JPWO2020013016A1 - 光波長変換部材及び発光装置 - Google Patents
光波長変換部材及び発光装置 Download PDFInfo
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- JPWO2020013016A1 JPWO2020013016A1 JP2019568422A JP2019568422A JPWO2020013016A1 JP WO2020013016 A1 JPWO2020013016 A1 JP WO2020013016A1 JP 2019568422 A JP2019568422 A JP 2019568422A JP 2019568422 A JP2019568422 A JP 2019568422A JP WO2020013016 A1 JPWO2020013016 A1 JP WO2020013016A1
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 80
- 239000002245 particle Substances 0.000 claims abstract description 123
- 239000013078 crystal Substances 0.000 claims abstract description 112
- 239000000919 ceramic Substances 0.000 claims abstract description 31
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000005204 segregation Methods 0.000 claims description 27
- 238000004458 analytical method Methods 0.000 claims description 23
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 19
- 238000005430 electron energy loss spectroscopy Methods 0.000 claims description 12
- 229910052733 gallium Inorganic materials 0.000 claims description 9
- 230000003287 optical effect Effects 0.000 claims description 5
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 4
- 150000002602 lanthanoids Chemical class 0.000 claims description 4
- 241000252073 Anguilliformes Species 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 17
- 238000010791 quenching Methods 0.000 abstract description 17
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052593 corundum Inorganic materials 0.000 abstract 1
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- 238000011156 evaluation Methods 0.000 description 6
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- 238000010586 diagram Methods 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
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- 238000004020 luminiscence type Methods 0.000 description 3
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- 238000013459 approach Methods 0.000 description 2
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- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
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- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
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Abstract
Description
A:Ce以外のランタノイド、Sc
B:Al、Ga
且つ、前記(Y、A)3B5O12:Ce結晶粒子は、(Y、A)3B5O12:Ce中のAについて、(Y、A)3B5O12:Ce結晶粒子の内部の濃度よりも、(Y、A)3B5O12:Ce結晶粒子の表面側の濃度が高い領域を有する。
・「主成分」とは、光波長変換部材中において、最も多い量(即ち体積)存在することを示している。例えば、光波長変換部材には、透光性粒子(即ち透光性を有する粒子)であるAl2O3結晶粒子と、蛍光性粒子(即ち蛍光を発することができる粒子)である化学式(Y、A)3B5O12:Ceで表される結晶粒子(即ち(Y、A)3B5O12:Ce結晶粒子)とを、合計で50体積%以上(好ましくは90体積%以上)含まれていてもよい。
5…発光素子
9…光波長変換部材
[1.実施形態]
[1−1.発光装置]
まず、本実施形態の光波長変換部材を備えた発光装置について説明する。
[1−2.光波長変換部材]
次に、光波長変換部材9について説明する。
B:Al、Ga
しかも、この光波長変換部材9では、(Y、A)3B5O12:Ce結晶粒子は、(Y、A)3B5O12:Ce中のAについて、(Y、A)3B5O12:Ce結晶粒子の内部の濃度(即ちイオン濃度)よりも、(Y、A)3B5O12:Ce結晶粒子の表面側(特にAl2O3結晶粒子に隣り合う表面側)の濃度が高い領域を有している。
[1−3.光波長変換部材の製造方法]
次に、光波長変換部材9を製造する際の概略の手順について、図2に基づいて、簡単に説明する。
[1−4.効果]
次に、本実施形態の効果を説明する。
[2.実験例]
次に、前記実施形態の具体的な実施例等について説明する。
[2−1.試料の評価方法]
まず、各試料に対して実施した各評価の方法について説明する。
各試料の光波長変換部材のセラミックス焼結体を、JIS R1634に規定される方法によって測定することにより、開気孔率を求めた。
各試料の光波長変換部材のセラミックス焼結体を鏡面加工し、FESEM(電界放出形走査電子顕微鏡)によって観察を行った。そして、各試料に対して任意の5箇所の測定点で画像を取得し、インターセプト法にて(Y、A)3B5O12:Ce結晶粒子の粒子径を求めた。なお、各測定点の範囲の大きさは、例えば縦30μm×横40μmである。
各試料の光波長変換部材のセラミックス焼結体を、φ3mm、厚さt=50〜100μmのディスク状に機械研磨加工した。次に、ディスク中心部分をディンプリングした後、イオンミリング法により中央部を貫通させて、STEM(走査型透過電子顕微鏡)用の試料を得た。
EELSによるマッピング分析は、複数個の(Y、A)3B5O12:Ce結晶粒子を同一視野内に含めた、縦5μm×横5μm以下の視野を、50×50ポイント以上の分解能で各ポイント0.1秒間EELSスペクトルを収集した。
また、前記EELSによるマッピング分析に用いた画像を、画像処理ソフト(Winloof)を用いて画像解析することで粒界を抽出した。また、(Y、A)3B5O12:Ce結晶粒子の中心は、(Y、A)3B5O12:Ce結晶粒子の各辺について前記画像処理ソフトによって近似線を取り、(Y、A)3B5O12:Ce結晶粒子の面積中心(即ち重心)を中心とした。
ライン分析は、STEM用の試料の開口部の最端位置の(Y、A)3B5O12:Ce結晶粒子に対して、開口端部に水平な方向(即ち試料の厚みの変化が少ない方向)において、(Y、A)3B5O12:Ce結晶粒子の内部と表面との間にて、100ポイントを1ポイント1秒で散乱電子を収集した。
各試料の光波長変換部材のセラミックス焼結体を、φ3mmのディスク形状に打ち抜き、研磨加工にて厚さ約50μmに調整した。次に、ディスク中心部分をディンプリングした後、イオンミリング法により中央部を貫通させて、貫通孔端部が極薄片化された試料を得た。
・・(S)
そして、図6に示すように、結晶粒子の外側表面に最も近い位置の測定範囲の濃度平均値から±5%の範囲(丸で囲んだ範囲H)の各測定範囲の濃度平均値を求め、±5%の範囲の各測定範囲の濃度平均値の平均値を求めて基準値とした。そして、その基準値を100%としたときに、濃度平均値の前記基準値の100%に対して60%に相当する位置をGdの偏析の境界とした。詳しくは、上述のように、結晶粒子の外側表面に最も近い位置から内部側に向かって測定を行った場合に、濃度平均値が前記基準値の100%から60%以下に低下した位置をGdの偏析の境界とした。
光波長変換部材の各試料として、縦13mm×横13mm×厚み0.2mmの試料を作製した。
光波長変換部材の各試料として、縦13mm×横13mm×厚み0.2mmの試料を作製した。
前記<発光強度>の測定の際と同様にして得られた光、即ちレンズにて集光した光に対して、色彩照度計により発光スペクトルを測定した。そして、そのスペクトルの中で最も高い点の波長を「発光ピーク波長」とし、発光スペクトルのシフト(即ち467nmからのシフト)を評価した。その結果を表2の「発光ピーク波長」の欄に記載した。
[2−2.試料の製造方法及び評価結果]
次に、各試料の製造方法と、各試料の評価結果について説明する。
下記表1に示す条件により、No.1〜8の光波長変換部材の試料を作製した。即ち、反応焼結によって、No.1〜8の光波長変換部材の試料を作製した。
下記表1に示す条件により、No.9、10の光波長変換部材の試料を作製した。
下記表1に示す条件により、No.11〜13の光波長変換部材の試料を作製した。即ち、反応焼結によって、No.11〜13の光波長変換部材の試料を作製した。
下記表1に示す条件により、No.14〜16の光波長変換部材の試料を作製した。
本開示は前記実施形態になんら限定されるものではなく、本開示を逸脱しない範囲において種々の態様で実施しうることはいうまでもない。
Claims (3)
- Al2O3結晶粒子と、化学式(Y、A)3B5O12:Ceで表される(Y、A)3B5O12:Ce結晶粒子と、を主成分とする多結晶体であるセラミックス焼結体から構成された光波長変換部材において、
前記(Y、A)3B5O12:Ce中のA、Bは、下記の元素群から選択される少なくとも1種の元素であり、
A:Ce以外のランタノイド、Sc
B:Al、Ga
且つ、前記(Y、A)3B5O12:Ce結晶粒子は、前記(Y、A)3B5O12:Ce中のAについて、前記(Y、A)3B5O12:Ce結晶粒子の内部の濃度よりも、前記(Y、A)3B5O12:Ce結晶粒子の表面側の濃度が高い領域を有する、
光波長変換部材。 - 前記(Y、A)3B5O12:Ce結晶粒子のEELS分析で得られる画像を用いて、前記(Y、A)3B5O12:Ce結晶粒子の表面から前記内部側に向かって、一定の間隔で、前記(Y、A)3B5O12:Ce中の前記Aの濃度に対応した測定値を求める場合に、
前記表面に最も近い位置における前記測定値から前記測定値が±5%の範囲となる複数の測定値について、当該複数の測定値の平均値を基準の100%とし、前記複数の測定値を求めた領域より前記内部側において、前記測定値が前記基準の100%に対して60%に相当する位置を前記Aの偏析の境界と規定したときに、
前記偏析の境界が、前記(Y、A)3B5O12:Ce結晶粒子の表面から粒子径の1%以上25%以下の範囲にある、
前記請求項1に記載の光波長変換部材。 - 前記請求項1又は請求項2に記載の光波長変換部材と、発光素子と、を備えた、
発光装置。
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