WO2016098830A1 - 蛍光体及びその用途 - Google Patents
蛍光体及びその用途 Download PDFInfo
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- WO2016098830A1 WO2016098830A1 PCT/JP2015/085274 JP2015085274W WO2016098830A1 WO 2016098830 A1 WO2016098830 A1 WO 2016098830A1 JP 2015085274 W JP2015085274 W JP 2015085274W WO 2016098830 A1 WO2016098830 A1 WO 2016098830A1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000001301 oxygen Substances 0.000 claims abstract description 15
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 15
- 239000006104 solid solution Substances 0.000 claims abstract description 9
- 230000003213 activating effect Effects 0.000 claims abstract description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 75
- 230000005284 excitation Effects 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 3
- 150000002602 lanthanoids Chemical class 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 239000011575 calcium Substances 0.000 description 40
- 230000000052 comparative effect Effects 0.000 description 15
- 239000000203 mixture Substances 0.000 description 13
- 239000013078 crystal Substances 0.000 description 12
- 239000000843 powder Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 229910052782 aluminium Inorganic materials 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 238000010306 acid treatment Methods 0.000 description 5
- 238000002189 fluorescence spectrum Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- -1 calcium nitride Chemical class 0.000 description 3
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 229910001940 europium oxide Inorganic materials 0.000 description 3
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 238000003991 Rietveld refinement Methods 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000001296 phosphorescence spectrum Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
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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
- C09K11/0883—Arsenides; Nitrides; Phosphides
-
- 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
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/77348—Silicon Aluminium Nitrides or Silicon Aluminium Oxynitrides
-
- 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
- C09K11/77928—Silicon Aluminium Nitrides or Silicon Aluminium Oxynitrides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
Definitions
- the present invention relates to a phosphor that emits red light, a light-emitting element including the phosphor, and a light-emitting device including the light-emitting element.
- a phosphor according to an embodiment of the present invention is a phosphor represented by a general formula Ca x + y Eu y SiAlN 3 .
- This phosphor is formed by bonding (Si, Al) -N 4 tetrahedrons, and Ca element is located in the gap.
- This composition is kept electrically neutral by a combination of Ca element occupancy, Si / Al ratio, and N / O ratio parameters.
- y is 0.004 or more and 0.012 or less, preferably 0.004 or more and 0.011 or less, more preferably 0.004 or more and 0.010 or less. It is. This is because if the Eu content is too low, the fluorescence intensity cannot be improved, and if the Eu content is too high, the fluorescence intensity due to fluorescence quenching due to energy transfer between Eu tends to decrease.
- the Eu content of the phosphor according to an embodiment of the present invention is 0.4% by mass or more and 1.2% by mass or less because if the Eu content is too small, the fluorescence intensity cannot be improved, and the Eu content This is because if the amount is too large, the fluorescence intensity due to fluorescence concentration quenching due to energy transfer between Eu tends to decrease.
- the Eu content is preferably 0.4% by mass or more and 1.1% by mass or less, more preferably 0.4% by mass or more and 1.0% by mass or less.
- An embodiment of the present invention provides a light emitting device including the light emitting element.
- the light emitting device include a lighting fixture, a lighting device, an image display device, a traffic light, and a projector.
- Table 1 shows values of x and y (preparation value and actual value), lattice constant (unit: nm), solid solution oxygen amount (unit: mass%), and Eu content in the general formulas of the phosphors of Examples and Comparative Examples. It shows the amount (unit: mass%), Ca content (unit: mass%), peak wavelength (unit: nm), and relative fluorescence peak intensity (unit:%).
- excitation / fluorescence spectrum measurement of the phosphor of Example 1 was performed using a spectrofluorometer (F7000, manufactured by Hitachi High-Technologies Corporation).
- the excitation wavelength of the fluorescence spectrum was 455 nm
- the monitor wavelength of the excitation spectrum was the peak wavelength of the fluorescence spectrum of 455 nm excitation.
- the raw material of the phosphor of Example 1 is ⁇ -type silicon nitride powder (SN-E10 grade manufactured by Ube Industries, Ltd., solid solution oxygen content 1.0 mass%) 37.6 mass%, aluminum nitride powder (manufactured by Tokuyama Corporation) E grade, solid solution oxygen content 0.8 mass%) 27.4 mass%, europium oxide (RU grade made by Shin-Etsu Chemical Co., Ltd.) 0.8 mass%, and calcium nitride powder (made by Materion, purity 99%, The particle size is 75 ⁇ m or less and the amount of dissolved oxygen is 0.6% by mass), which is 34.2% by mass.
- the ⁇ -type silicon nitride powder, the aluminum nitride powder, and the europium oxide were put in a nylon pot, a silicon nitride ball was used, and ball mill mixing was performed using ethanol as a solvent. . After removing the solvent by drying, the entire amount was passed through a sieve having an opening of 75 ⁇ m.
- the raw material from which this agglomeration was removed was carried into a glove box substituted with nitrogen, and the remaining raw material calcium nitride powder was mixed manually.
- the conventional “phosphor represented by the general formula Ca x + y Eu y SiAlN 3 and containing Eu as an activating element and part of the Ca element substituted with Eu” is equivalent to Comparative Example 1. .
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Luminescent Compositions (AREA)
- Led Device Packages (AREA)
Abstract
Description
蛍光体の格子定数は、X線回折装置(株式会社リガク製Ultima IV)を用い、CuKα線を用いた粉末X線回折(XRD)により、結晶相の同定を行った。
実施例1に係る蛍光体の結晶相は、CaAlSiN3単相であった。得られたX線回折パターンから、結晶構造解析ソフト(株式会社リガク製JADE)を用いてリートベルト解析を行い、格子定数精密化を行った。実施例1に係る蛍光体の格子定数aは0.9761nm、格子定数cは0.5051nmであった。
蛍光体のEu含有率及びCa含有量は、酸素窒素分析装置(株式会社堀場製作所製EMGA-920)により測定した。実施例1の蛍光体のEu含有量は0.67質量%、Ca含有量は28.4質量%であった。
蛍光体のピーク波長は、分光蛍光光度計(株式会社日立ハイテクノロジーズ製F7000)を用いて、実施例1の蛍光体の励起・蛍光スペクトル測定を行った。蛍光スペクトルの励起波長を455nmとし、励起スペクトルのモニター波長を455nm励起の蛍光スペクトルのピーク波長とした。
相対蛍光ピーク強度は、測定装置や条件によって変化するため単位は任意であり、同一条件で測定した実施例及び比較例での相対で比較した。基準として、160%以上が合格値である。
実施例1に係る蛍光体は、ピーク波長が653nmで赤色発光蛍光体であり、相対蛍光ピーク強度が170.4%の蛍光体であった。
実施例1の蛍光体の原料は、α型窒化ケイ素粉末(宇部興産株式会社製SN-E10グレード、固溶酸素量1.0質量%)37.6質量%、窒化アルミニウム粉末(トクヤマ株式会社製Eグレード、固溶酸素量0.8質量%)27.4質量%、酸化ユーロピウム(信越化学工業株式会社製RUグレード)0.8質量%、及び窒化カルシウム粉末(Materion社製、純度99%、粒度75μm以下、固溶酸素量0.6質量%)を34.2質量%である。
混合工程後の原料をグローブボックス内で蓋付きの円筒型窒化ホウ素製容器(電気化学工業株式会社製N-1グレード)に充填し、グローブボックスから取り出し、カーボンヒーターの電気炉にセットし、電気炉内を0.1Pa以下まで十分に真空排気した。真空排気したまま常温から加熱を開始した。600℃で窒素ガスを導入し、電気炉内の雰囲気圧力を0.1MPaとした。0.1MPaに圧力を設定後、1800℃まで昇温し、1800℃に達してから4時間この温度を保持する焼成を行った。
焼成粉末は、濃度1規定の塩酸に、スラリー濃度が25質量%となるように混合して酸処理を1時間行い、その後塩酸スラリーを攪拌しながら、煮沸処理を1時間行った。
比較例1の蛍光体において実施例1の蛍光体と異なる点は、原料配合比を窒化ケイ素粉末:窒化アルミニウム粉末:酸化ユーロピウム粉末:窒化カルシウム粉末=38.1:27.8:0.84:33.3質量%とした点である。
実施例1及び比較例1で使用した原料粉末を種々の配合比で混合し、それらの混合粉末を実施例1と同様の処理を行い、実施例2~4及び比較例2~6の蛍光体を作製し、評価した。Eu含有量の少ない比較例2及びCa含有量が少ない比較例3では、相対蛍光ピーク強度が低い値であった。酸素含有量が多い比較例4及び一般式組成から外れた比較例5は相対蛍光ピーク強度が低く格子定数が本発明範囲を逸脱していた。Eu含有量の多い比較例6では、ピーク波長が665nmと赤色発光蛍光体の範囲を逸脱していた。
実施例5の蛍光体は、実施例1の蛍光体のCaの一部をLiで置換したものである。
実施例5の蛍光体は、ピーク波長649nm、相対蛍光ピーク強度が170.8%の蛍光体であり電荷バランスを維持するために有効な方法であった。
Claims (4)
- 一般式Cax+yEuySiAlN3で示され、賦活元素としてのEuを含有すると共にCa元素の一部がEuで置換された蛍光体であって、当該x+yは1.0以上1.1以下であり、当該yは0.004以上0.012以下であり、当該蛍光体の格子定数aが0.9747nm以上0.9770nm以下であり、当該蛍光体の格子定数cが0.5050nm以上0.5055nm以下であり、そのCa含有量が27.8質量%以上28.8質量%以下であり、その固溶酸素量が0.3質量%以上1.2質量%以下であり、そのEu含有量が0.4質量%以上1.2質量%以下の蛍光体。
- 前記Caの一部が、Mg、Li、Y及びランタノイド(La、Ce及びEuを除く。)からなる群から選ばれる1種以上の元素によって置換されている請求項1に記載の蛍光体。
- 請求項1乃至2のいずれか1項に記載の蛍光体と、前記蛍光体に励起光を照射する発光光源とを有する発光素子。
- 請求項3に記載の発光素子を備える発光装置。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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JP2016564890A JP6715774B2 (ja) | 2014-12-16 | 2015-12-16 | 蛍光体及びその用途 |
KR1020177016967A KR102485860B1 (ko) | 2014-12-16 | 2015-12-16 | 형광체 및 그 용도 |
US15/537,123 US10519370B2 (en) | 2014-12-16 | 2015-12-16 | Phosphor and application therefor |
CN201580068437.1A CN107001933A (zh) | 2014-12-16 | 2015-12-16 | 荧光体及其用途 |
DE112015005609.2T DE112015005609B4 (de) | 2014-12-16 | 2015-12-16 | Leuchtstoff, lichtemittierendes element und lichtemittierende vorrichtung |
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JP2014253979 | 2014-12-16 | ||
JP2014-253979 | 2014-12-16 |
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WO2016098830A1 true WO2016098830A1 (ja) | 2016-06-23 |
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US (1) | US10519370B2 (ja) |
JP (1) | JP6715774B2 (ja) |
KR (1) | KR102485860B1 (ja) |
CN (1) | CN107001933A (ja) |
DE (1) | DE112015005609B4 (ja) |
TW (1) | TWI683887B (ja) |
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- 2015-12-16 JP JP2016564890A patent/JP6715774B2/ja active Active
- 2015-12-16 CN CN201580068437.1A patent/CN107001933A/zh not_active Withdrawn
- 2015-12-16 WO PCT/JP2015/085274 patent/WO2016098830A1/ja active Application Filing
- 2015-12-16 US US15/537,123 patent/US10519370B2/en active Active
- 2015-12-16 TW TW104142317A patent/TWI683887B/zh active
- 2015-12-16 DE DE112015005609.2T patent/DE112015005609B4/de active Active
- 2015-12-16 KR KR1020177016967A patent/KR102485860B1/ko active IP Right Grant
Patent Citations (6)
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KR20170094236A (ko) | 2017-08-17 |
TW201629186A (zh) | 2016-08-16 |
TWI683887B (zh) | 2020-02-01 |
JPWO2016098830A1 (ja) | 2017-09-21 |
JP6715774B2 (ja) | 2020-07-01 |
DE112015005609B4 (de) | 2024-04-25 |
KR102485860B1 (ko) | 2023-01-06 |
CN107001933A (zh) | 2017-08-01 |
US10519370B2 (en) | 2019-12-31 |
DE112015005609T5 (de) | 2017-09-07 |
US20180265781A1 (en) | 2018-09-20 |
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