JP5744033B2 - ナノ粒子を含む粒子、それの使用および方法 - Google Patents
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Description
本願は、2009年9月9日出願の米国特許出願第61/240932号(引用によって全体が本明細書に組み込まれる)に対する優先権を主張するものである。
本発明は、中央情報局提供の契約番号2004*H838109*000下の政府支援で行ったものである。本発明には政府が一定の権利を有する。
ある種の実施形態において、前記1以上の添加剤は、着色剤、散乱剤、結合剤、界面活性剤、UV吸収剤、および/またはそれらの1以上の混合物を含むことができる。
式中、kは2、34または5であり、nは1、2、3、4または5であって、k−nはゼロ以上となっており;XはO、OS、O−Se、O−N、O−P、O−As、S、S=O、SO2、Se、Se=O、N、N=O、P、P=O、C=OAsまたはAs=Oであり;YおよびLのそれぞれが独立に、H、OH、アリール、ヘテロアリール、または少なくとも1個の二重結合、少なくとも1個の三重結合もしくは少なくとも1個の二重結合と1個の三重結合を含んでいても良い直鎖もしくは分岐のC2−18炭化水素鎖である。炭化水素鎖は、1以上のC1−4アルキル、C2−4アルケニル、C2−4アルキニル、C1−4アルコキシ、ヒドロキシル、ハロ、アミノ、ニトロ、シアノ、C3−5シクロアルキル、3から5員複素環アルキル、アリール、ヘテロアリール、C1−4アルキルカルボニルオキシ、C1−4アルキルオキシカルボニル、C1−4アルキルカルボニルまたはホルミルで置換されていても良い。炭化水素鎖は、−O−、−S−、−N(Ra)−、−N(Ra)−C(O)−O−、−O−C(O)−N(Ra)−、−N(Ra)−C(O)−N(Rb)−、−O−C(O)−O−、−P(Ra)−または−P(O)(Ra)−によって中断されていても良い。各RaおよびRbは独立に、水素、アルキル、アルケニル、アルキニル、アルコキシ、ヒドロキシルアルキル、ヒドロキシルまたはハロアルキルである。アリール基は、置換されているか置換されていない環状芳香族基である。例としては、フェニル、ベンジル、ナフチル、トリル、アントらシル、ニトロフェニルまたはハロフェニルなどがある。ヘテロアリール基は、環中に1以上のヘテロ原子を有するアリール基であり、例えばフリル、ピリジル、ピロリル、フェナントリルがある。
下記において、分散剤としてポリビニルアルコールを用いる乳化光重合および保護オーバーコーティングを介したLMA/EGDAアクリルマイクロカプセル中のオクタデシルホスホン酸(ODPA)およびデシルアミンリガンドを持ったInP/ZnS量子ドットを含む粒子の製造例について説明する。
脱イオン水を用いる。メタクリル酸ラウリル(LMA)(Aldrich Chemical、96%ロット番号08118DE)およびジアクリル酸エチレングリコール(EGDA)(Aldrich Chemical、98%ロット番号15017PD)を、活性アルミナの短い層を通過させて重合阻害剤を除去することで精製する。カラムを通過させた後、モノマー類は密閉された琥珀色バイアル中に保管し、冷蔵し、24時間以内に使用する。Esacure KTO46光開始剤(Sartomer、ロット番号2008050005)、硫酸ナトリウム(Aldrich Chemical、無水)およびポリビニルアルコール(Fluka、4−98ロット番号454084)は、それ以上精製せずに用いる。他の溶媒はいずれも試薬用であり、それ以上精製せずに用いる。
量子ドット/モノマー製造。ラバーセプタムおよび磁気撹拌子を取り付けた50mLシュレンクフラスコに、アクリル酸ラウリル(6.08g、6.88mL)およびジアクリル酸エチレングリコール(1.52g、1.39mL)を入れる。トルエン中のInP/ZnS量子ドット(7mL、無機物基準で21mg/mL;合計無機物147mg)を注射器で加え、系の圧力が500ミリtorr以下に低下することで示されるようにトルエン溶媒が全て除去されるまで減圧を続ける。Esacure KTO−46光開始剤(0.28g)をアクリル酸ラウリル/量子ドット溶液に加え、磁気撹拌子を用いて十分に混和する。
温度が再度6℃になるまで反応混合物を冷却下に撹拌する。20%硫酸ナトリウム溶液42mLを、シリンジポンプを用いて5mL/分で加える(この体積は、6℃で4%4−98PVA溶液86mLの曇り点に達するように決定したものである)。溶液添加完了後、循環浴設定温度を30℃に設定し、反応溶液を20分間かけて昇温させて25℃とする。図1には、反応溶液中で生成するゲル粒子を示してある(200×ローダミンフィルター)(硫酸ナトリウム添加後のPVA水溶液)。
ゲルを500mLビーカーに移し入れ、メタノール250mLを加える。混合物をローター・固定子(低に設定)で温浸し、30分間分散させ、その間にゲルが崩壊して粒径低下が生じた。混合物を250mL遠心瓶に移し入れ、4000rpmで15分間遠心する。固体が管の底部にあり(黄褐色)、その上に薄い白色層がある。管の残りの部分は透明なメタノールであり、それは傾斜法で除去する。
本明細書で使用される場合、単数形である「一つの」、「1個の」および「その」は、文脈によって他の意味が明瞭に示されていない限り、複数形を含むものである。従って、例えば、発光材料に対する言及は、1以上のそのような材料に対する言及を含むものである。
Claims (38)
- 母材内に分散された、発光特性を有するナノ粒子を含む粒子を含む被覆粒子であって、該粒子は、該粒子の外表面にコーティングを含み、該コーティングが、置換ポリビニルアルコール化合物、非置換ポリビニルアルコール化合物、置換ポリビニリデンジクロライド化合物又は非置換ポリビニリデンジクロライド化合物を含む低酸素透過性の樹脂を含む、該被覆粒子。
- 前記コーティングが、少なくとも0.1ミクロンの厚さを有する、請求項1に記載の被覆粒子。
- 前記粒子が、0.01μm〜100μmの範囲の直径を有する、請求項1に記載の被覆粒子。
- 前記粒子が、少なくとも0.001重量%のナノ粒子を含む、請求項1に記載の被覆粒子。
- 前記粒子が、0.001〜25重量%のナノ粒子を含む、請求項1に記載の被覆粒子。
- 前記母材がポリマーを含む、請求項1に記載の被覆粒子。
- 前記母材がロウを含む、請求項1に記載の被覆粒子。
- 前記母材が光学的に透明である、請求項1に記載の被覆粒子。
- 前記ナノ粒子の少なくとも一部が、第1の半導体を含むコアおよび該コアの外表面の少なくとも一部の上に配置されたシェルを含み、該シェルが第2の半導体を含む、請求項1に記載の被覆粒子。
- 請求項1に記載の複数の被覆粒子を含む、粉末。
- 2以上の被覆粒子群が前記粉末に含まれ、少なくとも一つの被覆粒子群が、別の被覆粒子群に含まれるナノ粒子によって放出されるものと異なる波長の光を放出するナノ粒子を含む、請求項10に記載の粉末。
- 請求項1に記載の1以上の被覆粒子および固体もしくは液体媒体を含む、製剤。
- 被覆粒子が、媒体の重量基準で少なくとも0.1重量%の量で製剤中に存在する、請求項12に記載の製剤。
- 被覆粒子が、媒体の重量基準で少なくとも0.1〜75重量%の量で製剤中に存在する、請求項12に記載の製剤。
- 前記媒体が、モノマー類、ポリマー類、樹脂類および/または他のフィルム形成組成物を含む、請求項12に記載の製剤。
- 前記製剤が、1以上の添加剤をさらに含む、請求項12に記載の製剤。
- 前記1以上の添加剤が、着色剤、散乱剤、結合剤、界面活性剤、UV吸収剤および/またはこれらの1以上の混合物を含む、請求項16に記載の製剤。
- 請求項12に記載の製剤を含む、コーティング組成物。
- 前記コーティング組成物が、モノマー類、ポリマー類、樹脂類および/または他のフィルム形成組成物をさらに含む、請求項18に記載のコーティング組成物。
- 前記コーティング組成物が、1以上の添加剤をさらに含む、請求項18に記載のコーティング組成物。
- 前記1以上の添加剤が、着色剤、散乱剤、結合剤、界面活性剤、UV吸収剤および/またはこれらの1以上の温合物を含む、請求項20に記載のコーティング組成物。
- 請求項1に記載の複数の被覆粒子から製造されるフィルムを含む、コーティング組成物。
- 第2の母材中に分散した、請求項1に記載の1以上の被覆粒子を含む、組成物。
- 前記第2の母材が、ポリマーを含む、請求項23に記載の組成物。
- 前記第2の母材が、モノマーを含む、請求項23に記載の組成物。
- 前記第2の母材が、樹脂を含む、請求項23に記載の組成物。
- 母材中に分散させた、発光特性を有するナノ粒子を含む粒子を提供する段階、前記粒子の少なくとも一部の外表面の上にコーティングを形成する段階を有し、前記コーティングが、置換ポリビニルアルコール化合物、非置換ポリビニルアルコール化合物、置換ポリビニリデンジクロライド化合物又は非置換ポリビニリデンジクロライド化合物を含む低酸素透過性を有する樹脂を含む、カプセル化ナノ粒子の製造方法。
- 前記コーティングが、少なくとも0.1ミクロンの厚さを有する、請求項27に記載の方法。
- 前記母材が、ポリマーを含む、請求項27に記載の方法。
- 前記母材が、ロウを含む、請求項27に記載の方法。
- 前記母材が、ポリアクリレートを含む、請求項27に記載の方法。
- 前記母材が、無機材料を含む、請求項27に記載の方法。
- 前記母材が、ポリアクリレートを含む、請求項1に記載の被覆粒子。
- 前記母材が、ポリメタクリレートを含む、請求項1に記載の被覆粒子。
- 前記母材が、ポリメタクリル酸ラウリルを含む、請求項1に記載の被覆粒子。
- 前記母材が、無機材料を含む、請求項1に記載の被覆粒子。
- 請求項1に記載の1以上の被覆粒子を含む、組成物。
- 前記母材中に分散した、発光特性を有するナノ粒子を含む粒子を形成する段階、コーティング材料を不溶性とすることで液体媒体中の粒子の少なくとも一部の外表面の上にコーティング材料を含む層を形成する段階、前記コーティング材料を架橋することでコーティングを形成する段階を有し、該コーティングが、置換ポリビニルアルコール化合物、非置換ポリビニルアルコール化合物、置換ポリビニリデンジクロライド化合物又は非置換ポリビニリデンジクロライド化合物を含む、カプセル化ナノ粒子の製造方法。
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US24093209P | 2009-09-09 | 2009-09-09 | |
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PCT/US2010/048285 WO2011031871A1 (en) | 2009-09-09 | 2010-09-09 | Particles including nanoparticles, uses thereof, and methods |
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EP (1) | EP2475717A4 (ja) |
JP (1) | JP5744033B2 (ja) |
KR (1) | KR101865888B1 (ja) |
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Cited By (2)
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US11242481B2 (en) | 2016-12-19 | 2022-02-08 | Fujifilm Corporation | Wavelength conversion film and backlight unit |
US10784417B2 (en) | 2017-01-24 | 2020-09-22 | Fujifilm Corporation | Wavelength conversion film |
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US20120256141A1 (en) | 2012-10-11 |
EP2475717A1 (en) | 2012-07-18 |
CN102482457B (zh) | 2015-04-15 |
WO2011031871A1 (en) | 2011-03-17 |
KR101865888B1 (ko) | 2018-06-08 |
EP2475717A4 (en) | 2015-01-07 |
US9365701B2 (en) | 2016-06-14 |
KR20120083388A (ko) | 2012-07-25 |
JP2013504660A (ja) | 2013-02-07 |
CN102482457A (zh) | 2012-05-30 |
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