JP4891336B2 - 蛍光体及びその製造方法、並びに発光装置 - Google Patents
蛍光体及びその製造方法、並びに発光装置 Download PDFInfo
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- JP4891336B2 JP4891336B2 JP2008545403A JP2008545403A JP4891336B2 JP 4891336 B2 JP4891336 B2 JP 4891336B2 JP 2008545403 A JP2008545403 A JP 2008545403A JP 2008545403 A JP2008545403 A JP 2008545403A JP 4891336 B2 JP4891336 B2 JP 4891336B2
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- phosphor
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- sialon
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims description 123
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- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
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- 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
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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Description
<発明の経緯>
既に説明したように、従来のEu付活β型サイアロンを主成分とする蛍光体は、発光効率が低く、それを用いた白色LED等の発光装置は十分な輝度を得ることができず、実用に供することに難がある。
本実施形態の蛍光体は、一般式:Si6−zAlzOzN8−zで示されるβ型サイアロンをホスト結晶に、発光中心としてEu2+が含有されているものを主成分としている。
次に、本発明の蛍光体を得る方法について例示する。
まず、第一工程は、Euを含有するβ型サイアロンを生成させる工程である。これには、従来公知の製造方法が適用できるが、その具体例としては、次に例示する方法がある。即ち、Euを含有するβサイアロンの構成元素であるSi、Al、N、O、Euを主成分として含有し、他は不可避的不純物を含む混合組成物が得られるように、いろいろな原料を混合し、得られた混合組成物を窒素雰囲気中で加熱し、Euを含有するβサイアロンを合成する方法である。
本実施形態のβ型サイアロンを主成分とする蛍光体は、発光光源と蛍光体とを備える発光装置に使用され、特に350nm以上500nm以下の波長を含有している紫外光や可視光を励起源として照射することにより、520nm以上550nm以下の範囲の波長にピークを持つ発光特性を有するので、紫外LED又は青色LEDと、必要に応じて、更に赤色蛍光体及び/又は青色蛍光体と組み合わせることによって、容易に白色光が得られる。
以下、本実施形態の作用効果について再度まとめて説明する。
Eu含有βサイアロンの合成
宇部興産社製α型窒化ケイ素粉末(「SN−E10」グレード、酸素含有量1.2質量%、β相含有量4.5質量%)95.5質量%、トクヤマ社製窒化アルミニウム粉末(「F」グレード、酸素含有量0.9質量%)3.3質量%、大明化学社製酸化アルミニウム粉末(「TM−DAR」グレード)0.4質量%、信越化学工業社製酸化ユーロピウム粉末(「RU」グレード)0.8質量%を配合し、原料混合物1kgを得た。
磁場掃引範囲:3200〜3400gauss(320〜340mT)、
磁場変調:100kHz、5gauss、
照射マイクロ波:10mW、9.25GHz、
掃引時間:240秒、
データポイント数:2048ポイント、
標準試料:MgOにMn2+を熱拡散させたものを試料と同時に測定した。
直径60mm×高さ40mmの蓋付きの円筒型窒化ホウ素製容器(電気化学工業社製「N−1」グレード)に比較例1で合成した粉末20g充填し、カーボンヒーターの電気炉で大気圧窒素雰囲気中、1600℃で8時間の加熱処理を行った。得られた粉末は、焼結に伴う収縮はなく、加熱前とほとんど同じ性状である、目開き45μmの篩を全て通過した。
条件が9気圧のN2ガス圧雰囲気中、1950℃で8時間とする以外は実施例1と全く同じ加熱処理を行った。得られた粉末は、粒子間の焼結に伴う収縮が若干見られ、目開き45μmの篩の通過率も約60%であった。
条件が1Paの真空中、1400℃で8時間とする以外は実施例1と全く同じ加熱処理を行った。得られた粉末の色は処理前の緑色から茶色みがかった緑色へと変化した。得られた粉末は、焼結等に伴う収縮はなく、目開き45μmの篩を全て通過した。XRD測定の結果、微量のSiが検出された。
比較例3で得られた粉末を50%フッ化水素酸と70%硝酸の1:1混酸中で処理した。処理中に懸濁液は茶色っぽい緑色から鮮やかな緑色に変化した。その後、水洗及び乾燥して蛍光体粉末を得た。図1に、実施例2で得られた蛍光体粉末の励起・蛍光スペクトル測定結果を示す。
条件が大気圧アルゴン雰囲気中、1450℃で8時間とする以外は実施例1と全く同じ加熱処理を行った。得られた粉末の色は処理前の緑色から深緑色へ変化した。得られた粉末は、焼結等に伴う収縮はなく、目開き45μmの篩を全て通過した。
酸化ユーロピウム粉末を含まない原料配合とした以外は、比較例1と全く同じ条件でβ型サイアロンを主成分とする粉末を合成した。
比較例4で得られた粉末を実施例1と全く同じ条件で加熱処理を行い、粉末を得た。
実施例2で得た蛍光体とCa0.66Eu0.04Si9.9Al2.1O0.7N15.3の組成を持つCa−α型サイアロン:Eu蛍光体(発光ピーク波長:585nm、450nm励起での発光効率:60%)をそれぞれシランカップリング剤(信越シリコーン社製「KBE402」)で処理した。このシランカップリング処理された二種類の蛍光体を種々の比率で適量、エポキシ樹脂(サンユレック社製「NLD−SL−2101」)に混練し、発光波長450nmの青色LED素子の上にポッティングし、真空脱気、加熱硬化し、実施例4の表面実装型LED(発光装置)を作製した。
また、実施例4の発光装置における実施例2の蛍光体の代わりに、比較例1の蛍光体を用いて比較例6の白色光の発光装置を作製した。
実施例2で得た蛍光体とCa0.992Eu0.008AlSiN3の組成を持つ赤色蛍光体(発光ピーク波長:650nm、450nm励起での発光効率:70%)を使用し、実施例4と同様の方法により、色度座標(x、y)が(0.31、0.32)の実施例5の白色発光装置を作製した。実施例5の発光装置は、実施例4や比較例6の発光装置に比較して、演色性が優れていた。
宇部興産社製α型窒化ケイ素粉末(「SN−E10」グレード、酸素含有量1.2質量%、β相含有量4.5質量%)95.4質量%、トクヤマ社製窒化アルミニウム粉末(「E」グレード、酸素含有量0.8質量%)3.0質量%、大明化学社製酸化アルミニウム粉末(「TM−DAR」グレード)0.7質量%、信越化学工業社製酸化ユーロピウム粉末(「RU」グレード)0.8質量%を配合し、原料混合物1kgを得た。
実施例6及び実施例8の蛍光体に対して、湿式沈降法による微粉除去処理を行った(それぞれ実施例9及び実施例10)。蛍光体粉末10gを分散剤として、ヘキサメタ燐酸ナトリウムを添加した蒸留水500ml中に十分に分散した後、内寸80mm、高さ140mmの容器に移し、実施例9では12分間、実施例10では80分間静置し、水面から90mmの上澄み液を除去した。再び、ヘキサメタりん酸水溶液を追加し、分散し、所定時間静置した後、上澄み液を除去するという操作を上澄み液が透明になるまで繰り返した。その後、沈殿物をろ過し、分散剤を除去するために十分に水洗し、乾燥を行い微粉除去した蛍光体粉末を得た。ICP発光分光分析法により求めたEu含有量、粒度分布計により測定した粒度分布及びガス吸着法により測定し、BET多点解析により求めた比表面積を表7に、波長450nmの青色光で励起した時の蛍光特性を表8に示す。
Claims (4)
- Euを含有するβ型サイアロンを生成させる第一の工程と、真空中1200℃以上1550℃以下の温度範囲で熱処理し、更にフッ化水素酸と硝酸の混合物で酸処理することにより結晶欠陥密度を低減する第二の工程とを含む、蛍光体の製造方法により製造された蛍光体。
- Euを含有するβ型サイアロンを生成させる第一の工程と、窒素分圧が10kPa以下の窒素以外のガスを主成分とする不活性雰囲気中1300℃以上1600℃以下の温度範囲で熱処理し、更にフッ化水素酸と硝酸の混合物で酸処理することにより結晶欠陥密度を低減する第二の工程とを含む、蛍光体の製造方法により製造された蛍光体。
- Euを含有するβ型サイアロンを生成させる第一の工程と、真空中1200℃以上1550℃以下の温度範囲で熱処理し、更にフッ化水素酸と硝酸の混合物で酸処理することにより結晶欠陥密度を低減する第二の工程とを含む、蛍光体の製造方法。
- Euを含有するβ型サイアロンを生成させる第一の工程と、窒素分圧が10kPa以下の窒素以外のガスを主成分とする不活性雰囲気中1300℃以上1600℃以下の温度範囲で熱処理し、更にフッ化水素酸と硝酸の混合物で酸処理することにより結晶欠陥密度を低減する第二の工程とを含む、蛍光体の製造方法。
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US8404152B2 (en) | 2013-03-26 |
WO2008062781A1 (fr) | 2008-05-29 |
JPWO2008062781A1 (ja) | 2010-03-04 |
CN101600778B (zh) | 2013-10-23 |
JP2012052127A (ja) | 2012-03-15 |
EP2093272A1 (en) | 2009-08-26 |
TW200835776A (en) | 2008-09-01 |
EP2093272B1 (en) | 2016-11-02 |
TWI357927B (en) | 2012-02-11 |
KR20090084946A (ko) | 2009-08-05 |
CN101600778A (zh) | 2009-12-09 |
KR100985680B1 (ko) | 2010-10-05 |
EP2093272A4 (en) | 2009-12-30 |
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