JP5899304B2 - 色安定マンガンドープ蛍光体 - Google Patents
色安定マンガンドープ蛍光体 Download PDFInfo
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims description 128
- 239000000203 mixture Substances 0.000 claims description 37
- 239000000243 solution Substances 0.000 claims description 30
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 22
- 150000001875 compounds Chemical class 0.000 claims description 12
- 150000002500 ions Chemical class 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 229910052727 yttrium Inorganic materials 0.000 claims description 11
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 229910052732 germanium Inorganic materials 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229910052733 gallium Inorganic materials 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 229910052706 scandium Inorganic materials 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 229910052792 caesium Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 229910052701 rubidium Inorganic materials 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- FVIZARNDLVOMSU-UHFFFAOYSA-N ginsenoside K Natural products C1CC(C2(CCC3C(C)(C)C(O)CCC3(C)C2CC2O)C)(C)C2C1C(C)(CCC=C(C)C)OC1OC(CO)C(O)C(O)C1O FVIZARNDLVOMSU-UHFFFAOYSA-N 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- 239000011572 manganese Substances 0.000 description 55
- 239000000463 material Substances 0.000 description 24
- 239000004065 semiconductor Substances 0.000 description 14
- 239000008393 encapsulating agent Substances 0.000 description 12
- 230000005855 radiation Effects 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- 229910052748 manganese Inorganic materials 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 238000005286 illumination Methods 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 239000012047 saturated solution Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 229910052765 Lutetium Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000875 corresponding effect Effects 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 239000002861 polymer material Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 238000000790 scattering method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 102100032047 Alsin Human genes 0.000 description 1
- 101710187109 Alsin Proteins 0.000 description 1
- 229910015999 BaAl Inorganic materials 0.000 description 1
- 101100042630 Caenorhabditis elegans sin-3 gene Proteins 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- 229910005793 GeO 2 Inorganic materials 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 229910017639 MgSi Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910003564 SiAlON Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910000756 V alloy Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- FNCIDSNKNZQJTJ-UHFFFAOYSA-N alumane;terbium Chemical compound [AlH3].[Tb] FNCIDSNKNZQJTJ-UHFFFAOYSA-N 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- IPJKJLXEVHOKSE-UHFFFAOYSA-L manganese dihydroxide Chemical compound [OH-].[OH-].[Mn+2] IPJKJLXEVHOKSE-UHFFFAOYSA-L 0.000 description 1
- -1 nitride compound Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- XTUSEBKMEQERQV-UHFFFAOYSA-N propan-2-ol;hydrate Chemical compound O.CC(C)O XTUSEBKMEQERQV-UHFFFAOYSA-N 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000001721 transfer moulding Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- 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
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- 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
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- 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
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/42—Wire connectors; Manufacturing methods related thereto
- H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
- H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
- H01L2224/4805—Shape
- H01L2224/4809—Loop shape
- H01L2224/48091—Arched
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/42—Wire connectors; Manufacturing methods related thereto
- H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
- H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
- H01L2224/481—Disposition
- H01L2224/48151—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
- H01L2224/48221—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
- H01L2224/48245—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic
- H01L2224/48247—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic connecting the wire to a bond pad of the item
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L2924/15—Details of package parts other than the semiconductor or other solid state devices to be connected
- H01L2924/181—Encapsulation
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- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
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- H01L33/502—Wavelength conversion materials
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- 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
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Description
Ax[MFy]:Mn+4 I
粒子状の前記蛍光体を、式IIの組成物のフッ化水素酸飽和水溶液と接触させる段階とを含む。
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、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。
Ax[MnFy] IV
この溶液を、過剰A+イオンを含有する第2のフッ化水素酸水溶液と合わせる。用語「過剰A+イオン」は、化学量論量を超えるA+イオン、言い換えると、蛍光体の100%収率のために必要なA+イオン量を超えるA+イオンを意味する。一部の実施形態では、500%も過剰に使用するが、さらに多くの量又はより少ない量を使用することもできる。A+イオンが高濃度であると、式IIのホスト材料の形成と、蛍光体の沈殿とが同時に生じる。過剰A+イオンが「共通イオン効果」によって溶解性を抑制するため、両方の塩が過飽和となる。特定の実施形態では、AはK、Na又はこれらの組合せである。一部の実施形態では、式IIIの化合物は(NR4)2[MF6]であり、式IVの化合物はA2[MnF6]である。より具体的には、AはKであり、Mn+4ドープ蛍光体はK2SiF6:Mn+4であり、式IIIの化合物は(NH4)2SiF6であり、式IVの化合物はK2MnF6である。
50〜75wt%の蛍光体を充填してある二液型シリコーン(RTV615、Momentive社)に粉末を取り込む。これらシリコーン/粉末複合材料をその後、小さな窪みをもつAlプラークホルダへと注ぎ、450nm励起下における発光及び反射(BaSO4標準に対する)を試料毎に測定する。プラークの一部を、対照試料として確保し乾燥窒素下で保存する。その他のプラークを相対湿度約80%において約80℃で熟成させ、一定時間後、露光及び対照プラークの強度のスペクトルを再測定する。熟成前後のQEの比較が、その試料の劣化の一指標である。
水(21ml)にフッ化水素酸(49wt%、79ml)を添加して40%HF水溶液を形成し、その後このHF溶液にK2SiF6(10g、0.454モル)を添加した。この溶液を約70〜80℃まで加熱し、K2MnF6(1g、0.0040モル)を添加し、溶解するまで撹拌した。−20℃の半凍結40体積%イソプロパノール−水溶液、又は−48℃用半凍結58体積%エチレングリコール水溶液から構成される冷浴に溶液を移動させた。HFフッ化水素酸溶液が冷たくなった後、プラスチックビーカーの上のプラスチック漏斗内の中間多孔性のろ紙を通してHF蛍光体スラリーをろ過し、アセトンで洗浄し、空気乾燥させた。このPFS蛍光体をアルゴン雰囲気下で保存した。
出発材料K2SiF6及びK2MnF6(8モル%)を、プラスチック容器内で約70℃の70%HFに溶解させる。この溶液を撹拌しながら70℃で一定に保持する一方、溶媒を蒸発させることで、公称上8モル%のMnを含有するMn+4ドープPFS蛍光体の結晶化が生じる。溶媒除去後、粉末をアセトンで洗浄して残留HFがあれば除去し、その後真空ろ過し、乾燥させた。
49%水性HF(100ml)中(NH4)2SiF6(11.1g、0.454モル)及びK2MnF6(1g、0.00395モル、8モル%)の第1の溶液を、室温で調製した。49%HF(50ml)中にKF(20g)を含有する第2の溶液を、約0℃まで冷却した。第2の溶液に第1の溶液を撹拌しながら注ぎ、Mn+4ドープPFS蛍光体を沈殿させた。沈殿をアセトンで洗浄して残留HFがあれば除去し、その後真空ろ過し、乾燥させた。収量:12.5gK2[SiF6]:Mn4+(85%)。
それ以上溶解させることができなくなるまで(室温で約1.75g)40%HF100mLにK2SiF6を添加することによって、40%HF中K2SiF6の飽和溶液を調製した。その後、飽和溶液に実施例3からの蛍光体粉末を添加した。得られたスラリーを、約15分間撹拌しながら室温で保持した。処理した蛍光体を沈殿させ、40%HFをデカンテーションした。乾燥アセトンで洗浄することによって、残留HFを除去した。その後、処理した蛍光体を真空ろ過し、乾燥させた。
実施例3及び4の蛍光体に、記載のHHTH試験手順を施した。約48時間後、実施例2の未処理蛍光体は劣化したが、実施例4の処理した蛍光体は劣化を示さなかった。処理した試料のQEは、未処理試料のQEよりも初期で約15〜20%高かった。加えて、未処理PFSの体色はより橙色に見え、可視領域における吸収が減少した。HHTH処理後、未処理蛍光体のQEは初期値の約31〜33%であったが、処理した材料については、HHTH後のQEが初期値の約95%であった。結果を表1に示す。
Claims (12)
- 色安定Mn+4ドープ蛍光体の製造方法であって、
次の式IのMn+4ドープ蛍光体を準備する段階と、
Ax[MFy]:Mn+4 I
粒子状の前記蛍光体を、次の式IIの組成物のフッ化水素酸飽和水溶液と接触させる段階と
を含む方法。
Ax[MFy] II
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、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。 - MがSi、Ge、Sn、Ti、Zr又はこれらの組合せである、請求項1記載の方法。
- Mn+4ドープ蛍光体がK2SiF6:Mn+4であり、式IIの組成物がK2SiF6である、請求項1又は請求項2記載の方法。
- 前記接触段階が20℃〜50℃の温度で実施される、請求項1乃至請求項3のいずれか1項記載の方法。
- 前記接触段階が1分〜5時間実施される、請求項1乃至請求項4のいずれか1項記載の方法。
- 前記時間が5分〜1時間の範囲である、請求項5記載の方法。
- Mn+4ドープ蛍光体を準備する段階が、
60℃を超える温度で式Iの蛍光体のフッ化水素酸水溶液を準備する段階と、
溶液を30℃未満の温度まで冷却して溶液から蛍光体を粒子状に沈殿させる段階と
を含む、請求項1乃至請求項6のいずれか1項記載の方法。 - Mn+4ドープ蛍光体を準備する段階が、
式Iの蛍光体及び水性フッ化水素酸を含む溶液を準備する段階と、
溶液の溶媒を蒸発させながら、25℃〜120℃の温度で溶液を維持して溶液から蛍光体を粒子状に沈殿させる段階と
を含む、請求項1乃至請求項6のいずれか1項記載の方法。 - Mn+4ドープ蛍光体を準備する段階が、
以下の式IIIの化合物及び式IVの化合物を含む第1のフッ化水素酸水溶液を準備する段階と、
(NR4)x[MFy] III
Ax[MnFy] IV
第1の溶液を、過剰A+イオンを含む第2のフッ化水素酸水溶液と混合して、混合溶液からMn+4ドープ蛍光体を粒子状に沈殿させる段階と
を含む、請求項1乃至請求項6のいずれか1項記載の方法。 - AがK、Na又はこれらの組合せである、請求項9記載の方法。
- 式IIIの化合物が(NR4)2[MF6]であり、式IVの化合物がA2[MnF6]である、請求項9記載の方法。
- 式IIIの化合物が(NH4)2SiF6であり、式IVの化合物がK2MnF6である、請求項9記載の方法。
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