JP2009090378A - 金属ナノ粒子無機複合体の製造方法および金属ナノ粒子無機複合体 - Google Patents
金属ナノ粒子無機複合体の製造方法および金属ナノ粒子無機複合体 Download PDFInfo
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Abstract
【課題】化学合成方法を用いて、固体化したマトリックス中に均一に分散された、微細な金属ナノ粒子を有する金属ナノ粒子無機複合体の製造方法およびこの製造方法による金属ナノ粒子無機複合体を提供する。
【解決手段】基板上に、金属アルコキシドを酸触媒の作用により部分加水分解するゾルゲル法で、微細孔を有する酸化膜14を形成する酸化膜形成工程と、この酸化膜14を酸性の塩化スズ水溶液と接触させるSn析出工程と、微細孔からSn2+イオンを除去するSn2+イオン除去工程と、酸化膜14を金属キレート水溶液と接触させ、微細孔中に金属ナノ粒子12を析出させる金属ナノ粒子析出工程と、微細孔から金属イオンを除去する金属イオン除去工程を備えることを特徴とする金属ナノ粒子無機複合体10の製造方法およびこの製造方法による金属ナノ粒子無機複合体10。
【選択図】図1
Description
Y.Kobayashi,V.S.−Maceira and L.M.L.−Marzan,"Deposition of Silver Nanoparticles on Silica Sphereres by Pretreatment Steps in Electorores Plating,"Chem.Mater.,(2001),13,pp1630−1633. B.Zhang,H.Masumoto,Y.Someno and T.Goto,"Optical Properties of Au/SiO2 Nano−Composite Films Prepared by Induction−Coil−Coupled Plasma Sputtring,"Mater.Trans.,44[2],(2003),pp215−219
前記酸化物の割合をa(wt%)、前記金属ナノ粒子の割合をb(wt%)、前記スズ酸化物の割合をc(wt%)と表記した場合に、30≦a≦70、20≦b≦50、1≦c≦30であることを特徴とすることを特徴とする。
本発明の第1の実施の形態の金属ナノ粒子無機複合体の製造方法は、基板上に、金属アルコキシドを酸触媒の作用により部分加水分解するゾルゲル法で、微細孔を有する酸化膜を形成する酸化膜形成工程と、形成された酸化膜を酸性の塩化スズ水溶液と接触させるSn析出工程と、酸化膜中の微細孔からSn2+イオンを除去するSn2+イオン除去工程と、酸化膜を金属キレート水溶液と接触させ、微細孔中に金属ナノ粒子を析出させる金属ナノ粒子析出工程と、微細孔から金属イオンを除去する金属イオン除去工程を備えている。
本発明の第2の実施の形態の金属ナノ粒子無機複合体の製造方法は、Sn析出工程から金属イオン除去工程を複数回繰り返すことと、金属ナノ粒子析出工程の後、Sn析出工程の前に、微細孔からSn2+イオンを除去する第2のSn2+イオン除去工程を有すること以外は、基本的に第1の実施の形態と同様である。したがって、第1の実施の形態と重複する記述については、記載を省略する。
まず、石英ガラス基板の上に酸触媒を用いてSiO2膜を作製した。セパラブル・フラスコに、エタノール100ml、イオン交換水20ml、1mol/l塩酸水溶液10mlを加え、30℃に保持して30分程度混合した。次にTEOSを21g添加して、更に3h程度混合した。20×50×1mmの石英ガラス基板は、水、エタノール、アセトンで洗浄した後、UVドライ洗浄を行い、実験に供した。スピナーを使い、1000rpm×30sで調製した前駆体溶液を石英ガラス基板に塗布した。その後、室温で24h保持し、加水分解及び縮重合反応を起こさせた。
比較例として、塩基触媒を用いてSiO2膜を作製した。セパラブル・フラスコに、エタノール100ml、25%アンモニア水10mlを加え、30℃で30分程度混合し、ついでTEOSを3.5g添加し、3h程度混合した。これ以外は、実施例1と同様の処理を行った。
実施例1と同様にSiO2膜を作製した。まず、石英ガラス基板の上に酸触媒を用いてSiO2膜を作製した。セパラブル・フラスコに、エタノール150ml、イオン交換水27ml、1mol/l硝酸水溶液15mlを加え、30℃に保持して15分程度混合した。次にTEOSを31g添加して、更に2h程度混合した。
実施例1と同様にSiO2膜を作製した。まず、石英ガラス基板の上に酸触媒を用いてSiO2膜を作製した。セパラブル・フラスコに、エタノール100ml、イオン交換水20ml、1mol/l塩酸水溶液10mlを加え、30℃に保持して30分程度混合した。次にTEOSを21g添加して、更に3h程度混合した。20×50×1mmの石英ガラス基板は、水、エタノール、アセトンで洗浄した後、UVドライ洗浄を行い、実験に供した。スピナーを使い、1000rpm×30sで調製した前駆体溶液を石英ガラス基板に塗布した。その後、室温で24h保持し、加水分解及び縮重合反応を起こさせた。
実施例1と同様にSiO2膜を作製した。まず、石英ガラス基板の上に酸触媒を用いてSiO2膜を作製した。セパラブル・フラスコに、エタノール100ml、イオン交換水20ml、1mol/l塩酸水溶液10mlを加え、30℃に保持して30分程度混合した。次にTEOSを21g添加して、更に3h程度混合した。20×50×1mmの石英ガラス基板は、水、エタノール、アセトンで洗浄した後、UVドライ洗浄を行い、実験に供した。スピナーを使い、1000rpm×30sで調製した前駆体溶液を石英ガラス基板に塗布した。その後、室温で24h保持し、加水分解及び縮重合反応を起こさせた。
実施例1と同様にSiO2膜を作製した。まず、石英ガラス基板の上に酸触媒を用いてSiO2膜を作製した。セパラブル・フラスコに、エタノール100ml、イオン交換水20ml、1mol/l塩酸水溶液10mlを加え、30℃に保持して30分程度混合した。次にTEOSを21g添加して、更に3h程度混合した。20×50×1mmの石英ガラス基板は、水、エタノール、アセトンで洗浄した後、UVドライ洗浄を行い、実験に供した。スピナーを使い、1000rpm×30sで調製した前駆体溶液を石英ガラス基板に塗布した。その後、室温で24h保持し、加水分解及び縮重合反応を起こさせた。
実施例1と同様にSiO2膜を作製した。まず、石英ガラス基板の上に酸触媒を用いてSiO2膜を作製した。セパラブル・フラスコに、エタノール100ml、イオン交換水20ml、1mol/l塩酸水溶液10mlを加え、30℃に保持して30min.程度混合した。次にTEOSを21g添加して、更に3h程度混合した。20×50×1tmmの石英ガラス基板は、水、エタノール、アセトンで洗浄した後、UVドライ洗浄を行い、実験に供した。スピナーを使い、1000rpm×30sで調製した前駆体溶液を石英ガラス基板に塗布した。その後、室温で24h保持し、加水分解及び縮重合反応を起こさせた。
実施例1と同様にSiO2膜を作製した。まず、石英ガラス基板の上に酸触媒を用いてSiO2膜を作製した。セパラブル・フラスコに、エタノール100ml、イオン交換水20ml、1mol/l塩酸水溶液10mlを加え、30℃に保持して30分程度混合した。次にTEOSを21g添加して、更に3h程度混合した。20×50×1tmmの石英ガラス基板は、水、エタノール、アセトンで洗浄した後、UVドライ洗浄を行い、実験に供した。スピナーを使い、1000rpm×30sで調製した前駆体溶液を石英ガラス基板に塗布した。その後、室温で24h保持し、加水分解及び縮重合反応を起こさせた。
まず、石英ガラス基板の上に酸触媒を用いてAl2O3膜を作製した。セパラブル・フラスコに、エタノール150ml、イオン交換水27ml、1mol/l硝酸水溶液15mlを加え、30℃に保持して15min.程度混合した。次にAl(OC3H7)3を21g添加して、更に2h程度混合した。
12 Agナノ粒子
14 SiO2マトリックス相
20 洗浄装置
22 流入口
24 排出口
26 試料保持網台
28 試料
30 蒸留水
Claims (15)
- 基板上に、金属アルコキシドを酸触媒の作用により部分加水分解するゾルゲル法で、微細孔を有する酸化膜を形成する酸化膜形成工程と、
前記酸化膜を酸性の塩化スズ水溶液と接触させるSn析出工程と、
前記微細孔からSn2+イオンを除去するSn2+イオン除去工程と、
前記酸化膜を金属キレート水溶液と接触させ、前記微細孔中に金属ナノ粒子を析出させる金属ナノ粒子析出工程と、
前記微細孔から金属イオンを除去する金属イオン除去工程を備えることを特徴とする金属ナノ粒子無機複合体の製造方法。 - 前記Sn析出工程から前記金属イオン除去工程を複数回繰り返すことを特徴とする請求項1記載の金属ナノ粒子無機複合体の製造方法。
- 前記Sn析出工程と前記Sn2+イオン除去工程を連続して繰り返すことを特徴とする請求項1または請求項2に記載の金属ナノ粒子無機複合体の製造方法。
- 前記金属ナノ粒子析出工程の後、前記Sn析出工程の前に、前記微細孔からSn2+イオンを除去する第2のSn2+イオン除去工程を有することを特徴とする請求項2記載の金属ナノ粒子無機複合体の製造方法。
- 前記Sn2+イオン除去工程が、水または水溶液に前記酸化膜を浸漬する処理であることを特徴とする請求項1ないし請求項4いずれか一項に記載の金属ナノ粒子無機複合体の製造方法。
- 前記Sn2+イオン除去工程が、水または水溶液が循環する装置内に前記酸化膜を浸漬する処理であることを特徴とする請求項1ないし請求項4いずれか一項に記載の金属ナノ粒子無機複合体の製造方法。
- 前記第2のSn2+イオン除去工程が、前記金属ナノ粒子析出工程後、前記酸化膜を12時間以上溶液中あるいは大気中に保持することで、Sn2+をSn4+に変化させる処理であることを特徴とする請求項4記載の金属ナノ粒子無機複合体の製造方法。
- 前記第2のSn2+イオン除去工程が、前記金属ナノ粒子析出工程後、前記酸化膜を50℃以上100℃未満の温度で加熱をすることで、Sn2+をSn4+に変化させる処理であることを特徴とする請求項4記載の金属ナノ粒子無機複合体の製造方法。
- 前記金属アルコキシドがオルガノシランであって、前記酸化膜がSiO2膜であることを特徴とする請求項1ないし請求項8いずれか一項に記載の金属ナノ粒子無機複合体の製造方法。
- 前記金属キレート水溶液が、銀塩およびアンモニアを含む水溶液によって調製されたAg(NH3)2 +キレート水溶液であることを特徴とする請求項1ないし請求項9いずれか一項に記載の金属ナノ粒子無機複合体の製造方法。
- 前記SiO2膜形成工程後の前記SiO2膜が、IR測定において3400cm−1近傍および950cm−1近傍にOH基によるピークを示し、かつ、前記SiO2膜が含有するCl濃度が重量組成比で、SiO2/Cl=50〜80/1であり、かつ、前記微細孔の孔径が10nm以下であり、前記微細孔がネットワーク状に発達していることを特徴とする請求項9記載の金属ナノ粒子無機複合体の製造方法。
- SiO2,B2O3,Al2O3,TiO2,ZrO2,Na2O,CaO,SrOからなる群の中の少なくとも1つの酸化物を含む可視光に対して透明な酸化物と、
前記酸化物中に分散されたAu,Ag,Cu,Pt,Pb,Ph,Cd,In,Pdからなる群の中の少なくとも1つの金属を含む金属ナノ粒子と、
前記酸化物中に分散されたスズ酸化物(SnO2)とを含み、
前記酸化物の割合をa(wt%)、前記金属ナノ粒子の割合をb(wt%)、前記スズ酸化物の割合をc(wt%)と表記した場合に、
30≦a≦70、20≦b≦50、1≦c≦30であることを特徴とする金属ナノ粒子無機複合体。 - 前記酸化物がSiO2であり、前記金属がAgであることを特徴とする請求項12記載の金属ナノ粒子無機複合体。
- 前記酸化物の割合をa(wt%)、前記金属ナノ粒子の割合をb(wt%)、前記スズ酸化物の割合をc(wt%)と表記した場合に、
35≦a≦45、35≦b≦45、15≦c≦25であることを特徴とする請求項13記載の金属ナノ粒子無機複合体。 - Fを0.5〜3wt%、Clを0.1〜1.0wt%を含有することを特徴とする請求項13または請求項14記載の金属ナノ粒子無機複合体。
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