JP6831827B2 - ルミネセント材料ならびにそれを用いた発光デバイスおよび表示デバイス - Google Patents
ルミネセント材料ならびにそれを用いた発光デバイスおよび表示デバイス Download PDFInfo
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- JP6831827B2 JP6831827B2 JP2018227046A JP2018227046A JP6831827B2 JP 6831827 B2 JP6831827 B2 JP 6831827B2 JP 2018227046 A JP2018227046 A JP 2018227046A JP 2018227046 A JP2018227046 A JP 2018227046A JP 6831827 B2 JP6831827 B2 JP 6831827B2
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- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
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- 150000002987 phenanthrenes Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- KNCYXPMJDCCGSJ-UHFFFAOYSA-N piperidine-2,6-dione Chemical class O=C1CCCC(=O)N1 KNCYXPMJDCCGSJ-UHFFFAOYSA-N 0.000 description 1
- 229910052696 pnictogen Inorganic materials 0.000 description 1
- 229920001606 poly(lactic acid-co-glycolic acid) Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000003220 pyrenes Chemical class 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000822 sequential centrifugation Methods 0.000 description 1
- MTCFGRXMJLQNBG-UHFFFAOYSA-N serine Chemical compound OCC(N)C(O)=O MTCFGRXMJLQNBG-UHFFFAOYSA-N 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 229910052950 sphalerite Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- ZMBHCYHQLYEYDV-UHFFFAOYSA-N trioctylphosphine oxide Chemical compound CCCCCCCCP(=O)(CCCCCCCC)CCCCCCCC ZMBHCYHQLYEYDV-UHFFFAOYSA-N 0.000 description 1
- FIQMHBFVRAXMOP-UHFFFAOYSA-N triphenylphosphane oxide Chemical compound C=1C=CC=CC=1P(C=1C=CC=CC=1)(=O)C1=CC=CC=C1 FIQMHBFVRAXMOP-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- C09K11/0883—Arsenides; Nitrides; Phosphides
-
- 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
- C09K11/64—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing aluminium
- C09K11/646—Silicates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
- H01L33/507—Wavelength conversion elements the elements being in intimate contact with parts other than the semiconductor body or integrated with parts other than the semiconductor body
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
- H01L33/504—Elements with two or more wavelength conversion materials
Description
Ra nSi(ORb)4-n n=0〜3 式(I)
のシロキサン化合物に水を添加することにより行われる加水分解および縮合反応を介して得られる。
Rc mSi(ORd)4-m m=1〜3 式(II)
に示される有機シラン化合物を用いて表面上に親水性シラノール基を有する二酸化ケイ素粒子の表面を改質することにより得られうる。
18mgの酸化カドミウム(CdO)、813mgの酢酸亜鉛(ZnAc)、および7mgのオレイン酸を三口フラスコに添加した。次いで、15mlのオクタデセン(ODE)を添加し、そして120℃の温度の真空環境で溶液を加熱混合して反応させた。次いで、窒素ガスを三口フラスコに充填し、温度を290℃に上昇させた。次いで、2.1mlのトリオクチルホスフィンセレニド(TOP−Se)(0.0009mol)および58mgの硫黄(S)を注入し、290℃の温度で溶液を加熱して反応させた。次いで、0.5mlのn−ドデシルメルカプタン(DDT)および2.4mlのオクタデセンを注入し、525mgの酢酸亜鉛、1.83mlのオレイン酸、および4mlのオクタデセンを注入し、そして309mgの硫黄および5mlのトリオクチルホスフィンを注入した。次いで、溶液を撹拌して黄緑色懸濁液を生成させた。次いで、懸濁液を冷却し、そして沈殿物を得るために300mlのエタノールを用いて懸濁液の沈殿を行った。次いで、沈殿物に遠心分離を行って緑色量子ドットを生成した。これは、528nmのピーク波長および24nmの半値全幅を有する光を発することが可能である。
1.361gの酸化カドミウム(CdO)および20mgのオレイン酸を三口フラスコに添加した。次いで、30mlのオクタデセン(ODE)を添加し、そして180℃の温度の真空環境で溶液を加熱混合して反応させた。次いで、窒素ガスを三口フラスコに充填し、温度を250℃に上昇させた。次いで、0.7mlのトリオクチルホスフィンセレニド(TOPSe)(0.56mmol)を注入し、250℃の温度で溶液を加熱し、そして暗褐色溶液を生じるまで撹拌して反応させた。次いで、温度を120℃に冷却した。0.969gの酢酸亜鉛(Zn(Ac)2)を溶液に添加し、次いで、真空にすることにより溶液を脱水した。窒素ガスを三口フラスコに充填し、温度を250℃に上昇させた。次いで、8mlのトリオクチルホスフィン硫化物(TOPS)(12mmol)を溶液に注入した。溶液を250℃の窒素ガス下で反応させた。反応の終了後、溶液を室温に冷却した。次いで、沈殿物を得るために、300mlのエタノールを用いて溶液の沈殿を行った。次いで、沈殿物に遠心分離を行って赤色量子ドットを生成した。これは、650nmのピーク波長および35nmの半値全幅を有する光を発することが可能である。
量子ドット溶液(1)
量子ドットの合成例1の緑色量子ドットから溶媒を除去し、次いで、n−ヘキサンを添加して緑色量子ドットを1wt%の量子ドット溶液(1)にすることにより、量子ドット溶液(1)を作製した。
量子ドットの合成例2の赤色量子ドットから溶媒を除去し、次いで、n−ヘキサンを添加して赤色量子ドットを1wt.%の量子ドット溶液(2)にすることにより、量子ドット溶液(2)を作製した。
[コア溶液(1)]
3μmの平均直径および疎水性を有する、かつ10nmの平均表面開口直径および700m2/gの比表面積の多孔性マイクロ粒子である、二酸化ケイ素粒子をコアとして使用し、5wt%のコアを有するコア溶液(1)を生成するようにn−ヘキサンと混合した。
1μmの平均直径および疎水性を有する、かつ10nmの平均表面開口直径および400m2/gの比表面積の多孔性マイクロ粒子である、二酸化ケイ素粒子をコアとして使用し、5wt%のコアを有するコア溶液(2)を生成するようにn−ヘキサンと混合した。
0.15μmの平均直径および疎水性を有する、かつ5nmの平均表面開口直径および120m2/gの比表面積の多孔性マイクロ粒子である、二酸化ケイ素粒子をコアとして使用し、5wt%のコアを有するコア溶液(3)を生成するようにn−ヘキサンと混合した。
50μmの平均直径および疎水性を有する、かつ12nmの平均表面開口直径および120m2/gの比表面積の多孔性マイクロ粒子である、二酸化ケイ素粒子をコアとして使用し、5wt%のコアを有するコア溶液(4)を生成するようにn−ヘキサンと混合した。
0.25μmの平均直径を有する1gのヒュームドシリカ(商品名:SIS6960.0、Gelest製)を40gのジメチルスルホキシド中に分散し、改質剤として0.2gのヘキサデシルトリメトキシシランを添加した。窒素ガスの環境下で溶液を85℃に加熱し、そして72時間撹拌して反応させた。次いで、溶液を遠心分離処理し、エタノールで3回洗浄した。疎水性を有するヒュームドシリカマイクロ粒子をコアとして生成するように真空乾燥により溶液の溶媒を除去した。5wt%のコアを有するコア溶液(5)を生成するようにコアをn−ヘキサンと混合した。
[粒子の実施形態1]
0.25gの量子ドット溶液(1)と5gのコア溶液(1)とを混合して10分間放置した。次いで、遠心分離法により溶液を濾過し、量子ドットが装着されたコアを得た。次いで、量子ドットが装着されたコアを250gのエタノール中に均一に分散した。次いで、0.5gのテトラエトキシシラン(TEOS)および2.5gの29wt%水酸化アンモニウム(NH4OH)を溶液に添加し、室温で4時間撹拌した。その間、溶液のpH値は10〜11であった。遠心分離を行った。純水を用いて残渣を3回洗浄し、次いで、乾燥させてミクロンスケールの粒子を得た。粒子をエタノールと混合し、その中に均一に分散した。粒子を観察するために走査電子顕微鏡(SEM)を用いて溶液を分析し、Image−proPlus6.0のソフトウェアを用いて粒子の選択およびその性質たとえば平均直径などの測定を行った。PLを用いて粒子を分析し、ピークの光度を測定した。ルミネセンス保持率(単位:%)は、PL250対PL25の比である。PL25は、室温25℃で測定された粒子のPLピークの光度である。PL250は、250℃の環境下で粒子を2時間加熱した後に室温で測定された粒子のPLピークの光度である。
粒子の実施形態2および粒子の実施形態3は、粒子の実施形態1と異なり、表1に示される種類のコア溶液を用いた。
粒子の実施形態4は、粒子の実施形態1と異なり、表1に示される種類および量のコア溶液を用いた。
粒子の実施形態5は、粒子の実施形態5では量子ドット溶液(2)を用いたという点で粒子の実施形態4と異なっていた。
粒子の比較例1は、粒子の実施形態1と異なり、表1に示される種類のコア溶液を用いた。
粒子の比較例2は、粒子の比較例2では表1に示されるコア溶液を用いなかったという点で粒子の実施形態1と異なっていた。
粒子の比較例3は、0.25gの量子ドット溶液(1)から溶媒を除去することにより得られた粒子であった。
表2には、ルミネセント材料の実施例1〜5の組成およびルミネセント性質が列挙されている。ルミネセント材料の組成は、粒子および蛍光体の全重量を基準にしてルミネセント材料に占める粒子および蛍光体の重量パーセントが互いに異なる。
表6には、赤色蛍光体粉末(PFS)および青色LEDチップを適用するLED素子と共に表2の緑色ルミネセント材料の実施例1〜5をそれぞれ用いた発光デバイスの実施例1〜5の特性が列挙されている。青色LEDチップは、EPISTAR Corporationの製品型番ES−EEDBF11Pを使用する。これは、450nmの波長および(x,y)=(0.1409,0.0547)のCIE色度座標を有する光を発することが可能である。赤色蛍光体粉末は、GEの製品モデルTriGainのK2[SiF6]:Mn4+(フルオロケイ酸カリウムMn4+蛍光体、PFS)を使用する。これは、(x,y)=(0.691,0.307)のCIE色度座標、631nmの一次ルミネセントピーク波長、および10nmの半値全幅を有する光を発することが可能である。
22 蛍光体層
23 カプセル化層
100 ルミネセント材料
120 量子ドット
130 封止層
140 蛍光体
170 粒子
211 ベース
212 支承凹表面
213 発光素子
214 接続線
215 導線
Claims (5)
- 緑色量子ドットを含みかつ0.06μm〜30μmの平均直径を有する緑色粒子および前記緑色粒子と混合された緑色蛍光体β−SiAlONを含むルミネセント材料であって、
前記緑色粒子の1つはコアおよび前記コアを覆う封止層を含み、
前記緑色量子ドットは前記コアと前記封止層との間に配設され、
前記緑色蛍光体β−SiAlONの含有率は、前記緑色粒子および前記緑色蛍光体β−SiAlONの全含有率を100wt%として5wt%〜13.9wt%であり、
前記緑色蛍光体β−SiAlONは530nm〜550nmのメインピーク波長および40nm〜60nmの半値全幅を有し、
前記緑色粒子は520nm〜550nmのメインピーク波長および10nm〜30nmの半値全幅を有する、
前記ルミネセント材料。 - 前記コアが非フォトルミネセント材料である、請求項1に記載のルミネセント材料。
- 請求項1または2に記載のルミネセント材料を含む発光デバイス。
- 請求項3に記載の発光デバイスであって、
前記発光デバイスが赤色光変換材料および青色LEDチップを含み;
前記赤色光変換材料が600nm〜700nmのピーク波長を有する一次光を有し、かつ赤色蛍光体または赤色粒子を含む、前記発光デバイス。 - 請求項1または2に記載のルミネセント材料を含む表示デバイスであって、
前記表示デバイスが、テレビ、ディジタルカメラ、ディジタルビデオカメラ、ディジタルフォトフレーム、モバイルフォン、ラップトップ、コンピューターモニター、ポータブルミュージックプレーヤー、ゲームコンソール、自動車モニター、スマートウォッチ、またはバーチャルリアリティーメガネである、前記表示デバイス。
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