JP2012082502A - 金属ナノ粒子分散組成物 - Google Patents
金属ナノ粒子分散組成物 Download PDFInfo
- Publication number
- JP2012082502A JP2012082502A JP2010231901A JP2010231901A JP2012082502A JP 2012082502 A JP2012082502 A JP 2012082502A JP 2010231901 A JP2010231901 A JP 2010231901A JP 2010231901 A JP2010231901 A JP 2010231901A JP 2012082502 A JP2012082502 A JP 2012082502A
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- Prior art keywords
- metal
- nanoparticles
- compound
- particles
- metal nanoparticle
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 97
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 54
- 239000002184 metal Substances 0.000 title claims abstract description 54
- 239000002082 metal nanoparticle Substances 0.000 claims abstract description 228
- 239000002245 particle Substances 0.000 claims abstract description 154
- 150000001875 compounds Chemical class 0.000 claims abstract description 126
- 239000003960 organic solvent Substances 0.000 claims abstract description 26
- 125000002924 primary amino group Chemical class [H]N([H])* 0.000 claims abstract 3
- 239000006185 dispersion Substances 0.000 claims description 117
- 229920000642 polymer Polymers 0.000 claims description 65
- 239000010949 copper Substances 0.000 claims description 30
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 28
- 229910052802 copper Inorganic materials 0.000 claims description 28
- 150000003384 small molecules Chemical class 0.000 claims description 28
- 238000009835 boiling Methods 0.000 claims description 15
- 229910052709 silver Inorganic materials 0.000 claims description 13
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- 238000007641 inkjet printing Methods 0.000 claims description 2
- 239000010970 precious metal Substances 0.000 claims 1
- 238000000034 method Methods 0.000 description 61
- 239000002105 nanoparticle Substances 0.000 description 54
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 30
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- 230000000052 comparative effect Effects 0.000 description 25
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Abstract
【解決手段】 実施形態の金属ナノ粒子分散組成物は、有機溶媒と、前記有機溶媒に分散された金属含有粒子とを含有する。前記金属含有粒子は、第1の粒子と第2の粒子とを含む。前記第1の粒子は、重量平均分子量1000以上の高分子化合物を表面に有する第1の金属ナノ粒子からなり、前記第2の粒子は、重量平均分子量が500以下の低分子化合物を表面に有する第2の金属ナノ粒子からなる。前記低分子化合物の少なくとも一部は、一級アミンである。
【選択図】 なし
Description
一次粒子径が10nm以上100nm以下の範囲内の金属ナノ粒子であれば、こうした不都合は何等伴なうことはない。第1の金属ナノ粒子の最大粒径は、500nm以下であることが好ましく、200nm以下であることが特に好ましい。金属ナノ粒子の最大粒径とは、凝集粒子を含めた粒子径をさし、前述の粒度分布計測により求めることができる。
得られた銀ナノ粒子分散溶液にメタノールを加えると、表面に低分子化合物を有する銀ナノ粒子を凝集沈殿させることができる。こうして、ナノ粒子のみを取り出し、その後、所望の溶媒に分散させて分散組成物を得ることが可能となる。
まず、高分子化合物を表面に有する第1の金属ナノ粒子からなる第1の粒子の分散液を製造した。
第1の金属ナノ粒子として、銅ナノ粒子(日清エンジニアリング社製)を準備した。この銅ナノ粒子は、SEM観察による一次粒子径が約50nmであり、BET比表面積は16m2/gであった。
こうして得られた第1の粒子の分散液を用いた以外は実施例1と同様にして、実施例2の金属ナノ粒子分散組成物を作製した。
高分子化合物として、ポリエチレングリコール(重量平均分子量1500)を準備した。この高分子化合物を用いた以外は実施例2と同様にして、高分子化合物を表面に有する第1の金属ナノ粒子からなる第1の粒子の分散液を得た。
こうして得られた第1の粒子の分散液を用いた以外は実施例2と同様にして、実施例3の金属ナノ粒子分散組成物を作製した。
高分子化合物として、ゼラチン化合物(重量平均分子量100000)を準備した。この高分子化合物を用いた以外は実施例2と同様にして、高分子化合物を表面に有する第1の金属ナノ粒子からなる第1の粒子の分散液を得た。
こうして得られた第1の粒子の分散液を用いた以外は実施例2と同様にして、実施例4の金属ナノ粒子分散組成物を作製した。
第1の金属ナノ粒子として、5wt%のニッケルを含有した銅ナノ粒子(日清エンジニアリング社製)を準備した。この金属ナノ粒子を用いた以外は実施例1と同様にして、高分子化合物を表面に有する第1の金属ナノ粒子からなる第1の粒子の分散液を得た。
こうして得られた第1の粒子の分散液を用いた以外は実施例1と同様にして、実施例5の金属ナノ粒子分散組成物を作製した。
一級アミンとしてのヘキシルアミンをヘキサデシルアミンに変更した以外は、実施例1と同様の手法により、低分子化合物を表面に有する第2の金属ナノ粒子からなる第2の粒子を得た。なお、ヘキサデシルアミンの沸点は、約330℃である。この際の銀ナノ粒子の収率は、48%であった。また、低分子化合物の少なくとも一部は、一級アミンとしてのヘキサデシルアミンであることが確認された。このヘキシルアミンは、銀ナノ粒子の表面における低分子化合物の45%程度を占めていた。
こうして得られた第2の粒子を用いた以外は実施例1と同様にして、実施例6の金属ナノ粒子分散組成物を作製した。
低分子化合物を表面に有する第2の金属ナノ粒子からなる第2の粒子を用いない以外は実施例1と同様にして、比較例1の金属ナノ粒子分散組成物を作製した。本比較例の金属ナノ粒子分散組成物に含有されている金属ナノ粒子は、高分子化合物としてのポリビニルピロリドンを表面に有する銀ナノ粒子(第1の粒子)のみである。
低分子化合物を表面に有する第2の金属ナノ粒子からなる第2の粒子を用いない以外は実施例2と同様にして、比較例2の金属ナノ粒子分散組成物を作製した。本比較例の金属ナノ粒子分散組成物に含有されている金属ナノ粒子は、高分子化合物としてのポリビニルピロリドンを表面に有する銅ナノ粒子(第1の粒子)のみである。
高分子化合物を表面に有する第1の金属ナノ粒子からなる第1の粒子の分散液を用いない以外は、実施例6と同様にして、比較例3の金属ナノ粒子分散組成物を作製した。具体的には、実施例6と同様の低分子化合物を表面に有する銀ナノ粒子5gをトルエン10mlに加えた。ローリングミルを用いて、これを簡単に攪拌した後、超音波ホモジナイザーにより分散を行なって分散液を得た。超音波の条件は、周波数20kHz、出力約3Wとした。
ラウリン酸ナトリウムと硝酸銀とを当量混合し、イオン交換によりラウリン酸銀を合成した。得られたラウリン酸銀(30g)を1−オクタノール(300mL)中に加え、窒素雰囲気下180℃まで昇温して5時間保持した。反応溶液の温度を60℃に低下させたところ、銀ナノ粒子の生成が確認された。メタノール(500mL)を加えて銀ナノ粒子を凝集させ、吸引ろ過により回収した。
Claims (7)
- 有機溶媒と、前記有機溶媒に分散された金属含有粒子とを含有し、
前記金属含有粒子は、
重量平均分子量1000以上の高分子化合物を表面に有する第1の金属ナノ粒子からなる第1の粒子と、
重量平均分子量が500以下で少なくとも一部が一級アミンである低分子化合物を表面に有する第2の金属ナノ粒子からなる第2の粒子と
を含むことを特徴とする金属ナノ粒子分散組成物。 - 前記第2の金属ナノ粒子は、貴金属を主成分とすることを特徴とする請求項1に記載の金属ナノ粒子分散組成物。
- 前記第1の金属ナノ粒子は、銅を主成分とすることを特徴とする請求項1または2に記載の金属ナノ粒子分散組成物。
- 前記第2の金属ナノ粒子は、銀を主成分とすることを特徴とする請求項1乃至3のいずれか1項に記載の金属ナノ粒子分散組成物。
- 前記一級アミンの沸点は、250℃以下であることを特徴とする請求項1乃至4のいずれか1項に記載の金属ナノ粒子分散組成物。
- インクであることを特徴とする請求項1乃至5のいずれか1項に記載の金属ナノ粒子分散組成物。
- インクジェット印刷用インクであることを特徴とする請求項6に記載の金属ナノ粒子分散組成物。
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CN201110050460.1A CN102453374B (zh) | 2010-10-14 | 2011-03-02 | 金属纳米粒子分散体 |
US13/041,599 US8828276B2 (en) | 2010-10-14 | 2011-03-07 | Metal nanoparticle dispersion |
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Also Published As
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US20120091401A1 (en) | 2012-04-19 |
KR101354873B1 (ko) | 2014-01-22 |
EP2441922A1 (en) | 2012-04-18 |
CN102453374B (zh) | 2016-04-06 |
CN102453374A (zh) | 2012-05-16 |
EP2441922B1 (en) | 2015-08-26 |
KR20120038878A (ko) | 2012-04-24 |
JP5623861B2 (ja) | 2014-11-12 |
US8828276B2 (en) | 2014-09-09 |
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