JP6507284B2 - 多孔質粒子内の封止量子ドット - Google Patents
多孔質粒子内の封止量子ドット Download PDFInfo
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- JP6507284B2 JP6507284B2 JP2018079653A JP2018079653A JP6507284B2 JP 6507284 B2 JP6507284 B2 JP 6507284B2 JP 2018079653 A JP2018079653 A JP 2018079653A JP 2018079653 A JP2018079653 A JP 2018079653A JP 6507284 B2 JP6507284 B2 JP 6507284B2
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
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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
- 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
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21K—NON-ELECTRIC LIGHT SOURCES USING LUMINESCENCE; LIGHT SOURCES USING ELECTROCHEMILUMINESCENCE; LIGHT SOURCES USING CHARGES OF COMBUSTIBLE MATERIAL; LIGHT SOURCES USING SEMICONDUCTOR DEVICES AS LIGHT-GENERATING ELEMENTS; LIGHT SOURCES NOT OTHERWISE PROVIDED FOR
- F21K9/00—Light sources using semiconductor devices as light-generating elements, e.g. using light-emitting diodes [LED] or lasers
- F21K9/60—Optical arrangements integrated in the light source, e.g. for improving the colour rendering index or the light extraction
- F21K9/64—Optical arrangements integrated in the light source, e.g. for improving the colour rendering index or the light extraction using wavelength conversion means distinct or spaced from the light-generating element, e.g. a remote phosphor layer
-
- 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
- F21V7/00—Reflectors for light sources
- F21V7/22—Reflectors for light sources characterised by materials, surface treatments or coatings, e.g. dichroic reflectors
- F21V7/28—Reflectors for light sources characterised by materials, surface treatments or coatings, e.g. dichroic reflectors characterised by coatings
- F21V7/30—Reflectors for light sources characterised by materials, surface treatments or coatings, e.g. dichroic reflectors characterised by coatings the coatings comprising photoluminescent substances
-
- 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
- F21V9/30—Elements containing photoluminescent material distinct from or spaced from the light source
- F21V9/32—Elements containing photoluminescent material distinct from or spaced from the light source characterised by the arrangement of the photoluminescent material
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21Y—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES F21K, F21L, F21S and F21V, RELATING TO THE FORM OR THE KIND OF THE LIGHT SOURCES OR OF THE COLOUR OF THE LIGHT EMITTED
- F21Y2115/00—Light-generating elements of semiconductor light sources
- F21Y2115/10—Light-emitting diodes [LED]
Description
「アルミニウム含有酸化物」と言う用語は、MgAl2O4、BaMgAl10O17、Y3Al5O12、および特にAl2O3など、アルミニウム含有酸化物の種類に関する。「チタン含有酸化物」と言う用語は、Ba2TiO4、CaTiO3、Li2TiO3、および特にTiO2などのチタン酸塩のような、チタン含有酸化物の種類に関する。別の実施例では、無機コーティングは、インジウム金属酸化物コーティングからなる群から選定され、例えばインジウムスズ酸化物(ITO)コーティングからなる群から選定され、インジウム亜鉛酸化物コーティングが設置されてもよい。さらに別の実施例では、コーティングは、ジルコニア(ZrO2)コーティングおよびスズ酸化物(SnO2)(SNO)コーティングからなる群から選定された無機コーティングを有する。特に、(覆いの実施例としての)コーティングは、シリカ、アルミナ、ITO、およびSNOの群の1または2以上から選定される。そのような材料の組み合わせ、または前述のような、異なる組成の層を有するマルチレイヤコーティングが設置されてもよい。ガラスの例は、例えば、ホウ酸ガラス、リン酸ガラス、ボロシリケートガラス等である。
(Y-)k-n-(X)-(-L)n
を有する。ここで、kは2、3、4、または5であり、nは1、2、3、4または5であり、k-nはゼロ以上である;XはO、OS、O-Se、O-N、O-P、O-As、S、S=0、S02、Se、Se=0、N、N=0、P、P=0、C=0 AsまたはAs=0;YおよびLは、それぞれ独立に、H、OH、アリール、ヘテロアリール、または任意で、少なくとも一つの二重結合、少なくとも一つの三重結合、もしくは少なくとも一つの二重結合と一つの三重結合とを含む、直鎖もしくは分岐鎖のC2〜18炭化水素鎖である。炭化水素鎖は、任意で、C1〜4アルキル、C2〜4アルケニル、C2〜4アルキニル、C1〜4アルコキシ、ヒドロキシ、ハロ、アミノ、ニトロ、シアノ、C3〜5シクロアルキル、3〜5員ヘテロシクロアルキル、アリール、ヘテロアリール、Cl〜4アルキルカルボニルオキシ、Cl〜4アルコキシカルボニル、Cl〜4アルキルカルボニルまたはホルミルの、1または2以上と置換され得る。また炭化水素鎖は、任意で、-0-、-S-、-N(Ra)-、-N(Ra)-C(0)-0-、-0-C(0)-N(Ra)-、-N(Ra)-C(0)-N(Rb)-、-O-C(0)-0-、-P(Ra)-、または-P(0)(Ra)-により中断されてもよい。RaおよびRbの各々は、独立して、水素、アルキル、アルケニル、アルキニル、アルコキシ、ヒドロキシルアルキル、ヒドロキシル、またはハロアルキルであってもよい。アリール基は、置換されたまたは未置換の環状芳香族基である。一例には、フェニル、ベンジル、ナフチル、トリル、アントラシル、ニトロフェニル、またはハロフェニルが含まれる。ヘテロアリール基は、環内に、1または2以上のヘテロ原子を有するアリール基であり、例えばフリル、ピリジル、ピロリル、フェナントリルである。
実施例を概略的に示す。ここでは、これは、例えば、LEDのLED色素17である。
−アクリレート(モノマーまたはオリゴマー)に分散されたQD
−シリコーン(主としてオリゴマー)に分散されたQD
−エポキシに分散されたQD(モノマーまたはオリゴマー)
−任意の他の硬化性高分子樹脂(モノマーまたはオリゴマー)に分散されたQD。
−流動床反応器を用いた、ガス相からの成膜技術(PVD、ALD等)
−化学(湿式化学または化学気相成膜)合成における、前駆体材料からの無機シェルの成長法
を用いてシールされる。
1− ebecryl150、またはIBMA/HDDAの80/20の混合物中に、QD(0.1〜1wt%)を混合する
2− 0.5wt%のirgacureを添加する(任意)
3− 5gのQD−アクリル混合物に、1gのtriosperl多孔質シリカ粒子を添加する
4− 10分間、静かに撹拌/振動する
5− ブフナー漏斗に配置されたフィルタ(ろ紙)上に、QD−アクリル多孔質シリカ粒子混合物を設置する
6− 漏斗を1〜10分間、真空にする
7− フィルタ上の多孔質シリカ粒子を、エタノール、ヘプタン、トルエン、または別の溶媒で洗浄する(任意)
8− フィルタから粉末を除去する
9− ガラス板またはガラス瓶に粉末を広げ、N2流通の下、UVで硬化させる
10− 硬化された粉末をトルエンに分散させ、超音波処理を実施する
11− トルエンを除去して、含浸された粉末を得る。
以下のように、Trisoperl粒子を含浸した:ヘプタン中のCrystalplexのQDの5wt%分散液1gを、IBMA/HDDA(5g)に添加した。この結果、IBMA/HDDA中の1wt%の分散QDが得られる。これに1gのPSP、および0.5wt%の光開始剤(irgacure184)を加えた。粉末−アクリレート混合物をブフナー漏斗にのせ、グローブボックス中で数分間、ろ過した。ろ過処理の後、グローブボックス内でUV光を用いて、4分間、粉末を硬化した。この結果、粘着性の粉末が得られた。これは、密閉ガラス瓶内で、すなわち周囲空気と接触させずに、トルエンに分散させ、15分間US処理を行うことにより、個々のPSPの浮遊粉末に変換された。次に、デカンタ法により、グローブボックス内でトルエンが除去され、その後の数時間の気化により、全てのトルエンが除去された。FTIR測定では、アクリルが95%の変換率を有し、これは、アクリレートがほぼ完全に硬化されていることを意味する。これらの粒子のサブセットは、QEおよび安定性評価のため、ebecryl150に混合された。2回の異なる含浸実験では、これらのQDのQEは、51%および52%と測定された。含浸していないHDDA/IBMA中のQDのQEは、69%と測定された。これは、含浸、硬化、および第2のマトリクスに取入れる際に、QEにロスがあることを意味する。この低下の理由は不明であるが、追加の処理ステップによるものである可能性がある。表3には、QEデータをまとめて示す。
(グローブボックスの外で)シリコンウェハの上に、50mgの含浸PSP(バッチ1)を広げ、ASMジュアルチャンバALDシステムの(プラズマ加速ALD用の)エメラルドチャンバに導入した。100℃で、プラズマ加速ALDプロセスを用いて、50mのアルミナ層を設置した。反応ガスとして、TMA(トリメチルアルミニウム)およびO2を用いた。成膜後、粉末が回収され、これがEbecryl150(1wt%のirgacure184)と混合され、二次マトリクスに、ALDコーティングされたPSPの硬化膜が得られた。前述の例1のように、IBMA/HDDAにおける平坦QDの膜(非含浸)に加えて、ALDを有さない同じ含浸PSPの参照サンプルも作製した。全ての場合において、サンプルは、2つのガラス板の間の、100μmのアクリル層からなる。プラズマ加速ALDプロセスを用いたALDコーティングPSP(以降、サンプルALD−aと称する)のQEは、50%のQEを有し、これは、ALDコーティング前(バッチ1 52%)と同じである。従って、ALDコーティングは、QDのQEには、(ほとんど)影響を及ぼさない。
(グローブボックスの外で)30mgの含浸PSP(バッチ1)をシリコンウェハ上に広げ、ASMジュアルチャンバALDシステムの(熱ALD用)パルサーチャンバに導入した。熱ALDプロセスを用いて、反応ガスとしてTMA(トリメチルアルミニウム)およびO3を用いて、150℃で、50nmのアルミナ層を設置した。成膜後に、粉末を回収し、Ebecryl150(1wt%のirgacure184を含む)と混合し、二次マトリクスにおいて、ALDコーティングPSPの硬化膜を形成した。150℃での熱ALDを用いて、ALDコーティングされたPSP(以降、サンプルALD−bと称する)のQEは、31%のQEを有し、これは、ALDコーティング前(バッチ1、QEは52%)に比べて20%の低下である。
(グローブボックスの外で)10mgの含浸PSP(バッチ2)をシリコンウェハ上に広げ、ASMジュアルチャンバALDシステムの(熱ALD用)パルサーチャンバに導入した。熱ALDプロセスを用い、150℃で、反応ガスとしてTMA(トリメチルアルミニウム)およびO3を使用して、50nmのアルミナ層を設置した。成膜後に、粉末を回収し、Ebecryl150(0.5wt%のirgacure184を含む)に混合し、二次マトリクスにおいて、ALD−コーティングPSPの硬化膜を形成した。熱ALDを用いたALD−コーティングPSP(以降、サンプルALD−cと称される)のQEは、33%であり、これは、ALDコーティング前(バッチ2、51%)に比べて20%の低下である。この結果および前述の例は、熱ALDプロセスにより、QEに相当の低下が生じることを示しており、これは、単に温度だけの影響ではない。ALD−a(プラズマ加速)は、100℃でも実施されたからである。熱ALDプロセスにおいて使用されるオゾンが、QE低下の原因である可能性があるが、本願では、これ以上検討しない。
PCT/IB2013/059577(本願の参照として取り入れられる)に記載の方法で、Crystalplex社から市販されているQDを、シロキサンリガンドで改質した。使用したリガンドは、側鎖にアミン官能基を有する、5000Mwのシロキサン分子(AB109373、粘度~100cSt)であり、アミン基は、最初リガンド交換の前に、PCT/IB2013/059577に記載のように、カルボン酸に変換された。リガンドは、カルボン酸を介してQD表面に結合し、シロキサンリガンドは、混和性のQDを、低分子量のシリコーンにする(100cSt未満)。
Claims (8)
- ポアを有する多孔質無機材料コアを有する粒子を有する発光材料であって、
前記ポアは、少なくとも一部が、発光量子ドットが埋設された高分子材料で充填され、
前記粒子は、前記コアの少なくとも一部が被覆された覆いを有し、
前記覆いは、コーティングを有し、該コーティングは、シリコン含有酸化物、アルミニウム含有酸化物、ジルコニウム含有酸化物、ガラス、チタン含有酸化物、ハフニウム含有酸化物、およびイットリウム含有酸化物からなる群から選定された無機コーティングで、前記粒子の少なくとも一部を被覆し、
前記多孔質無機材料は、多孔質シリカ、多孔質アルミナ、多孔質ジルコニア、および多孔質チタニアの1または2以上を有する、発光材料。 - 前記覆いは、前記粒子を被覆するマルチレイヤコーティングを有し、
前記マルチレイヤコーティングは、有機高分子コーティングおよび無機コーティング、またはシリコン含有酸化物、アルミニウム含有酸化物、ジルコニウム含有酸化物、ガラス、チタン含有酸化物、ハフニウム含有酸化物、およびイットリウム含有酸化物の群から選定された、少なくとも2つのコーティングを有する、請求項1に記載の発光材料。 - 前記粒子は、1〜500μmの範囲の粒子サイズを有し、
前記ポアは、0.1〜10μmの範囲の平均ポアサイズを有し、
前記高分子材料は、アクリレート、シリコーン、またはエポキシタイプの高分子の1または2以上を有し、
前記覆いは、無機コーティングを有する、請求項1または2に記載の発光材料。 - 波長変換器であって、
請求項1乃至3のいずれか一つに記載の発光材料を有する、光透過性固体マトリクスを有する、波長変換器。 - さらに、第2の発光材料を有する、請求項4に記載の波長変換器。
- 照明装置であって、
光源光を生成するように構成された光源と、
請求項1乃至3のいずれか一つに記載の発光材料と、
を有し、
前記発光材料は、前記光源光の少なくとも一部を、可視発光量子ドット光に変換するように構成される、照明装置。 - 前記発光量子ドットは、コア−シェル量子ドットからなる群から選択され、
前記コアは、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、HgZnSTe、GaN、GaP、GaAs、AlN、AlP、AlAs、InN、InP、InGaP、InAs、GaNP、GaNAs、GaPAs、AlNP、AlNAs、AlPAs、InNP、InNAs、InPAs、GaAlNP、GaAlNAs、GaAlPAs、GaInNP、GaInNAs、GaInPAs、InAlNP、InAlNA、およびInAlPAsナノ粒子からなる群から選定される、請求項6に記載の照明装置。 - 前記光源から、ゼロまたはゼロ以外の距離で配置された、請求項4または5に記載の波長変換器を有し、
さらに、第2の発光材料を有し、該第2の発光材料は、光による励起の下、前記発光量子ドットとは別の発光の波長分布を示す、請求項6または7に記載の照明装置。
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