JP7473050B2 - 量子ドット、量子ドットを用いた波長変換部材、照明部材、バックライト装置、並びに、表示装置 - Google Patents
量子ドット、量子ドットを用いた波長変換部材、照明部材、バックライト装置、並びに、表示装置 Download PDFInfo
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- JP7473050B2 JP7473050B2 JP2023078630A JP2023078630A JP7473050B2 JP 7473050 B2 JP7473050 B2 JP 7473050B2 JP 2023078630 A JP2023078630 A JP 2023078630A JP 2023078630 A JP2023078630 A JP 2023078630A JP 7473050 B2 JP7473050 B2 JP 7473050B2
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- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- ZMBHCYHQLYEYDV-UHFFFAOYSA-N trioctylphosphine oxide Chemical compound CCCCCCCCP(=O)(CCCCCCCC)CCCCCCCC ZMBHCYHQLYEYDV-UHFFFAOYSA-N 0.000 description 1
- FIQMHBFVRAXMOP-UHFFFAOYSA-N triphenylphosphane oxide Chemical compound C=1C=CC=CC=1P(C=1C=CC=CC=1)(=O)C1=CC=CC=C1 FIQMHBFVRAXMOP-UHFFFAOYSA-N 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 description 1
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 229940102001 zinc bromide Drugs 0.000 description 1
- BOXSVZNGTQTENJ-UHFFFAOYSA-L zinc dibutyldithiocarbamate Chemical compound [Zn+2].CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC BOXSVZNGTQTENJ-UHFFFAOYSA-L 0.000 description 1
- RKQOSDAEEGPRER-UHFFFAOYSA-L zinc diethyldithiocarbamate Chemical compound [Zn+2].CCN(CC)C([S-])=S.CCN(CC)C([S-])=S RKQOSDAEEGPRER-UHFFFAOYSA-L 0.000 description 1
- 229940105125 zinc myristate Drugs 0.000 description 1
- 229940012185 zinc palmitate Drugs 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- NRINZBKAERVHFW-UHFFFAOYSA-L zinc;dicarbamate Chemical class [Zn+2].NC([O-])=O.NC([O-])=O NRINZBKAERVHFW-UHFFFAOYSA-L 0.000 description 1
- GPYYEEJOMCKTPR-UHFFFAOYSA-L zinc;dodecanoate Chemical compound [Zn+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O GPYYEEJOMCKTPR-UHFFFAOYSA-L 0.000 description 1
- GJAPSKMAVXDBIU-UHFFFAOYSA-L zinc;hexadecanoate Chemical compound [Zn+2].CCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCC([O-])=O GJAPSKMAVXDBIU-UHFFFAOYSA-L 0.000 description 1
- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- GBFLQPIIIRJQLU-UHFFFAOYSA-L zinc;tetradecanoate Chemical compound [Zn+2].CCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCC([O-])=O GBFLQPIIIRJQLU-UHFFFAOYSA-L 0.000 description 1
- DUBNHZYBDBBJHD-UHFFFAOYSA-L ziram Chemical compound [Zn+2].CN(C)C([S-])=S.CN(C)C([S-])=S DUBNHZYBDBBJHD-UHFFFAOYSA-L 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
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Description
脂肪族1級アミン系、オレイルアミン:C18H35NH2、ステアリル(オクタデシル)アミン:C18H37NH2、ドデシル(ラウリル)アミン:C12H25NH2、デシルアミン:C10H21NH2、オクチルアミン:C8H17NH2
脂肪酸、オレイン酸:C17H33COOH、ステアリン酸:C17H35COOH、パルミチン酸:C15H31COOH、ミリスチン酸:C13H27COOH、ラウリル(ドデカン)酸:C11H23COOH、デカン酸:C9H19COOH、オクタン酸:C7H15COOH
チオール系、オクタデカンチオール:C18H37SH、ヘキサンデカンチオール:C16H33SH、テトラデカンチオール:C14H29SH、ドデカンチオール:C12H25SH、デカンチオール:C10H21SH、オクタンチオール:C8H17SH
ホスフィン系、トリオクチルホスフィン:(C8H17)3P、トリフェニルホスフィン:(C6H5)3P、トリブチルホスフィン:(C4H9)3P
ホスフィンオキシド系、トリオクチルホスフィンオキシド:(C8H17)3P=O、トリフェニルホスフィンオキシド:(C6H5)3P=O、トリブチルホスフィンオキシド:(C4H9)3P=O
本発明では、カドミウムを含まない量子ドットを合成するにあたり以下の原料を用いた。
溶媒
オクタデセン:Aldrich株式会社製、出光興産株式会社製
オレイルアミン:花王株式会社製:ファーミン
オレイン酸:花王株式会社製:ルナックO-V
トリオクチルホスフィン:北興化学株式会社製
塩化亜鉛:Aldrich株式会社製、又はキシダ化学株式会社製
ヨウ化亜鉛:Aldrich株式会社製
酢酸亜鉛2水和物:生駒化学株式会社製
無水酢酸亜鉛:Aldrich株式会社製
セレン(4N:99.99%):新興化学株式会社製、又はAldrich株式会社製
硫黄:キシダ化学株式会社製
<測定機器>
蛍光分光計:日本分光株式会社製 F-2700
紫外-可視光分光光度計:日立株式会社製 V-770
量子収率測定装置:大塚電子株式会社製 QE-1100
X線回折装置(XRD):Bruker社製 D2 PHASER
走査線電子顕微鏡(SEM):日立株式会社製 SU9000
100mL反応容器に、アセチルアセトナト銅:Cu(acac)2 131mgと、ドデカンチオール:DDT 1.5mLと、オレイルアミン:OLAm 4.75mLと、オクタデセン:ODE 6.25mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
100mL反応容器に、無水酢酸銅:Cu(OAc)2 36.3mgと、ドデカンチオール:DDT 0.3mLと、Se-DDT/OLAm溶液(0.5M)0.4mLと、オクタデセン:ODE 10mLを入れた。そして、不活性ガス(N2)雰囲気下、220℃で10分間、攪拌しつつ加熱した。得られた反応溶液(Cu2Se(S))を、室温まで冷却した。
100mL反応容器に、アセチルアセトナト銅:Cu(acac)2 131mgと、ドデカンチオール:DDT 1.5mLと、オレイルアミン:OLAm 4.75mLと、オクタデセン:ODE 6.25mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
100mL反応容器に、オレイン酸銅のオクタデセン溶液(0.2M):Cu(OLAc)2-ODE 1.2mLと、Se-ODE溶液 3mLと、溶液ドデカンチオール:DDT 0.4mLと、オクタデセン:ODE 3mLを入れた。この溶液を200℃で60分間、攪拌しつつ加熱した。得られた反応溶液(Cu2SeS)を、室温まで冷却した。
300mL反応容器に、無水酢酸銅:Cu(OAc)2 543mgと、ドデカンチオール:DDT 9mLと、オレイルアミン:OLAm 28.5mLと、オクタデセン:ODE 37.5mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
300mL反応容器に、無水酢酸銅:Cu(OAc)2 543mgと、ドデカンチオール:DDT 9mLと、オレイルアミン:OLAm 9mLと、オクタデセン:ODE 57mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
300mL反応容器に、無水酢酸銅:Cu(OAc)2 546mgと、ドデカンチオール:DDT 9mLと、オレイルアミン:OLAm 9mLと、オクタデセン:ODE 57mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
100mL反応容器に、無水酢酸銅:Cu(OAc)2 72.6mgと、オレイルアミン:OLAm 0.263mLと、オクタデセン:ODE 10mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
100mL反応容器に、無水酢酸銅:Cu(OAc)2 182mgと、ドデカンチオール:DDT 3mLと、オレイルアミン:OLAm 9.5mLと、オクタデセン:ODE 12.5mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
実施例6の反応溶液に、ドデシルアミン:DDA 0.6mLを入れ、不活性ガス(N2)雰囲気下にて、220℃で5分間、攪拌しつつ加熱した。
実施例6の反応溶液100mLに、ドデシルアミン:DDA 1mLを入れ、不活性ガス(N2)雰囲気下にて、220℃で5分間、攪拌しつつ加熱した。
実施例5の反応溶液10mLに、エタノールを加え沈殿を発生させ、遠心分離を施して沈殿を回収し、その沈殿にODEを加えて分散させた。
実施例6の反応溶液12.5mLに、エタノールを加え沈殿を発生させ、遠心分離を施して沈殿を回収し、その沈殿にODEを加えて分散させた。
実施例7の反応溶液10mLに、エタノールを加え沈殿を発生させ、遠心分離を施して沈殿を回収し、その沈殿にODEを加えて分散させた。
実施例7の反応溶液10mLに、エタノールを加え沈殿を発生させ、遠心分離を施して沈殿を回収し、その沈殿にODEを加えて分散させた。
100mL反応容器に、オレイン酸亜鉛:Zn(OLAc)2-ODE溶液(0.4M)0.833mLと、Se-ODE溶液(0.1M)10mLを入れ、不活性ガス(N2)雰囲気下、280℃で35分間攪拌しつつ加熱した。
100mL反応容器に、Se-ODE溶液(0.1M)20mLを入れ、不活性ガス(N2)雰囲気下、260℃で3分間攪拌しつつ加熱した。
100mL反応容器に、無水酢酸銅:Cu(OAc)2 183mgと、オレイルアミン:OLAm 0.66mLと、オクタン酸 0.64mL、オクタデセン:ODE 8.7mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
100mL反応容器に、オクタン酸亜鉛:141mgと、オクタデセン:ODE 20mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
Claims (9)
- カドミウムを含まない量子ドットであって、蛍光半値幅が、25nm以下であり、
Cuの残存量が100ppm以下であり、
前記量子ドットは、亜鉛とセレン、或いは、亜鉛とセレンと硫黄とを含有するナノクリスタルであることを特徴とする量子ドット。 - 前記量子ドットは、前記ナノクリスタルをコアとし、前記コアの表面にシェルが被覆されたコアシェル構造を有することを特徴とする請求項1に記載の量子ドット。
- 前記コアが、ZnSeSで形成されていることを特徴とする請求項2に記載の量子ドット。
- 前記量子ドットの表面が配位子で覆われていることを特徴とする請求項1から請求項3のいずれかに記載の量子ドット。
- 前記配位子は、脂肪族アミン系、ホスフィン系、及び、脂肪族カルボン酸系の少なくともいずれか1種から選択されることを特徴とする請求項4に記載の量子ドット。
- 請求項1から請求項5のいずれかに記載の量子ドットを含むことを特徴とする波長変換 部材。
- 請求項1から請求項5のいずれかに記載の量子ドットを含むことを特徴とする照明部材。
- 請求項1から請求項5のいずれかに記載の量子ドットを含むことを特徴とするバックライト装置。
- 請求項1から請求項5のいずれかに記載の量子ドットを含むことを特徴とする表示装置。
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WO2021070858A1 (ja) * | 2019-10-09 | 2021-04-15 | Nsマテリアルズ株式会社 | 量子ドット、及び、その製造方法 |
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JP2023101543A (ja) | 2023-07-21 |
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CN113583677A (zh) | 2021-11-02 |
US20240124774A1 (en) | 2024-04-18 |
TW201923036A (zh) | 2019-06-16 |
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