JP2019504811A - GaPおよびAlPシェルを有するInP量子ドット、ならびにその製造方法 - Google Patents
GaPおよびAlPシェルを有するInP量子ドット、ならびにその製造方法 Download PDFInfo
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- JP2019504811A JP2019504811A JP2018536410A JP2018536410A JP2019504811A JP 2019504811 A JP2019504811 A JP 2019504811A JP 2018536410 A JP2018536410 A JP 2018536410A JP 2018536410 A JP2018536410 A JP 2018536410A JP 2019504811 A JP2019504811 A JP 2019504811A
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- shell
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- alp
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- H05B33/12—Light sources with substantially two-dimensional radiating surfaces
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Abstract
Description
(a)放射線を放出する層と、
(b)放射線放出層の上に配置される本明細書に記載のナノ構造の集団を含むフィルム層と、
(c)フィルム層の上の光透過性バリア層と、
(d)バリア層の上に配置される光学素子と、
を含む表示装置を提供する。
InPナノ構造のコロイド合成方法は当技術分野において周知である。そのような方法は、たとえば結果として得られるナノ構造のサイズおよび/または形状の分布を制御するための、ナノ構造の成長を制御する技術を含む。
いくつかの実施形態では、本発明のナノ構造は、コアと、少なくとも1つのGaPまたはAlPのシェル層とを含む。いくつかの実施形態では、本発明のナノ構造は、コアと、少なくとも2つのシェル層とを含む。シェルは、たとえば、ナノ構造の量子収率および/または安定性を高めることができる。特に、InPコア上のGaPまたはAlPのシェルは、GaPまたはAlPとZnSとの間の格子不整合が小さいため、ZnSなどのさらなるシェルの格子整合層として機能することができる。
いくつかの実施形態では、追加のシェル前駆体を加えた後、高温で維持することによって、さらなるシェル層が形成される。典型的には、前の層の反応が実質的に完了した後(たとえば、前の前駆体の少なくとも1つがなくなる、または反応から除去されるとき、またはさらなる成長が検出できないとき)に、追加の前駆体が供給される。別の実施形態では、InP/GaPまたはInP/AlPナノ構造が単離され、次に、1つ以上の別の反応にさらなるシェル層が加えられる。
InP/GaP/シェルナノ構造またはInP/AlP/シェルナノ構造の集団は、フィルムを形成するマトリックス(たとえば、有機ポリマー、ケイ素含有ポリマー、無機、ガラス質、および/または別のマトリックス)中に場合により埋め込まれる。このフィルムは、ナノ構造発光体の集団中で、および/またはデバイス、たとえば、LED、バックライト、ダウンライト、または別の表示もしくは照明装置、または光学フィルター中に組み込んで使用することができる。代表的な発光体および照明装置は、たとえば、所望の波長またはその付近の放出極大を有するナノ構造の集団を組み込むことによって特定の色の光を発生させることができ、または異なる放出極大を有する2つ以上の異なるナノ構造の集団を組み込むことによって幅広い色域を発生させることができる。種々のマトリックスが当技術分野において周知となっている。たとえば、米国特許第7,068,898号、ならびに米国特許出願公開第2010/0276638号、同開第2007/0034833号、および同第2012/0113672号を参照されたい。代表的なナノ構造発光体フィルム、LED、バックライト装置などは、たとえば、米国特許出願公開第2010/0276638号、同第2012/0113672号、同第2008/0237540号、同第2010/0110728号、および同第2010/0155749号、ならびに米国特許第7,374,807号、同第7,645,397号、同第6,501,091号、および同第6,803,719号に記載されている。
(a)放射線を放出する層と、
(b)放射線放出層の上に配置されるInP/GaP/シェルナノ構造またはInP/AlP/シェルナノ構造の集団を含むフィルム層と、
(c)フィルム層の上の光透過性バリア層と、
(d)バリア層の上に配置される光学素子と、
を含む表示装置をも提供する。
以下の実施例は、本明細書に記載の生成物および方法の説明的で非限定的なものである。当分野において通常遭遇し本開示を考慮すれば当業者には明らかとなる種々の条件、処方、およびその他のパラメーターの適切な修正および適応は、本発明の意図および範囲に含まれる。
InP/GaPの形成。3mLのTOP中に溶解させたGaCl3(90mg、0.51mmol)の120℃の溶液に、1.7mLのヘキサン中に溶解させたInPコア(140mg、0.96mmol)を加え、フラスコに短時間通気して、溶液からヘキサンを沸騰させ除去した。反応混合物から採取したアリコートによって、この温度でコアの吸収が475nmから481nmまで5nmだけシフトすることが示された。混合物を120℃で1時間維持した後、周囲温度まで冷却した。
InP/GaPの形成:3mLのTOPに、2mLのヘキサン中のInPコア(171mg、1.17mmol)の溶液を105℃で加え、フラスコに短時間通気して、TOP溶液からヘキサンを沸騰させ除去した。溶液を125℃まで加熱し、その温度でGaCl3を固体として加えた。溶液を125℃で20分間維持し、次に150℃まで加熱し、その温度で、0.75mLのTOP中のP(SiMe3)3(120mg、0.47mmol)の溶液を5分間かけて加えた。こうして得た混合物を150℃で20分間撹拌した後、温度を200℃まで上昇させ、その温度でさらに20分間維持した。この時間の後、混合物を周囲温度まで冷却した。
InP/GaP/ZnSの形成:3mLのTOP中に溶解させたGaCl3(90mg、0.51mmol)の120℃の溶液に、1.7mLのヘキサン中に溶解させたInPコア(140mg、0.96mmol)を加え、フラスコに短時間通気して、TOP溶液からヘキサンを沸騰させ除去した。反応混合物から採取したアリコートによって、この温度でコアの吸収が475nmから480nmまで5nmだけシフトすることが示された。次に混合物をゆっくり150℃まで加熱すると吸収スペクトルは変化せず、次に200℃なで加熱すると、この温度で吸収帯が490nmにシフトした。200℃において、1mLのTOP中のP(SiMe3)3(600mg、0.48mmol)の溶液を反応混合物に加え、これを200℃で20分間維持した。この結果、吸収帯が499nmまでさらに10nmのレッドシフトを示した(合計で、吸収帯の24nmレッドシフトがGaPシェル成長中に確認された)。
InP/AlPの形成:3mLのTOPに、2mLのヘキサン中のInPコア(171mg、1.17mmol)の溶液を110℃において加え、フラスコに短時間通気して、TOP溶液からヘキサンを沸騰させ除去した。次に同じ温度で、AlCl3を固体として加えた。AlCl3の添加後、UV−visにおける局所吸光度は、8.5nm(475nmから487.5nmまで)だけシフトし、溶液は自発的に115℃まで上昇した。この温度を20分間維持した後、混合物を150℃にさらに20分間加熱した。この時間の後、混合物を周囲温度まで冷却した。UV−visスペクトルは、InP/AlPナノ結晶が487nmで最大吸光度を有することを示した。この反応中のUV−visスペクトルの変化を図2中に示している。
InP/AlP/ZnSの形成:5mLのTOP中に溶解させたAlCl3(90mg、0.51mmol)の110℃の溶液に、3mLのTOP中に溶解させたInPコア(140mg、0.96mmol)を加えた。反応混合物から採取したアリコートによって、この温度でナノ結晶の吸収が475nmから489nmまで14nmシフトすることが示された。混合物を次にゆっくり150℃まで加熱すると、吸収スペクトルの変化は見られなかった。次に、150℃において、1mLのTOP中のP(SiMe3)3(600mg、0.48mmol)の溶液を反応混合物に加えると、吸収スペクトルのさらなるレッドシフトは見られなかった。続いて混合物を200℃に20分間加熱すると、今回の吸収帯の変化は見られなかった。
ガリウムラウレエート(gallium laureate)を用いてGa3+ドーピングを試みた。500mgのInPコア(473.5nmにおける吸収を有する)、2.3gのラウリン酸(ガリウムトリメチルガリウムとラウリン酸との反応によって調製される)、および30mLのODEを250mLのフラスコに投入した。反応混合物を280℃に40分間加熱した。その時間の間、InPコアは473.5nmから444nmへの29.5nmのブルーシフトを示した(図3)。反応混合物をICP−AESによって分析すると、結果はガリウムがコア中に混入されていないことを示した。ICP−AES(重量%):Zn、0.09%;P、0.22%;In、2.07%;Ga、検出されず.
ラウリン酸のみを用いる対照実験:ラウリン酸のみを使用し、ガリウムラウレエート(gallium laureate)は使用せずに、実施例5の手順を繰り返した。この結果15nmだけ吸収のブルーシフトが生じた(図4)。
オレイン酸のみを用いる対照実験:80℃において、ODE中に溶解させたInPコアにオレイン酸を加えた。次の10分間、吸収ピークは465nm〜458nmまで、すなわち合計7nmのブルーシフトが起こった。
三塩化ガリウムおよびオレイン酸を用いて文献報告の繰り返しを試みた(Kim et al., J. Am. Chem. Soc. 134: 3804-3809 (2012)。
オレイン酸のみを用いる文献報告の繰り返しを試みた。この実験の目的は、Kim et al., J. Am. Chem. Soc. 134: 3804-3809 (2012)に報告される文献を再現するためにガリウムが必要かどうかを調べることであった。同じ手順に従ったが、ガリウム源は全く使用しなかった。
Claims (29)
- InPコアと、第1のGaPまたはAlPのシェルとを含む、ナノ構造。
- 前記InPと前記第1のGaPまたはAlPのシェルとの間の合金を含む請求項1に記載のナノ構造。
- 前記第1のGaPまたはAlPのシェルを取り囲む第2のシェルをさらに含む、請求項1または2に記載のナノ構造。
- 前記第2のシェルが、CdS、CdSe、CdO、CdTe、ZnS、ZnO、ZnSe、ZnTe、MgTe、GaAs、GaSb、GaN、HgO、HgS、HgSe、HgTe、InAs、InSb、InN、AlAs、AlN、AlSb、AlS、PbS、PbO、PbSe、PbTe、MgO、MgS、MgSe、MgTe、CuCl、Ge、Si、およびそれらの合金からなる群から選択される、請求項3に記載のナノ構造。
- 第1のGaPシェルで取り囲まれ、ZnSシェルでさらに取り囲まれたInPコアを含む、請求項1に記載のナノ構造。
- 第1のAlPシェルで取り囲まれ、ZnSシェルでさらに取り囲まれたInPコアを含む、請求項1に記載のナノ構造。
- 請求項1に記載のナノ構造の製造方法であって、
(a)InPコアを、MX3(式中、M=AlまたはGaであり、X=アニオンである)およびリン化物源と溶媒中で接触させて、第1のGaPまたはAlPのシェルで取り囲まれたInPコアを得ることを含む、方法。 - 前記ナノ構造を単離することをさらに含む、請求項7に記載の方法。
- 前記リン化物源が(トリアルキルシリル)3ホスフィンである、請求項7または8に記載の方法。
- 前記(トリアルキルシリル)3ホスフィンが(トリメチルシリル)3ホスフィンである、請求項9に記載の方法。
- 前記アニオンが、F−、Cl−、Br−、I−、OH−、またはOSO2R−であり、式中、Rはアルキルまたは場合によりアルキル置換アリール基である、請求項7〜10のいずれか一項に記載の方法。
- 前記溶媒がトリオクチルホスフィン(TOP)である、請求項7〜11のいずれか一項に記載の方法。
- 前記第1のGaPまたはAlPのシェルで取り囲まれた前記InPコアを加熱することによって、前記InPとGaPまたはAlPとの間に合金を形成することをさらに含む、請求項7〜12のいずれか一項に記載の方法。
- 前記InPコアと前記第1のGaPまたはAlPのシェルとを取り囲む第2のシェルを形成することをさらに含む、請求項7〜13のいずれか一項に記載の方法。
- 前記第2のシェルがZnSを含む、請求項14に記載の方法。
- 前記第1のGaPまたはAlPのシェルで取り囲まれた前記InPコアを亜鉛源および硫黄源と溶媒中で接触させることを含む、請求項15に記載の方法。
- 前記亜鉛源がジカルボン酸亜鉛である、請求項16に記載の方法。
- 前記ジカルボン酸亜鉛がジオレイン酸亜鉛である、請求項17に記載の方法。
- 前記硫黄源がアルキルメルカプタンである、請求項16〜18のいずれか一項に記載の方法。
- 前記アルキルメルカプタンがオクタン−1−チオールである、請求項19に記載の方法。
- 前記溶媒がトリオクチルホスフィン(TOP)である、請求項7〜20のいずれか一項に記載の方法。
- (a)における前記接触が酸の非存在下で行われる、請求項7〜21のいずれか一項に記載の方法。
- マトリックスと、請求項1〜6のいずれか一項に記載のナノ構造の集団とを含むフィルム。
- 放射線を放出する層と、
前記放射線放出層の上に配置される、請求項1〜6のいずれか一項に記載のナノ構造の集団を含むフィルム層と、
前記フィルム層の上の光透過性バリア層と、
前記バリア層の上に配置される光学素子と、
を含む表示装置。 - 前記放射線放出層、前記フィルム層、および前記光学素子が前記表示装置のピクセル単位の一部である、請求項24に記載の表示装置。
- 前記光学素子がカラーフィルターである、請求項24または25に記載の表示装置。
- 前記バリア層が酸化物を含む、請求項24〜26のいずれか一項に記載の表示装置。
- 前記フィルム層が、前記光透過性バリア層に結合する界面活性剤またはリガンドをさらに含む、請求項24〜27のいずれか一項に記載の表示装置。
- 前記光透過性バリア層が、光束、熱、酸素、水分、またはそれらの組合せによる劣化から前記ナノ構造を保護するように構成される、請求項24〜28のいずれか一項に記載の表示装置。
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EP3405550A1 (en) | 2018-11-28 |
KR20180104010A (ko) | 2018-09-19 |
US10066161B2 (en) | 2018-09-04 |
EP3405550B1 (en) | 2021-04-21 |
US20200347295A1 (en) | 2020-11-05 |
US20170204326A1 (en) | 2017-07-20 |
US20180320068A1 (en) | 2018-11-08 |
CN108699434A (zh) | 2018-10-23 |
US10611958B2 (en) | 2020-04-07 |
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