JP2014198905A - 被覆銀超微粒子とその製造方法 - Google Patents
被覆銀超微粒子とその製造方法 Download PDFInfo
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- JP2014198905A JP2014198905A JP2014111297A JP2014111297A JP2014198905A JP 2014198905 A JP2014198905 A JP 2014198905A JP 2014111297 A JP2014111297 A JP 2014111297A JP 2014111297 A JP2014111297 A JP 2014111297A JP 2014198905 A JP2014198905 A JP 2014198905A
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- 150000003973 alkyl amines Chemical class 0.000 claims abstract description 90
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- Powder Metallurgy (AREA)
- Conductive Materials (AREA)
- Non-Insulated Conductors (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
【解決手段】粒子径が30nm以下の、保護分子アミンにより覆われた有機溶剤に分散可能な被覆銀超微粒子であって、熱重量測定において160℃の温度における重量減少率が30%以上であること、そして、100℃以下の温度において1時間以下で焼結し銀色の焼結膜となることを特徴とする。この被覆銀超微粒子は、加熱により分解して金属銀を生成する銀化合物と、アルキルアミン、アルキルジアミンとを混合して錯化合物とし、これを加熱することにより当該銀化合物を熱分解することにより調製する。
【選択図】図3
Description
(シュウ酸銀)
シュウ酸銀は、銀含有率が高く、通常200℃で分解する。熱分解すると、シュウ酸イオンが二酸化炭素として除去され金属銀がそのまま得られるため、還元剤を必要とせず、不純物が残留しにくい点で有利である。このため、本発明において被覆銀超微粒子を得るための銀の原料となる銀化合物としてはシュウ酸銀が好ましく用いられるため、以下、銀化合物としてシュウ酸銀を用いた場合について本発明を説明する。ただし、上記のように、銀化合物と所定のアミンとの間で生成する錯化合物において、当該アミンが銀原子に配位した状態で熱分解可能な銀化合物であればシュウ酸銀に限定されずに用いられることはいうまでもない。
(中短鎖アルキルジアミン、中短鎖アルキルアミン)
特に、沸点が250℃以下のアルキルアミン及びアルキルジアミンを含んだシュウ酸イオン・アルキルアミン・アルキルジアミン・銀錯化合物では、100℃以下の低い温度での熱分解で被覆銀超微粒子を高効率で得ることができる。
中短鎖アルキルジアミンとしては、前記錯化合物の熱分解温度を考慮すれば100℃以上の沸点であること、また、得られた被覆銀超微粒子の低温焼結性を考慮すれば、250℃以下の沸点であることが考慮される。例えば、エチレンジアミン(118℃)、N,N−ジメチルエチレンジアミン(105℃)、N,N’−ジメチルエチレンジアミン(119℃)、N,N-ジエチルエチレンジアミン(146℃)、N,N’−ジエチルエチレンジアミン(153℃)、1,3−プロパンジアミン(140℃)、2,2-ジメチル−1,3−プロパンジアミン(153℃)、N,N−ジメチル−1,3−ジアミノプロパン(136℃)、N,N’−ジメチル−1,3−ジアミノプロパン(145℃)、N,N−ジエチル−1,3−ジアミノプロパン(171℃)、1,4−ジアミノブタン(159℃)、1,5−ジアミノ−2−メチルペンタン(193℃)、1,6−ジアミノヘキサン(204℃)、N,N’−ジメチル−1,6−ジアミノヘキサン(228℃)、1,7−ジアミノヘプタン(224℃)、1,8−ジアミノオクタン(225℃)等が挙げられるが、これらに限定されるものではない。
得られた青色光沢の固体物について、粉末X線回折計(リガク MiniFlex II )により解析を行ったところ、粉末X線回折パターン(図1)から金属銀が生成していることが確認された。また、そのシグナル半値幅から、単結晶子サイズが4.0nmの被覆銀超微粒子であることが分かった。
4g(3.37 mmol)を混合し、この混合液にシュウ酸銀3.04g(10.0 mmol)を加え、10分間撹拌し、シュウ酸イオン・アルキルアミン・銀錯化合物を調製した。これを100℃で60分加熱撹拌すると、青色光沢を呈する懸濁液へと変化した。これにメタノール5 mLを加え、遠心分離により得られた沈殿物を自然乾燥すると、青色光沢の被覆銀超微粒子の固体物2.25g(銀基準収率94.5%)が得られた。
[解析と評価]
得られた青色光沢の固体物について、粉末X線回折計により解析を行ったところ、粉末X線回折パターン(図6)から金属銀が生成していることが確認された。また、そのシグナル半値幅から、単結晶子サイズが4.1nmの被覆銀超微粒子であることが分かった。得られた被覆銀超微粒子を透過型電子顕微鏡で観察した。10〜20nm程度の球状粒子が観察された(図7)。FT−IRスペクトルから得られた固体物にはアルキルアミンが含有していることが確認された。熱重量分析から、得られた固体物には9.30重量%アルキルアミンが保護分子として含有されており、使用したシュウ酸銀に対する銀基準収率は94.5%であることが明らかになった。
<比較例1>
<比較評価>
Claims (4)
- 平均粒径が30nm以下であり、保護分子により覆われた有機溶剤に分散可能な被覆銀超微粒子であって、熱重量測定において160℃まで加熱した際の当該保護分子の重量減少率が30%以上であることを特徴とする被覆銀超微粒子。
- 平均粒径が30nm以下であり、保護分子により覆われた有機溶剤に分散可能な被覆銀超微粒子であって、100℃以下の温度において1時間以下で焼結して銀色の金属膜を形成可能であることを特徴とする被覆銀超微粒子。
- 平均粒径が30nm以下であり、保護分子により覆われた被覆銀超微粒子であって、前記保護分子は、沸点が100〜250℃の範囲内にあるアルキルアミンと、沸点が100〜250℃の範囲内にあるアルキルジアミンを主成分として含むことを特徴とする被覆銀超微粒子。
- 請求項1から3のいずれかに記載の被覆銀超微粒子を分散媒に分散させたことを特徴とする被覆銀超微粒子分散液。
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