JP2017513960A - 安定性と発光効率が向上した量子ドットナノ粒子 - Google Patents
安定性と発光効率が向上した量子ドットナノ粒子 Download PDFInfo
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- JP2017513960A JP2017513960A JP2016550505A JP2016550505A JP2017513960A JP 2017513960 A JP2017513960 A JP 2017513960A JP 2016550505 A JP2016550505 A JP 2016550505A JP 2016550505 A JP2016550505 A JP 2016550505A JP 2017513960 A JP2017513960 A JP 2017513960A
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- C—CHEMISTRY; METALLURGY
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Abstract
Description
本願は、2014年2月7日に出願された米国仮出願第61/937,073号の利益を主張する。
自由なアミンのクエンチング効果を、オレイルアミンの存在下と不存在下とで、InP合金を用いたコアにシェルを形成することで実証した。InPZnS合金を用いたコアを、ほぼ米国特許第7,558,828号に記載されているようにして調製した。InP合金を用いたコアの2つのサンプルの各々を、THERMINOLに懸濁させた。酢酸亜鉛(0.862g)を各混合物に加えて、それら混合物を230℃で2時間加熱した。ドデカンチオール(1.69mL)を両混合物に加えて、一方の混合物にオレイルアミン(0.2mL)を加えた。両混合物を、さらに1時間半反応させた。
InPZnS合金を用いたコアを、ほぼ米国特許第7,558,828号に記載されているようにして調製した。コアをTHERMINOL(40mL)に懸濁させて、酢酸亜鉛(5.76g)、ミリスチン酸(1.5g)、ステアリン酸亜鉛(11.32g)を更に加えた。混合物を180℃に加熱して、その後、亜鉛ジエチルジチオカルバメート(2.295g)を加えて、20分間放置した。高い濁度が観察されて、反応混合物のフォトルミネセンスは、非常に低いままであり、その温度での低い反応度/反応度を示唆した。混合物を230℃に加熱して3時間放置した。粉末は次第に溶解したが、QYは、全体にわたって非常に低いままであった。
180℃でジエチルジチオカルバメートを加えた後にオレイルアミン(5mL)を混合物に加えた点を除いて、InPZnS合金を用いたコアに、実施例2に記載したものと同じ条件下でシェルを形成した。混合物を、180℃で更に20分間加熱した。得られた量子ドットは、523nmでフォトルミネセンスを示し、FWHMは53nmであり、QYは73%であった。実施例2と実施例3の違いは、アミンがシェル形成に極めて重要であることを示唆している。
InPZnS合金を用いたコアを、ほぼ米国特許第7,558,828号に記載されているようにして調製し、亜鉛ジエチルジチオカルバメートとオレイルアミンを共に窒素下にて、50℃に設定した水槽を用いて予め混合することで、シェル形成反応に加える前に、亜鉛ジエチルジチオカルバメートを最初にオレイルアミンで錯体化した点を除いて、実施例3に記載したようにシェルを形成した。シェル化反応によって、ルミネッセンスのQYが75%である量子ドットを得た。同じ反応で、ルミネッセンスのQYが85%に達する量子ドットを得た。
InPZnS合金を用いたコアを、ほぼ米国特許第7,558,828号に記載されているようにして調製し、亜鉛ジエチルジチオカルバメートに代えてエチルキサンチン酸亜鉛を用いた点を除いて、実施例4に記載したようにシェルを形成した。InPZnS合金を用いたコア(500mg)、ミリスチン酸(1.5g)、酢酸亜鉛(2.4g)、ステアリン酸亜鉛(5.3g)を、THERMINOL中にて真空下にて100℃で1時間撹拌し、その後215℃に加熱して、140℃に冷却した。エチルキサンチン酸亜鉛(0.97g)とオレイルアミン(1.05mL)を予め混合したTHERMINOL(5mL)溶液を、コア溶液に加えた。その溶液を、1時間撹拌し、その後180℃で1時間撹拌した。オクタノール(2.4mL)を加えて、溶液を更に30分撹拌した。反応により、ルミネッセンスのQYが85%である量子ドットを得た。
Claims (20)
- 複数の第1ジチオカルバメートキャッピングリガンドを含む量子ドット(QD)ナノ粒子。
- Rは親水基である、請求項2に記載のQDナノ粒子。
- Rは両親媒性部である、請求項2に記載のQDナノ粒子。
- R’はエチル基である、請求項2に記載のQDナノ粒子。
- 複数の第1ジチオカルボネートキャッピングリガンドを含む量子ドット(QD)ナノ粒子。
- R及びR’は、炭化水素である、請求項8に記載のQDナノ粒子。
- R基は、C12炭化水素鎖であり、カルボン酸官能性がC12位置にある、請求項8に記載のQDナノ粒子。
- 複数の第1ジチオカルバメートキャッピングリガンドを含む量子ドット(QD)ナノ粒子を調製する方法であって、
分子クラスタ化合物の存在下でコア材料前駆体を反応させて、ナノ粒子コアを作製する工程と、
コアを単離する工程と、
単離したコアをシェル前駆体と反応させて、少なくとも1つの半導体シェルをコア上に成長させる工程と、
ナノ粒子の最外の半導体表面にキャッピングリガンドを結合させる工程と、
キャッピングリガンドの少なくとも一部をジチオリガンドと交換する工程と、
を含んでいる方法。 - コアのサイズに関する光学特性を監視して、コアが所定のサイズに至ると反応を停止させる工程を更に含む、請求項11に記載の方法。
- 光学特性は、吸収スペクトルである、請求項12に記載の方法。
- 光学特性は、放射スペクトルである、請求項12に記載の方法。
- コアは、濾過によって単離される、請求項11に記載の方法。
- 反応混合物に非溶媒を加えてコアの沈殿を誘起する工程を更に含む、請求項15に記載の方法。
- 少量の物質をコアからエッチングした後に、コアをシェル前駆体と反応させる工程を更に含む、請求項11に記載の方法。
- フッ化水素酸が使用されて、コアがエッチングされる、請求項17に記載の方法。
- シェル形成反応中に配位リガンドを加えて、シェル形成反応を安定化させる工程を更に含む、請求項11に記載の方法。
- 配位リガンドは、ミリスチン酸である、請求項19に記載の方法。
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TW201536895A (zh) | 2015-10-01 |
US20170229618A1 (en) | 2017-08-10 |
TW201631120A (zh) | 2016-09-01 |
TWI580763B (zh) | 2017-05-01 |
JP6483716B2 (ja) | 2019-03-13 |
EP3473692B1 (en) | 2020-12-09 |
CN110003883A (zh) | 2019-07-12 |
JP2019023297A (ja) | 2019-02-14 |
KR101819573B1 (ko) | 2018-01-18 |
EP3102649A1 (en) | 2016-12-14 |
KR20180007013A (ko) | 2018-01-19 |
KR101912782B1 (ko) | 2018-10-29 |
US9666768B2 (en) | 2017-05-30 |
EP3473692A1 (en) | 2019-04-24 |
US10468559B2 (en) | 2019-11-05 |
KR20160103068A (ko) | 2016-08-31 |
WO2015118346A1 (en) | 2015-08-13 |
US20150228866A1 (en) | 2015-08-13 |
CN105992807A (zh) | 2016-10-05 |
CN105992807B (zh) | 2019-02-12 |
TWI621692B (zh) | 2018-04-21 |
EP3102649B1 (en) | 2018-10-10 |
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