JP5820606B2 - 蛍光体材料の製造方法、蛍光体材料、及び発光装置 - Google Patents
蛍光体材料の製造方法、蛍光体材料、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 95
- 239000000463 material Substances 0.000 title claims description 56
- 238000004519 manufacturing process Methods 0.000 title claims description 25
- 238000000034 method Methods 0.000 title claims description 13
- 239000002245 particle Substances 0.000 claims description 94
- 239000010419 fine particle Substances 0.000 claims description 46
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- 239000002002 slurry Substances 0.000 claims description 37
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- 239000012298 atmosphere Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 6
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 238000007738 vacuum evaporation Methods 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
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- PSNPEOOEWZZFPJ-UHFFFAOYSA-N alumane;yttrium Chemical compound [AlH3].[Y] PSNPEOOEWZZFPJ-UHFFFAOYSA-N 0.000 claims 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 10
- 230000006866 deterioration Effects 0.000 description 9
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 229910052727 yttrium Inorganic materials 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 229910044991 metal oxide Inorganic materials 0.000 description 5
- 150000004706 metal oxides Chemical class 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
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- 229910052688 Gadolinium Inorganic materials 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 2
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- 229910052712 strontium Inorganic materials 0.000 description 2
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910015999 BaAl Inorganic materials 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 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
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
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Description
平均粒子径20nm、最大粒子径50nmの酸化イットリウム(Y2O3)よりなるセラミックス微粒子12Aを有機溶媒に分散させたものに、平均粒子径が10μm程度の緑色系の蛍光体粒子11を混合してスラリーを調製した(ステップS101)。次いで、ロータリーエバポレーターを用い、このスラリーを減圧蒸発乾燥法により乾燥させ、有機溶媒を除去した(ステップS102)。その際、スラリーを収納した容器を回転させることによりスラリーを撹拌しながら乾燥させた。続いて、乾燥させた粉末、すなわちセラミックス微粒子12Aを付着させた蛍光体粒子11を窒素雰囲気中において400℃で2時間熱処理した(ステップS103)。そののち、得られた粉末、すなわち被覆層12を形成した蛍光体粒子11について、同様にしてスラリーの調製(ステップS101)、乾燥(ステップS102)、熱処理(ステップS103)をもう1回繰り返し、蛍光体材料10を得た。得られた蛍光体材料10について、原料に用いた蛍光体粒子11の収率を調べたところ、95%以上であった。なお、収率は、収率=処理後の総重量/(処理前の蛍光体粒子重量+セラミックス微粒子の重量)により求めた。
スラリーを噴霧乾燥により乾燥させたことを除き、他は実施例1と同様にして蛍光体材料を作製した。得られた蛍光材料について、原料に用いた蛍光体粒子の収率を調べたところ、約70%であった。
スラリーを自然乾燥により乾燥させたことを除き、他は実施例1と同様にして蛍光体材料を作製した。比較例1−2では、実施例1と同量のスラリーを乾燥させるのに、実施例1の10倍以上の時間がかかった。
実施例1により作製した蛍光体材料10を用い、図3に示したような発光装置20を作製した。発光素子22には紫外光を発するものを用いた。
熱処理を酸化雰囲気中(大気雰囲気中)において行ったことを除き、他は実施例1と同様にして蛍光体材料10を作製し、実施例2−1と同様にして、発光装置20を作製した。
蛍光体粒子に被覆層を形成せずに、そのまま蛍光体材料として用い、実施例2−1と同様にして発光装置を作製した。
実施例2−1,2−2及び比較例2の各発光装置20について、発光試験を行い、輝度の経時変化を調べた。得られた結果を表2に示す。表2において、相対輝度というのは、被覆層を形成していない比較例2の初期輝度を100%とした場合の相対値である。
セラミックス微粒子12Aの平均粒子径及び最大粒子径を変化させたことを除き、他は実施例1と同様にして蛍光体材料10を作製し、実施例2−1と同様にして発光装置20を作製した。実施例3−1では平均粒子径が40nm、最大粒子径が50nm、実施例3−2では平均粒子径が30nm、最大粒子径が50nm、実施例3−3では平均粒子径が25nm、最大粒子径が50nm、実施例3−4では平均粒子径が20nm、最大粒子径が40nm、実施例3−5では平均粒子径が15nm、最大粒子径が40nmのセラミックス微粒子12Aを用いた。得られた発光装置20について実施例2−1と同様にして発光試験を行い、輝度の経時変化を調べた。得られた結果を実施例2−1及び比較例2の結果と共に表3に示す。表3において、2000時間後の輝度維持率というのは、被覆層を形成していない比較例2の初期輝度を100%とした場合の相対値である。
Claims (7)
- 蛍光体粒子の表面に被覆層を有する蛍光体材料の製造方法であって、
蛍光体粒子と、セラミックス微粒子と、液体とを含むスラリーを減圧蒸発乾燥法により乾燥させ、液体を除去することにより、蛍光体粒子の表面に被覆層を形成する工程と、
前記スラリーを乾燥させたのち、窒素及び長周期表第18族元素からなる群のうちの少なくとも1種を含む不活性ガス雰囲気中において熱処理する工程と
を含むことを特徴とする蛍光体材料の製造方法。 - 前記熱処理の温度は、450℃以下とすることを特徴とする請求項1記載の蛍光体材料の製造方法。
- 前記スラリーを乾燥させる際に、スラリーを撹拌することを特徴とする請求項1又は請求項2記載の蛍光体材料の製造方法。
- 前記スラリーを乾燥させる際に、ロータリーエバポレーター又はフラッシュエバポレーターを用いることを特徴とする請求項1から請求項3のいずれか1に記載の蛍光体材料の製造方法。
- 前記セラミックス微粒子の平均粒径を40nm以下とすることを特徴とする請求項1から請求項4のいずれか1に記載の蛍光体材料の製造方法。
- 前記セラミックス微粒子の最大粒径を50nm以下とすることを特徴とする請求項1から請求項5のいずれか1に記載の蛍光体材料の製造方法。
- 前記セラミックス微粒子は、希土類酸化物,酸化ジルコニウム,酸化チタン,酸化亜鉛,酸化アルミニウム,イットリウムとアルミニウムの複合酸化物,酸化マグネシウム及びアルミニウムとマグネシウムの複合酸化物からなる群のうちの少なくとも1種の金属酸化物を含むことを特徴とする請求項1から請求項6のいずれか1に記載の蛍光体材料の製造方法。
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JP2011096645A JP5820606B2 (ja) | 2011-04-23 | 2011-04-23 | 蛍光体材料の製造方法、蛍光体材料、及び発光装置 |
TW100122371A TWI599638B (zh) | 2011-04-23 | 2011-06-27 | 螢光體材料之製造方法、螢光體材料、及發光裝置 |
KR1020137001755A KR101771448B1 (ko) | 2011-04-23 | 2011-06-28 | 형광체 재료의 제조방법, 형광체 재료 및 발광장치 |
CN201180036915.2A CN103038310B (zh) | 2011-04-23 | 2011-06-28 | 荧光体材料的制造方法、荧光体材料及发光装置 |
PCT/JP2011/064792 WO2012147215A1 (ja) | 2011-04-23 | 2011-06-28 | 蛍光体材料の製造方法、蛍光体材料、及び発光装置 |
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