JP5700326B2 - 青色に発光する蛍光体とその製造方法および利用 - Google Patents
青色に発光する蛍光体とその製造方法および利用 Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000000126 substance Substances 0.000 title 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 73
- 238000005342 ion exchange Methods 0.000 claims description 66
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 58
- 229910021536 Zeolite Inorganic materials 0.000 claims description 53
- 239000010457 zeolite Substances 0.000 claims description 53
- 150000002500 ions Chemical class 0.000 claims description 33
- 239000013078 crystal Substances 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000011248 coating agent Substances 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 15
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- 239000000758 substrate Substances 0.000 claims description 7
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- 150000003839 salts Chemical class 0.000 claims description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 13
- 238000002189 fluorescence spectrum Methods 0.000 description 11
- 230000003647 oxidation Effects 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 8
- 230000005284 excitation Effects 0.000 description 8
- 229910052684 Cerium Inorganic materials 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 239000000976 ink Substances 0.000 description 7
- 238000001354 calcination Methods 0.000 description 6
- -1 rare earth metal ions Chemical class 0.000 description 6
- 229910052693 Europium Inorganic materials 0.000 description 5
- 150000002910 rare earth metals Chemical class 0.000 description 5
- 229910052771 Terbium Inorganic materials 0.000 description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 4
- XQTIWNLDFPPCIU-UHFFFAOYSA-N cerium(3+) Chemical compound [Ce+3] XQTIWNLDFPPCIU-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
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- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
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- 238000004020 luminiscence type Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
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- 238000003746 solid phase reaction Methods 0.000 description 2
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- 229910052727 yttrium Inorganic materials 0.000 description 2
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- TVGGZXXPVMJCCL-UHFFFAOYSA-N [Si].[La] Chemical compound [Si].[La] TVGGZXXPVMJCCL-UHFFFAOYSA-N 0.000 description 1
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- 239000002253 acid Substances 0.000 description 1
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- 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
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- JYIBXUUINYLWLR-UHFFFAOYSA-N aluminum;calcium;potassium;silicon;sodium;trihydrate Chemical compound O.O.O.[Na].[Al].[Si].[K].[Ca] JYIBXUUINYLWLR-UHFFFAOYSA-N 0.000 description 1
- 238000005280 amorphization Methods 0.000 description 1
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- 150000001553 barium compounds Chemical class 0.000 description 1
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- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 150000001785 cerium compounds Chemical class 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 229910001603 clinoptilolite Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
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- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical compound [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
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- 239000012266 salt solution Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
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- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- Luminescent Compositions (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Description
1)リンデQゼオライトのイオン交換によって、リンデQの構造内に青色発光の中心となるCe3+を均一に分散させることができる。Ceイオンの交換率は、イオン交換に用いたCe塩溶液の濃度に比例する。
2)Ceイオンで交換したリンデQ(イオン交換率47.6%)を還元性雰囲気で900℃に加熱することによって、波長295nmの紫外光で励起したとき410nm付近にピークを有する青色に発光する蛍光体が得られる。加熱を大気中で行なった試料は発光せず、これはCe3+が酸化されCe4+になったためと思われる。
3)Ceイオン交換リンデQの青色発光ピークは、イオン交換率の増加にともない強くなる。
4)Ceイオン交換により、リンデQの熱安定性が向上する。熱安定性の向上の程度は、Ceイオン交換率に依存する。
5)イオン交換率が80.5%のCe交換リンデQは、加熱温度が800℃までは、ゼオライト構造を維持する。900℃以上に加熱すると、非晶質となる。
6)イオン交換率80.5%のCe交換リンデQは、加熱温度が900℃に至るまでは、ゼオライト構造が維持されるかこわれるかにかかわらず、六角板状の形態を維持する。
7)Ce交換リンデQは、加熱温度により、発光のピーク波長が異なる。加熱温度が高くなるにつれてピーク波長は長波長側にシフトし、900℃の加熱試料からは、励起波長295nmにおいて410nm付近にピークを有する青色の発光がみられる。
8)ゼオライト構造を維持する加熱試料は、水分を吸着して復水するが、復水後も発光特性を維持する。しかしながら、Ce3+の酸化により、発光特性を喪失する。これに対して非晶質の加熱試料は復水することがなく、かつ、酸化による発光強度の減少もない。
Claims (8)
- K2O・Al2O3・2SiO2・xH2Oの組成を有し、六角板状の結晶形態をもつ「リンデQ」型ゼオライトにイオン交換を行なってCe3+イオンを分散させ、かつ、Ce 3+ を酸化させることのない条件下で加熱してゼオライトの結晶構造を破壊することにより非晶質としたが、板状の外形には変更が加えられていない材料からなり、295nmの紫外線により励起されて410nmに波長のピークを有する青色の蛍光を発する板状蛍光体。
- 請求項1に記載した板状蛍光体を製造する方法であって、K2O・Al2O3・2SiO2・xH2Oの組成を有し、六角板状の結晶形態をもつ「リンデQ」型ゼオライトを、Ceの可溶性塩の水溶液に浸漬し、温度100℃以下でゼオライト中のK+とCe3+イオンとのイオン交換を行なって、少なくとも20%の交換率でCeイオンを存在させたのち、Ce 3+ を酸化させることのない非酸化性の雰囲気下で850℃以上1000℃未満の温度で焼成することにより、ゼオライトの結晶構造を破壊して非晶質とするが、板状の外形を維持した蛍光体を得ることからなる製造方法。
- 非酸化性の雰囲気下の焼成を、900℃近辺の温度において行なう請求項2の製造方法。
- 請求項1に記載した板状蛍光体をビヒクルに分散させて形成した蛍光塗料または印刷インク。
- 請求項4の蛍光塗料または印刷インクを、板状体蛍光体が基材の面に沿って配向される塗布手段を用いて基材に塗布し、厚さ方向にナノサイズの板状蛍光体が存在する塗膜を得ることからなる板状蛍光体の塗膜形成方法。
- 偽造を防止すべき書類を基材とし、その表面に請求項4に記載した蛍光塗料または印刷インクの塗膜を形成して得た、偽造防止処理を施した書類。
- 偽造を防止すべき書類が、有価証券または製品ラベルである請求項6の偽造防止処理を施した書類。
- 請求項6に記載の偽造防止処理を施した書類に対して紫外線を照射し、励起された発光体から生じる青色光を検出することからなる偽造を検知する方法。
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