JP2017501268A - 色安定性マンガンドープ複合フッ化物蛍光体の製造方法 - Google Patents
色安定性マンガンドープ複合フッ化物蛍光体の製造方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 25
- XPIIDKFHGDPTIY-UHFFFAOYSA-N F.F.F.P Chemical compound F.F.F.P XPIIDKFHGDPTIY-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 56
- 150000001875 compounds Chemical class 0.000 claims abstract description 28
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 15
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 150000002500 ions Chemical class 0.000 claims abstract description 12
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 9
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 7
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 7
- 150000001450 anions Chemical group 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 6
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 4
- 229910052738 indium Inorganic materials 0.000 claims abstract description 4
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 4
- 229910052701 rubidium Inorganic materials 0.000 claims abstract description 4
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 4
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 3
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 3
- 229910052718 tin Inorganic materials 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 40
- 230000001376 precipitating effect Effects 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 61
- 239000011572 manganese Substances 0.000 description 33
- 239000000463 material Substances 0.000 description 26
- 229910052791 calcium Inorganic materials 0.000 description 25
- 239000000203 mixture Substances 0.000 description 25
- 229910052712 strontium Inorganic materials 0.000 description 23
- 229910052788 barium Inorganic materials 0.000 description 15
- 239000008393 encapsulating agent Substances 0.000 description 14
- 238000003756 stirring Methods 0.000 description 14
- 239000012190 activator Substances 0.000 description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 239000004065 semiconductor Substances 0.000 description 12
- 239000002245 particle Substances 0.000 description 11
- 230000005855 radiation Effects 0.000 description 11
- 229920001296 polysiloxane Polymers 0.000 description 10
- 229920000642 polymer Polymers 0.000 description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- -1 fluoride ions Chemical class 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000003085 diluting agent Substances 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- 229910052684 Cerium Inorganic materials 0.000 description 4
- 239000004809 Teflon Substances 0.000 description 4
- 229920006362 Teflon® Polymers 0.000 description 4
- 229910052771 Terbium Inorganic materials 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 229910052746 lanthanum Inorganic materials 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 239000012047 saturated solution Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 102100032047 Alsin Human genes 0.000 description 3
- 101710187109 Alsin Proteins 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
- 229910052772 Samarium Inorganic materials 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
- 239000002019 doping agent Substances 0.000 description 3
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- 229910052731 fluorine Inorganic materials 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
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- 239000006228 supernatant Substances 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
- 229910004261 CaF 2 Inorganic materials 0.000 description 2
- 239000004743 Polypropylene Substances 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
- 238000010521 absorption reaction Methods 0.000 description 2
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- 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
- 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
- 239000004677 Nylon Substances 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229910004298 SiO 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
- OJOWXSLGSMTXEO-UHFFFAOYSA-H [Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[K+].[K+].[K+].[K+].[K+].[K+] Chemical compound [Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[Mn](=O)(=O)([O-])F.[K+].[K+].[K+].[K+].[K+].[K+] OJOWXSLGSMTXEO-UHFFFAOYSA-H 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 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
- 238000011109 contamination Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 150000008040 ionic compounds Chemical group 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
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- 229920001643 poly(ether ketone) Polymers 0.000 description 1
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- 230000000171 quenching effect Effects 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000004448 titration Methods 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
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- 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
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- H01L33/50—Wavelength conversion elements
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Abstract
Description
Ax(M(1-m),Mnm)Fy (I)
(1−m)部の式HxMFyの化合物を含む第1のHF水溶液を、m×n部の式Ax[MnFy]の化合物を含む第2のHF水溶液を、(1−n)部の式Ax[MnFy]の化合物及び式AaXの化合物を含む第3のHF水溶液と接触させて、色安定性Mn4+ドープ複合フッ化物蛍光体を含む沈殿を生じさせる工程を含む方法に関する。
式中、
Aは、Li、Na、K、Rb、Cs、NR4又はこれらの組合せであり、
Mは、Si、Ge、Sn、Ti、Zr、Al、Ga、In、Sc、Hf、Y、La、Nb、Ta、Bi、Gd又はこれらの組合せであり、
Rは、H、低級アルキル又はそれらの組合せであり、
Xはアニオンであり、
aはXアニオンの電荷の絶対値であり、
xは[MFy]イオンの電荷の絶対値であり、
yは5、6又は7であり、
0<m≦0.08であり、
0.1≦n≦1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+((Ca,Sr,Ce)3(Al,Si)(O,F)5(SASOF))、
(Ba,Sr,Ca)5(PO4)3(Cl,F,Br,OH):Eu2+,Mn2+、(Ba,Sr,Ca)BPO5:Eu2+,Mn2+、(Sr,Ca)10(PO4)6・vB2O3:Eu2+(式中、0<v≦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+(式中、0≦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+(式中、0≦α≦0.5)、(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+(式中、2β+4γ=3μ)、Ca3(SiO4)Cl2:Eu2+、(Lu,Sc,Y,Tb)2-u-vCevCa1+uLiwMg2-wPw(Si,Ge)3-wO12-u/2(式中、−0.5≦u≦1、0<v≦0.1、及び0≦w≦0.2)、(Y,Lu,Gd)2-φCaφSi4N6+φC1-φ:Ce3+,(式中、0≦φ≦0.5)、(Lu,Ca,Li,Mg,Y),Eu2+及び/又はCe3+ドープα−SiAlON、β−SiAlON:Eu2+、(Ca,Sr,)AlSiN3:Eu2+(Ca,Sr,Ba)SiO2N2:Eu2+,Ce3+、3.5MgO・0.5MgF2・GeO2:Mn4+、Ca1-c-fCecEufAl1+cSi1-cN3,(式中、0≦c≦0.2、0≦f≦0.2)、Ca1-h-rCehEurAl1-h(Mg,Zn)hSiN3,(式中、0≦h≦0.2、0≦r≦0.2)、Ca1-2s-tCes(Li,Na)sEutAlSiN3,(式中、0≦s≦0.2、0≦f≦0.2、s+t>0)、Ca1-σ-χ-φCeσ(Li,Na)χEuφAl1+σ-χSi1-σ+χN3,(式中、0≦σ≦0.2、0≦χ≦0.4、0≦φ≦0.2)。
(Ca,Ce)3Sc2Si3O12(CaSiG)、
(Sr,Ca,Ba)3Al1-xSixO4+xF1-x:Ce3+((Ca,Sr,Ce)3(Al,Si)(O,F)5(SASOF))、
(Ba,Sr,Ca)2Si1-ξO4-2ξ:Eu2+(式中、0≦ξ≦0.2)、
(Y,Gd,Tb,La,Sm,Pr,Lu)3(Al,Ga)5-αO12-3/2α:Ce3+(式中、0≦α≦0.5)、
(Ba,Sr,Ca)βSiγNμ:Eu2+(式中、2β+4γ=3μ)、(Y,Lu,Gd)2-φCaφSi4N6+φC1-φ:Ce3+,(式中、0≦φ≦0.5)、β−SiAlON:Eu2+、及び(Ca,Sr,)AlSiN3:Eu2+。
K2MnF6は、KMnO4、KF、H2O2、及びHF水溶液からBode(Angew.Chem.65(11):304)に基づく1工程の1ポット方法によって合成された:
2KMnO4+KF+10HF+3H2O2→2K2MnF6↓+8H2O+3O2
Teflonコーティングされた磁性撹拌棒を備えた4Lのポリエチレンビーカーに、50%HF水溶液(1L)を充填し、氷浴で冷却した。次いでKF(240g、4.13mol)及び微粉末化KMnO4(15g、94.9mmol)を添加し、混合物を15分間激しく撹拌した。撹拌を停止し、未溶解材料を沈降させた。上清溶液を第2のビーカーにデカントして、後続の滴定工程において終点認識を困難にし得る未溶解KMnO4の不存在を確実にした。冷暗紫色溶液に、30%の水性H2O2を点眼器で徐々に添加した。各5〜10滴の添加の後、さらなる添加は、O2の発生が終わるまで停止される。約20mLのH2O2の添加後、終点に近づきつつあった。褐色がかった金色沈殿が形成したが、終点は、撹拌を停止し、上清溶液の色を観察することによって、判断できる。反応は、溶液の色が紫色から中位の赤味がかった褐色に変化したときに完了したと判断された。山吹色のK2MnF6沈殿を、Teflon濾紙を有するプラスチックブフナー漏斗を用いて回収した。沈殿は、冷アセトン(各10mL)で2回洗浄し、ポンプで吸引して乾燥させ、18.44g(78.6%、KMnO4に基づく)の黄色K2MnF6を得た。
HF中の飽和又はほぼ飽和のK2MnF6溶液を、20.3gのK2MnF6及び282mLの48重量%のHFを用いて調製し、生成物を真空濾過した。41mLの48%HF中に溶解した40.6gのKFの処理溶液も調製した。KF溶液を、撹拌しながらK2MnF6溶液に滴下し、沈殿を形成した。上清を捨て、次いで真空フィルタスラリーを真空濾過し、冷アセトンで4回洗浄して、真空デシケーター中で乾燥した。
70%HF中のK2MnF6の飽和又はほぼ飽和溶液を、40mlの70重量%HF中の10グラムのK2MnF6を用いて調製した。10mlの48%HF中に溶解した10gのKHF2の処理溶液も調製した。KHF2溶液を撹拌しながらK2MnF6溶液に添加した。得られたスラリーを真空濾過し、アセトンで4回覆い、K2MnF6生成物を真空デシケーター中で乾燥した。
合成されたままの蛍光体及び実施例2の蛍光体サンプル中のAl、Ca、Cr、Cu、Fe、Na、Ni及びZrのレベルを決定した。結果を表1に示す。汚染物質のレベルは、精製プロセスによって顕著に低減された。
一般的手順
蛍光体調製
フルオロケイ酸、H2SiF6、及びHFを撹拌しながら混合して、第1の溶液を形成した。K+の供給源を含有するフッ化水素酸溶液は、フッ化水素酸をKF又はKHF2及びカリウムヘキサフルオロマンガネート(PFM)、K2MnF6を含有するビーカーに、固体を溶解するために撹拌しながら注ぐことによって調製される。これを受容液と呼ぶ。HF水溶液及びK2MnF6を含有する第3の溶液を調製する。これをPFM溶液と呼ぶ。フルオロケイ酸及びPFM溶液を、撹拌しながら受容液に、別々に、約10分間にわたって徐々に添加する。フルオロケイ酸溶液の添加は、PFM添加の前に、通常1〜2分早く始める。添加が完了した後、懸濁液を数分撹拌し、次いで撹拌を停止して、蛍光体を沈降させ、上清をデカントする。
48%のフッ化水素酸中のKHF2の溶液は、65mLの48%フッ化水素酸を、8.1グラムのKHF2を含有するビーカー(ビーカーA)に注ぐことによって調製した。次いでK2MnF6(0.219g、0.00089mol)を、固体を溶解するために撹拌しながら溶液に添加した。H2SiF6(15mlの35%のH2SiF6、0.036mol)及び60mlの48%HFを第2のビーカー(ビーカーB)に注ぎ、撹拌した。HF(21mLの48%HF)をK2MnF6(0.219g、0.00089mol)を含有する第3のビーカー(ビーカーC)に注ぎ、固体を溶解するために撹拌した。ビーカーAを撹拌する間、ビーカーB及びCの内容物を約7分間かけて滴下した。添加が完了した後、懸濁液をさらに5分間撹拌し、次いで撹拌を停止して、蛍光体を沈降させ、上清をデカントした。処理溶液(80mL)をビーカーに添加し、生成物を15分間撹拌した。撹拌を停止し、蛍光体を沈降させ、処理溶液をデカントした。蛍光体を真空濾過し、アセトンで3回すすぎ、真空下で乾燥させ、選別し、MnドープされたK2SiF6を得た。
Claims (14)
- 式Iの色安定性Mn4+ドープ複合フッ化物蛍光体の製造方法であって、
Ax(M(1-m),Mnm)Fy (I)
(1−m)部の式HxMFyの化合物を含む第1のHF水溶液及びm×n部の式Ax[MnFy]の化合物を含む第2のHF水溶液を、(1−n)部の式Ax[MnFy]の化合物及び式AaXの化合物を含む第3のHF水溶液と接触させて、色安定性Mn4+ドープ複合フッ化物蛍光体を含む沈殿を生じさせる工程を含む方法。
式中、
AはLi、Na、K、Rb、Cs、NR4又はこれらの組合せであり、
MはSi、Ge、Sn、Ti、Zr、Al、Ga、In、Sc、Hf、Y、La、Nb、Ta、Bi、Gd又はこれらの組合せであり、
RはH、低級アルキル又はそれらの組合せであり、
Xはアニオンであり、
aはXアニオンの電荷の絶対値であり、
xは[MFy]イオンの電荷の絶対値であり、
yは5、6又は7であり、
0<m≦0.05であり、
0.1≦n≦1である。 - nが0.25〜0.95である、請求項1に記載の方法。
- nが0.5〜0.9である、請求項1に記載の方法。
- nが0.6〜0.8である、請求項1に記載の方法。
- nが約0.7である、請求項1に記載の方法。
- 式IのMn4+ドープ複合フッ化物がK2(Si(1-m),Mnm)F6である、請求項1に記載の方法。
- 式AaXの塩がKF、KHF2及びこれらの組合せから選択される、請求項1に記載の方法。
- 第1及び第2のHF水溶液を、第3の溶液に徐々に添加される、請求項1に記載の方法。
- 接触させる工程の前に、式AxMnFyの化合物を濃HF水溶液から沈澱させ、沈殿を単離する工程をさらに含む、請求項1に記載の方法。
- 請求項1に記載の方法で製造された複合フッ化物を含むLED照明装置(10)。
- LEDチップ(12)と、
LEDチップ(12)の表面に配設された請求項1に記載の方法で製造された複合フッ化物と
を備えるLED照明装置(10)。 - 式K2(Si(1-m),Mnm)F6の色安定性Mn4+ドープ複合フッ化物蛍光体の製造方法であって、
(1−m)部の式H2SiF6の化合物を含む第1のHF水溶液及びm×n部の式K2MnF6の化合物を含む第2のHF水溶液を、(1−n)部の式K2MnF6の化合物とKF、KHF2及びそれらの組合せから選択される化合物とを含む第3のHF水溶液と接触させて、色安定性Mn4+ドープ複合フッ化物を含む沈殿を生じさせる工程
を含む方法。
式中、0<m≦0.08、0.1≦n≦1である。 - nが0.6〜0.8である、請求項1に記載の方法。
- 段階的添加工程の前に、式K2(Si(1-m),Mnm)F6の化合物を濃HF水溶液から沈澱させ、沈殿を単離する工程をさらに含む、請求項1に記載の方法。
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TWI633171B (zh) | 2018-08-21 |
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CN105793389A (zh) | 2016-07-20 |
US9388336B2 (en) | 2016-07-12 |
AU2014362239A1 (en) | 2016-06-16 |
EP3080230B1 (en) | 2018-07-04 |
WO2015089345A1 (en) | 2015-06-18 |
MY183192A (en) | 2021-02-18 |
TW201529801A (zh) | 2015-08-01 |
CN105793389B (zh) | 2018-12-04 |
JP6595998B2 (ja) | 2019-10-23 |
KR102434076B1 (ko) | 2022-08-19 |
US20150166887A1 (en) | 2015-06-18 |
MX2016007678A (es) | 2016-10-14 |
KR20160096709A (ko) | 2016-08-16 |
AU2014362239B2 (en) | 2018-06-07 |
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