JP5519552B2 - 蛍光体の材料 - Google Patents

蛍光体の材料 Download PDF

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Publication number
JP5519552B2
JP5519552B2 JP2011035197A JP2011035197A JP5519552B2 JP 5519552 B2 JP5519552 B2 JP 5519552B2 JP 2011035197 A JP2011035197 A JP 2011035197A JP 2011035197 A JP2011035197 A JP 2011035197A JP 5519552 B2 JP5519552 B2 JP 5519552B2
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Japan
Prior art keywords
light
phosphor
led
emission
sio
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Expired - Lifetime
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JP2011035197A
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JP2011105951A (ja
Inventor
タッシュ、シュテファン
パハラー、ペーター
ロート、グンドゥラ
テウス、ヴァルター
ケンプフェルト、ヴォルフガング
シュタリック、デトレフ
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Toyoda Gosei Co Ltd
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Toyoda Gosei Co Ltd
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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
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • 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
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
    • C09K11/7795—Phosphates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • C—CHEMISTRY; METALLURGY
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
    • C09K11/7734—Aluminates
    • C—CHEMISTRY; METALLURGY
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
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    • C09K11/77344—Aluminosilicates
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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    • C09K11/774—Borates
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
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    • G02B6/0011—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings specially adapted for lighting devices or systems the light guides being planar or of plate-like form
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    • F21Y2105/00—Planar light sources
    • F21Y2105/10—Planar light sources comprising a two-dimensional array of point-like light-generating elements
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    • F21Y2115/00—Light-generating elements of semiconductor light sources
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Description

本発明は、発光素子と、蛍光体とを備え、発光素子が第１のスペクトル範囲、特に光スペクトルの青色および／または紫外線範囲で発光し、蛍光体がアルカリ土類金属オルト珪酸塩（Ｅｒｄａｌｋａｌｉｏｒｔｈｏｓｉｌｉｋａｔｅ）の群に由来するか又はこの発光物質群の少なくとも１つの成分を含み、発光素子の発光の一部を吸収し、別のスペクトル範囲、特に黄緑色、黄色又はオレンジ色の範囲で発光する光源に関する。選択された蛍光体はこの群の他の蛍光体および／またはこの群に属していない別の発光物質と混合されて使用される。
発光素子は特に無機ＬＥＤであるが、有機ＬＥＤ、レーザーダイオード、無機厚膜エレクトロルミネセンスシートまたは無機薄膜エレクトロルミネセンス部品であってもよい。
無機ＬＥＤはとりわけ、長寿命、省スペース、耐震性、さらにスペクトル狭帯域での発光という点で優れている。
多数の発光色、特にスペクトル広帯域の多数の発光色は、ＬＥＤ内の活性半導体材料の内部発光によって実現できないか又は非効率にしか実現することができない。とりわけこのことは白色光を得る場合にあてはまる。
従来の技術によれば、半導体を用いて内部で実現することができない発光色は色変換によって得られる。
この色変換の技術は主として、少なくとも１つの蛍光体をＬＥＤダイ上に配置する原理に基づいている。その蛍光体は、このダイから発光された放射の一部を吸収し、ホトルミネセンスへ励起される。光源の発光色すなわち光色はダイの伝送された放射と発光物質の発光された放射との混合によって生じる。
蛍光体としては基本的に有機系ならびに無機系を使用することもできる。無機顔料の主要な利点は有機系に比べて高い化学的な温度および放射安定性にある。無機ＬＥＤの長寿命に関連して、長寿命の無機蛍光体は２つの構成要素から構成される光源の高い色位置安定性を保証する。
青色発光ＬＥＤから放出された放射が白色光に変換されるべき場合、青色光（４５０〜４９０ｎｍ）を有効に吸収し高効率で大部分黄色のルミネセンス放射に変換する発光物質が必要とされる。当然、少数の無機蛍光体しかこの要求を満たすことができない。現時点では多くの場合、ＹＡＧ発光物質クラスの材料が青色ＬＥＤに対する色変換顔料として使用されている（国際公開第９８／０５０７８号、第９８／１２７５７号パンフレット参照）。しかしながら、この材料には、該材料が５６０ｎｍ以下の発光最大値の場合にしか充分に高い効率を示さないという欠点がある。このような理由から青色ダイオード（４５０
〜４９０ｎｍ）と組み合わされたＹＡＧ顔料を用いて、６０００〜８０００Ｋの色温度および比較的低い演色（演色評価数Ｒａの標準的な値は７０〜７５である）を有する冷たい感じの白色の光色のみを実現することができる。これにより用途範囲が非常に強く制限される。一方では、全般照明に白色光源を適用すると通常は照明手段の演色に高い要求が出され、他方では、とりわけ欧州および北米における顧客からは２７００〜５０００Ｋの色温度を持つ温かい光色が好まれている。
さらに国際公開第００／３３３８９号パンフレットから、青色ＬＥＤの光を変換するための蛍光体としてとりわけＢａ２ＳｉＯ４：Ｅｕ２＋を使用することが公知である。発光物質Ｂａ２ＳｉＯ４：Ｅｕ２＋の発光最大値は５０５ｎｍにあり、それゆえこのような組合わせを用いると確実に白色光を発生することができない。
Ｓ．Ｈ．Ｍ． Ｐｏｏｒｔ等による論文、“Ｏｐｔｉｃａｌ ｐｒｏｐｅｒｔｉｅｓ ｏｆ Ｅｕ２＋−ａｋｔｉｖａｔｅｄ ｏｒｔｈｏｓｉｌｉｃａｔｅｓ ａｎｄ ｏｒｔｈｏｐｈｏｓｐａｔｅｓ”（刊行物「Ｊｏｒｎａｌ ｏｆ Ａｌｌｏｙｓ ａｎｄ Ｃｏｍｐｏｕｎｄｓ 」２６０巻、１９９７年発行、第９３〜９７頁）では、Ｅｕで活性化されたＢａ２ＳｉＯ４ならびにリン酸塩（例えばＫＢａＰＯ４、ＫＳｒＰＯ４）の性質が研究されている。また同文献では、Ｂａ２ＳｉＯ４の発光が５０５ｎｍにあることが確認されている。
国際公開第００／３３３８９号パンフレット
本発明の課題は、冒頭に記載した種類の光源を、高い効率および高い演色を同時に得ると共に高温の色温度を持つ白光色、特に国際照明委員会（ＣＩＥ）から全般照明用に決定された公差楕円内に位置する色位置を発生できるように変更することにある。
この課題は、青色の第１発光の一部を吸収して、黄緑色、黄色又はオレンジ色の領域の第２発光を発する蛍光体であり、前記蛍光体は、Ｍ ２ Ｓｉ １−Ｘ Ｎ Ｘ Ｏ ４ ：Ｅｕ（ただし、Ｍは、ＳｒＢａ、ＳｒＣａ、あるいはＳｒＢａＣａであり、Ｎは、Ｇａ、Ｇｅ、Ｂ、ＰあるいはＡｌであり、ｘは０．０５以下である）によって示され、前記第２発光は前記第１発光の前記一部を除いた残りの部分の青色の光と混合されて白色光を発生する蛍光体によって解決される。
また、前記課題は、３７０〜３９０ｎｍの紫外の第１発光を吸収して、黄緑色、黄色又はオレンジ色の領域の第２発光を発する蛍光体であり、前記蛍光体は、Ｍ ２ Ｓｉ １−Ｘ Ｎ Ｘ Ｏ ４ ：Ｅｕ（ただし、Ｍは、ＳｒＢａ、ＳｒＣａ、あるいはＳｒＢａＣａであり、Ｎは、Ｇａ、Ｇｅ、Ｂ、ＰあるいはＡｌであり、ｘは０．０５以下である）によって示され、前記第２発光は、青色の第３発光と混合されて白色光を発生する蛍光体によって解決される。
本発明によるＬＥＤ光源のスペクトル（波長に依存する相対強度）を示す図 本発明によるＬＥＤ光源のスペクトル（波長に依存する相対強度）を示す図 本発明によるＬＥＤ光源のスペクトル（波長に依存する相対強度）を示す図 本発明によるＬＥＤ光源のスペクトル（波長に依存する相対強度）を示す図 本発明によるＬＥＤ光源のスペクトル（波長に依存する相対強度）を示す図 本発明によるＬＥＤ光源のスペクトル（波長に依存する相対強度）を示す図 本発明によるＬＥＤ光源の第１実施例の概略断面図 本発明によるＬＥＤ光源の第２実施例の概略断面図 本発明によるＬＥＤ光源の第３実施例の概略断面図 本発明によるＬＥＤ光源の第４実施例の概略断面図
本発明の他の利点を以下において実施例および図面に基づいて詳細に説明する。
図１〜６は本発明による種々のＬＥＤ光源のスペクトル（波長に依存する相対強度）を示し、図７〜１０は本発明によるＬＥＤ光源の種々の実施例を示す。
図１は、４６４ｎｍの重心波長を有する第１のスペクトル範囲において発光する青色ＬＥＤと、５９６ｎｍの最大値を有する第２のスペクトル範囲において発光する組成（Ｓｒ１．４Ｃａ０．６ＳｉＯ４：Ｅｕ２＋）の本発明による蛍光体との組合わせによって形成されている２７００Ｋの色温度を有する白色ＬＥＤの発光スペクトルを示す。
４６４ｎｍで発光するＬＥＤと、本発明によるオルト珪酸塩蛍光体のそれぞれ１つとの組合わせの他の例が図２および図３に示されている。組成Ｓｒ１．９０Ｂａ０．０８Ｃａ０．０２ＳｉＯ４：Ｅｕ２＋を持ち黄色光を発する蛍光体が色変換のために使用されると、４１００Ｋの色温度を有する白光色が生じ、一方蛍光体Ｓｒ１．８４Ｂａ０．１６ＳｉＯ４：Ｅｕ２＋を使用すると例えば６５００Ｋの色温度を有する白色光源が製造される。
４６４ｎｍＬＥＤと、本発明による２つのオルト珪酸塩蛍光体との組合わせの標準的なスペクトルが図４に示されている。使用された発光物質は組成Ｓｒ１．４Ｃａ０．６ＳｉＯ４：Ｅｕ２＋およびＳｒ１．００Ｂａ１．００ＳｉＯ４：Ｅｕ２＋を有している。図４に示された具体的なスペクトルのために５０８８Ｋの色温度と８２の演色評価数Ｒａとが保たれている。当然、全ての色温度は蛍光体の選定された量比率に応じて約３５００Ｋ〜７５００Ｋの範囲で実現されており、本発明による２つのアルカリ土類金属オルト珪酸塩蛍光体から成るこの種の混合物の大きな利点はとりわけ８０以上のＲａ値が同時に得られることにある。
この一例が図５に示されている。図示されているスペクトルは、４６４ｎｍＬＥＤと、２つの蛍光体Ｓｒ１．６Ｃａ０．４Ｓｉ０．９８Ｇａ０．０２Ｏ４：Ｅｕ２＋およびＳｒ１．１０Ｂａ０．９０ＳｉＯ４：Ｅｕ２＋から成る混合物との組合わせを示し、５０００Ｋの色温度で８２のＲａ値を提供する。
発光素子として、３７０〜３９０ｎｍの最大値を有する第１のスペクトル範囲において発光するＵＶ−ＬＥＤが使用される場合、そのＬＥＤと、図４に示された本発明による蛍光体および同時に青緑色光を発するバリウム−マグネシウムアルミン酸塩発光物質：Ｅｕ，Ｍｎの特定の成分を含んでいる発光物質混合物との組合わせによって、９０以上のＲａ値が実現される。図６は６５００Ｋの色温度で９１のＲａを有する白色光源の発光スペクトルを示す。
他の例は次の一覧表に記載されている。使用された無機ＬＥＤの発光波長および本発明による蛍光体のそれぞれの組成のほかに、生じた色温度およびＲａ値ならびに光源の色位置が示されている。
Ｔ＝２７７８Ｋ（４６４ｎｍ＋Ｓｒ１．４Ｃａ０．６ＳｉＯ４：Ｅｕ２＋）；ｘ＝０．４６１９、ｙ＝０．４２４７、Ｒａ＝７２、
Ｔ＝２９５０Ｋ（４６４ｎｍ＋Ｓｒ１．４Ｃａ０．６ＳｉＯ４：Ｅｕ２＋）；
ｘ＝０．４３８０、ｙ＝０．４００４、Ｒａ＝７３、
Ｔ＝３４９７Ｋ（４６４ｎｍ＋Ｓｒ１．６Ｂａ０．４ＳｉＯ４：Ｅｕ２＋）；
ｘ＝０．４０８６、ｙ＝０．３９９６、Ｒａ＝７４、
Ｔ＝４１８３Ｋ（４６４ｎｍ＋Ｓｒ１．９Ｂａ０．０８Ｃａ０．０２ＳｉＯ４：Ｅｕ２＋）；
ｘ＝０．３７６２、ｙ＝０．３８７３、Ｒａ＝７５、
Ｔ＝６６２４Ｋ（４６４ｎｍ＋Ｓｒ１．９Ｂａ０．０２Ｃａ０．０８ＳｉＯ４：Ｅｕ２＋）；
ｘ＝０．３１０１、ｙ＝０．３３０６、Ｒａ＝７６、
Ｔ＝６３８５Ｋ（４６４ｎｍ＋Ｓｒ１．６Ｃａ０．４ＳｉＯ４：Ｅｕ２＋＋Ｓｒ０．４Ｂａ１．６ＳｉＯ４：Ｅｕ２＋）；
ｘ＝０．３１３５、ｙ＝０．３３９７、Ｒａ＝８２、
Ｔ＝４２１６Ｋ（４６４ｎｍ＋Ｓｒ１．９Ｂａ０．０８Ｃａ０．０２ＳｉＯ４：Ｅｕ２＋））；
ｘ＝０．３７１０、ｙ＝０．３６９６、Ｒａ＝８２、
Ｔ＝３９５４Ｋ（４６４ｎｍ＋Ｓｒ１．６Ｂａ０．４ＳｉＯ４：Ｅｕ２＋＋Ｓｒ０．４Ｂａ１．６ＳｉＯ４：Ｅｕ２＋＋ＹＶＯ４：Ｅｕ３＋）；
ｘ＝０．３７５６、ｙ＝０．３８１６、Ｒａ＝８４、
Ｔ＝６４８９Ｋ（ＵＶ−ＬＥＤ＋Ｓｒ１．６Ｃａ０．４ＳｉＯ４：Ｅｕ２＋＋Ｓｒ０．４Ｂａ１．６ＳｉＯ４：Ｅｕ２＋＋バリウム−マグネシウムアルミン酸塩：Ｅｕ２＋）；
ｘ＝０．３１１５、ｙ＝０．３３９０、Ｒａ＝８６、
Ｔ＝５０９７Ｋ（４６４ｎｍ＋Ｓｒ１．６Ｂａ０．４（Ｓｉ０．９８Ｂ０．０２）Ｏ４：Ｅｕ２＋＋Ｓｒ０．６Ｂａ１．４ＳｉＯ４：Ｅｕ２＋）；
ｘ＝０．３４２３、ｙ＝０．３４８５、Ｒａ＝８２、
Ｔ＝５０８４Ｋ（ＵＶ−ＬＥＤ＋Ｓｒ１．６Ｃａ０．４（Ｓｉ０．９９Ｂ０．０１）Ｏ４：Ｅｕ２＋＋Ｓｒ０．６Ｂａ１．４ＳｉＯ４：Ｅｕ２＋＋ストロンチウム−マグネシウム
アルミン酸塩：Ｅｕ２＋）；
ｘ＝０．３４３０、ｙ＝０．３５３１、Ｒａ＝８３、
Ｔ＝３３６９Ｋ（４６４ｎｍ＋Ｓｒ１．４Ｃａ０．６Ｓｉ０．９５Ｇｅ０．０５Ｏ４：Ｅｕ２＋）；
ｘ＝０．４１３４、ｙ＝０．３９５９、Ｒａ＝７４、
Ｔ＝２７８７Ｋ（４６６ｎｍ＋Ｓｒ１．４Ｃａ０．６Ｓｉ０．９８Ｐ０．０２Ｏ４．０１：Ｅｕ２＋）；
ｘ＝０．４６３０、ｙ＝０．４２８０、Ｒａ＝７２、
Ｔ＝２９１３Ｋ（４６４ｎｍ＋Ｓｒ１．４Ｃａ０．６Ｓｉ０．９８Ａｌ０．０２Ｏ４：Ｅｕ２＋）；
ｘ＝０．４４２５、ｙ＝０．４０５０、Ｒａ＝７３
Ｔ＝４２０１Ｋ。
本発明の有利な実施例において、色変換は次のとおり実施される。
１つ又は複数のＬＥＤチップ１（図７参照）をプリント板２上で組み立てる。ＬＥＤ上に直接、（一方ではＬＥＤチップの保護のために、他方ではＬＥＤチップ内で発生した光をより良好に出射させることができるようにするために）封止材料（カプセル化材料）３を半球もしくは半楕円の形で配置する。この封止材料３は、各ダイを個々に包含することもできるし、封止材料が全てのＬＥＤのための共通の１個の形であってもよい。このようにして実装したプリント板２を反射鏡４内に設置するか、またはこの反射鏡４をＬＥＤチップ１の上にかぶせる。
反射鏡４に透光板５を設置する。一方ではこの透光板５は装置の保護のために使用され、他方ではこの透光板５中に蛍光体６が混入されている。透光板５を透過する青色光（もしくは紫外放射）は、その透過の際に部分的に蛍光体６によって第２のスペクトル範囲へ変換され、その結果全体的に白色の色印象が得られる。平面平行な板の間で生じるような導波作用による損失は、該透光板の不透明性および散乱特性によって減少される。さらに反射鏡４によって、すでに調整された光のみが透光板５に入射するようにされ、その結果全反射作用が始めから減少される。
図８に示されているように、蛍光体６を反射鏡４に被着することも可能である。この場合には透光板は必要とされない。
これとは別に、各ＬＥＤチップ１上に反射鏡４´がかぶせられていてもよく、この反射鏡４´は封止材料（カプセル化材料）３´をドーム形に注型され、透光板５が各反射鏡４´上につまりこの装置全体の上に配置されている（図９参照）。
照明光源を製造するために、個別ＬＥＤの代りにＬＥＤアレイを使用すると有利である。本発明の優れた変形例において、色変換は、ＬＥＤチップ１が直接プリント板２上に組み立てられているＬＥＤアレイ１´（図１０参照）で次のように実施される。
ＬＥＤアレイ１´を注型材料（例えばエポキシ樹脂）３を用いて、別の材料（例えばＰＭＭＡ）からなる透明なポリマーレンズ７に接着する。ポリマーレンズ７および注型材料３の材料は、できるだけ近似する屈折率を有するように、すなわち位相整合されているように選択される。注型材料３は、ポリマーレンズ７の最大で球形または楕円形の窪みの中に存在する。この窪みの形状は、注型材料３中に色変換物質が分散されているという点で重要であり、従ってこの形状付与によって、角度に関係しない発光色が得られることが保証される。これとは別に前記アレイは、最初に透明な注型材料で注型され、引き続いて色変換物質を含有している注型材料を用いてポリマーレンズに接着されていてもよい。
少なくとも２つの異なる蛍光体が使用されている特に良好な演色を有する白色ＬＥＤを製造するために、これらの蛍光体を一緒に１つのマトリックス中に分散させるのではなく、これら蛍光体を別々に分散させて設けると有利である。これは、最終的な光色が複数段の色変換プロセスによって得られる組合せに特に該当する。すなわち、最長波の発光色が１つの発光プロセスによって生成されることであり、この発光プロセスは次のとおり、すなわち、ＬＥＤの発光を第１の蛍光体が吸収する―第１の蛍光体が発光する―第１の蛍光体の発光を第２の蛍光体が吸収する―第２の蛍光体が発光する、というように進行する。特に、この種のプロセスにとって、個々の蛍光体を光の伝搬方向に相前後して配置すると有利である。というのは、それによって、種々の材料を一様に分散させた場合よりも材料の濃度を減少させることができるからである。
本発明は上述の実施例に限定されない。蛍光体はポリマーレンズ（または別の光学部品）中に組み込まれていてもよい。蛍光体をＬＥＤダイ上に直接配置することもできるし、透明な注型材料の表面上に配置することもできる。また蛍光体を散乱粒子と共に１つのマトリックス中に組み込むこともできる。このことによって、マトリックス中での沈降が防止され、均一な光出射が保証される。
１ ＬＥＤチップ
１´ ＬＥＤアレイ
２ プリント板
３、３´ 封止材料
４、４´ 反射鏡
５ 透光板
６ 蛍光体
７ ポリマーレンズ

Claims (2)

  1. 青色の第１発光の一部を吸収して、黄緑色、黄色又はオレンジ色の領域の第２発光を発する蛍光体であり、
    前記蛍光体は、
    Ｍ２ＳｉＯ ４：Ｅｕ（ただし、Ｍは、ＳｒＢａ、ＳｒＣａ、あるいはＳｒＢａＣａである）によって示され、
    前記第２発光は前記第１発光の前記一部を除いた残りの部分の青色の光と混合されて白色光を発生する青色光励起用蛍光体。
  2. ３７０〜３９０ｎｍの紫外の第１発光を吸収して、黄緑色、黄色又はオレンジ色の領域の第２発光を発する蛍光体であり、
    前記蛍光体は、
    Ｍ２ＳｉＯ ４：Ｅｕ（ただし、Ｍは、ＳｒＢａ、ＳｒＣａ、あるいはＳｒＢａＣａである）によって示され、
    前記第２発光は、青色の第３発光と混合されて白色光を発生する３７０〜３９０ｎｍの紫外光励起用蛍光体。
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