JP4928775B2 - 半導体ナノ粒子表面修飾方法 - Google Patents
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Description
[実施例]
(サイズ選択光エッチング法を用いる場合)
まず、30℃の超純水1000ml入った容器に、ヘキサメタリン酸ナトリウム61.8mg(0.1mmol)と過塩素酸カドミウム84.4mg(0.2mmol)を加え、さらにリン酸水素二ナトリウム141.960mg(1mmol)を加え、この溶液を、窒素バブリングしながら密閉した容器中で30分間攪拌した。その後、前記容器を激しく振りながら、S2−とCd2+が等量となるように、硫化水素ガス4.96cm−3(1atm、25°)を加えた後、室温で数時間攪拌を行った。このとき、溶液の色は、光学的に透明な無色から光学的に透明な黄色へ変化する。さらに、溶液を窒素バブリングすることにより、該溶液中の未反応の硫化水素を取り除いた後、酸素バブリングを10分間行ない、メチルビオロゲン25.7mg(0.1mmol)を加えた。ここで、前記溶液に対し、レーザー等を用いた単色光、あるいは、カラーフィルターを介した水銀ランプ光を照射し、サイズ選択光エッチング法による粒径制御を行った。その後、前記溶液を窒素バブリングしながら30分間攪拌し、3−メルカプトプロピオン酸50μlを加え、遮光下で一晩攪拌を行った。
まず、30℃の超純水1000ml入った容器に、ヘキサメタリン酸ナトリウム61.8mg(0.1mmol)と過塩素酸カドミウム84.4mg(0.2mmol)を加え、さらにリン酸水素二ナトリウム28.392mg(0.2mmol)とリン酸二水素ナトリウム95.984mg(0.8mmol)を加え、この溶液を、窒素バブリングしながら密閉した容器中で30分間攪拌した。その後、前記容器を激しく振りながら、S2−とCd2+が等量となるように、硫化水素ガス4.96cm−3(1atm、25°)を加えた後、室温で数時間攪拌を行った。さらに、溶液を窒素バブリングすることにより、該溶液中の未反応の硫化水素を取り除いた後、3-メルカプトプロピオン酸50μlを加え、遮光下で一晩攪拌を行った。
上記のようにして得られた有機溶媒中に完全に分散したナノ粒子を用いて、両親媒性分子による被覆を行った。前記有機溶媒中に完全に分散したナノ粒子溶液10mlを共栓付試験管やナスフラスコ等の容器にいれ、エバポレーションを行ない容器内壁にて膜状とする。その後、クロロホルム中に塩化ドデシルトリメチルアンモニウムを5mMとなるように溶かした溶液を2ml加えて粒子を再溶解させ、エバポレーションを行ない再度容器内壁にて膜状とする。さらに90℃に加温して残留しているクロロホルムを除去し、メタノールを2ml加えて再度粒子を溶解させた。その後、超純水を10ml加え90℃に加温しながらしばらく攪拌することでメタノールを除去した。最終的に遠心分離を行ない、沈殿を除去することにより、光学的に透明な黄色の溶液を得ることができた。このときの構造模式図を図2に、光学スペクトルを図3に示す。
上記のようにして得られた有機溶媒中に完全に分散したCdSナノ粒子10mlをナス型フラスコに入れ、エバポレーションによりヘキサンを除去した。これに、クロロホルム2mlとオクタデシルアミンを0.5mMとなるように加え、超音波を用いて溶解させた。さらに、エバポレーションによりクロロホルムを除去し、THFを2ml加えて再溶解させた。ここでは、超音波処理を用いてもよい。その後、ナス型フラスコに10mlの超純水と撹拌子を入れ、スターラーで撹拌しながら、THF中に溶解させたCdSナノ粒子を、急激に注入した。この溶液を超音波処理等により溶解させ、エバポレーションによりTHFのみを除去して水溶液とした後、遠沈管に溶液を入れ、遠心分離により沈殿を取り除いた。このとき得られるのは、表面にアミノ基が配列した水溶性ナノ粒子である。
Claims (25)
- 半導体ナノ粒子に官能基を有するポリマーが静電的に結合し、該半導体ナノ粒子が該ポリマーで修飾され、前記官能基を有するポリマーの官能基が、−COOH、−OH、−NH 2 、−SH、−OCN、−CNO、−CH=O、−CH=CH 2 、−C≡CHから選択される1種以上であることを特徴とする半導体ナノ粒子。
- 前記半導体ナノ粒子表面に電子供与性基が配列し、該電子供与性基の外側に前記ポリマーが静電的に結合していることを特徴とする請求項1に記載の半導体ナノ粒子。
- 前記電子供与性基が、−OR、−OCH2R、−OCOCH2R、−NHR、−N(CH2R)2、−NHCOCH2R、−CH2R、−C6H4R[ここで、Rは水素、置換または無置換の炭化水素基から選ばれる]の少なくとも1種以上であることを特徴とする請求項2に記載の半導体ナノ粒子。
- 前記官能基を有するポリマーが、架橋剤によりクロスリンクしていることを特徴とする請求項1乃至3のいずれかに記載の半導体ナノ粒子。
- 前記クロスリンク結合が、エステル結合、アミド結合、イミド結合、エーテル結合、ウレタン結合、スルフィド結合、ポリスルフィド結合、カーボネート結合、チオール結合、チオエステル結合、チオウレタン結合から選択される1種以上であることを特徴とする請求項4に記載の半導体ナノ粒子。
- 前記クロスリンク結合が、炭素−炭素2重結合または炭素−炭素3重結合の重合によるものであることを特徴とする請求項4に記載の半導体ナノ粒子。
- 前記官能基を有するポリマーがポリアクリル酸であり、前記架橋剤がアルキレンジアミンであることを特徴とする請求項4乃至6のいずれかに記載の半導体ナノ粒子。
- 前記官能基を有するポリマーが半導体ナノ粒子を被覆する化合物を介して半導体ナノ粒子表面と結合していることを特徴とする請求項1乃至7のいずれかに記載の半導体ナノ粒子。
- 前記半導体ナノ粒子表面を被覆する化合物が、第1級アミン類(R1NH2)、第2級アミン類(R1R2NH)、第3級アミン類(R1R2R3N)、第4級アンモニウム化合物類(R4R5R6R7N+)[ここで、R1〜R7は、それぞれ水素、置換または無置換の炭化水素基から選ばれる]から選択される1種以上であることを特徴とする請求項8に記載の半導体ナノ粒子。
- 前記R1〜R7が、アミノ基又はアンモニウム基とは逆の末端に置換基を有することを特徴とする請求項9に記載の半導体ナノ粒子。
- 前記半導体ナノ粒子の材質が、ZnO、ZnS、ZnSe、ZnTe、CdO、CdS、CdMnS、CdSe、CdMnSe、CdTe、CdMnTe、HgS、HgSe、HgTe、InP、InAs、InSb、InN、GaN、GaP、GaAs、GaSb、TiO2、WO3、PbS、PbSe、MgTe、AlAs、AlP、AlSb、AlS、Ge、Siから選択される1種以上の半導体ナノ粒子、又はこれら半導体材質がコア部とシェル部の複層構造を有する半導体ナノ粒子であることを特徴とする請求項1乃至10のいずれかに記載の半導体ナノ粒子。
- 前記半導体ナノ粒子の粒径が、直径において10%rms未満の偏差を示す単分散であることを特徴とする請求項1乃至11のいずれかに記載の半導体ナノ粒子。
- 前記半導体ナノ粒子が、励起光を照射されたときに半値全幅(FWHM)で60nm以下の狭いスペクトル範囲で光を放出することを特徴とする請求項1乃至12のいずれかに記載の半導体ナノ粒子。
- 半導体ナノ粒子表面に、官能基を有するポリマーを静電的に結合させる工程と該ポリマーの官能基を架橋剤によってクロスリンクさせる工程とを含み、前記官能基を有するポリマーが官能基として、−COOH、−OH、−NH 2 、−SH、−OCN、−CNO、−CH=O、−CH=CH 2 、−C≡CHから選択される1種以上を有することを特徴とする半導体ナノ粒子の製造方法。
- 半導体ナノ粒子に1種以上の電子供与性基を与える表面処理材料を加え、半導体ナノ粒子表面に電子供与性基を配列させる工程と、該半導体ナノ粒子表面に官能基を有するポリマーを静電的に結合させる工程、該ポリマーの官能基を架橋剤によってクロスリンクさせる工程とを含み、前記官能基を有するポリマーが官能基として、−COOH、−OH、−NH 2 、−SH、−OCN、−CNO、−CH=O、−CH=CH 2 、−C≡CHから選択される1種以上を有することを特徴とする半導体ナノ粒子の製造方法。
- 半導体ナノ粒子表面に電子供与性基を与える表面処理材料が、純金属および金属化合物、アンモニア、アミン類、アンモニウム類、ニトリル類、イソシアネート類から選択される含窒素化合物、又は、アルコール類、フェノール類、ケトン類、アルデヒド類、カルボン酸類、有機酸または無機酸のエステル類、エーテル類、酸アミド類、酸無水物類から選択される含酸素化合物の少なくとも1種以上であることを特徴とする請求項15に記載の半導体ナノ粒子製造方法。
- 前記電子供与性基を配列させた半導体ナノ粒子を被覆する工程を含むことを特徴とする請求項15に記載の半導体ナノ粒子の製造方法。
- 前記半導体ナノ粒子を被覆する材料が、第1級アミン類(R1NH2)、第2級アミン類(R1R2NH)、第3級アミン類(R1R2R3N)、第4級アンモニウム化合物類(R4R5R6R7N+)[ここで、R1〜R7は水素、置換または無置換の炭化水素基から選ばれる]の少なくとも1種以上であることを特徴とする請求項17に記載の半導体ナノ粒子の製造方法。
- 前記R1〜R7が、アミノ基又はアンモニウム基とは逆の末端に置換基を有することを特徴とする請求項18に記載の半導体ナノ粒子の製造方法。
- 前記クロスリンクが、エステル化反応、アミド化反応、イミド化反応、エーテル化反応、ウレタン化反応、スルフィド化反応、ポリスルフィド化反応、カーボネート化反応、チオール化反応、チオエステル化反応、チオウレタン化反応から選択される1種以上で行われることを特徴とする請求項14乃至19のいずれかに記載の半導体ナノ粒子の製造方法。
- 前記クロスリンクが、炭素−炭素2重結合または炭素−炭素3重結合の重合反応で行われることを特徴とする請求項14乃至19のいずれかに記載の半導体ナノ粒子の製造方法。
- 前記官能基を有するポリマーがポリアクリル酸であり、前記架橋剤がアルキレンジアミンであることを特徴とする請求項14乃至21のいずれかに記載の半導体ナノ粒子の製造方法。
- 前記半導体ナノ粒子の材質が、ZnO、ZnS、ZnSe、ZnTe、CdO、CdS、CdMnS、CdSe、CdMnSe、CdTe、CdMnTe、HgS、HgSe、HgTe、InP、InAs、InSb、InN、GaN、GaP、GaAs、GaSb、TiO2、WO3、PbS、PbSe、MgTe、AlAs、AlP、AlSb、AlS、Ge、Siから選択される1種以上の半導体ナノ粒子、又はこれら半導体材質がコア部とシェル部の複層構造を有する半導体ナノ粒子であることを特徴とする請求項14乃至22のいずれかに記載の半導体ナノ粒子の製造方法。
- 請求項1乃至13のいずれかに記載の半導体ナノ粒子からなる蛍光試薬。
- 請求項1乃至13のいずれかに記載の半導体ナノ粒子からなる光デバイス。
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