JP2017164740A - 表面修飾ナノ粒子 - Google Patents
表面修飾ナノ粒子 Download PDFInfo
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Abstract
【解決手段】溶媒中でリガンド相互作用剤102をナノ粒子100と会合させて、リガンド相互作用剤−ナノ粒子会合錯体110を含む混合物を形成し、混合物に結合/架橋剤106と、特異な溶解性及び/又は相溶性を与えるように調整された表面改質リガンド107とを加え、リガンド相互作用剤−ナノ粒子会合錯体110と、結合/架橋剤106と表面改質リガンド107とを反応させて、表面改質リガンドを含む外面を有する機能化ナノ粒子120を形成する技術。
【選択図】図1
Description
大きさが2〜100nmのオーダーであって、多くの場合、量子ドット及び/又はナノ粒子と称される粒子からなる化合物半導体の調製及びキャラクタリゼーション(characterization)に大きな関心が持たれてきた。これらの研究は、ナノ粒子におけるサイズ調整可能な電子、光学及び化学特性に主に焦点を当ててきた。生物学的ラベリング(biological labeling)、太陽電池、触媒作用、生物学的イメージング、発光ダイオードのような多様な商業的用途への適用可能性から、半導体ナノ粒子は、大きな関心を集めている。
ナノ粒子の多くの用途は、半導体ナノ粒子が、特定の媒体と相溶性を有する(compatible)ことを要求している。例えば、蛍光標識、インビボ(in vivo)イメージングや治療学などの幾つかの生物学的用途は、ナノ粒子が水性環境と相溶性を有することを要求している。その他の用途では、ナノ粒子は、芳香族化合物、アルコール、エステルやケトンなどの有機媒体中に分散可能であることが望ましい。例えば、有機系分散剤中に分散した半導体ナノ粒子を含有するインク配合物は、光起電(PV)デバイス用の半導体材料の薄膜を製造するために重要である。
608nmで赤色発光する、カドミウムフリーの量子ドットナノ粒子(CFQD)(InP/ZnS)(200mg)を、イソプロピルミリステート(100マイクロリットル)と共にトルエン(1mL)中に分散させた。混合物を約1乃至2分間50℃で加熱し、その後、室温で15時間ゆっくりと振とうさせた。HMMM(Cymel 303) (400mg)、モノヒドロキシポリジメチルシロキサン(MW 5kD) (200mg)、及びp−トルエンスルホン酸(70mg)のトルエン溶液(4mL)を、ナノ粒子分散液に加えた。混合液を脱気し、電磁撹拌機を用いて300rpmで撹拌しつつ、140℃で4時間還流させた。窒素のストリームを1時間、フラスコに通して、求核基とHMMMの反応で生じる揮発性の副産物を確実に除去した。混合物を室温まで冷めるままにし、不活性ガス下で保存した。表面修飾ナノ粒子は、未修飾のナノ粒子と比べて、蛍光量子収率の損失が小さく又は無く、発光ピーク又は半値全幅(FWHM)値に変化はなかった。表面修飾ナノ粒子は、様々な分子量の(10乃至1000kD)PDMSポリマーに良好に分散し、残留トルエンを除去した後でさえ、分散したままであった。反対に、PDMSに分散させた同じ濃度の未修飾ナノ粒子は、凝集して、ホストシリコーンから分離した。
525nmで緑色発光する、カドミウムフリーの量子ドットナノ粒子(CFQD)(InP/ZnS)(200mg)を、イソプロピルミリステート(100マイクロリットル)と共にトルエン(1mL)中に分散させた。混合物を約1乃至2分間50℃で加熱し、その後、室温で15時間ゆっくりと振とうさせた。HMMM(Cymel 303) (400mg)、トリメチロールプロパントリグリシジルエーテル(200mg)、サリチル酸(70mg)のトルエン溶液(4mL)を、ナノ粒子分散液に加えた。混合液を脱気し、電磁撹拌機を用いて300rpmで撹拌しつつ、140℃で4時間還流させた。窒素のストリームを1時間、フラスコに通して、求核基とHMMMの反応で生じる揮発性の副産物を確実に除去した。混合物を室温まで冷めるままにし、不活性ガス下で保存した。表面修飾ナノ粒子は、未修飾のナノ粒子と比べて、蛍光量子収率の損失が小さく又は無く、発光ピーク又は半値全幅(FWHM)値に変化はなかった。表面修飾ナノ粒子は、様々な分子量のエポキシポリマーに良好に分散し、残留トルエンを除去した後でさえ、分散したままであった。反対に、同じ濃度の未修飾ナノ粒子は、凝集して、ホストマトリクスから分離した。
608nmで赤色発光する、カドミウムフリーの量子ドットナノ粒子(CFQD)(InP/ZnS)(200mg)を、イソプロピルミリステート(100マイクロリットル)と共にトルエン(1mL)中に分散させた。混合物を約1乃至2分間50℃で加熱し、その後、室温で15時間ゆっくりと振とうさせた。HMMM(Cymel 303) (400mg)、モノメトキシポリエチレンオキシド(CH3O−PEG2000−OH)(400mg)、サリチル酸(50mg)のトルエン溶液(4mL)を、ナノ粒子分散液に加えた。混合液を脱気し、電磁撹拌機を用いて300rpmで撹拌しつつ、130℃で2時間還流させた。窒素のストリームを1時間、フラスコに通して、求核基とHMMMの反応で生じる揮発性の副産物を確実に除去した。混合物を室温まで冷めるままにし、不活性ガス下で保存した。表面修飾ナノ粒子は、未修飾のナノ粒子と比べて、蛍光量子収率の損失が小さく又は無く、発光ピーク又は半値全幅(FWHM)値に変化はなかった。修飾されたドットのアリコートをポリスチレン樹脂又はポリスチレンコポリマー樹脂(トルエン中5%固形分、例えば、スチレン−エチレン/ブチレン−スチレン又はスチレン−エチレン/プロピレン−スチレン(SEPS、SEBS、Kraton))と混合し、修飾されたナノ粒子は、ホストポリスチレン樹脂に非常に良く分散し、残留トルエンを除去した後でも分散したままであった。同じナノ粒子濃度にて、未修飾でそのままのナノ粒子は、凝集して、ホスト樹脂から分離した。表面修飾ナノ粒子のフィルムは均一であるが、未修飾のナノ粒子のフィルムでは、ナノ粒子は顕著に凝集した。
608nmで赤色発光する、カドミウムフリーの量子ドットナノ粒子(CFQD)(InP/ZnS/ZnO)(200mg)を、イソプロピルミリステート(100マイクロリットル)と共にトルエン(1mL)中に分散させた。混合物を約1乃至2分間50℃で加熱し、その後、室温で15時間ゆっくりと振とうさせた。HMMM(Cymel 303) (400mg)、モノメトキシポリエチレンオキシド(CH3O−PEG2000−OH)(400mg)、サリチル酸(50mg)のトルエン溶液(4mL)を、ナノ粒子分散液に加えた。混合液を脱気し、電磁撹拌機を用いて300rpmで撹拌しつつ、140℃で4時間還流させた。窒素のストリームを1時間、フラスコに通して、求核基とHMMMの反応で生じる揮発性の副産物を確実に除去した。混合物を室温まで冷めるままにし、不活性ガス下で保存した。表面修飾ナノ粒子は、未修飾のナノ粒子と比べて、蛍光量子収率の損失が小さく又は無く、発光ピーク又は半値全幅(FWHM)値に変化はなかった。
エポキシ相溶性ナノ粒子を、実施例2について説明したように調整した。エポキシ相溶性ナノ粒子を、LEDエポキシ封止剤(EX135)に加えた。封止剤と青色発光LEDチップとを用いて、LEDを調整した。図8Aは、表面修飾ナノ粒子を組み込んでいるLEDの発光曲線を示している。発光測定を、一週間毎日、その後、毎週行った。図8Bは、未修飾のナノ粒子を組み込んでいるLEDの発光曲線を示している。未修飾のナノ粒子を、最初にアクリルビーズに組み込み、その後、ビーズをエポキシに封入した。予想したように、両方のLEDの発光強度は、LEDが劣化するにつれて、時間と共に減少した。しかしながら、表面修飾ナノ粒子を組み込んでいるLEDの絶対発光強度は、未修飾ナノ粒子を組み込んでいるLEDの強度の約2倍となっている。
Claims (9)
- ナノ粒子を機能化する方法であって、
溶媒中でリガンド相互作用剤をナノ粒子と会合させて、リガンド相互作用剤−ナノ粒子会合錯体を含む混合物を形成する工程と、
混合物に結合/架橋剤と表面改質リガンドとを加える工程と、
リガンド相互作用剤−ナノ粒子会合錯体と、結合/架橋剤と、表面改質リガンドとを反応させて、表面改質リガンドを含む外面を有する機能化ナノ粒子を形成する工程と、
を含む方法。 - ナノ粒子にキャッピングリガンドを与える工程を更に含んでおり、リガンド相互作用剤をナノ粒子と会合させる工程は、リガンド相互作用剤とキャッピングリガンドをインターカレーションさせる工程を含む、請求項1に記載の方法。
- 結合/架橋剤は、表面改質リガンドをリガンド相互作用剤に結合させるための結合部位を提供する、請求項1に記載の方法。
- 表面修飾リガンドは水溶性である、請求項1に記載の方法。
- 表面修飾リガンドは、ポリエーテルを含む、請求項1に記載の方法。
- 表面修飾リガンドは、モノメトキシポリエチレングリコールである、請求項1に記載の方法。
- 表面修飾リガンドは、シリコーンを含む、請求項1に記載の方法。
- 混合物に触媒を加える工程を更に含む、請求項1に記載の方法。
- 触媒は、サリチル酸及びp−トルエンスルホン酸の一方である、請求項8に記載の方法。
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JP6381713B2 (ja) | 2018-08-29 |
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JP6827447B2 (ja) | 2021-02-10 |
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US20180142146A1 (en) | 2018-05-24 |
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US9115097B2 (en) | 2015-08-25 |
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US20160046859A1 (en) | 2016-02-18 |
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US10377944B2 (en) | 2019-08-13 |
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