JP6752803B2 - 色安定赤色発光蛍光体 - Google Patents
色安定赤色発光蛍光体 Download PDFInfo
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- JP6752803B2 JP6752803B2 JP2017541767A JP2017541767A JP6752803B2 JP 6752803 B2 JP6752803 B2 JP 6752803B2 JP 2017541767 A JP2017541767 A JP 2017541767A JP 2017541767 A JP2017541767 A JP 2017541767A JP 6752803 B2 JP6752803 B2 JP 6752803B2
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims description 121
- 239000002994 raw material Substances 0.000 claims description 35
- 239000002245 particle Substances 0.000 claims description 32
- 239000012263 liquid product Substances 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 21
- 229910052731 fluorine Inorganic materials 0.000 claims description 17
- 229910052727 yttrium Inorganic materials 0.000 claims description 14
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 12
- 239000011737 fluorine Substances 0.000 claims description 12
- 239000007800 oxidant agent Substances 0.000 claims description 12
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 11
- 230000001590 oxidative effect Effects 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- 229910052733 gallium Inorganic materials 0.000 claims description 8
- 229910052732 germanium Inorganic materials 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 229910052701 rubidium Inorganic materials 0.000 claims description 5
- 229910052706 scandium Inorganic materials 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910052792 caesium Inorganic materials 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- 239000011572 manganese Substances 0.000 description 58
- 239000000203 mixture Substances 0.000 description 45
- 239000000243 solution Substances 0.000 description 30
- 239000000047 product Substances 0.000 description 27
- 229910052791 calcium Inorganic materials 0.000 description 20
- 229910052712 strontium Inorganic materials 0.000 description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 18
- 238000001816 cooling Methods 0.000 description 17
- 238000009826 distribution Methods 0.000 description 17
- 229910052788 barium Inorganic materials 0.000 description 16
- 239000008393 encapsulating agent Substances 0.000 description 15
- 239000004065 semiconductor Substances 0.000 description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 239000012527 feed solution Substances 0.000 description 12
- 239000012298 atmosphere Substances 0.000 description 11
- 150000001875 compounds Chemical class 0.000 description 11
- 229920000642 polymer Polymers 0.000 description 11
- 229920001296 polysiloxane Polymers 0.000 description 11
- 239000000843 powder Substances 0.000 description 11
- 239000002904 solvent Substances 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 230000005855 radiation Effects 0.000 description 8
- 239000012047 saturated solution Substances 0.000 description 8
- 238000010923 batch production Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 239000002223 garnet Substances 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 6
- 239000003085 diluting agent Substances 0.000 description 5
- 230000005284 excitation Effects 0.000 description 5
- -1 fluoride ions Chemical class 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- 229910052748 manganese Inorganic materials 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 229910052765 Lutetium Inorganic materials 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 229910003564 SiAlON Inorganic materials 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- LMBFAGIMSUYTBN-MPZNNTNKSA-N teixobactin Chemical compound C([C@H](C(=O)N[C@@H]([C@@H](C)CC)C(=O)N[C@@H](CO)C(=O)N[C@H](CCC(N)=O)C(=O)N[C@H]([C@@H](C)CC)C(=O)N[C@@H]([C@@H](C)CC)C(=O)N[C@@H](CO)C(=O)N[C@H]1C(N[C@@H](C)C(=O)N[C@@H](C[C@@H]2NC(=N)NC2)C(=O)N[C@H](C(=O)O[C@H]1C)[C@@H](C)CC)=O)NC)C1=CC=CC=C1 LMBFAGIMSUYTBN-MPZNNTNKSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- MCSXGCZMEPXKIW-UHFFFAOYSA-N 3-hydroxy-4-[(4-methyl-2-nitrophenyl)diazenyl]-N-(3-nitrophenyl)naphthalene-2-carboxamide Chemical compound Cc1ccc(N=Nc2c(O)c(cc3ccccc23)C(=O)Nc2cccc(c2)[N+]([O-])=O)c(c1)[N+]([O-])=O MCSXGCZMEPXKIW-UHFFFAOYSA-N 0.000 description 2
- 229910016569 AlF 3 Inorganic materials 0.000 description 2
- 102100032047 Alsin Human genes 0.000 description 2
- 101710187109 Alsin Proteins 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910004261 CaF 2 Inorganic materials 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 239000001045 blue dye Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 150000002222 fluorine compounds Chemical class 0.000 description 2
- 239000001046 green dye Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000001044 red dye Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 2
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 229910015999 BaAl Inorganic materials 0.000 description 1
- 101100042630 Caenorhabditis elegans sin-3 gene Proteins 0.000 description 1
- 229910004573 CdF 2 Inorganic materials 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910020313 ClF Inorganic materials 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 229910005793 GeO 2 Inorganic materials 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 229910017639 MgSi Inorganic materials 0.000 description 1
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 1
- 229910017855 NH 4 F Inorganic materials 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229920000291 Poly(9,9-dioctylfluorene) Polymers 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910018287 SbF 5 Inorganic materials 0.000 description 1
- 229910008449 SnF 2 Inorganic materials 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002591 computed tomography Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000005112 continuous flow technique Methods 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- MILUBEOXRNEUHS-UHFFFAOYSA-N iridium(3+) Chemical compound [Ir+3] MILUBEOXRNEUHS-UHFFFAOYSA-N 0.000 description 1
- NKVDKFWRVDHWGC-UHFFFAOYSA-N iridium(3+);1-phenylisoquinoline Chemical compound [Ir+3].C1=CC=CC=C1C1=NC=CC2=CC=CC=C12.C1=CC=CC=C1C1=NC=CC2=CC=CC=C12.C1=CC=CC=C1C1=NC=CC2=CC=CC=C12 NKVDKFWRVDHWGC-UHFFFAOYSA-N 0.000 description 1
- UEEXRMUCXBPYOV-UHFFFAOYSA-N iridium;2-phenylpyridine Chemical compound [Ir].C1=CC=CC=C1C1=CC=CC=N1.C1=CC=CC=C1C1=CC=CC=N1.C1=CC=CC=C1C1=CC=CC=N1 UEEXRMUCXBPYOV-UHFFFAOYSA-N 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000009828 non-uniform distribution Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920003227 poly(N-vinyl carbazole) Polymers 0.000 description 1
- 229920001643 poly(ether ketone) Polymers 0.000 description 1
- 229920000553 poly(phenylenevinylene) Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920002098 polyfluorene Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000013074 reference sample Substances 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000001721 transfer moulding Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
Classifications
-
- 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
- C09K11/61—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing fluorine, chlorine, bromine, iodine or unspecified halogen elements
- C09K11/617—Silicates
-
- 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
- C09K11/61—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing fluorine, chlorine, bromine, iodine or unspecified halogen elements
- C09K11/615—Halogenides
- C09K11/616—Halogenides with alkali or alkaline earth metals
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
- Led Device Packages (AREA)
Description
式中、
AはLi、Na、K、Rb、Cs又はこれらの組合せであり、
MはSi、Ge、Sn、Ti、Zr、Al、Ga、In、Sc、Y、La、Nb、Ta、Bi、Gd又はこれらの組合せであり、
xは[MFy]イオンの電荷の絶対値であり、
yは5、6又は7である。
式中、
A1はH、Li、Na、K、Rb、Cs又はそれらの組合せであり、
MはSi、Ge、Sn、Ti、Zr、Al、Ga、In、Sc、Y、La、Nb、Ta、Bi、Gd又はそれらの組合せであり
xは[MFy]イオンの電荷の絶対値であり、
yは5、6又は7である。
D50は体積分布でのメジアン粒径であり、
D90は、体積分布で分布粒子の90%の粒径よりも大きい粒径であり、
D10は、体積分布で分布粒子の10%の粒径よりも大きい粒径である。
((Sr1-z(Ca,Ba,Mg,Zn)z)1-(x+w)(Li,Na,K,Rb)wCex)3(Al1-ySiy)O4+y+3(x-w)F1-y-3(x-w)(0<x≦0.10,0≦y≦0.5,0≦z≦0.5,0≦w≦x);
(Ca,Ce)3Sc2Si3O12(CaSiG);
(Sr,Ca,Ba)3Al1-xSixO4+xF1-x:Ce3+(SASOF));
(Ba,Sr,Ca)5(PO4)3(Cl,F,Br,OH):Eu2+,Mn2+;(Ba,Sr,Ca)BPO5:Eu2+,Mn2+;(Sr,Ca)10(PO4)6*νB2O3:Eu2+(0<ν≦1);Sr2Si3O8*2SrCl2:Eu2+;(Ca,Sr,Ba)3MgSi2O8:Eu2+,Mn2+;BaAl8O13:Eu2+;2SrO*0.84P2O5*0.16B2O3:Eu2+;(Ba,Sr,Ca)MgAl10O17:Eu2+,Mn2+;(Ba,Sr,Ca)Al2O4:Eu2+;(Y,Gd,Lu,Sc,La)BO3:Ce3+,Tb3+;ZnS:Cu+,Cl-;ZnS:Cu+,Al3+;ZnS:Ag+,Cl-;ZnS:Ag+,Al3+;(Ba,Sr,Ca)2Si1-ξO4-2ξ:Eu2+(−0.2≦ξ≦0.2);(Ba,Sr,Ca)2(Mg,Zn)Si2O7:Eu2+;(Sr,Ca,Ba)(Al,Ga,In)2S4:Eu2+;(Y,Gd,Tb,La,Sm,Pr,Lu)3(Al,Ga)5-αO12-3/2α:Ce3+(0≦α≦0.5);
(Y,Gd,Lu,Tb)3(Al,Ga)5O12:Ce3+;(Ca,Sr)8(Mg,Zn)(SiO4)4Cl2:Eu2+,Mn2+;Na2Gd2B2O7:Ce3+,Tb3+;(Sr,Ca,Ba,Mg,Zn)2P2O7:Eu2+,Mn2+;(Gd,Y,Lu,La)2O3:Eu3+,Bi3+;(Gd,Y,Lu,La)2O2S:Eu3+,Bi3+;(Gd,Y,Lu,La)VO4:Eu3+,Bi3+;(Ca,Sr)S:Eu2+,Ce3+;SrY2S4:Eu2+;CaLa2S4:Ce3+;(Ba,Sr,Ca)MgP2O7:Eu2+,Mn2+;(Y,Lu)2WO6:Eu3+,Mo6+;(Ba,Sr,Ca)βSiγNμ:Eu2+(2β+4γ=3μ);
(Ba,Sr,Ca)2Si5-xAlxN8-xOx:Eu2+(0≦x≦2);Ca3(SiO4)Cl2:Eu2+;
(Lu,Sc,Y,Tb)2-u-vCevCa1+uLiwMg2-wPw(Si,Ge)3-wO12-u/2(−0.5≦u≦1,0<v≦0.1,0≦w≦0.2);(Y,Lu,Gd)2-φCaφSi4N6+φC1-φ:Ce3+(0≦φ≦0.5);
Eu2+及び/又はCe3+をドープしたα−SiAlON;(Ca,Sr,Ba)SiO2N2:Eu2+,Ce3+;
β−SiAlON:Eu2+,3.5MgO*0.5MgF2*GeO2:Mn4+;(Sr,Ca,Ba,Mg)AlSiN3:Eu2+;
(Sr,Ca,Ba)3SiO5:Eu2+;Ca1-c-fCecEufAl1+cSi1-cN3(0≦c≦0.2,0≦f≦0.2);
Ca1-h-rCehEurAl1-h(Mg,Zn)hSiN3(0≦h≦0.2,0≦r≦0.2);
Ca1-2s-tCes(Li,Na)sEutAlSiN3(0≦s≦0.2,0≦f≦0.2,s+t>0);及び
Ca1-σ-χ-φCeσ(Li,Na)χEuφAl1+σ-χSi1-σ+χN3(0≦σ≦0.2,0≦χ≦0.4,0≦φ≦0.2)。
ビーカーA〜C間の原料の量及び配分を表1に示す。ビーカーAを積極的に撹拌し、ビーカーBの内容物を約5分間かけてそこに滴下した。ビーカーBの内容物の約1分後に、ビーカーCの内容物のビーカーAへの滴下を開始し、約4分間にわたって続けた。沈殿物を5分間温浸し、撹拌を停止した。上清をデカントし、沈殿物を減圧濾過し、酢酸で1回、アセトンで2回すすぎ、次いで真空下で乾燥させた。乾燥粉末を170メッシュの篩に通して篩い分けし、20%F2/80%窒素雰囲気下で、540℃で8時間アニールした。アニールした蛍光体を、K2SiF6で飽和した49%HFの溶液で洗浄し、真空下で乾燥させ、170メッシュの篩に通して篩い分けした。
手順
反応容器として使用した2000mlの分液漏斗を約300RPMの速度で撹拌した。3つの蠕動ポンプを使用して、すべての流量に対して厳密な制御を維持した。流量は、溶液A及び溶液Bについては15〜40mL/分、溶液3については30〜100mL/分の間に設定した。実施例1〜6の溶液A〜Cの間の原料の量及び配分を表2に示す。
Claims (6)
- 次の式IのMn+4ドープ蛍光体の調製方法であって、
Ax[MFy]:Mn+4 I
(式中、
AはLi、Na、K、Rb、Cs又はそれらの組合せであり、
Mは、Si、Ge、Sn、Ti、Zr、Al、Ga、In、Sc、Y、La、Nb、Ta、Bi、Gd又はそれらの組合せであり、
xは[MFy]イオンの電荷の絶対値であり、
yは5、6又は7である。)
Mの原料及びHFを含む第1の溶液並びにMnの原料を含む第2の溶液を、Aの原料の存
在下で反応器に徐々に添加して、Mn+4ドープ蛍光体を含む液体生成物を形成するステッ
プと、
反応器から液体生成物を排出するステップであって、液体生成物を反応器から排出する際の反応器内の液体生成物の体積の変動が50%未満であるステップと、
さらに、
Mn +4 ドープ蛍光体を液体生成物から単離するステップと、
Mn +4 ドープ蛍光体を昇温下でガス状のフッ素含有酸化剤と接触させ、式Iの色安定Mn 4+ ドープ蛍光体を形成するステップと、
を含む方法。 - Aの原料を含む第3の溶液を反応器に徐々に添加するステップをさらに含む、請求項1に記載の方法。
- 液体生成物を排出することなく第1及び第2の溶液を反応器に徐々に添加する初期期間をさらに含む、請求項1に記載の方法。
- HF、Aの原料、Mn+4ドープ蛍光体の予備形成粒子又はそれらの組合せから選択された材料を反応器に予め仕込むステップをさらに含む、請求項1に記載の方法。
- 液体生成物を反応器から排出する際の反応器内の液体生成物の体積の変動が10%未満
である、請求項1に記載の方法。 - フッ素含有酸化剤がF2である、請求項1に記載の方法。
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