JP2014514368A - 蛍光体成分を有する発光複合材 - Google Patents
蛍光体成分を有する発光複合材 Download PDFInfo
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- JP2014514368A JP2014514368A JP2013555535A JP2013555535A JP2014514368A JP 2014514368 A JP2014514368 A JP 2014514368A JP 2013555535 A JP2013555535 A JP 2013555535A JP 2013555535 A JP2013555535 A JP 2013555535A JP 2014514368 A JP2014514368 A JP 2014514368A
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- Prior art keywords
- layer
- ceramic body
- dopant
- thickness
- light emitting
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- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
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- WEAPVABOECTMGR-UHFFFAOYSA-N triethyl 2-acetyloxypropane-1,2,3-tricarboxylate Chemical compound CCOC(=O)CC(C(=O)OCC)(OC(C)=O)CC(=O)OCC WEAPVABOECTMGR-UHFFFAOYSA-N 0.000 description 1
- 239000001069 triethyl citrate Substances 0.000 description 1
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 description 1
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- TUUQISRYLMFKOG-UHFFFAOYSA-N trihexyl 2-acetyloxypropane-1,2,3-tricarboxylate Chemical compound CCCCCCOC(=O)CC(C(=O)OCCCCCC)(OC(C)=O)CC(=O)OCCCCCC TUUQISRYLMFKOG-UHFFFAOYSA-N 0.000 description 1
- AMMPRZCMKXDUNE-UHFFFAOYSA-N trihexyl 2-hydroxypropane-1,2,3-tricarboxylate Chemical compound CCCCCCOC(=O)CC(O)(C(=O)OCCCCCC)CC(=O)OCCCCCC AMMPRZCMKXDUNE-UHFFFAOYSA-N 0.000 description 1
- APVVRLGIFCYZHJ-UHFFFAOYSA-N trioctyl 2-hydroxypropane-1,2,3-tricarboxylate Chemical compound CCCCCCCCOC(=O)CC(O)(C(=O)OCCCCCCCC)CC(=O)OCCCCCCCC APVVRLGIFCYZHJ-UHFFFAOYSA-N 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
- C09K11/7774—Aluminates
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- 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
- H01L33/02—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 bodies
- H01L33/26—Materials of the light emitting region
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
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- E21B47/00—Survey of boreholes or wells
- E21B47/12—Means for transmitting measuring-signals or control signals from the well to the surface, or from the surface to the well, e.g. for logging while drilling
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Abstract
【選択図】図19B
Description
本願は、2011年2月24日出願の米国特許出願第61/446,346号の優先権の恩典を主張するものであり、該出願は、その全体が参照により本明細書に援用されている。
本願は、蛍光体成分を有する発光セラミック材料に関する。
発光セラミック
一部の実施形態においては、蛍光体組成物は、式I(A1−x−zGdxDz)3B5O12(式中、Dは、Nd、Er、Eu、Mn、Cr、Yb、Sm、Tb、Ce、Pr、Dy、Ho、Luおよびこれらの組み合わせから選択される第1ドーパントであり;Aは、Y、Lu、Ca、La、Tbおよびこれらの組み合わせから選択され;Bは、Al、Mg、Si、Ga、Inおよびこれらの組み合わせから選択され;xは、約0.20から約0.80までの範囲であり;およびzは、約0.001から約0.10までの範囲である)によって表すことができる。
[式1]
に等しいだろう。一例として、図4に描写されているGd濃度プロファイル410の平均ドーパント濃度は、最大ドーパント濃度となる。対照的に、図6に描写されている第1ドーパント濃度勾配600およびGd濃度勾配610は、それらのそれぞれの最大濃度より低い平均濃度を例証する。
本明細書に開示する一部の実施形態は、式Iの組成物を含む発光セラミックの製造方法を含む。前記方法は、たとえば、集成体を焼結させてセラミック体を形成することを含む場合がある。前記方法を用いて、上で開示した任意のセラミック体を調製することができる。
一部の実施形態は、光源と、該光源によって放射される放射線の少なくとも一部分を受け取るように構成されたセラミック体とを有する照明器具を提供する。前記セラミック体は、式Iの組成物、たとえば、上に開示した任意の組成物を含むことができる。
(a)(Y0.635Ce0.015Gd0.35)3Al5O12層:1.826gの硝酸イットリウム(III)・六水和物(hex hydrate)(純度99.9%、Sigma−Aldrich)、4.756gの硝酸アルミニウム・九水和物(純度98.6%、Sigma−Aldrich)、1.185gの硝酸ガドリニウム・六水和物(hex hydrate)(純度99.9%、Sigma−Aldrich)、および0.049gの硝酸セリウム(III)・六水和物(純度99.99%、Sigma−Aldrich)を脱イオン水に溶解し、その後、30分間超音波処理して、完全透明溶液を調製した。
従来、LED−YAGの組み合わせは、封止体樹脂、たとえばエポキシおよびシリコーン、中に分散された黄色光発光YAG蛍光体粉末という構成に基づいて製造されてきた。しかし、YAG蛍光体粉末の粒径はおよそ1〜10μmであるので、YAG粉末が分散された封止体樹脂媒体は光散乱特性を示す。これにより、青色LEDからの入射光およびYAGから出る黄色発光の少なからぬ部分が、後方散乱され、白色光発光の減損として散逸されることとなる。
幾つかの装置(Ceが%で1.5のYAG粉末((Y0.985Ce0.015)3Al5O12)およびCeが%で1.5でGdが%で35のYAG粉末((Y0.635Ce0.015Gd0.35)3Al5O12)、Ceが%で1.5のYAGセラミック((Y0.985Ce0.015)3Al5O12)およびCeが%で1.5でGdが%で35のYAGセラミック((Y0.635Ce0.015Gd0.35)3Al5O12)を、実施例1および2で説明したように構築した。各装置の相対強度および該装置の温度を測定した。図19Aは、1.5%Ceおよび1.5%Ce、35%Gd粉末、たとえば約150℃での約30%(5.8/8.2)の1滴、を有する装置の相対強度の減少を示す。図19Bは、図19Aにおいて説明したのと同じドーパント濃度を含むセラミック発光層についての150℃で約5%(8.2/8.6)の相対強度向上を示す。加えて、同じ駆動電流で、粉末実施形態の温度(約150℃)は、セラミック実施形態のもの(約55℃)よりはるかに高いので(図18を参照されたし)、粉末実施形態と比較したセラミック実施形態の相対効率は、約167%である。
実施例1において調製したセラミック体をSEM−EDX特性づけに用いた。このセラミック体サンプルは、(Y0.635Ce0.015Gd0.35)3Al5O12が2層のY3Al5O12層間に挿入されている共ドープ層を有する集成体からのものであった。調製したセラミックサンプルの断面を研磨して、その内側部分を露出させ、熱エッチングおよび不純物除去のために箱型炉内で、空気中で、約1400Cで2時間加熱した。処理した断面をSEMで観察した。そのSEMにおけるEDX付属装置を用いて、その断面上の一定の距離を横断する元素ラインスキャンを行って、図20に示すような、そのラインに沿った元素プロファイルを得た。Ceドーパントは、共ドープ層から隣接する層へと広く拡散した。Gdドーパントは、共ドープ層内により多く拘束され、より狭い分布を呈示した。
図21A〜Bに示したような集成体を構成したことを除き、一般に実施例1と同じ手順を用いて2つのさらなるセラミック体を調製した。各集成体は、共ドープ層の両側に(Y0.65Gd0.35)3Al5O12を有する層を含む。これらのガドリニウムドープ層は、焼結中の限られたGd拡散を補償することができる、より広いGd分布をセラミック体内に生じさせると予想される。
図21C(図中、Xは、共ドープ層中におよび共ドープ層の両側の2層の層中にドープされたガドリニウムの量である)に示したような集成体を構成したことを除き、一般に実施例1と同じ手順を用いて4つのセラミック体を調製した。Xについての試験値は、%で0、%で15、%で25、および%で35であった。共ドープ層は、固相反応から調製し、約78μmの厚さであった。他の層は、各々約200μm厚であった。IQEおよびピーク発光波長を実施例1での手順に従って決定した。
図23Aから23Dに示すような4群の構造を調製した。図23Aから23D(図中、Zは、セリウムの量であり、Xは、共ドープ層中にドープされたもの、および場合により共ドープ層の両側の層中にドープされたもの、両方のガドリニウムの量である)に示したような集成体を構成したことを除き、一般に実施例1と同じ手順を用いてこれらのセラミック体を調製した。Tは、各層の厚みである。Zについての試験値は、%で0.2から%で2(%で0.2、%で1.0、%で1.5、および%で2.0)であり、Xは、%で5から%で50(%で5、%で10、%で15、%で25、%で35および%で50)であり、およびTは、40μmから400μm(40μm、200μmおよび400μm)であった。一般に実施例1の場合と同じ手順を用いて、各セラミック体についての光学特性を試験した。結果を下の表3に示す。4群すべての構造が、カラーポイントを所望の目標カラービニングへとシフト(一般に、CCy値減少およびCCx値増加に伴って赤方シフト)させ、それらはすべて量子効率(IQE)および熱的性質を維持した。
Claims (25)
- 発光層を含有する熱安定性セラミック体であって、該発光層が、式(A1−X−ZGdxDz)3B5O12(式中、
Dは、Nd、Er、Eu、Mn、Cr、Yb、Sm、Tb、Ce、Pr、Dy、Ho、Luおよびこれらの組み合わせからなる群より選択される第1ドーパントであり;
Aは、Y、Lu、Ca、La、Tbおよびこれらの組み合わせからなる群より選択され;
Bは、Al、Mg、Si、Ga、Inおよびこれらの組み合わせからなる群より選択され;
xは、約0.20から約0.80までの範囲内であり;および
zは、約0.001から約0.10までの範囲内である)
によって表される化合物を含有するものである、熱安定性セラミック体。 - DがCeを含む、請求項1に記載のセラミック体。
- DがCeである、請求項2に記載のセラミック体。
- AがYである、請求項1に記載のセラミック体。
- BがAlである、請求項1に記載のセラミック体。
- 少なくとも8W/mKの熱伝導率を呈示する、請求項1に記載のセラミック体。
- 前記発光層中の第1ドーパントが、該発光層の厚みに沿って第1ドーパント濃度勾配を有する、請求項1に記載のセラミック体。
- 前記第1ドーパント濃度勾配が、前記発光層の厚みに沿ったその中央にまたは該中央付近に最大第1ドーパント濃度を含む、請求項7に記載のセラミック体。
- 前記第1ドーパント濃度勾配が、前記発光層の厚みに沿った表面にまたは該表面付近に最大第1ドーパント濃度を含む、請求項7に記載のセラミック体。
- 前記発光層が、該発光層の厚みに沿ってGd濃度勾配を含む、請求項1に記載のセラミック体。
- 前記第1ドーパント濃度勾配が、前記Gd濃度勾配に比べて広い、請求項10に記載のセラミック体。
- 前記Gd濃度勾配が、前記発光層の厚みに沿った前記最大第1ドーパント濃度にまたは該濃度付近に最大Gd濃度を含む、請求項10に記載のセラミック体。
- 熱安定性セラミック体の形成方法であって、集成体を焼結させることを含み、該集成体が、約10μmから約400μmの範囲の厚みを有する共ドープ層を含有し、該共ドープ層が、
イットリウム・アルミニウム・ガーネット(YAG)、YAG前駆体またはこれらの組み合わせと;
Nd、Er、Eu、Mn、Cr、Yb、Sm、Tb、Ce、Pr、Dy、Ho、Luおよびこれらの組み合わせからなる群より選択される第1ドーパントと;
YAGの量、YAG前駆体の相当量またはこれらの組み合わせに対して%で約20から%で約80のGdと
を含有するものである方法。 - 前記集成体が、前記ドープ層の一方の側面に配置された第1の層をさらに含有し、該第1の層が、YAG、YAG前駆体またはこれらの組み合わせを含有し、該第1の層には前記第1ドーパントが実質的になく、および該第1の層が、約40μmから約800μmの範囲の厚みを有する、請求項13に記載の方法。
- 前記共ドープ層が、前記第1の層と第2の層の間に配置され、該第2の層が、YAG、YAG前駆体またはこれらの組み合わせを含有し、該第2の層には前記第1ドーパントが実質的になく、および前記第1および第2の層が、各々独立して、約40μmから約400μmの範囲の厚みを有する、請求項14に記載の方法。
- 前記第2の層が、Gdをさらに含有する、請求項15に記載の方法。
- 前記第2の層が、%で約20から%で約80のGdを含有する、請求項16に記載の方法。
- 前記共ドープ層が、%で約20から%で約80のGdを含有する、請求項13に記載の方法。
- 前記共ドープ層が、%で約0.1から%で約10の第1ドーパントを含有する、請求項13に記載の方法。
- 前記第1ドーパントがCeである、請求項13に記載の方法。
- 前記集成体の焼結が、約1000℃から約1900℃の範囲の温度で少なくとも約2時間の前記集成体の加熱を含む、請求項13に記載の方法。
- 前記共ドープ層中の第1ドーパントの少なくとも約30%が、前記工程中に該共ドープ層から出て拡散する、請求項14に記載の方法。
- 請求項13に記載の方法によって製造されるセラミック体。
- 照明器具であって、
青色放射線を放射するように構成された光源と、
請求項1に記載のセラミック体と
を含み、
該セラミック体が、該青色放射線の少なくとも一部分を受け取るように構成されているものである、照明器具。 - 請求項1に記載のセラミック体を青色放射線に曝露することを含む、光生成方法。
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KR20210066929A (ko) * | 2018-11-21 | 2021-06-07 | 오스람 옵토 세미컨덕터스 게엠베하 | 세라믹 파장 컨버터 어셈블리 및 이를 제조하는 방법 |
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WO2020195250A1 (ja) * | 2019-03-27 | 2020-10-01 | Tdk株式会社 | 蛍光体および光照射装置 |
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CN103476903A (zh) | 2013-12-25 |
EP2678404A1 (en) | 2014-01-01 |
KR20140015392A (ko) | 2014-02-06 |
EP2678404B1 (en) | 2017-10-18 |
KR101952138B1 (ko) | 2019-02-26 |
JP6133791B2 (ja) | 2017-05-24 |
TWI573290B (zh) | 2017-03-01 |
US8968600B2 (en) | 2015-03-03 |
US20120218736A1 (en) | 2012-08-30 |
CN103476903B (zh) | 2016-08-24 |
TW201244165A (en) | 2012-11-01 |
WO2012116114A1 (en) | 2012-08-30 |
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