JP4567436B2 - 発光ナノ粒子およびそれらの調製方法 - Google Patents
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Description
従って、単離された半導体コアを提供する工程、第1のシェル前駆物質、第2のシェル前駆物質、溶媒、ならびに付加物とコアを混合する工程を包含する方法に従って調製される発光性ナノ粒子を提供することによって、上述の当該分野における必要性に取り組むことが、本発明の主な目的である。この付加物としては、2族元素、12族元素、13族元素、14族元素、15族元素、16族元素、またはFe、Nb、Cr、Mn、Co、Cu、およびNiが挙げられ得る。このようにして形成される反応分散物は、半導体コア上に無機のシェルの形成を引き起こすのに十分な温度および期間、加熱される。
(概要および定義)
本発明を詳細に説明する前に、他に示されない限り、本発明は、特定のナノ粒子物質または製造プロセス(これらは、変動し得るので)に限定されないことが理解されるべきである。本明細書中で使用される用語は、特定の実施形態を説明することのみを目的とし、そして制限されることが意図されないこともまた理解されるべきである。
新規のコア−シェル構造を包含する発光ナノ粒子の調製方法を、本明細書中に開示する。この方法によって調製された発光ナノ粒子もまた開示される。理論に束縛されることは望まれないが、これらの方法は、コア物質とシェル物質との間の格子構造の不一致を補うことによって半導体コア上の高品質の厚いシェルの過成長を促進するようである。この補償は、以下に提案されるいくつかのコア−シェル構造の1つ以上を生じ得る。簡便なコア−シェル構造を、図1に示す。
本明細書中に記載される方法は、半導体コアおよび無機物シェルの合成の間、元素の導入の程度および性質を制御するために、体系的な合成様式において使用され得る。この方法は、単一の反応容器内(すなわち、「ワンポット(one−pot)」合成)で行なわれ得るか、または半導体コアおよび無機物シェルの分離合成を使用して行なわれ得る。
(追加のジメチルカドミウムを用いるコア−シェルナノクリスタルの調製)
トリ−n−オクチルホスフィンオキシド(TOPO、30g)を、マントルヒーター上の攪拌子を含み、そしてバンプトラップおよび熱電対(および温度コントローラー)を備えた、3つ首丸底フラスコ中で、180℃で減圧下1時間脱気した。溶融反応物を、乾燥N2雰囲気下に置いて、350℃に加熱した。不活性雰囲気のグローブボックスの中で、Se(360mg)を、トリ−n−オクチルホスフィン(TOP、20mL)の中でジメチルカドミウム(230μl)と混合した。シングルラピッドインジェクションにおいて、このTOP溶液を、反応物から熱源を取り除いた後に、熱TOPOポットに添加した。インジェクションの後、温度を、265℃まで下げ、そして290℃に加熱した。1℃/時間の傾きで熱を上げながら、粒子の最大発光が608nmに達するまで、6.5時間反応に供した。この反応物を、100℃まで冷却した。デシルアミン(11mL)をシリンジを介して添加し、そして加熱を一晩維持した。
(追加のカドミウムジアセテートを用いるコア−シェルナノクリスタルの調製)
ナノクリスタルを、シェルオーバーコーティング手順におけるジメチルカドミウム/TOP溶液を、カドミウムジアセテート/TOP溶液と交換した以外、実施例1に記載されるのと類似の様式で調製した。カドミウムジアセテート/TOP溶液の0.67M溶液の0.25mLを用いた。得られたオーバーコーティングされたナノクリスタルは、実施例1で調製されたものと類似のシェル厚を表した。光安定性もまた同等であった。
(添加剤として非常に大量のシェル前駆体を用いるコア−シェルナノクリスタルの調製)
コア反応を、ナノ粒子の発光ピークが608nmではなく622nmに達した時に、反応を停止した以外、実施例1に記載されるように実行した。ジメチルカドミウムも、カルシウムジアセテートもシェル反応物に添加しなかった。シェルストック溶液は、TOP(6.3g)、ジエチル亜鉛(206mg)、およびビス(トリメチルシリル)スルフィド(450mg)を含んだ。シェル反応を、図5に示されるS前駆体:Zn前駆体比で含んで行った。さらに、コントロール反応を、1:1のモル比のS前駆体とZn前駆体を用いて行った。シェル厚および粒子の形態を、全てのS前駆体:Zn前駆体比について評価した。劇的な差異を、粒子の明るさにおいて観察し:0.76および0.22の発光量子収率を、それぞれ、1.5:1のS前駆体:Zn前駆体モル比反応物およびコントロール反応物について測定した(図5を参照のこと)。
(イオン性前駆体のみを用いるコアおよび改変型シェル)
(CdSeコア合成)
セレンの第1の前駆体溶液を、10mLのTBP(トリ−n−ブチルホスフィン)中に0.79gのSeを溶解することにより調製した。カドミウムの第2の前駆体溶液を、50gの最終重量までTOP中の5.76g無水カドミウムアセテートを溶解することにより調製した。
上で調製したCdSe粒子(「コア」)の10mLを、20mLの75%メタノール/25%イソプロパノール(v/v)で凝集させた。遠心分離後、コアを5mLのヘキサン中に再分散させた。
(CdTe/ZnSコア−シェル構造)
(CdTeコアの調製)
TDPA(0.56g)、TOPO(5.00g)、およびTeflon(登録商標)をコーティングした小さな攪拌子を、3つ首丸底フラスコ中に置いた。このフラスコを、マグネチックスターラープレート上の60Wマントルヒーター内の所定の位置に固定し、白いゴム製のセプタムを装着し、コンデンサーを真空−窒素マニホルドに接続し、そして熱電対を温度コントローラーに接続した。リアクタを真空にし、そして窒素を三回充填し、そして減圧下で攪拌しながら100℃に加熱し、これを3時間維持した。容器を窒素で充填し、そして窒素ブランケットを維持した。シリンジにより、TOP中のカドミウムアセテート(0.5m、2.00g)を、セプタムを通して添加した。2つの18ゲージの針をセプタムに挿入し、そしてリアクタに窒素を噴霧しながら、温度を320℃まで上げた。これら2つの針を、250℃で取り除いた。温度が初めて310℃になった10分後、TOP中のTOP:Te(1.75m、0.86g)をシリンジにより添加した。マントルヒーターを4.25分後に取り除き、そして反応物を冷却させた。反応物が100℃に冷却されたとき、トルエン(4.8mL)を添加した。攪拌しながら、メタノール(14.5mL)を添加し、そして凝集したコアを遠心分離により単離した。コアを5mLのメタノールでリンスし、そして風乾させた。ヘキサン(14mL)を添加してコアを分散させた。
ヘキサン(3.5mL)中に分散させたCdTeコアを、TOPO(5.00g)を含む3つ首丸底フラスコに添加した。フラスコに、真空−窒素マニホルドに接続した6インチコンデンサー、白色のゴム製セプタム、および温度コントローラーに接続された熱電対を装着した。ヘキサンを加熱なしに減圧下で除去し、温度を室温未満に低下させた。一旦真空になると、反応物を100℃に加熱し、そして90分間維持した。窒素に切り替えた後、TOP(2.50g)およびデシルアミン(4.35mL)を添加した。反応物を100℃にて一晩維持した。TDPA(0.336g)を、ゴム製セプタム、真空−窒素マニホルド接続部、および温度コントローラーに接続した熱電対を備えた、25mLの3つ首丸底フラスコ中に置いた。リアクタを真空にし、そして窒素を3回充填した。TOP中のカドミウムアセテート(0.5m、1.21g)およびTOP(1.30g)を、窒素下で添加し、そして反応物を250℃に加熱し、引き続いて、100℃に冷却した。熱液体をコアに移した。混合しながら、ジエチル亜鉛(0.075g)を、TOP(0.50g)を含むバイアルに添加した。この混合物に、ビス(トリメチルシリル)スルフィド(0.108g)を混合しながら添加した。このバイアルを旋回させて内容物を混合し、シリンジに移した。CdTeコア溶液を215℃に加熱し、そして亜鉛/イオウ/TOP溶液を、1mL/時間で添加した。最後に、温度を90℃に低下させ、これを1日維持した。ストック溶液添加の関数としての発光の発生のプロットを、図5に表す。
(コアをシェルを有するCd(II)前駆体から作製する:添加剤としてのコア反応物の成分の使用)
(コア合成)
セレン(Se)の第1の前駆体溶液を、10mlのTBP中に0.79gのSeを溶解することにより調製した。カドミウムの第2の前駆体溶液を、40mLの最終容量まで、TOP中に6.15gの無水カドミウムアセテートを溶解することにより調製した。
2.0mLのデシルアミンを、コア分散物に添加した。それによって形成された、デシルアミン/コア分散物を100℃にて一晩維持した。11gのTOPO(Alfa、工業用グレード)を、丸底フラスコ中で減圧下で180℃にて1時間脱気した。3mlのデシルアミン/コア分散物を、TOPOに添加して、TOPO/デシルアミン/コア分散物を形成させた。フラスコを200℃に加熱した。シェル前駆体ストック溶液を5.0gのTOP、30mgのジエチル亜鉛、および43mgのビス−トリメチルシリルスルフィドを混合することにより作製した。2.9mLのシェル前駆体ストックを、100μl/分の速度でTOPO/デシルアミン/コア分散物に添加した。次いで、フラスコを冷却させ、そしてこのように形成したコア−シェル分散物の保存の前に、トルエンを添加した。
Claims (8)
- 以下の工程:
a)単離された半導体コアを提供する工程;
b)該コアと、以下:
i.第1のシェル前駆体、
ii.第2のシェル前駆体、
iii.溶媒、および
iv.CdまたはSから選択される元素を含む、添加剤、
を混合して、反応分散物を形成する工程;
c)該半導体コア上への無機シェルの形成を誘導する温度で、それに十分な時間にわたって、該反応分散物を加熱する工程、
を包含する方法によって調製された、半導体コア、無機シェル、およびその間の界面領域からなる発光ナノ粒子であって、
該半導体コアが、実質的にCdSeまたはCdTeであり、かつ
該無機シェルが、実質的にZnSであり、
該添加剤は、該界面領域と該シェルの両方に存在し、
該シェルは、該半導体コアから外向き方向で、該添加剤の減少する濃度の勾配を示す、発光ナノ粒子。 - 前記溶媒および前記添加剤が、前記第1のシェル前駆体および第2のシェル前駆体の添加の前に、前記コアと混合され、そして工程(c)が、該第1のシェル前駆体および第2のシェル前駆体の添加と同時である、請求項1に記載のナノ粒子。
- 前記溶媒および前記半導体コアが、前記第2のシェル前駆体の添加の前に、前記添加剤と混合され、そして工程(c)が、該第2のシェル前駆体の添加と同時である、請求項1に記載のナノ粒子。
- 前記溶媒および前記半導体コアが、前記添加剤の添加の前に、前記第1のシェル前駆体と混合され、そして工程(c)が、該第2のシェル前駆体の添加と同時である、請求項1に記載のナノ粒子。
- 以下の工程:
a)単離された半導体コアを提供する工程;
b)該コアと、以下:
i.第1のシェル前駆体、
ii.第2のシェル前駆体、
iii.溶媒、および
iv.CdまたはSから選択される元素を含む、添加剤、
を混合して、反応分散物を形成する工程;
c)該半導体コア上への無機シェルの形成を誘導する温度で、それに十分な時間にわたって、該反応分散物を加熱する工程、
を包含する、半導体コア、無機シェル、およびその間の界面領域からなる発光ナノ粒子を調製する方法であって、
該半導体コアが、実質的にCdSeまたはCdTeであり、かつ
該無機シェルが、実質的にZnSであり、
該添加剤は、該界面領域と該シェルの両方に存在し、
該シェルは、該半導体コアから外向き方向で、該添加剤の減少する濃度の勾配を示す、方法。 - 前記溶媒および前記添加剤が、前記第1のシェル前駆体および第2のシェル前駆体の添加の前に、前記コアと混合され、そして工程(c)が、該第1のシェル前駆体および第2のシェル前駆体の添加と同時である、請求項5に記載の方法。
- 前記溶媒および前記半導体コアが、前記第2のシェル前駆体の添加の前に、前記添加剤および前記第1のシェル前駆体と混合され、そして工程(c)が、該第2のシェル前駆体の添加と同時である、請求項5に記載の方法。
- 前記溶媒および前記半導体コアが、前記添加剤および第2のシェル前駆体の添加の前に、前記第1のシェル前駆体と混合され、そして工程(c)が、該第2のシェル前駆体の添加と同時である、請求項5に記載の方法。
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US30678701P | 2001-07-20 | 2001-07-20 | |
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