JP5912121B2 - Mn賦活蛍光物質 - Google Patents
Mn賦活蛍光物質 Download PDFInfo
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- JP5912121B2 JP5912121B2 JP2013532060A JP2013532060A JP5912121B2 JP 5912121 B2 JP5912121 B2 JP 5912121B2 JP 2013532060 A JP2013532060 A JP 2013532060A JP 2013532060 A JP2013532060 A JP 2013532060A JP 5912121 B2 JP5912121 B2 JP 5912121B2
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- 239000000463 material Substances 0.000 title claims description 34
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 56
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 31
- 239000011575 calcium Substances 0.000 claims description 30
- 239000011572 manganese Substances 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 23
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- 239000000126 substance Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 12
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- 239000007858 starting material Substances 0.000 claims description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 4
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- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
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- 229910002601 GaN Inorganic materials 0.000 claims description 3
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- AUCDRFABNLOFRE-UHFFFAOYSA-N alumane;indium Chemical compound [AlH3].[In] AUCDRFABNLOFRE-UHFFFAOYSA-N 0.000 claims description 3
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- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims description 2
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- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
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- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 4
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 2
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- 101710187109 Alsin Proteins 0.000 description 1
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- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
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- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 150000001169 Lutetium Chemical class 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
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- 229910052783 alkali metal Inorganic materials 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 description 1
- 229910001632 barium fluoride Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
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- 238000005424 photoluminescence Methods 0.000 description 1
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- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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- FVRNDBHWWSPNOM-UHFFFAOYSA-L strontium fluoride Chemical compound [F-].[F-].[Sr+2] FVRNDBHWWSPNOM-UHFFFAOYSA-L 0.000 description 1
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- 239000000758 substrate Substances 0.000 description 1
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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
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7767—Chalcogenides
- C09K11/7769—Oxides
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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
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
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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
- C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
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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
- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
- C09K11/71—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus also containing alkaline earth metals
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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
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7701—Chalogenides
- C09K11/7703—Chalogenides with alkaline earth metals
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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
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7706—Aluminates
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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
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7774—Aluminates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- 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
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/12—Light sources with substantially two-dimensional radiating surfaces
- H05B33/14—Light sources with substantially two-dimensional radiating surfaces characterised by the chemical or physical composition or the arrangement of the electroluminescent material, or by the simultaneous addition of the electroluminescent material in or onto the light source
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
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Description
例えば、(Ca,Sr)S:Eu、(Ca,Sr,Ba)2Si5N8:Euおよび(Ca,Sr)AlSiN3:Euまたはこれらの発光団の混合物などの好適な一連の赤色発光蛍光物質は、既に多様な特許出願においてこの目的のために提案されている。
驚くべきことに、今回、Mn4+賦活ルテチウム含有ガーネット蛍光物質が上述した課題を達成することを見出した。
ここで、3価のアルミニウムの格子サイトでの4価のマンガンの取り込みは、Lu3+サイトでの2価イオン、例えばCa2+またはSr2+などの取り込みによって補償されなければならない。
Lu3−x−zAxAl5−y−zScyO12:MnzCaz (I)
式中、
Aは、Y、GdまたはTbを表し、
xは、0〜2.90の範囲からの値を表し、
yは、0〜0.50の範囲からの値を表し、
zは、0.005〜0.05の範囲からの値を表す、
で表される化合物である。
yは、好ましくは0.10〜0.45、特に好ましくは0.20〜0.40の範囲からの値を表す。
本発明による式Iで表される化合物は、以下、簡略化して蛍光物質ともいう。
上述のすべての品質を、当業者によく知られる方法によって光源の発光スペクトルから計算する。
a)ルテチウム、スカンジウム、カルシウム、アルミニウム、マンガン、イットリウム、テルビウムおよび/またはガドリニウム含有材料の混合、
b)少なくとも1つのさらなる無機および/または有機物質の添加、
c)混合物の熱処理。
・ NH4HCO3溶液を用いた共沈(例えば、Jander, Blasius Lehrbuch der analyt. u. praep. anorg. Chem. 2002参照)
・ クエン酸およびエチレングリコールの溶液を使用したPecchiniプロセス(例えば、Annual Review of Materials Research Vol. 36: 2006, 281-331参照)
・ 尿素を用いた燃焼法
・ 水性または有機塩溶液(出発材料)の噴霧乾燥
・ 水性または有機塩溶液(出発材料)の噴霧熱分解
・ 硝酸塩溶液の蒸発および残留物の熱変換
・ クエン酸またはシュウ酸塩を含む溶液を用いた沈殿
薄片の寸法(長さ×幅)は、配置に依存する。薄片はまた、とくにそれらがとくに小さい寸法を有する場合には、変換層内の散乱の中心として適する。
IniGajAlkN、式中0≦i、0≦j、0≦k、およびi+j+k=1
で表される発光窒化インジウムアルミニウムガリウムである。
例1:Lu2.995Al4.995O12:Mn0.005Ca0.005の製造
5.0125g(0.0126mol)のLu 2O3、0.0042gのCaCO3(4.2115*10−5mol)および0.0075g(4.2115*10−5mol)のMnC2O4*2H2Oを濃HNO3に加温しながら溶解する。300mlの水中の15.7827g(0.0427mol)のAl(NO3)3*9H2Oを、次に10gのクエン酸を30分間撹拌しながら、この溶液に添加する。溶液を150℃で、乾燥キャビネット内で終夜乾燥させ、得られたクエン酸塩前駆体を細かく粉砕する。粉末を1000℃で3時間か焼し、その後空気中で1750℃で5時間か焼する。
5.0125gのLu2O3および0.5808gのSc2O3を濃HNO3に加温しながら溶解し、0.0042gのCaCO3をその後添加する。
14.2028のAl(NO3)3*9H2Oおよび0.0075gのシュウ酸マンガンを蒸留水に溶解し、先の溶液に添加する。
10gのクエン酸をこの溶液に添加し、加温しながら30分間撹拌する。溶液を130℃で、乾燥キャビネット内で終夜蒸発させ、得られたクエン酸塩前駆体を細かく粉砕する。粉末を1000℃で3時間か焼し、その後空気中で1700℃で4時間か焼する。
2.507gのLu2O3および1.4226gのY2O3を濃HNO3に加温しながら溶解し、4.2mgのCaCO3を添加する。15.783gのAl(NO3)3*9H2Oおよび7.5mgのシュウ酸マンガンを蒸留水に溶解し、先の溶液に添加する。10gのクエン酸をこの溶液に添加し、加温しながら30分間撹拌する。溶液を130℃で、乾燥キャビネット内で終夜蒸発させ、得られたクエン酸塩前駆体を粉砕する。粉末を1000℃で3時間か焼し、その後空気中で1700℃で4時間か焼する。
23.507gのLu2O3および2.284gのGd2O3を濃HNO3に加温しながら溶解し、その後4.2mgのCaCO3をこの溶液に添加する。15.783gのAl(NO3)3*9H2Oおよび7.5mgのシュウ酸マンガンを蒸留水に溶解し、先の溶液に添加する。10g量のクエン酸をこの溶液に添加し、加温しながら30分間撹拌する。溶液を130℃で、乾燥キャビネット内で終夜蒸発させ、得られたクエン酸塩前駆体を粉砕する。粉末を1000℃で3時間か焼し、その後空気中で1700℃で4時間か焼する。
例1〜4からの蛍光物質を、二成分系シリコーン(Dow CorningからのOE 6550)と、タンブルミキサー(tumble mixer)中で、等量の蛍光物質がシリコーンの2種の構成成分中に分散するように混合する;蛍光物質混合物のシリコーン中の合計濃度は、8重量%である。2つの蛍光物質含有シリコーン構成成分を各5ml、互いに均質に混合し、ディスペンサー中に移送する。100μm2のGaNチップを含む、OSA optoelectronics, Berlinからの空のLEDパッケージを、ディスペンサーを用いて満たす。次に、LEDを加熱チャンバーに配置して、シリコーンを1時間にわたり150℃で凝固させる。
上記で述べたすべての量を、当業者によく知られる方法によって光源の発光スペクトルから計算する。
Claims (15)
- 式I
Lu3−x−zAxAl5−y−zScyO12:MnzCaz (I)
式中、
Aは、Y、GdまたはTbを表し、
xは、0〜2.90の範囲からの値を表し、
yは、0〜0.50の範囲からの値を表し、
zは、0.005〜0.05の範囲からの値を表す、
で表される化合物。 - xが、0〜2.0の範囲からの値を表すことを特徴とする、請求項1に記載の化合物。
- xが、0.10〜0.90の範囲からの値を表すことを特徴とする、請求項1または2に記載の化合物。
- yが、0.10〜0.45の範囲からの値を表すことを特徴とする、請求項1〜3のいずれか一項に記載の化合物。
- yが、0.20〜0.40の範囲からの値を表すことを特徴とする、請求項1〜3のいずれか一項に記載の化合物。
- 請求項1〜5のいずれか一項に記載の化合物の、湿式化学法を用いた製造方法であって、以下の方法ステップ:
a)請求項1〜5のいずれか一項に記載の化合物の製造のための出発材料としての、ルテチウム、スカンジウム、カルシウム、アルミニウム、マンガン、イットリウム、テルビウムおよび/またはガドリニウム含有材料の混合、
b)クエン酸および/またはシュウ酸の添加、
c)混合物の、最初に温度>900℃での空気下で、次に温度>1500℃での、か焼を行う熱処理、
を含む、前記方法。 - 方法ステップbにおいてクエン酸が添加されることを特徴とする、請求項6に記載の方法。
- 混合物の熱処理が、複数のステップで実行されることを特徴とする、請求項6または7に記載の方法。
- 半導体および請求項1〜5のいずれか一項に記載の式Iで表される少なくとも1つの化合物を含むことを特徴とする、光源。
- 半導体が、発光窒化インジウムアルミニウムガリウムであることを特徴とする、請求項9に記載の光源。
- 半導体が、式In i Ga j Al k Nで表され、式中0<i、0<j、0<kおよびi+j+k=1である発光窒化インジウムアルミニウムガリウムであることを特徴とする、請求項9または10に記載の光源。
- 請求項9〜11のいずれか一項に記載の少なくとも1つの光源を含むことを特徴とする、照明ユニット。
- 化合物と半導体との間の光結合を、光伝導配置によって達成することを特徴とする、請求項12に記載の照明ユニット。
- ディスプレイデバイスであって、請求項12または13に記載の少なくとも1つの照明ユニットを含むことを特徴とする、前記ディスプレイデバイス。
- 請求項1〜5のいずれか一項に記載の少なくとも1つの化合物の、発光ダイオードからの青色または近UV放射の部分的な、または完全な変換のための変換蛍光物質としての使用。
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DE102006037730A1 (de) | 2006-08-11 | 2008-02-14 | Merck Patent Gmbh | LED-Konversionsleuchtstoffe in Form von keramischen Körpern |
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