JP2006152327A - 銀粉およびその製造方法 - Google Patents
銀粉およびその製造方法 Download PDFInfo
- Publication number
- JP2006152327A JP2006152327A JP2004340789A JP2004340789A JP2006152327A JP 2006152327 A JP2006152327 A JP 2006152327A JP 2004340789 A JP2004340789 A JP 2004340789A JP 2004340789 A JP2004340789 A JP 2004340789A JP 2006152327 A JP2006152327 A JP 2006152327A
- Authority
- JP
- Japan
- Prior art keywords
- silver powder
- silver
- acid
- reducing agent
- reaction system
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 229910052709 silver Inorganic materials 0.000 claims abstract description 37
- 239000004332 silver Substances 0.000 claims abstract description 37
- -1 silver ions Chemical class 0.000 claims abstract description 27
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 12
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 11
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 10
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 10
- 239000000194 fatty acid Substances 0.000 claims description 10
- 229930195729 fatty acid Natural products 0.000 claims description 10
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 8
- 230000009467 reduction Effects 0.000 claims description 8
- 235000010323 ascorbic acid Nutrition 0.000 claims description 5
- 239000011668 ascorbic acid Substances 0.000 claims description 5
- 229960005070 ascorbic acid Drugs 0.000 claims description 5
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- 125000002524 organometallic group Chemical group 0.000 claims 1
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- 238000000151 deposition Methods 0.000 abstract 1
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- 238000006722 reduction reaction Methods 0.000 description 8
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- 230000000052 comparative effect Effects 0.000 description 5
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- 229910052751 metal Inorganic materials 0.000 description 4
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- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 230000020169 heat generation Effects 0.000 description 3
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- 229920000178 Acrylic resin Polymers 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 2
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- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
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- 229910021529 ammonia Inorganic materials 0.000 description 2
- YZXBAPSDXZZRGB-DOFZRALJSA-N arachidonic acid Chemical compound CCCCC\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O YZXBAPSDXZZRGB-DOFZRALJSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 2
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- 238000010304 firing Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 2
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
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- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 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
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- AXAZMDOAUQTMOW-UHFFFAOYSA-N dimethylzinc Chemical compound C[Zn]C AXAZMDOAUQTMOW-UHFFFAOYSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
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- 238000011156 evaluation Methods 0.000 description 1
- 125000005313 fatty acid group Chemical group 0.000 description 1
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- 235000004515 gallic acid Nutrition 0.000 description 1
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- 235000019322 gelatine Nutrition 0.000 description 1
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- 238000009423 ventilation Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
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Abstract
【解決手段】 銀イオンを含有する水性反応系に還元剤を添加して銀粒子を還元析出させた後、乾燥することにより得られた銀粉を100℃より高く且つ400℃より低い温度で熱処理することにより、50℃から800℃における最大熱膨張率が1.5%以下であり、50℃から800℃まで加熱した際に発熱ピークがなく、800℃で恒量になるまで強熱したときの強熱減量が1.0%以下、タップ密度が2g/cm3以上、BET比表面積が5m2/g以下である銀粉を製造する。
【選択図】 図1
Description
銀イオンとして12g/Lの硝酸銀溶液3600mLに、工業用のアンモニア水180mLを加えて、銀のアンミン錯体溶液を生成した。この銀のアンミン錯体溶液に水酸化ナトリウム1gを加えてpH調整した後、還元剤として工業用のホルマリン192mLを15秒で加えた。その直後に、ステアリン酸0.1gを加えて銀のスラリーを得た。この銀のスラリーをろ過、水洗した後、乾燥して銀粉を得た。この銀粉を大気中において150℃で6時間熱処理した。
T℃における熱膨張率(%)=(LT−L50)/L50×100
ここで、L50およびLTは、それぞれ試料温度が50℃およびT℃におけるペレット状の銀粉試料の長さ(mm)である。
強熱減量(%)=(w1−w2)/w1×100
熱処理の条件を250℃で2時間とした以外は実施例1と同様の方法により得られた銀粉について、実施例1と同様の方法により熱膨張率、強熱減量、発熱量、BET比表面積およびタップ密度を測定し、焼成体の評価を行った。
銀イオンとして12g/Lの硝酸銀溶液3600mLに、工業用のアンモニア140mLを加えて、銀のアンミン錯体溶液を生成した。この銀のアンミン錯体溶液に還元剤としてヒドラジンの60%溶液17mLを加えた。その直後に、分散剤としてオレイン酸0.2gを加えて銀のスラリーを得た。この銀のスラリーをろ過、水洗した後、乾燥して銀粉を得た。この銀粉を大気中において150℃で6時間熱処理した。
熱処理を施さなかった以外は実施例1と同様の方法により得られた銀粉について、実施例1と同様の方法により熱膨張率、強熱減量、発熱量、BET比表面積およびタップ密度を測定し、焼成体の評価を行った。
熱処理の条件を100℃で20時間とした以外は実施例1と同様の方法により得られた銀粉について、実施例1と同様の方法により熱膨張率、強熱減量、発熱量、BET比表面積およびタップ密度を測定し、焼成体の評価を行った。
熱処理の条件を450℃で2時間とした以外は実施例1と同様の方法により得られた銀粉について、実施例1と同様の方法により熱膨張率、強熱減量、発熱量、BET比表面積およびタップ密度を測定し、焼成体の評価を行った。
Claims (8)
- 銀イオンを含有する水性反応系に還元剤を添加して銀粒子を還元析出させた後、乾燥することにより得られた銀粉を100℃より高く且つ400℃より低い温度で熱処理することを特徴とする、銀粉の製造方法。
- 前記銀粒子の還元析出前または還元析出後のスラリー状の反応系に分散剤を添加することを特徴とする、請求項1に記載の銀粉の製造方法。
- 前記分散剤が、脂肪酸、脂肪酸塩、界面活性剤、有機金属、キレート形成剤および保護コロイドからなる群から選ばれる1種類以上の分散剤であることを特徴とする、請求項2に記載の銀粉の製造方法。
- 前記還元剤が、アスコルビン酸、アルカノールアミン、ヒドロキノン、ヒドラジンおよびホルマリンからなる群から選ばれる1種以上の還元剤であることを特徴とする、請求項1乃至3のいずれかに記載の銀粉の製造方法。
- 前記還元剤を、前記銀イオンを含有する水性反応系の銀の含有量に対して1当量/分以上の速度で添加することを特徴とする、請求項1乃至4のいずれかに記載の銀粉の製造方法。
- 50℃から800℃における最大熱膨張率が1.5%以下であり、800℃で恒量になるまで強熱したときの強熱減量が1.0%以下であることを特徴とする、銀粉。
- 50℃から800℃まで加熱した際に発熱ピークがないことを特徴とする、請求項6に記載の銀粉。
- タップ密度が2g/cm3以上であり、BET比表面積が5m2/g以下であることを特徴とする、請求項6または7に記載の銀粉。
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JP2004340789A JP5028695B2 (ja) | 2004-11-25 | 2004-11-25 | 銀粉およびその製造方法 |
US11/285,140 US8282702B2 (en) | 2004-11-25 | 2005-11-21 | Silver powder and method for producing same |
DE602005023402T DE602005023402D1 (de) | 2004-11-25 | 2005-11-23 | Silberpulver sowie Verfahren zu dessen Herstellung |
TW094141185A TWI367137B (en) | 2004-11-25 | 2005-11-23 | Silver powder and method for producing same |
EP05025568A EP1666174B1 (en) | 2004-11-25 | 2005-11-23 | Silver powder and method for producing same |
AT05025568T ATE480350T1 (de) | 2004-11-25 | 2005-11-23 | Silberpulver sowie verfahren zu dessen herstellung |
KR1020050113277A KR101141839B1 (ko) | 2004-11-25 | 2005-11-25 | 은분 및 그의 제조 방법 |
CN2009100044047A CN101513671B (zh) | 2004-11-25 | 2005-11-25 | 银粉及其制造方法 |
CN2005101287156A CN1781630B (zh) | 2004-11-25 | 2005-11-25 | 银粉及其制造方法 |
US13/468,468 US8992701B2 (en) | 2004-11-25 | 2012-05-10 | Silver powder and method for producing same |
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2005
- 2005-11-21 US US11/285,140 patent/US8282702B2/en active Active
- 2005-11-23 DE DE602005023402T patent/DE602005023402D1/de active Active
- 2005-11-23 AT AT05025568T patent/ATE480350T1/de not_active IP Right Cessation
- 2005-11-23 TW TW094141185A patent/TWI367137B/zh active
- 2005-11-23 EP EP05025568A patent/EP1666174B1/en not_active Ceased
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Publication number | Priority date | Publication date | Assignee | Title |
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WO2007004649A1 (ja) * | 2005-07-05 | 2007-01-11 | Mitsui Mining & Smelting Co., Ltd. | 高結晶銀粉及びその高結晶銀粉の製造方法 |
KR101061841B1 (ko) | 2009-01-13 | 2011-09-05 | 충남대학교산학협력단 | 화학환원법에 의한 단분산 구형 은 분말의 제조방법 |
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JP2012153979A (ja) * | 2012-04-02 | 2012-08-16 | Dowa Holdings Co Ltd | 銀粉およびその製造方法 |
JP2015071814A (ja) * | 2013-10-03 | 2015-04-16 | 住友金属鉱山株式会社 | 銀粉の製造方法 |
Also Published As
Publication number | Publication date |
---|---|
DE602005023402D1 (de) | 2010-10-21 |
CN101513671A (zh) | 2009-08-26 |
US20120219453A1 (en) | 2012-08-30 |
KR20060058655A (ko) | 2006-05-30 |
TWI367137B (en) | 2012-07-01 |
EP1666174B1 (en) | 2010-09-08 |
CN101513671B (zh) | 2010-12-08 |
EP1666174A3 (en) | 2006-09-13 |
US8992701B2 (en) | 2015-03-31 |
TW200626262A (en) | 2006-08-01 |
ATE480350T1 (de) | 2010-09-15 |
CN1781630B (zh) | 2010-08-04 |
US8282702B2 (en) | 2012-10-09 |
JP5028695B2 (ja) | 2012-09-19 |
CN1781630A (zh) | 2006-06-07 |
KR101141839B1 (ko) | 2012-05-07 |
EP1666174A2 (en) | 2006-06-07 |
US20060107791A1 (en) | 2006-05-25 |
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