JP2011052284A - 金属微粒子の製造方法 - Google Patents
金属微粒子の製造方法 Download PDFInfo
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- JP2011052284A JP2011052284A JP2009202945A JP2009202945A JP2011052284A JP 2011052284 A JP2011052284 A JP 2011052284A JP 2009202945 A JP2009202945 A JP 2009202945A JP 2009202945 A JP2009202945 A JP 2009202945A JP 2011052284 A JP2011052284 A JP 2011052284A
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- Prior art keywords
- gelatin
- fine particles
- metal fine
- metal
- molecular weight
- Prior art date
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- 239000002184 metal Substances 0.000 title claims abstract description 71
- 239000010419 fine particle Substances 0.000 title claims abstract description 70
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 27
- 229920000159 gelatin Polymers 0.000 claims abstract description 77
- 108010010803 Gelatin Proteins 0.000 claims abstract description 73
- 235000019322 gelatine Nutrition 0.000 claims abstract description 73
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 73
- 239000008273 gelatin Substances 0.000 claims abstract description 71
- 239000002245 particle Substances 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 31
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 16
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 11
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- 238000009826 distribution Methods 0.000 claims abstract description 7
- 238000007385 chemical modification Methods 0.000 claims description 14
- 239000002923 metal particle Substances 0.000 claims description 9
- 229910001111 Fine metal Inorganic materials 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 3
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- -1 halogen ions Chemical class 0.000 description 25
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- 239000011593 sulfur Substances 0.000 description 23
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- 238000011282 treatment Methods 0.000 description 18
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- 229940055729 papain Drugs 0.000 description 3
- 235000019834 papain Nutrition 0.000 description 3
- 235000019419 proteases Nutrition 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 3
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- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 2
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Abstract
【解決手段】金属化合物が溶解あるいは分散している液中で、ゼラチンの存在下、前記金属化合物が持つ金属イオンを還元することにより、金属微粒子を得る方法において、前記ゼラチンの種類を選択することによって前記金属微粒子の粒子径を制御することを特徴とする、金属微粒子の製造方法。粒子径の制御とともに粒子径分布の制御をも行うことが出来る。
【選択図】なし
Description
本発明にかかる金属微粒子の製造方法は、遷移金属元素、典型金属元素のいずれにも適用でき、例えば、種々の用途に汎用的に用いられている、周期表第VIII族に属する鉄、コバルト、ニッケル、ルテニウム、ロジウム、パラジウム、オスミウム、イリジウム、白金や、周期表第IB族に属する銅、銀、金などへの適用が好ましい。中でも、導電性に優れる金、銀、白金、パラジウム、銅、ニッケルが好ましく、銅、銀、ニッケルがより好ましく、特に、廉価な銅が好ましい。また、これらは、1種に限らず、2種以上組み合せても良く、合金であっても良い。
本発明に用いるゼラチンは、牛や豚などの哺乳動物の骨、皮部分や、サメやティラピアなどの魚類の骨、皮、鱗部分などのコラーゲンを含有する原料から従来公知の方法で得ることができ、具体的には、例えば、熱水抽出、アルカリ処理、酸処理などによって得ることができる。
本発明にかかる金属微粒子の製造方法における還元処理としては、特に限定されず、例えば、還元剤を添加することによって行っても良いし、還元剤を用いない電解還元などによる還元処理であっても良い。
本発明にかかる金属微粒子の製造方法により得られる金属微粒子は、所望の平均粒子径を有するものであり、金属微粒子が使用される一般的な用途、例えば、塗料、インキ、金属微粒子ペーストなどとして好適に利用できる。より具体的には、平均粒子径が10〜50nmのものであれば塗料などに好適に利用でき、平均粒子径が30〜500nmのものであれば金属微粒子ペーストなどに好適に利用できる。なお、ここにいう平均粒子径の値は、後述の実施例記載の方法で測定される値を基準としている。
ゼラチンやその加水分解物の重量平均分子量や数平均分子量は、パギイ法により測定した。ここで「パギイ法」とは、高速液体クロマトグラフィーを用いたゲル濾過法によって、試料溶液のクロマトグラムを求め、分子量分布を推定する方法である。具体的には、以下の方法により測定した。
カラム温度:50℃
測定波長:230nm
分子量既知のプルラン(P−82、昭和電工社製)で溶出時間を求めて検量線を作成した。その後、ゼラチンを分析し、検体の重量平均分子量と数平均分子量を下式から求めた。下式において、Siは各ポイントでの吸光度、Miは溶出時間Tiでの分子量である。
数平均分子量=ΣSi/(ΣSi/Mi)
<金属微粒子の平均粒子径>
SEM写真観察により視野から無作為に粒子を選択して平均粒子径を求めた。
「G−0749K」(魚由来のゼラチン、重量平均分子量110000、数平均分子量24000、新田ゼラチン社製)200gを50℃の温水1800gに溶解し、WSC(水溶性カルボジイミド、同仁化学社製)46gを添加し、さらにメチオニン48gを添加して、50℃、pH7.0の条件で2時間反応させた。つぎに、化学修飾後のゼラチン90gを60℃の温水210gに溶解した。前記ゼラチンゾルにパパイン(タンパク質分解酵素、メルク社製)9mgを添加し、前記酵素の加水分解最適条件下となるように温度60℃、pH7.0に調整して、90分間加水分解処理を行った後、ゾルを75℃に加熱することにより、酵素を失活させた。
製造例1において、メチオニン48gに代えて、リジン44gを用いた以外は同様にして、化学修飾および加水分解がなされたゼラチンを得た。このゼラチンの重量平均分子量は9100、数平均分子量は2200であった。
「G−0749K」(魚由来のゼラチン、重量平均分子量110000、数平均分子量24000、新田ゼラチン社製)90gを60℃の温水210gに溶解した。前記ゼラチンゾルにパパイン(タンパク質分解酵素、メルク社製)9mgを添加し、前記酵素の加水分解最適条件下となるように温度60℃、pH7.0に調整して、90分間加水分解処理を行った後、ゾルを75℃に加熱することにより、酵素を失活させた。
製造例3において、酵素量を27mg、加水分解処理時間を100分間に変更したこと以外は同様にして、重量平均分子量5900、数平均分量700の加水分解ゼラチンを得た。
上記製造例1〜4のゼラチンを保護コロイドとして用いて、以下の操作により、各金属微粒子を製造した。
「G−0749K」(魚由来のゼラチン、重量平均分子量110000、数平均分子量24000、新田ゼラチン社製)を用いたこと以外は、実施例1〜4と同様にして、金属微粒子を製造した。
「G−0750」(魚由来のゼラチン、重量平均分子量170000、数平均分子量39000、新田ゼラチン社製)を用いたこと以外は、実施例1〜4と同様にして、金属微粒子を製造した。
「G−0746K」(牛由来のゼラチン、重量平均分子量190000、数平均分子量50000、新田ゼラチン社製)を用いたこと以外は、実施例1〜4と同様にして、金属微粒子を製造した。
各実施例1〜7で得られた金属微粒子の平均粒子径を表1に示すとともに、各実施例1〜7で得られた各金属微粒子について、各SEM写真を図1〜7に示す。
Claims (5)
- 金属化合物が溶解あるいは分散している液中で、ゼラチンの存在下、前記金属化合物が持つ金属イオンを還元することにより、金属微粒子を得る方法において、前記ゼラチンの種類を選択することによって前記金属微粒子の粒子径を制御することを特徴とする、金属微粒子の製造方法。
- 前記粒子径の制御とともに粒子径分布の制御をも行う、請求項1に記載の金属微粒子の製造方法。
- 前記ゼラチンの種類の選択が、ゼラチンの平均分子量の大小の選択である、請求項1または2に記載の金属微粒子の製造方法。
- 前記ゼラチンの種類の選択が、ゼラチンに対する化学修飾の有無の選択か、および/または、化学修飾の内容の選択である、請求項1から3までのいずれかに記載の金属微粒子の製造方法。
- 前記ゼラチンの種類の選択が、ゼラチンを得るための原料の選択である、請求項1から4までのいずれかに記載の金属微粒子の製造方法。
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