JP6118825B2 - 新規材料並びに高量子収率及び高安定性を有するナノ粒子のマトリックス中への分散方法 - Google Patents
新規材料並びに高量子収率及び高安定性を有するナノ粒子のマトリックス中への分散方法 Download PDFInfo
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- JP6118825B2 JP6118825B2 JP2014555354A JP2014555354A JP6118825B2 JP 6118825 B2 JP6118825 B2 JP 6118825B2 JP 2014555354 A JP2014555354 A JP 2014555354A JP 2014555354 A JP2014555354 A JP 2014555354A JP 6118825 B2 JP6118825 B2 JP 6118825B2
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V9/00—Elements for modifying spectral properties, polarisation or intensity of the light emitted, e.g. filters
- F21V9/08—Elements for modifying spectral properties, polarisation or intensity of the light emitted, e.g. filters for producing coloured light, e.g. monochromatic; for reducing intensity of light
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- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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Description
(1)(i)第1の官能基と第2の官能基とを含むキャッピング分子でコーティングされた外表面を有するナノ粒子、特に発光ナノ粒子と、(ii)固体ポリマーの前駆体(本明細書では、「ポリマー前駆体」とも表記される)とを混合するプロセス要素、及び
(2)固体ポリマーを生成させ、埋め込まれたナノ粒子を有する固体ポリマーを製造するプロセス要素
を含み、
第1の官能基は量子ドットの外表面に結合するように構成され、且つ第2の官能基は、(a)固体ポリマーの前駆体と混和し得る機能、及び(b)固体ポリマーの前駆体と反応し得る機能からなる群から選択される1つ以上の機能を有する方法を提供する。
キャッピング分子の調製:
亜鉛及びシリコーン含有界面活性剤が、ジエチル亜鉛等の高反応性有機金属亜鉛と、酸、チオール等の官能基を有し、ジエチル亜鉛と反応できるシリコーンポリマーとの反応により調製される。例えば、
Zn−PDMSキャッピング分子の調製:ジエチル亜鉛+モノカルボキシデシル末端PDMS
ZnEt2+PDMS−CxH2xCOOH=(PDMS−CxH2xCOO)2Zn
CdリッチのCdSe/CdSのQRに対する交換:文献(L. Carbone, et al.“Synthesis and micrometer-scale assembly of colloidal CdSe/CdS nanorods prepared by a seeded growth approach”Nano Lett., 2007, 7 (10), 2942-2950)に従って、CdSe/CdSのロッドが予め合成される。合成後、QRは精製され、トルエンに再溶解され、2.5E−08M/mlの溶液を生成する。
表面改質QDが2つの方法によりシリコーンマトリックスに混合される。
QD−SylgardPDMSの例としてのQD−シリコーンポリマーマトリックスの調製:
Zn−PDMS及びアミノ−PDMSで改質されたQDを、トルエン又はクロロホルム等の溶媒に溶解させ、QD溶液を生成する。まず、Sylgard 184(成分B)等の、PDMSモノマーを含有するPDMS成分が溶液に加えられ、撹拌により透明な混合物を与える。その後、架橋剤及び触媒を含有する、Sylgard 184(成分A)等の他方の成分が、所望の重量比(Sylgard 184の場合、この比は10%である)で混合物に加えられる。その後、透明な混合物は、乾燥され、ある温度で硬化され(Sylgard 184の場合、150℃で、30分間である)、透明なQD−PDMSマトリックスを与える。
QD−Silres(登録商標)の例としてのQD−シリコーンポリマーマトリックスの調製:
上記ウンデシル酸亜鉛及び(3−メルカプトプロピル)−トリメトキシシランで改質されたQDをトルエン又はクロロホルム等の溶媒に溶解させ、QD溶液を生成する。Silres(登録商標) 610等のSilres(登録商標)モノマーが、所望の重量比で混合物に加えられる。その後、透明な混合物は乾燥され、ある温度で硬化され(Silres(登録商標) 610の場合、200℃で、30分間である)、透明なQD−Silres(登録商標)マトリックスを与える。
QD−アクリレートの例としてのQD−シリコーンポリマーマトリックスの調製:
メタクリル酸亜鉛で改質されたQDをトルエン又はクロロホルム等の溶媒に溶解させ、QD溶液を生成する。その後、メチルメタクリレート等のアクリレートモノマーが溶液に加えられる。その後、混合物は透明になるまで攪拌され、1重量%の光開始剤が加えられ、その後、混合物はUV照射下で硬化され、透明なQD−アクリレートマトリックスを与える。
材料のキャラクタリゼーション
QD−シリコーンポリマー複合体の成分及び構造は、容易に検出され得るであろう。構造は、TEM、XRDのキャラクタリゼーション法によってキャラクタライズされ得るであろう。成分は、IR、NMR、UV−可視、PL、ICPMS及びXPSにより、成分の種類、元素比についてキャラクタライズされ得るであろう。
量子収率は、積分球の中で、標準物質として、またQD−PDMSフィルムの吸収及び透過に使用するUV吸収体として、YAG蛍光体粉末(95%QE)を用いて測定される。QD−シリコーンフィルムの一例では、450nm〜700nmで90%を超える透明度を有し、また、マトリックス中にQDが0.3重量%含まれ、100μmの厚さのとき、最大90%のQEを有する。
Claims (14)
- ポリマー中に埋め込まれた発光ナノ粒子を有する固体ポリマーの製造方法であって、
(1)(i)第1の官能基と第2の官能基とを含むキャッピング分子でコーティングされた外表面を有する発光ナノ粒子と、(ii)前記固体ポリマーの前駆体とを混合するプロセス要素、及び
(2)前記固体ポリマーを生成させ、これにより埋め込まれたナノ粒子を有する前記固体ポリマーを製造するプロセス要素
を含み、
前記第1の官能基は量子ドットの外表面に結合し、且つ前記第2の官能基は、(a)前記固体ポリマーの前駆体と混和し得る機能、及び(b)前記固体ポリマーの前駆体と反応し得る機能からなる群から選択される1つ以上の機能を有し、
前記キャッピング分子は、2種類のキャッピング分子を含み、第1の種類のキャッピング分子の前記第1の官能基は、配位機能を有する金属イオンを含み、且つ第2の種類のキャッピング分子の前記第1の官能基は、ルイス塩基の機能を有する、方法。 - 前記第1の種類のキャッピング分子の前記第2の官能基と、前記第2の種類のキャッピング分子の前記第2の官能基とが同じである、請求項1に記載の方法。
- 固体ポリマーの前記前駆体が、重合により前記ポリマーを生成できるモノマーを含む、請求項1又は2に記載の方法。
- 固体ポリマーの前記前駆体がポリマーを含み、且つ前記第1のプロセス要素が、(1)(i)前記第1の官能基と前記第2の官能基とを含むキャッピング分子でコーティングされた外表面を有するナノ粒子と、(ii)前記固体ポリマーの前駆体と、(iii)前記固体ポリマーの前駆体用溶媒とを混合することを含む、請求項1又は2に記載の方法。
- 前記第2の官能基が、シロキサン、スチレン及びアクリレートからなる群から選択され、且つ前記固体ポリマーが、ポリシロキサン、ポリスチレン及びポリアクリレートからなる群から選択されるポリマーを含む、請求項1乃至4のいずれか一項に記載の方法。
- 前記ナノ粒子が、CdS、CdSe、CdTe、ZnS、ZnSe、ZnTe、HgS、HgSe、HgTe、CdSeS、CdSeTe、CdSTe、ZnSeS、ZnSeTe、ZnSTe、HgSeS、HgSeTe、HgSTe、CdZnS、CdZnSe、CdZnTe、CdHgS、CdHgSe、CdHgTe、HgZnS、HgZnSe、HgZnTe、CdZnSeS、CdZnSeTe、CdZnSTe、CdHgSeS、CdHgSeTe、CdHgSTe、HgZnSeS、HgZnSeTe及びHgZnSTeからなる群から選択される、請求項1乃至5のいずれか一項に記載の方法。
- 発光ポリマー製品に埋め込まれた、第1の官能基と第2の官能基とを含むキャッピング分子でコーティングされた外表面を有する発光ナノ粒子を有する固体ポリマーを含み、前記キャッピング分子は、2種類のキャッピング分子を含み、第1の種類のキャッピング分子の前記第1の官能基は、配位機能を有する金属イオンを含み、且つ第2の種類のキャッピング分子の前記第1の官能基は、ルイス塩基の機能を有する、発光ポリマー製品。
- 少なくとも一部の前記キャッピング分子の少なくとも一部の前記第2の官能基が、前記固体ポリマーのポリマー鎖と織り合わされている、請求項7に記載の発光ポリマー製品。
- 前記キャッピング分子の少なくとも一部の前記第2の官能基が、前記固体ポリマーのポリマー鎖の一部である、請求項7又は8に記載の発光ポリマー製品。
- 前記第1の種類のキャッピング分子の前記第2の種類のキャッピング分子に対するモル比が0.8〜1.2の範囲である、請求項7乃至9のいずれか一項に記載の発光ポリマー製品。
- 前記第2の官能基が、シロキサン、スチレン及びアクリレートからなる群から選択され、且つ前記固体ポリマーが、ポリシロキサン、ポリスチレン及びポリアクリレートからなる群から選択されるポリマーを含む、請求項7乃至10のいずれか一項に記載の発光ポリマー製品。
- 前記ナノ粒子が、CdS、CdSe、CdTe、ZnS、ZnSe、ZnTe、HgS、HgSe、HgTe、CdSeS、CdSeTe、CdSTe、ZnSeS、ZnSeTe、ZnSTe、HgSeS、HgSeTe、HgSTe、CdZnS、CdZnSe、CdZnTe、CdHgS、CdHgSe、CdHgTe、HgZnS、HgZnSe、HgZnTe、CdZnSeS、CdZnSeTe、CdZnSTe、CdHgSeS、CdHgSeTe、CdHgSTe、HgZnSeS、HgZnSeTe及びHgZnSTeからなる群から選択され、前記ポリマー製品が、コーティング、自立層、及びプレートからなる群から選択され、且つ前記ポリマー製品が、380〜750nmの範囲から選択される波長の光に対して透過性を有する、請求項7乃至11のいずれか一項に記載の発光ポリマー製品。
- (i)光源光を発生する光源、及び(ii)前記光源光の少なくとも一部をコンバーター光に変換する光コンバーターを含む照明ユニットであって、前記光コンバーターが、請求項7乃至12のいずれか一項に記載のポリマー製品を含む、照明ユニット。
- 複数のナノ粒子を含む発光材料であって、前記ナノ粒子が、第1の官能基と第2の官能基とを含むキャッピング分子によってコーティングされた外表面を含む量子ドット粒子を含み、前記キャッピング分子が−[−Si(R)2−O−]n(但し、n=1〜20で、Rがメチル基及びフェニル基から選択される)を含み、前記キャッピング分子は、2種類のキャッピング分子を含み、第1の種類のキャッピング分子の前記第1の官能基は、配位機能を有する金属イオンを含み、且つ第2の種類のキャッピング分子の前記第1の官能基は、ルイス塩基の機能を有する、発光材料。
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EP2809710A2 (en) | 2014-12-10 |
EP2809710B1 (en) | 2017-03-15 |
US9701897B2 (en) | 2017-07-11 |
KR20140126363A (ko) | 2014-10-30 |
CN104105739A (zh) | 2014-10-15 |
RU2627378C2 (ru) | 2017-08-08 |
JP2015516467A (ja) | 2015-06-11 |
RU2014135769A (ru) | 2016-03-27 |
CN104105739B (zh) | 2016-08-17 |
WO2013114254A3 (en) | 2014-01-09 |
BR112014018744A8 (pt) | 2017-07-11 |
ES2627005T3 (es) | 2017-07-26 |
KR102043269B1 (ko) | 2019-11-12 |
BR112014018744B1 (pt) | 2020-12-15 |
US20140369024A1 (en) | 2014-12-18 |
WO2013114254A2 (en) | 2013-08-08 |
BR112014018744A2 (ja) | 2017-06-20 |
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