JP2008075181A - マイクロ波を用いた銅ナノ粒子の製造方法 - Google Patents
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Abstract
【解決手段】本発明は、(a)銅塩、分散剤、還元剤及び有機溶媒を含む混合溶液を調製する段階と、(b)前記混合溶液の温度を30ないし50℃に昇温させて撹拌する段階と、(c)前記混合溶液にマイクロ波を照射する段階と、及び(d)前記混合溶液の温度を低下させて銅ナノ粒子を得る段階と、を含む銅ナノ粒子の製造方法を提供する。
【選択図】図2
Description
(a)銅塩、分散剤、還元剤及び有機溶媒を含む混合溶液を調製する段階と、
(b)前記混合溶液の温度を30ないし50℃に昇温させて撹拌する段階と、
(c)前記混合溶液にマイクロ波を照射する段階と、及び
(d)前記混合溶液の温度を低下させて銅ナノ粒子を得る段階と
を含む銅ナノ粒子の製造方法が提供される。
(a)銅塩、分散剤、還元剤及び有機溶媒を含む混合溶液を調製する段階と、(b)前記混合溶液の温度を30ないし50℃に昇温させて撹拌する段階と、(c)前記混合溶液にマイクロ波を照射する段階と、及び(d)前記混合溶液の温度を低下させて銅ナノ粒子を得る段階とを含む。
硫酸銅0.1モル、次亜リン酸ナトリウム0.4モル、PVP1モル及びエチレングリコール500mlをビーカーで混合して40℃に昇温した後、撹拌機を用いて溶解させて混合溶液を製造した。製造した混合溶液をマイクロ波オーブンに投入して3分間マイクロ波を照射した。還元反応により黒褐色の反応物が得られたらマイクロ波の照射を止め、前記混合溶液に予め冷却した蒸留水500mlを投入して急冷した。遠心分離により黒褐色の銅ナノ粒子を回収し、アセトンと蒸留水とを用いて3回洗浄した後、50℃の真空乾燥器で3時間乾燥して、最終的に粉末形態の銅ナノ粒子6gを得た。
硫酸銅0.2モル、次亜リン酸ナトリウム0.8モル、PVP2モル及びエチレングリコール1000mlをビーカー中で混合して40℃に昇温した後、撹拌機を用いて溶解させて混合溶液を製造した。製造した混合溶液をマイクロ波オーブンに投入して7分間マイクロ波を照射した。還元反応により黒褐色の反応物が得られたら、マイクロ波の照射を止め、前記混合溶液に予め冷却した蒸留水1000mlを投入して急冷した。遠心分離により黒褐色の銅ナノ粒子を回収し、アセトンと蒸留水とを用いて3回洗浄した後、50℃の真空乾燥器で3時間乾燥して最終的に粉末形態の銅ナノ粒子12gを得た。
Claims (12)
- (a)銅塩、分散剤、還元剤及び有機溶媒を含む混合溶液を調製する段階と、
(b)前記混合溶液の温度を30ないし50℃に昇温させて撹拌する段階と、
(c)前記混合溶液にマイクロ波を照射する段階と、及び
(d)前記混合溶液の温度を低下させて銅ナノ粒子を得る段階と
を含む銅ナノ粒子の製造方法。 - 前記銅塩が、塩化銅(CuCl2)、硝酸銅(Cu(NO3)2)、硫酸銅(CuSO4)、酢酸銅((CH3COO)2Cu)、アセチルアセトナト銅(copper(II)acetylacetonate)、炭酸銅(copper(II)carbonate)、銅シクロヘキサンブチレート(copper(II)cyclohexanebutyrate)、ステアリン酸銅(copper(II)stearate)、過塩素酸銅(copper(II)perchlorate)、エチレンジアミン銅(copper(II)ethylenediamine)及び水酸化銅(Cu(OH)2)からなる群より選ばれる少なくとも一つである請求項1に記載の銅ナノ粒子の製造方法。
- 前記銅塩が、0.001ないし1mol/Lの範囲で前記混合溶液に含まれる請求項1に記載の銅ナノ粒子の製造方法。
- 前記分散剤が、ポリビニルピロリドン(Polyvinylpyrrolidone、PVP)、セチルトリメチルアンモニウムブロミド(Cetyltrimethyl ammonium bromide、CTAB)、ドデシル硫酸ナトリウム(Sodium dodecyl sulfate、SDS)及びソジウムカルボキシメチルセルロース(Sodiumcarboxymethylcellulose、Na−CMC)からなる群より選ばれる少なくとも一つである請求項1に記載の銅ナノ粒子の製造方法。
- 前記分散剤が、銅塩1モルに対して1ないし20モルの比率で前記混合溶液に含まれる請求項1に記載の銅ナノ粒子の製造方法。
- 前記還元剤が、次亜リン酸ナトリウム(NaH2PO2)、ヒドラジン(N2H4)、塩化水素及びソジウムボロハイドライド(NaBH4)からなる群より選ばれる少なくとも一つである請求項1に記載の銅ナノ粒子の製造方法。
- 前記還元剤が、銅塩1モルに対して2ないし6モルの比率で前記混合溶液に含まれる請求項1に記載の銅ナノ粒子の製造方法。
- 前記有機溶媒が、エチレングリコール、ジエチレングリコール、トリエチレングリコール及びポリエチレングリコールからなる群より選ばれる少なくとも一つである請求項1に記載の銅ナノ粒子の製造方法。
- 前記マイクロ波の照射強度が、0.01ないし0.5W/cm3である請求項1に記載の銅ナノ粒子の製造方法。
- 前記マイクロ波の照射時間が、2ないし10分間である請求項1に記載の銅ナノ粒子の製造方法。
- (d)段階が、冷却した蒸留水を用いて混合溶液を急冷して行われる請求項1に記載の銅ナノ粒子の製造方法。
- (d)段階が、さらに前記混合溶液を遠心分離して銅ナノ粒子を分離する段階と、前記分離した銅ナノ粒子を洗浄した後乾燥させる段階とを含む請求項1に記載の銅ナノ粒子の製造方法。
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US8864871B2 (en) | 2014-10-21 |
US20080072706A1 (en) | 2008-03-27 |
JP5068614B2 (ja) | 2012-11-07 |
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