JP6602066B2 - Yag系蛍光体の製造方法 - Google Patents
Yag系蛍光体の製造方法 Download PDFInfo
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- JP6602066B2 JP6602066B2 JP2015122976A JP2015122976A JP6602066B2 JP 6602066 B2 JP6602066 B2 JP 6602066B2 JP 2015122976 A JP2015122976 A JP 2015122976A JP 2015122976 A JP2015122976 A JP 2015122976A JP 6602066 B2 JP6602066 B2 JP 6602066B2
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims description 42
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000000843 powder Substances 0.000 claims description 75
- 239000002994 raw material Substances 0.000 claims description 29
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 28
- 229910016036 BaF 2 Inorganic materials 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 20
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 16
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical group [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 claims description 2
- 229910001632 barium fluoride Inorganic materials 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims 1
- 238000005049 combustion synthesis Methods 0.000 description 39
- 238000006243 chemical reaction Methods 0.000 description 18
- 238000002485 combustion reaction Methods 0.000 description 13
- 238000002441 X-ray diffraction Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 230000004907 flux Effects 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 238000004020 luminiscence type Methods 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 230000004927 fusion Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 238000003746 solid phase reaction Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000009103 reabsorption Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Description
本発明者らは、反応温度を制御するための希釈剤として、YAGのAl源としてのAl2O3を利用することを検討し、その適正な添加量の検討を行った。
原料となる素粉末の純度が、燃焼合成で得られるYAG系蛍光体の品質(発光特性)に及ぼす影響について検討した。
原料として、Y2O3粉末(関東化学製:純度99.99%)、CeO2粉末(高純度化学製:純度99.99%、平均径0.2μm)、金属Al粉末(高純度化学製:純度99.99%、平均径45μm)、Al2O3粉末(高純度化学製:純度99.99%)、NaClO4粉末(ALDRICH製:純度98.0%)を原料とし、Ceを1.0at%、2.0at%、3.0at%、4.0at%、および5.0at%含有するYAG蛍光体(YAG:Ce)を燃焼合成した。この時の条件は、x=1.725とした。それぞれの合成時の反応式は、下式(13)〜(17)のとおりである。
フラックスは、複合酸化物等を合成する際に、その合成に必要な温度を引き下げ、均質性を高める効果があることが知られており、BaF2、CaF2、NaCl等が用いられる。このうち、BaF2は、比較的安価であり融点が1626Kと比較的高いこと、また、湯で洗浄することでほぼ取り除くことができるという利点がある(特許文献4や非特許文献7を参照)。そこで、本発明者らは、フラックスとしてのBaF2の添加量の検討を行った。
燃焼合成法により得られたYAG系蛍光体の上述発光特性を、固相反応法で合成したYAG系蛍光体の発光特性と比較した。
20 坩堝
30 断熱材
40 カーボンホイル
50 ロータリーポンプ
60 ガス導入口
70 ガス排出口
80 コントロールボックス
100 燃焼合成装置
Claims (9)
- 酸化イットリウム(Y2O3)粉末と酸化アルミニウム(Al2O3)粉末と金属Al粉末を含む素粉末を原料とし、前記金属Al粉末の酸化熱を利用してYAG(Y3Al5O12)系蛍光体を燃焼合成する、YAG系蛍光体の製造方法であって、
前記原料中のY 2 O 3 粉末と前記Al 2 O 3 粉末と前記金属Al粉末の比をモル比でY 2 O 3 :Al 2 O 3 :Al=1.5:x:(5−2x)としたときに、前記xを1.5〜1.8の範囲に設定する、YAG系蛍光体の製造方法。 - 前記原料中に、さらにセリウム酸化物(CeO2)粉末を添加し、前記Y2O3粉末と前記CeO2粉末と前記Al2O3粉末と前記金属Al粉末の比をモル比でY2O3:CeO2:Al2O3:Al=(1.5−α):2α:x:(5−2x)としたときに、前記xを1.5〜1.8の範囲に設定する、請求項1に記載のYAG系蛍光体の製造方法。
- 2α/[2(1.5−α)+2α]で定義される前記αと(1.5−α)の比を、1.0%以上で5.0%以下に設定する、請求項2に記載のYAG系蛍光体の製造方法。
- 前記xを1.70〜1.75の範囲に設定する、請求項1〜3の何れか1項に記載のYAG系蛍光体の製造方法。
- 前記原料に、さらに酸素供給剤として過塩素酸物を加える、請求項1〜4の何れか1項に記載のYAG系蛍光体の製造方法。
- 前記酸素供給剤はNaClO4である、請求項5に記載のYAG系蛍光体の製造方法。
- 前記原料に、更にフッ化バリウム(BaF2)粉末を添加する、請求項2〜6の何れか1項に記載のYAG系蛍光体の製造方法。
- 前記BaF2粉末の添加量を、原料の素粉末の全量に対して4〜6wt%の範囲に設定する、請求項7に記載のYAG系蛍光体の製造方法。
- 前記Al2O3粉末および金属Al粉末として、純度99.99%以上のものを用いる、請求項1〜8の何れか1項に記載のYAG系蛍光体の製造方法。
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CN107090290A (zh) * | 2017-04-25 | 2017-08-25 | 江苏师范大学 | 一种快速低耗高效制备yag粉体的方法 |
KR102510280B1 (ko) * | 2021-01-14 | 2023-03-15 | 목포대학교산학협력단 | 고순도 및 고밀도 이트륨 알루미늄 가넷 소결체 및 이의 제조방법 |
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WO1990011249A1 (en) * | 1989-03-29 | 1990-10-04 | Institut Strukturnoi Makrokinetiki Akademii Nauk Sssr | Method of obtaining complex oxides |
JP2609376B2 (ja) * | 1991-06-28 | 1997-05-14 | 修 山田 | 金属間化合物およびセラミックスの製造方法 |
JPH06247775A (ja) * | 1993-02-19 | 1994-09-06 | Yoshio Miyamoto | ガス圧燃焼焼結法 |
JP4325629B2 (ja) * | 2005-02-28 | 2009-09-02 | 三菱化学株式会社 | 蛍光体及びその製造方法並びにそれを使用した発光装置 |
JP2006347823A (ja) * | 2005-06-16 | 2006-12-28 | Ntn Corp | 燃焼合成方法および誘電体セラミックス |
JP2007091523A (ja) * | 2005-09-28 | 2007-04-12 | Ntn Corp | 燃焼合成方法および誘電体セラミックス |
JP5190835B2 (ja) * | 2007-04-03 | 2013-04-24 | 独立行政法人産業技術総合研究所 | 多元系酸窒化物蛍光体の製造方法 |
KR101013146B1 (ko) * | 2010-02-16 | 2011-02-10 | 충남대학교산학협력단 | 이트륨 알루미늄 가넷 황색-발광 형광체의 급속 고상 합성방법 |
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