JP6093340B2 - 蛍光体、蛍光体の作製方法及び発光装置 - Google Patents
蛍光体、蛍光体の作製方法及び発光装置 Download PDFInfo
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims description 205
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- 239000000463 material Substances 0.000 claims description 68
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- 238000009826 distribution Methods 0.000 claims description 15
- 229910052733 gallium Inorganic materials 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- 229910052727 yttrium Inorganic materials 0.000 claims description 11
- 229910052738 indium Inorganic materials 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 229910052706 scandium Inorganic materials 0.000 claims description 10
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 7
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- 238000005406 washing Methods 0.000 claims description 7
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- 229910052771 Terbium Inorganic materials 0.000 claims description 6
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- 239000002245 particle Substances 0.000 description 26
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 22
- 235000019353 potassium silicate Nutrition 0.000 description 21
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
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- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 2
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
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- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical class [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
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- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
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- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
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- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229940110728 nitrogen / oxygen Drugs 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012788 optical film Substances 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- RLQWHDODQVOVKU-UHFFFAOYSA-N tetrapotassium;silicate Chemical compound [K+].[K+].[K+].[K+].[O-][Si]([O-])([O-])[O-] RLQWHDODQVOVKU-UHFFFAOYSA-N 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7767—Chalcogenides
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- H—ELECTRICITY
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Description
実験例は以下のように説明される。
(1)蛍光体の直径(D10、D50、D90)の分析はBeckman CoulterのMultisizer−3によって行う。
蛍光体から放出される光の特性の測定装置は図2に示されるようなものである。測定を以下のように行う。1.8gのサンプルを直径12cmのサンプルホルダー12に入れ、サンプルがサンプルホルダー12内に均一に分散するように押し付ける。次いで、サンプルホルダー12を暗箱体11内に設置する。波長455nmの光源13、例えば炭化ケイ素基板を有するInGaN青色発光ダイオード素子を、サンプルから5cm離してサンプル上に垂直に配置する。光源13でサンプルに照射する。蛍光を輝度計16(TOPCON、SR−3A)に反射鏡15を介して水平に指向する。反射鏡15は直径2cmの導光管14内に配置し、蛍光材料から放出される蛍光を指向する。導光管14及び光源は45度の角度を成すようにする。反射鏡15とサンプルホルダー12との距離は8cmとし、輝度計16と反射鏡15との距離は40cmとする。輝度計16はフィールド1度の検出モードを適用する。輝度値の測定誤差は±0.3%以内とする。蛍光体からの光の主波長をJobin YVONのFluoro Max−3によって測定した。
(3−1a)機器:
測定は、誘導結合プラズマ(ICP)原子発光分光計(ULTIMA−2型、Jobin Yvon Technology)を用いて行った。
0.1gのサンプルを正確に秤量し、白金坩堝内に入れた。1gのNa2CO3を白金坩堝に添加し、サンプルと均一に混合した。次いで、混合物を1200℃の高温炉によって融合させた(温度条件:温度を室温から1200℃まで2時間かけて上昇させ、1200℃で5時間保持した)。次いで、融合生成物を冷却し、25mlのHCl(36%)等の酸性溶液中に添加した後、加熱して溶液が透明になるまで溶解させた。次いで、溶液を冷却後、100mL容のPFAメスフラスコ内に入れ、純水をフラスコの標線まで適量(quantitatively)添加した。
窒素/酸素分析装置(株式会社堀場製作所、EMGA−620W)。
20mgの蛍光体をSnカプセルに入れた後、カプセルを坩堝に入れ、測定した。
実施形態及び比較例の蛍光体は、表1〜表3に示される違いを除いて同様の方法によって作製する。表1は原料混合物の蛍光体原料の各々の元素のモル比(mole relation)、すなわち式A3−aCeaQ5−eEeO12(式中のA元素はイットリウム(Y)元素及びガドリニウム(Gd)元素であり、Q元素はガリウム(Ga)元素であり、E元素はアルミニウム(Al)元素である)の各々の元素及び原料混合物の融剤YF3の金属元素イットリウム(Y)のモル比を示す。表2及び表3は水ガラス溶液の濃度を示す。蛍光体の作製方法を、以下の実施形態3を一例として開示する。
Claims (6)
- 式A 3−a Ce a Q 5−e E e O 12 (式中、AがY、La、Gd、Tb及びLuの少なくとも1つを含み、QがGa、Al、In及びScの少なくとも1つを含み、EがGa、In、Sc、Alの少なくとも1つを含み、Ceはセリウムであり、Oは酸素であり、0<a≦3であり、0≦e≦5である)からなる、直径分布スパンが0.7未満であって、且つ該直径分布スパンは(D90−D10)/D50と定義される蛍光体の作製方法であって、
原料混合物を焼結することであって、それにより焼結蛍光体材料を得ることと、
前記焼結蛍光体材料をアルカリ金属ケイ酸塩水溶液と混合することであって、それにより蛍光体混合物を得ることと、
続いて前記蛍光体混合物に対して後続処理プロセスを行うことであって、それにより蛍光体を得ることと、
を含み、
前記後続処理プロセスが水洗工程を含む、作製方法。 - 前記蛍光体の中央径(D50)が13μmを超える場合、10μm〜20μmである蛍光体の含量が該蛍光体の体積の80%超であって、10μm未満である蛍光体の含量が該蛍光体の体積の15%未満である、請求項1に記載の蛍光体の作製方法。
- 前記蛍光体の中央径(D50)が13μmを超える場合、10μm〜20μmである蛍光体の含量が該蛍光体の体積の80%超かつ87%未満であって、10μm未満である蛍光体の含量が該蛍光体の体積の15%未満かつ10%超である、請求項1に記載の蛍光体の作製方法。
- 前記蛍光体の中央径(D50)が13μmを超える場合、20μmを超える蛍光体の含量が該蛍光体の体積の5%未満であって、10μm〜20μmである蛍光体の含量が該蛍光体の体積の80%超であって、10μm未満である蛍光体の含量が該蛍光体の体積の15%未満である、請求項1に記載の蛍光体の作製方法。
- 前記蛍光体の中央径(D50)が13μmを超える場合、20μmを超える蛍光体の含量が該蛍光体の体積の5%未満かつ3%超であって、10μm〜20μmである蛍光体の含量が該蛍光体の体積の80%超かつ87%未満であって、10μm未満である蛍光体の含量が該蛍光体の体積の15%未満かつ10%超である、請求項1に記載の蛍光体の作製方法。
- 前記蛍光体の中央径(D50)が13μm未満である場合、10μm〜15μmである蛍光体の含量が該蛍光体の体積の50%超である、請求項1に記載の蛍光体の作製方法。
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JP6273394B1 (ja) * | 2017-06-14 | 2018-01-31 | デンカ株式会社 | フッ化物蛍光体とそれを用いた発光装置 |
JP6273395B1 (ja) * | 2017-06-14 | 2018-01-31 | デンカ株式会社 | フッ化物蛍光体とそれを用いた発光装置 |
JP6917244B2 (ja) * | 2017-08-23 | 2021-08-11 | 日本特殊陶業株式会社 | 蛍光体ホイール、ホイールデバイスおよびプロジェクター |
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JP4991026B2 (ja) | 2003-02-26 | 2012-08-01 | 日亜化学工業株式会社 | 発光装置 |
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