性が確認された。
Claims (3)
- 請求項2に記載の金属微粒子分散液を基材に塗布し焼結してなることを特徴とする焼結体。
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2012035198A (ja) * | 2010-08-06 | 2012-02-23 | Miyoshi Oil & Fat Co Ltd | 銀微粒子による新規触媒 |
JP2012117173A (ja) * | 2010-12-01 | 2012-06-21 | Miyoshi Oil & Fat Co Ltd | 金属微粒子担持材料 |
RU2584288C2 (ru) * | 2014-07-09 | 2016-05-20 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский политехнический университет" | Синтез ноль-валентных наночастиц металлов переходной группы с поверхностью, ковалентно модифицированной органическими функциональными группами |
Families Citing this family (1)
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JP6778371B2 (ja) * | 2015-01-23 | 2020-11-04 | ミヨシ油脂株式会社 | 金微粒子マトリックスメタロプロテアーゼ阻害剤 |
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- 2009-02-25 JP JP2009042862A patent/JP5438994B2/ja active Active
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JP2004263222A (ja) * | 2003-02-28 | 2004-09-24 | Tanaka Kikinzoku Kogyo Kk | 一元系又は多元系金属コロイド及び一元系又は多元系金属コロイドの製造方法 |
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JP2007302915A (ja) * | 2006-05-08 | 2007-11-22 | Katsuro Sato | 金属錯体微粒子及びその製造方法 |
JP2008083605A (ja) * | 2006-09-29 | 2008-04-10 | Az Electronic Materials Kk | 金属微粒子分散液からなるパターン形成用組成物およびパターン形成法 |
Non-Patent Citations (1)
Title |
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JPN6013042467; Fakhradin Mirkhalaf, Jerzy Paprotny, David J. Schiffrin: 'Synthesis of Metal Nanoparticles Stabilized by Metal-Carbon Bond' J. Am. Chem. Soc. Vol.128 No.23, 20060614, p.7400-7401 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2012035198A (ja) * | 2010-08-06 | 2012-02-23 | Miyoshi Oil & Fat Co Ltd | 銀微粒子による新規触媒 |
JP2012117173A (ja) * | 2010-12-01 | 2012-06-21 | Miyoshi Oil & Fat Co Ltd | 金属微粒子担持材料 |
RU2584288C2 (ru) * | 2014-07-09 | 2016-05-20 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский политехнический университет" | Синтез ноль-валентных наночастиц металлов переходной группы с поверхностью, ковалентно модифицированной органическими функциональными группами |
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