JP5223339B2 - ナノ半導体粒子の製造方法 - Google Patents
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- C—CHEMISTRY; METALLURGY
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
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Description
本発明でいう「ナノ粒子」とは、ナノメートルオーダーの平均粒子径を有する微細粒子を意味する。ナノ半導体粒子の形状は、球状、棒状、板状、チューブ状などが考えられるが、本発明の製造方法から得られるナノ半導体粒子は、球状またはほぼ球状であると考えられ、粒子径はその直径を表している。本発明のナノ半導体粒子は、全体のサイズ(コア部とシェル部とを合せた部分の直径であるが、シェル部表面にさらに高分子鎖などが付される場合には、当該鎖も含める)として、通常は1000nm以下の平均粒子径である。
本発明のナノ半導体粒子は、コア・シェル構造をもつナノ半導体粒子であり、シェリングされた粒子の平均粒子径は100nm以下であり、かつ、コア部粒子径の変動係数が30%以内であることが好ましい。
高い発光効率が安定して得るようにコア部のサイズとシェル部のサイズとの関係が次のように規定される。本発明のコア・シェル構造をもつナノ半導体粒子の好ましい態様は、コア部粒子径が1nm以上であり、かつ、シェル部の厚みが最小で0.2nmであり、さらにコア部粒子径に対して1/100〜1/2のシェル厚みをもつことが好ましい。
本発明のナノ半導体粒子は、上記のように優れた性能の発光粒子として有望であるが、粒子サイズがナノオーダーであることからこの超微小粒子が発光集合体となった場合にバルク粒子とは異なる特性が発現される。ナノ粒子の光学特性に関してその粒子径分布との関係から見ると、ナノ粒子のサイズが量子効果として発光効率に大きく影響を及ぼすため、粒子径の分布の幅が大きい、換言すると粒子径の変動係数が大きいと、量子収率は上昇しない。結果的に標識分子としての発光性物質であっても、あるいは基板に固定されている発光体でも高性能のものでなくなる。
本発明のコア・シェル構造のナノ半導体粒子を作製する方法としては、特に限定されず、例えば、気相法、液相法(例えば、逆ミセル法、ホットソープ法、共沈を利用した方法)などの方法が知られている。しかしながら、ナノ半導体粒子は超微細粒であるがゆえに、粒子径分布のばらつきが少ない、なるべく均一なナノ粒子の集団を効率よく、しかも大量に製造することは容易ではない。ナノ粒子の製造に当たっては、多くの場合、その粒子径を微小とするために多数の核を同時に生成させることが必要となり、このため核の生成時に前駆体濃度を急上昇させなければならないことが、特開2003−225900号公報に記載されている。その際、反応系内での前駆体濃度、温度などが不均一になることが避けられない。そうした条件に起こる不均一性は、得られるナノ粒子の粒子径分布に著しい影響を与え、特にスケールアップした場合に、より顕著となることが予想される。
四塩化ケイ素を0.1mol/Lとなるように純水に溶解し、これをA液とした。硫酸ヒドラジンを0.1mol/Lとなるように純水に溶解し、これをB液とした。両液を60℃に保持し、ポンプAを用いて直径1mmのY字型反応装置に導入して反応させ、空気中、60℃で1時間加熱処理した。これにより平均粒子径4.5nmのSiナノ半導体粒子を得た。これをサンプル1とした。反応中のY字型反応装置における圧力変動係数は18%であった。
四塩化ケイ素を0.1mol/Lとなるように純水に溶解し、これをA液とした。硫酸ヒドラジンを0.1mol/Lとなるように純水に溶解し、これをB液とした。両液を60℃に保持し、ポンプBを用いて直径1mmのY字型反応装置に導入して反応させ、空気中、60℃で1時間加熱処理した。これにより平均粒子径4.4nmのSiナノ半導体粒子を得た。これをサンプル2とした。反応中のY字型反応装置における圧力変動係数は4%であった。
四塩化ケイ素を0.1mol/Lとなるように純水に溶解し、これをA液とした。硫酸ヒドラジンを0.1mol/Lとなるように純水に溶解し、これをB液とした。両液を60℃に保持し、ポンプCを用いて直径1mmのY字型反応装置に導入して反応させ、空気中、60℃1時間加熱処理した。これにより平均粒子径4.6nmのSiナノ半導体粒子を得た。これをサンプル3とした。反応中のY字型反応装置における圧力変動係数は1%であった。
Claims (3)
- コア部とシェル部とから構成されるコア・シェル構造を有し、シェリングされた粒子の平均粒子径が100nm以下であり、かつ、該コア部の粒子径の変動係数が30%以内であり、該コア部がシリコン核であり、該シェル部が酸化シリコン(SiO 2 )主体の層であるナノ半導体粒子の製造方法であって、
(i)四塩化ケイ素溶液と還元剤とを一様連続的に混合して反応させる工程と、(ii)形成されたシリコンナノ粒子を加熱酸化する工程とを含むことを特徴とするナノ半導体粒子の製造方法。 - 前記シェリングされた粒子の粒子径の変動係数が、30%以内であることを特徴とする請求の範囲第1項に記載のナノ半導体粒子の製造方法。
- 前記シェル部は、前記コア部よりもバンドギャップが大きい組成物から構成されていることを特徴とする請求の範囲第1項または第2項に記載のナノ半導体粒子の製造方法。
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PCT/JP2007/050783 WO2007086321A1 (ja) | 2006-01-27 | 2007-01-19 | ナノ半導体粒子 |
JP2007555912A JP5223339B2 (ja) | 2006-01-27 | 2007-01-19 | ナノ半導体粒子の製造方法 |
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US (1) | US7431867B2 (ja) |
EP (1) | EP1977992B1 (ja) |
JP (1) | JP5223339B2 (ja) |
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JP2007515361A (ja) * | 2003-03-06 | 2007-06-14 | レンセラー・ポリテクニック・インスティチュート | ナノ粒子の、室温におけるバルク固体からの迅速な生成 |
US20100255462A1 (en) * | 2006-01-27 | 2010-10-07 | Konica Minolta Medical & Graphic, Inc. | Fluorescent marker for living organism and fluorescent marking method for the same |
WO2007086188A1 (ja) * | 2006-01-30 | 2007-08-02 | Konica Minolta Medical & Graphic, Inc. | 三層型半導体ナノ粒子および三層型半導体ナノロッド |
JP5045876B2 (ja) * | 2006-03-15 | 2012-10-10 | 学校法人東京電機大学 | 発光輝度の持続性に優れたナノシリコン粒子とその製造方法 |
JP5151993B2 (ja) * | 2007-01-22 | 2013-02-27 | コニカミノルタエムジー株式会社 | コア/シェル型半導体ナノ粒子とその製造方法 |
WO2009050639A1 (en) * | 2007-10-16 | 2009-04-23 | Nxp B.V. | Particle comprising core and shell and applications thereof |
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US7431867B2 (en) | 2008-10-07 |
WO2007086321A1 (ja) | 2007-08-02 |
EP1977992A1 (en) | 2008-10-08 |
US20070187463A1 (en) | 2007-08-16 |
ES2402812T3 (es) | 2013-05-09 |
EP1977992A4 (en) | 2010-03-10 |
EP1977992B1 (en) | 2012-12-12 |
JPWO2007086321A1 (ja) | 2009-06-18 |
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