JP6890299B2 - ガーネット珪酸塩、ガーネット珪酸塩蛍光体、並びにガーネット珪酸塩蛍光体を用いた波長変換体及び発光装置 - Google Patents
ガーネット珪酸塩、ガーネット珪酸塩蛍光体、並びにガーネット珪酸塩蛍光体を用いた波長変換体及び発光装置 Download PDFInfo
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- JP6890299B2 JP6890299B2 JP2019525206A JP2019525206A JP6890299B2 JP 6890299 B2 JP6890299 B2 JP 6890299B2 JP 2019525206 A JP2019525206 A JP 2019525206A JP 2019525206 A JP2019525206 A JP 2019525206A JP 6890299 B2 JP6890299 B2 JP 6890299B2
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- 239000002223 garnet Substances 0.000 title claims description 222
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims description 213
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims description 203
- 239000002245 particle Substances 0.000 claims description 65
- 229910004283 SiO 4 Inorganic materials 0.000 claims description 50
- 239000013078 crystal Substances 0.000 claims description 49
- 239000011164 primary particle Substances 0.000 claims description 37
- 230000005284 excitation Effects 0.000 claims description 25
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 16
- 229910052744 lithium Inorganic materials 0.000 claims description 16
- 238000005286 illumination Methods 0.000 claims description 11
- 150000002500 ions Chemical class 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 description 37
- 230000000052 comparative effect Effects 0.000 description 32
- 229910052783 alkali metal Inorganic materials 0.000 description 15
- 150000001340 alkali metals Chemical class 0.000 description 15
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 14
- 239000002994 raw material Substances 0.000 description 13
- 239000011575 calcium Substances 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- 238000000295 emission spectrum Methods 0.000 description 11
- 238000010304 firing Methods 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 8
- 230000031700 light absorption Effects 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000006104 solid solution Substances 0.000 description 8
- 238000000635 electron micrograph Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- -1 rare earth ions Chemical class 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 238000001308 synthesis method Methods 0.000 description 6
- 238000010189 synthetic method Methods 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910000323 aluminium silicate Inorganic materials 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 229910010272 inorganic material Inorganic materials 0.000 description 4
- 239000011147 inorganic material Substances 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011368 organic material Substances 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000004323 axial length Effects 0.000 description 3
- WETINTNJFLGREW-UHFFFAOYSA-N calcium;iron;tetrahydrate Chemical compound O.O.O.O.[Ca].[Fe].[Fe] WETINTNJFLGREW-UHFFFAOYSA-N 0.000 description 3
- 238000007580 dry-mixing Methods 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 150000004760 silicates Chemical class 0.000 description 3
- 238000003746 solid phase reaction Methods 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910020068 MgAl Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052586 apatite Inorganic materials 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000008393 encapsulating agent Substances 0.000 description 2
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- 238000002844 melting Methods 0.000 description 2
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- 230000004048 modification Effects 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 229910052609 olivine Inorganic materials 0.000 description 2
- 239000010450 olivine Substances 0.000 description 2
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
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- 239000011347 resin Substances 0.000 description 2
- 239000011163 secondary particle Substances 0.000 description 2
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- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910001428 transition metal ion Inorganic materials 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- 229910015999 BaAl Inorganic materials 0.000 description 1
- XPIIDKFHGDPTIY-UHFFFAOYSA-N F.F.F.P Chemical compound F.F.F.P XPIIDKFHGDPTIY-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910017414 LaAl Inorganic materials 0.000 description 1
- 229910018250 LaSi Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- KEXULJHMZPYREB-UHFFFAOYSA-N cerium(3+) lutetium(3+) oxygen(2-) Chemical compound [O-2].[Ce+3].[Lu+3].[O-2].[O-2] KEXULJHMZPYREB-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
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- 239000007789 gas Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910003443 lutetium oxide Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- MPARYNQUYZOBJM-UHFFFAOYSA-N oxo(oxolutetiooxy)lutetium Chemical compound O=[Lu]O[Lu]=O MPARYNQUYZOBJM-UHFFFAOYSA-N 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 230000001443 photoexcitation Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- F21V9/38—Combination of two or more photoluminescent elements of different materials
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- G03B21/00—Projectors or projection-type viewers; Accessories therefor
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Description
本実施形態に係るガーネット珪酸塩は、一般式:Lu2CaMg2(SiO4)3で表される珪酸塩を主成分とするガーネット珪酸塩である。そして、ガーネット珪酸塩は、ガーネットの結晶構造に由来する粒子形状を持つ一次粒子を含んでいる。このようなガーネット珪酸塩は結晶性が良好であるため、単分散性に優れ、高発光効率と高光吸収率を兼ね備える蛍光体を得ることが可能となる。
[化1]
Lu2O3+CaCO3+2MgO+3SiO2+xLiCl→Lu2CaMg2(SiO4)3+xLiCl(+CO2↑)
次に、本実施形態に係るガーネット珪酸塩蛍光体について詳細に説明する。本実施形態に係るガーネット珪酸塩蛍光体は、ガーネット珪酸塩と、ガーネット珪酸塩に含まれる、発光中心として機能するイオンとを含む。これにより、ガーネット珪酸塩蛍光体は、外部刺激、例えば粒子線(α線、β線、電子線)や電磁波(γ線、X線、真空紫外線、紫外線、可視光線)の照射などによって容易に励起され、蛍光を放つことが可能となる。なお、ガーネット珪酸塩蛍光体から放出される蛍光は、紫外線、可視光線及び赤外線から選ばれるいずれかの電磁波であれは、後述する発光装置用として用いることができるが、実用面で好ましい蛍光は可視光である。放出される蛍光が可視光であれば、表示装置や照明装置用の発光装置として広範囲に利用できるものになる。
次に、本実施形態に係る波長変換体について詳細に説明する。本実施形態の波長変換体は、ガーネット珪酸塩蛍光体を備えるものである。波長変換体は、例えば、発光ダイオードなどの固体発光素子が放つエネルギーを吸収し、吸収したエネルギーを色調制御された可視光に変換する機能を有する。固体発光素子を用いた発光装置にこのような波長変換体を用いることにより、固体発光素子が放つ光を色調制御し、所望の照明光を得ることが可能となる。
次に、本実施形態に係る発光装置を説明する。本実施形態の発光装置は、上述のガーネット珪酸塩蛍光体または波長変換体を備えている。
酸化ルテチウムセリウム((Lu0.97Ce0.03)2O3):純度3N、日本イットリウム株式会社製
炭酸カルシウム(CaCO3):純度2N5、関東化学株式会社製
酸化マグネシウム(MgO):純度3N、和光純薬工業株式会社製
二酸化ケイ素(SiO2):純度>3N、日本アエロジル株式会社製
塩化リチウム(LiCl):純度2N、和光純薬工業株式会社製
実施例では、反応式2に沿って、ガーネット珪酸塩蛍光体の合成を試みた。なお、反応式2から分かるように、実施例は、合成する1モルのガーネット珪酸塩蛍光体(Lu2CaMg2(SiO4)3:Ce3+)に対して、3モルの反応促進剤(LiCl)を利用する合成法である。
[化2]
(Lu,Ce)2O3+CaCO3+2MgO+3SiO2+3LiCl→(Lu,Ce)2CaMg2(SiO4)3+3LiCl(+CO2↑)
比較例では、反応式3に沿って、フラックスを一切利用しないオーソドックスな固相反応を利用して、ガーネット珪酸塩蛍光体の合成を試みた。具体的には、反応促進剤を添加しなかったこと以外は実施例と同様の手順で、比較例のガーネット珪酸塩蛍光体を得た。なお、比較例のガーネット珪酸塩蛍光体は、淡い橙色の焼成物であった。
[化3]
(Lu,Ce)2O3+CaCO3+2MgO+3SiO2→(Lu,Ce)2CaMg2(SiO4)3(+CO2↑)
参考例では、反応式4に沿って、ガーネット珪酸塩蛍光体の合成を試みた。反応式4におけるxは、0.1、0.3、1、10から選択される数値である。そして、参考例1、参考例2、参考例3及び参考例4のxは、各々0.1、0.3、1及び10である。
[化4]
(Lu,Ce)2O3+CaCO3+2MgO+3SiO2+xLiCl→(Lu,Ce)2CaMg2(SiO4)3+xLiCl(+CO2↑)
上述のようにして得られた実施例、比較例、及び参考例1乃至4のガーネット珪酸塩蛍光体について、電子顕微鏡を用いた観察、結晶構造解析、及び発光スペクトル測定を行った。また、実施例及び比較例のガーネット珪酸塩蛍光体について、金属不純物の含有量を測定した。
実施例、比較例及び参考例のガーネット珪酸塩蛍光体を、電子顕微鏡(製品名:VE−9800、株式会社キーエンス製)を用いて観察した。図7(a)は実施例のガーネット珪酸塩蛍光体の観察結果を示し、図7(b)は比較例のガーネット珪酸塩蛍光体の観察結果を示す。
実施例及び比較例のガーネット珪酸塩蛍光体の結晶構造解析を、X線回折装置(製品名:MultiFlex、株式会社リガク製)を用いて行った。実施例のガーネット珪酸塩蛍光体の測定結果を図10(a)に示す。また、比較例のガーネット珪酸塩蛍光体の測定結果を図10(b)に示す。参考のため、図10(c)には、PDF(Power Diffraction Files)に登録されている、ガーネット型の結晶構造を持つY3Al5O12のパターン(PDF No.330040)を示す。
次に、実施例のガーネット珪酸塩蛍光体を青色光で励起したときの発光スペクトルを、瞬間マルチ測光システム(製品名:QE−1100、大塚電子株式会社製)を用いて評価した。なお、発光スペクトル測定時の励起波長は450nmとした。実施例の発光スペクトルの測定結果を図11中に(a)として示した。また、図11中の(b)は、同様に測定した比較例のガーネット珪酸塩蛍光体の発光スペクトルである。
次に、実施例及び比較例のガーネット珪酸塩蛍光体における金属不純物を、誘導結合プラズマ発光分光分析装置(製品名:CIROS−120、Spectro社製)を用いて評価した。なお、分析に際しては、乾燥させたサンプルを過酸化ナトリウムでアルカリ融解し、得られた融成物を塩酸で溶解した後、純水で希釈して分析に供した。金属不純物分析の結果、実施例のガーネット珪酸塩蛍光体からは、リチウムが検出された。これに対して、比較例のガーネット珪酸塩蛍光体からリチウムは検出されなかった。
100,100A,100B,100C,100D 波長変換体
Claims (8)
- 一般式:Lu2CaMg2(SiO4)3で表される珪酸塩を主成分とするガーネット珪酸塩であって、
ガーネットの結晶構造に由来する粒子形状を持つ一次粒子を含み、
リチウムを含有し、リチウムの含有量が50ppm以上2000ppm未満であるガーネット珪酸塩。 - 平均粒子径が3μm以上である、請求項1に記載のガーネット珪酸塩。
- 請求項1又は2に記載のガーネット珪酸塩と、
前記ガーネット珪酸塩に含まれる、発光中心として機能するイオンと、
を含むガーネット珪酸塩蛍光体。 - 前記イオンはCe3+である、請求項3に記載のガーネット珪酸塩蛍光体。
- 請求項3又は4に記載のガーネット珪酸塩蛍光体を備える波長変換体。
- 請求項3若しくは4に記載のガーネット珪酸塩蛍光体、又は請求項5に記載の波長変換体を備える発光装置。
- 励起源として、440nm以上475nm未満の波長範囲内にピークを持つ青色光を放つ発光素子をさらに備え、
前記青色光は前記ガーネット珪酸塩蛍光体を励起する、請求項6に記載の発光装置。 - 前記ガーネット珪酸塩蛍光体が放つ蛍光成分は、照明光又は表示画素として利用される、請求項6又は7に記載の発光装置。
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