JP5878570B2 - 窒化物ナノ粒子の製造 - Google Patents
窒化物ナノ粒子の製造 Download PDFInfo
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- JP5878570B2 JP5878570B2 JP2014030049A JP2014030049A JP5878570B2 JP 5878570 B2 JP5878570 B2 JP 5878570B2 JP 2014030049 A JP2014030049 A JP 2014030049A JP 2014030049 A JP2014030049 A JP 2014030049A JP 5878570 B2 JP5878570 B2 JP 5878570B2
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- nanoparticles
- nitride
- nanocrystals
- electron
- capping agent
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
- C30B7/06—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent using non-aqueous solvents
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0632—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with gallium, indium or thallium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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Description
ヨウ化インジウム(300mg、0.6mmol)、ナトリウムアミド(500mg、12.8mmol)、ヘキサデカンチオール(380μl、1.0mmol)、ステアリン酸亜鉛(379mg、0.6mmol)およびジフェニルエーテル(20ml)(沸点259℃、溶媒として作用)を225℃まで急速に加熱した。構成成分のうち、ヨウ化インジウムは第III族金属(インジウム)を供給し、ナトリウムアミドは窒素を供給し、ヘキサデカンチオールは電子供与基を有するキャッピング剤であり、ステアリン酸亜鉛は電子求引基を有するキャッピング剤であり、そしてジフェニルエーテルは溶媒として働く。60分の経過の間、反応混合物の一部(0.25ml)を数回取り出し、それをシクロヘキサン(3ml)に希釈し、あらゆる不溶性物質を遠心分離機を用いて取り除いた。これにより得られる澄んだ溶液について、吸光光度法および発光分光法により分析をおこなった。その結果、図1および図2に示されるように、反応が経過している間、最大発光波長が、480nmから850nmまで変化することが示された。発光スペクトルにおけるピークは、ほぼ150nm程度の半値全幅強度を有していた。
ヨウ化インジウム(300mg、0.6mmol)、ナトリウムアミド(500mg、12.8mmol)、ヘキサデカンチオール(380μl、1.0mmol)、ステアリン酸亜鉛(379mg、0.6mmol)およびジフェニルエーテル(20ml)を250℃まで急速に加熱した。40分の経過の間、反応混合物の一部(0.25ml)を数回取り出し、それをシクロヘキサン(3ml)を用いて希釈し、あらゆる不溶性物質を遠心分離機を用いて取り除いた。これにより、放射性の窒化インジウムナノ結晶体の澄んだ溶液が得られる。実施例1と同様に、得られたナノ結晶体の吸収/放射特性は反応に依存しており、図1および図2に類似した時間依存性を示した。
ヨウ化インジウム(300mg、0.6mmol)、ナトリウムアミド(500mg、12.8mmol)、パルミチン酸(256.4、1.0mmol)、ステアリン酸亜鉛(379mg、0.6mmol)およびジフェニルエーテル(20ml)を225℃まで急速に加熱した。本実施例において、ヘキサデカンチオールではなく、パルミチン酸が、電子供与基を有するキャッピング剤として用いられている。
ナトリウムアミド(100mg、2.56mmol)、ステアリン酸亜鉛(76mg、0.12mmol)およびジフェニルエーテル(3ml)の混合物を、250℃に加熱した、ヨウ化インジウム(60mg、0.12mmol)とヘキサデカンチオール(62μl、0.2mmol)とを含むジフェニルエーテル(20ml)溶液中に、素早く添加した。試料(0.5ml)を、6〜20分の規則的な間隔で取り出し、トルエン(3ml)を用いて希釈した。結果として得られた試料の発光スペクトルは、試料を取り出した時間に応じて、最大値が420nm〜670nmに及ぶピークを示し、半値全幅は140〜200nmに広がっていた。
ヨウ化インジウム(InI3)(300mg、0.6mmol)を含むジフェニルエーテル(3ml)の高温溶液を、225℃に加熱した、ナトリウムアミド(500mg、12.8mmol)、ヘキサデカンチオール(612μl、2.0mmol)、ステアリン酸亜鉛(760mg、1.2mmol)およびジフェニルエーテル(20ml)を含む溶液に添加した。試料(0.5ml)を、1〜15分の規則的な間隔で取り出し、ヘキサン(3ml)を用いて希釈した。結果として得られた試料の発光スペクトルは、試料を取り出した時間に応じて、最大値が610nm〜810nmに及ぶピークを示し、半値全幅は152〜230nmに広がっていた。
窒素源としてナトリウムアミドを使用した場合と比較して、溶解性の窒素源を使用することにより、発光ピークの半値全幅強度が低減することが示されている。好適な溶解性窒素源の一つは、(CH3CH2)2NLi−ジエチルアミドリチウムである。用語「溶解性の」は、窒素源が反応混合物中に溶解できることを意味している。このことは、通常、反応が行われる溶媒に対して窒素源が溶解できることを要することと同等である。なぜなら、溶媒は、反応混合物の大部分(体積換算)を構成するであろうためである。窒素源は、完全に溶解できることを必要としないが、向上した溶解性は有益である。他の好適な溶解性の窒素源は、他の金属アミドであり、ジメチルアミドリチウム[(CH3)2NLi]、ジプロピルアミドリチウム[CH3(CH2)3NLi]、ジブチルアミドリチウム[CH3(CH2)4NLi]および一般式R2NMを有する他の金属アミドなどである。ここで、Mは、金属であり、Rは直鎖状または分枝鎖状のアルキル鎖である。発光ピークのピーク幅の減少は、窒素源の溶解性が増加することによって、より均質な反応混合物が得られ、これにより、個々のナノ結晶体の成長が互いに同じ時間に開始でき、それゆえ、反応の間、個々のナノ結晶体は、互いに、より類似したサイズとなり、これにより、結果物であるナノ結晶体における発光スペクトルの幅がより狭くなったことによるものと考えられる。
ヨウ化インジウム(600mg、1.2mmol)、ナトリウムアミド(1g、15.6mmol)、ヘキサデカンチオール(600μl、1.0mmol)、ステアリン酸亜鉛(760mg、1.2mmol)および1−オクタデセン(40ml)を250℃まで急速に加熱した。混合物を250℃で30分間保持した後、室温まで冷却し、遠心分離によりあらゆる不溶性物質を取り除いた。暗い色の溶液を、デカントで固体から移しとり、ジエチルジチオカルバミン酸亜鉛(1g、2.7mmol)とともに、175℃で60分間、さらに処理した。混合物を室温まで冷却し、あらゆる不溶性物質を遠心分離により取り除き、InN−ZnSコア−シェルナノ結晶体の溶液を残した。ジエチルジチオカルバミン酸亜鉛は、シェルのZnSの前駆物質である。ナノ結晶体は、シクロヘキサンにすぐに溶解する暗い固体を残すような、200mlの無水エタノールを用いた沈殿により、単離された。コア−シェルナノ結晶体は、対応するコアのみのナノ結晶体と比較して、向上したPLQYを示している。
ヨウ化ガリウム(113mg、0.25mmol)、ヨウ化インジウム(124mg、0.25mmol)、ナトリウムアミド(390 mg、10mmol)、ヘキサデカンチオール(153μl、0.5mmol)、ステアリン酸亜鉛(316mg、0.5mmol)および1−オクタデセン(40ml)を225℃まで急速に加熱し、225℃で保持した。20分、40分、および60分後に試料(0.25ml)を取り出し、シクロヘキサンを用いて希釈し、PLQYを測定した。結果、20分、40分、および60分の試料における値は、それぞれ14%、11%、および10.5%であった。反応混合物中にヨウ化ガリウムを追加することにより、結果として得られるナノ結晶体のPLQYが増加することが見られた。これはおそらくは、ガリウムがナノ結晶体中に組み込まれたためである。
ヨウ化ガリウム(113mg、0.25mmol)、ヨウ化インジウム(124mg、0.25mmol)、ナトリウムアミド(390 mg、10mmol)、ヘキサデカンチオール(153μl、0.5mmol)、ステアリン酸亜鉛(316mg、0.5mmol)および1−オクタデセン(40ml)を225℃まで急速に加熱した。混合物を225℃で60分間保持した後、混合物を室温まで冷却し、遠心分離してあらゆる不溶性物質を取り除いた。結果として得られる暗い色の溶液を、デカントで固体から移しとり、ジエチルジチオカルバミン酸亜鉛(1g、2.7mmol)とともに、175℃で60分間、さらに処理した。混合物を室温まで冷却し、あらゆる不溶性物質を遠心分離により取り除き、InGaN−ZnSコア−シェルナノ結晶体の溶液を残した。ナノ結晶体のPLQYを測定した結果、18%であった。このことは、InGaNナノ結晶体上にZnSシェルを成長させることによりPLQYが向上し、ナノ結晶体の長期にわたる安定性が向上したことを示している。
ヨウ化ガリウム(113mg、0.25mmol)、ヨウ化インジウム(124mg、0.25mmol)、ナトリウムアミド(390 mg、10mmol)、ヘキサデカンチオール(153μl、0.5mmol)、ステアリン酸亜鉛(316mg、0.5mmol)および1−オクタデセン(40ml)を225℃まで急速に加熱した。混合物を225℃で20分間保持した後、混合物を室温まで冷却し、遠心分離してあらゆる不溶性物質を取り除いた。結果として得られる濃い色つきの溶液を、デカントで固体から移しとり、試料4mlをジエチルジチオカルバミン酸亜鉛(100mg、0.27mmol)とともに、175℃で40分間、処理した。結果として得られたナノ結晶体は、PLQYが23%であった。このことは、InGaNナノ結晶体上にZnSシェルを成長させることによりPLQYおよび安定性が向上することを再び示している。
ヨウ化ガリウム(113mg、0.25mmol)、ヨウ化インジウム(124mg、0.25mmol)、ナトリウムアミド(390 mg、10mmol)、ヘキサデカンチオール(153μl、0.5mmol)、ステアリン酸亜鉛(316mg、0.5mmol)および1−オクタデセン(40ml)を225℃まで急速に加熱した。混合物を225℃で20分間保持した後、混合物を室温まで冷却し、遠心分離してあらゆる不溶性物質を取り除いた。結果として得られる溶液20mlを、ヨウ化ガリウム(113mg、0.25mmol)およびナトリウムアミド(185mg、5mmol)とともにさらに処理して、225℃まで加熱し、225℃で20分間保持した。得られたナノ結晶体を測定した結果、PLQYは28%であった。このことは、InGaNナノ結晶体上に窒化ガリウムシェルを成長させることによって、硫化亜鉛のシェルの場合よりもPLQYが大幅に向上することを示している。
ヨウ化ガリウム(113mg、0.25mmol)、ヨウ化インジウム(124mg、0.25mmol)、ナトリウムアミド(390 mg、10mmol)、ヘキサデカンチオール(153μl、0.5mmol)、ステアリン酸亜鉛(316mg、0.5mmol)および1−オクタデセン(40ml)を225℃まで急速に加熱した。混合物を225℃で20分間保持した後、混合物を室温まで冷却し、遠心分離してあらゆる不溶性物質を取り除いた。結果として得られる溶液20mlを、ヨウ化ガリウム(113mg、0.25mmol)およびナトリウムアミド(185mg、5mmol)とともにさらに処理して、225℃まで20分間加熱した。得られた溶液を遠心分離してあらゆる不溶性物質を取り除き、次いで、ジエチルジチオカルバミン酸亜鉛(500mg、1.35mmol)とともに処理し、175℃まで加熱して、175℃で60分間保持した。得られたナノ結晶体を測定した結果、PLQYは21.5%であった。これは、GaNによって被覆されているInGaNナノ結晶体上にZnSシェルを成長させることにより、コア−シェル−シェル構造体となる一つの例である。他のコア−シェル構造体と同様に、シェルがナノ結晶体の長期にわたる安定性を向上させる。
Claims (14)
- 発光窒化物ナノ粒子を製造する方法であって、
金属を包含する第1材料と、窒素を包含する第2材料と、窒化物ナノ粒子の光輝性量子収量を増加させるための電子求引基を有するキャッピング剤および電子供与基を有するキャッピング剤とを、第1の溶媒中で反応させることにより、窒化物ナノ粒子を製造する工程を含み、
上記第1材料は、第III族金属のヨウ化物であり、
上記第2材料は、金属アミドであり、
上記電子求引基を有するキャッピング剤は、カルボン酸亜鉛であり、
上記電子供与基を有するキャッピング剤は、カルボン酸またはチオールであり、
上記第1の溶媒は、沸点が少なくとも200℃である溶媒である、方法。 - 窒化物ナノ粒子を製造する方法であって、
金属を包含する第1材料と、窒素を包含する第2材料と、電子求引基を有するキャッピング剤および電子供与基を有するキャッピング剤とを、第1の溶媒中で反応させることにより、窒化物ナノ粒子を製造する工程を含み、
上記第1材料は、第III族金属のヨウ化物であり、
上記第2材料は、金属アミドであり、
上記電子求引基を有するキャッピング剤は、カルボン酸亜鉛であり、
上記電子供与基を有するキャッピング剤は、カルボン酸またはチオールであり、
上記第1の溶媒は、沸点が少なくとも200℃である溶媒である、方法。 - 上記窒化物ナノ粒子は、異なる2以上の金属を含む、請求項1または2に記載の方法。
- 上記第2材料は、上記第1の溶媒に対して溶解性である、請求項1〜3の何れか1項に記載の方法。
- 上記電子求引基を有する上記キャッピング剤および上記電子供与基を有する上記キャッピング剤のうちの少なくとも1つは、(i)メタノール、エタノールもしくは水、または(ii)トルエン、ヘキサンもしくはエーテルへの、上記窒化物ナノ粒子の溶解性を促進させる基を含む、請求項1〜4の何れか1項に記載の方法。
- 上記窒化物ナノ粒子の溶解性を促進させる上記基は、アルキル鎖である、請求項5に記載の方法。
- 上記窒化物ナノ粒子は、第III族窒化物ナノ粒子である、請求項1〜6の何れか1項に記載の方法。
- 上記窒化物ナノ粒子は、窒化インジウムナノ粒子である、請求項7に記載の方法。
- 上記第1材料は、ヨウ化インジウムであり、上記第2材料は、NaNH2、LiNH2またはKNH2である、請求項8に記載の方法。
- 上記第1材料、上記第2材料、上記電子求引基を有する上記キャッピング剤および上記電子供与基を有する上記キャッピング剤を150℃〜300℃の温度で反応させることにより、上記窒化物ナノ粒子を製造する工程を含む、請求項1〜9の何れか1項に記載の方法。
- 上記第1材料、上記第2材料、上記電子求引基を有する上記キャッピング剤および上記電子供与基を有する上記キャッピング剤を210℃〜250℃の温度で反応させることにより、上記窒化物ナノ粒子を製造する工程を含む、請求項10に記載の方法。
- 所望の寸法を有するナノ粒子を得るために、上記第1材料、上記第2材料、上記電子求引基を有する上記キャッピング剤および上記電子供与基を有する上記キャッピング剤を反応させる時間の長さを調節する工程を含む、請求項1〜11の何れか1項に記載の方法。
- コア−シェルナノ粒子を形成する方法であって、
請求項1〜12の何れか1項に記載の方法にしたがって窒化物結晶体を形成する工程を含み、該窒化物結晶体はナノ粒子のコアを形成しており、
さらに、上記コアの周囲にシェルを形成する工程を含む、方法。 - コア−シェルナノ粒子を形成する方法であって、
ナノ粒子のコアの周囲にシェルを形成する工程を含み、該シェルは、請求項1〜12の何れか1項に記載の方法によって形成される、方法。
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