JP6764200B2 - 金属酸化物の薄膜、該薄膜を備えた有機エレクトロルミネッセンス素子、太陽電池、および薄膜の製造方法 - Google Patents
金属酸化物の薄膜、該薄膜を備えた有機エレクトロルミネッセンス素子、太陽電池、および薄膜の製造方法 Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims description 224
- 229910044991 metal oxide Inorganic materials 0.000 title claims description 155
- 150000004706 metal oxides Chemical class 0.000 title claims description 155
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- 238000004519 manufacturing process Methods 0.000 title claims description 25
- 238000000034 method Methods 0.000 title description 51
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- 239000007789 gas Substances 0.000 claims description 26
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Images
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Description
薄膜であって、
前記薄膜は、亜鉛(Zn)、錫(Sn)、ケイ素(Si)および酸素(O)を含み、
酸化物換算で、前記薄膜の酸化物の合計100mol%に対して、SnO2が15mol%超、95mol%以下である、金属酸化物の薄膜を提供する。
薄膜を有する有機エレクトロルミネッセンス素子であって、
前記薄膜は、亜鉛(Zn)、錫(Sn)および酸素(O)を含み、酸化物換算で、前記薄膜の酸化物の合計100mol%に対して、SnO2が15mol%超、95mol%以下の金属酸化物の薄膜である、有機エレクトロルミネッセンス素子を提供する。
薄膜を有する太陽電池であって、
前記薄膜は、亜鉛(Zn)、錫(Sn)および酸素(O)を含み、酸化物換算で、前記薄膜の酸化物の合計100mol%に対して、SnO2が15mol%超、95mol%以下の金属酸化物の薄膜である、太陽電池を提供する。
前記の薄膜の製造方法であって、
スパッタリング法によりチャンバー内で薄膜を形成する前に前記チャンバー内の圧力を8×10−4Pa以下とした後にスパッタリングガスを導入し、その後に前記チャンバー内の圧力を0.1Pa〜5.0Paとし成膜する薄膜の製造方法を提供する。
本発明の一実施例では、亜鉛(Zn)、錫(Sn)および酸素(O)を含み、酸化物換算で、前記薄膜の酸化物の合計100mol%に対して、SnO2が15mol%超、95mol%以下の金属酸化物(ZTOおよびZTSO)の薄膜が提供される。金属酸化物の薄膜のうち、ケイ素(Si)を含む薄膜がZTSOの薄膜、ケイ素(Si)を実質的に含まない薄膜がZTOの薄膜である。
本発明の一実施例では、亜鉛(Zn)、錫(Sn)、ケイ素(Si)および酸素(O)を含み、酸化物換算で、前記薄膜の合計100mol%に対して、SnO2が15mol%超、95mol%以下である金属酸化物(ZTSO)の薄膜が提供される。SnO2は、酸化物換算で、前記金属酸化物の合計100mol%に対して、15mol%以下の場合、結晶化温度が低く、各種のプロセスにおいて施される熱処理工程において結晶化しやすく、非晶質、微結晶、または非晶質と微結晶とが混在する薄膜の状態に保てない。SnO2は、酸化物換算で、前記金属酸化物の合計100mol%に対して、95mol%超の場合、焼結が難しく、良好な酸化物ターゲットが得られないので薄膜をつくるのが難しい。
本発明の一実施例では、亜鉛(Zn)、錫(Sn)および酸素(O)を含み、酸化物換算で、前記金属酸化物の合計100mol%に対して、SnO2が15mol%超、95mol%以下であり、ケイ素(Si)を実質的に含まない金属酸化物(ZTO)の薄膜が提供される。SnO2は、酸化物換算で、前記金属酸化物の合計100mol%に対して、15mol%以下の場合、結晶化温度が低く、各種のプロセスにおいて施される熱処理工程において結晶化しやすく、非晶質、微結晶、または非晶質と微結晶とが混在する状態に保てない。SnO2は、酸化物換算で、前記金属酸化物の合計100mol%に対して、95mol%超の場合、焼結が難しく、良好な酸化物ターゲットが得られないので薄膜を得るのが難しい。
L=Kλ/(βcosθ) 式(1)
で表される。シェラー定数Kは0.9である。X線波長λは0.154nmである。
EA=4.0×(ZnO)+1.0×(SiO2)+4.7×(SnO2) 式(2)
ここで、(ZnO)、(SiO2)および(SnO2)は、それぞれZnO、SiO2およびSnO2のモル分率である。
本発明の一実施例による金属酸化物の薄膜は、有機エレクトロルミネッセンス素子の層部材として用いることができる。本発明の一実施例による有機エレクトロルミネッセンス素子は、一対の電極である陽極および陰極と、陽極と陰極の間に発光層とを有し、発光層と陰極の間には、「金属酸化物の薄膜」が配置される。この「金属酸化物の薄膜」は、電子輸送層、電子注入層、およびホールブロック層から選ばれる一以上の層として配置されればよい。
金属酸化物の薄膜が電子輸送層として配置された構造;
金属酸化物の薄膜が電子注入層として配置された構造;
金属酸化物の薄膜がホールブロック層として配置された構造;
金属酸化物の薄膜が電子輸送層と電子注入層とを兼ねて配置された構造;
金属酸化物の薄膜が電子輸送層とホールブロック層とを兼ねて配置された構造;
金属酸化物の薄膜が電子輸送層と電子注入層とホールブロック層とを兼ねて配置された構造;のいずれかであってよい。
金属酸化物の薄膜が陰極に接して配置された構造;
金属酸化物の薄膜が発光層に接して配置された構造;
金属酸化物の薄膜が陰極および発光層に接して配置された構造;
金属酸化物の薄膜が陰極と発光層のいずれにも接せずに配置された構造;
のいずれかであってよい。金属酸化物の薄膜が発光層に接して配置される場合、金属酸化物の薄膜は発光層との屈折率差が小さいため、金属酸化物の薄膜と発光層の界面における全反射による損失が少ないという効果が得られる。
(a)陰極\金属酸化物の薄膜\発光層\陽極
(b)陰極\電子注入層\金属酸化物の薄膜\発光層\陽極
(c)陰極\電子注入層\金属酸化物の薄膜\ホールブロック層\発光層\陽極
(d)陰極\金属酸化物の薄膜\ホールブロック層\発光層\陽極
(e)陰極\金属酸化物の薄膜\電子輸送層\発光層\陽極
(f)陰極\金属酸化物の薄膜\電子輸送層\ホールブロック層\発光層\陽極
(g)陰極\電子輸送層\金属酸化物の薄膜\発光層\陽極
(h)陰極\電子注入層\電子輸送層\金属酸化物の薄膜\発光層\陽極
なお、上記の素子構成は例示であり、本発明の有機エレクトロルミネッセンス素子の構成はこれに限定されるものではない。また、陽極と発光層との間には、陽極側から順に、ホール注入層、ホール輸送層、および電子ブロック層からなる群から選択される一以上の層が設けられていてもよい。
基板110は、上部に有機EL素子100を構成する各層を支持する役割を有する。基板110の材質は特に限られない。図1において、有機EL素子100の光取り出し面を下側(すなわち基板110側)とする場合、基板110は、透明な材料で構成される。例えば、基板110として、ガラス基板またはプラスチック基板等が使用される。
陰極120は、通常、金属で構成される。なお、有機EL素子100の光取り出し面を下側(すなわち基板110側)とする場合、陰極120は、透明な材料で構成される。陰極120として、例えばITO(インジウムスズ酸化物)のような透明金属酸化物薄膜が使用される。
電子注入層130は、電子注入性を有する材料から選定される。電子注入層130は、フッ化リチウム、炭酸セシウム、塩化ナトリウム、フッ化セシウム、酸化リチウム、酸化バリウム、炭酸バリウム、および8−キノリノラトリチウムからなる群から選ばれる一以上であってもよい。
(1)Ca原子の一部乃至全部が、Sr、Mg、および/またはBaなどの金属原子に置換された同型化合物。例えば、Ca原子の一部乃至全部がSrに置換された化合物としては、ストロンチウムアルミネートSr12Al14O33があり、CaとSrの混合比が任意に変化された混晶として、カルシウムストロンチウムアルミネートCa12−xSrXAl14O33(xは1〜11の整数;平均値の場合は0超12未満の数)などがある。
(2)Al原子の一部乃至全部が、Si、Ge、Ga、In、およびBからなる群から選択される一種以上の原子に置換された同型化合物。例えば、Ca12Al10Si4O35などが挙げられる。
(3)12CaO・7Al2O3(上記(1)、(2)の化合物を含む)中の金属原子および/または非金属原子(ただし、酸素原子を除く)の一部が、Ti、V、Cr、Mn、Fe、Co、Ni、およびCuからなる群から選択される一種以上の遷移金属原子もしくは典型金属原子、Li、Na、およびKからなる群から選択される一種以上のアルカリ金属原子、またはCe、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、およびYbからなる群から選択される一種以上の希土類原子と置換された同型化合物。
(4)ケージに包接されているフリー酸素イオンの一部乃至全部が、他の陰イオンに置換された化合物。他の陰イオンとしては、例えば、H−、H2 −、H2−、O−、O2 −、OH−、F−、Cl−、およびS2−などの陰イオンや、窒素(N)の陰イオンなどがある。
(5)ケージの骨格の酸素の一部が、窒素(N)などで置換された化合物。
なお、電子注入層130は、省略してもよい。
前述のように、有機EL素子100において、電子輸送層140には、金属酸化物の薄膜が使用される。
ホールブロック層145は、ホールブロック性を有する材料から選定される。ホールブロック層は、例えば最高被占分子軌道(Highest Occupied Molecular Orbital、略称HOMO)基準の高い材料等であってもよい。あるいは、無機酸化物、金属酸化物等であってもよい。例えば、IGZO(In−Ga−Zn−O)、ITO(In−Sn−O)、ISZO(In−Si−Zn−O)、IGO(In−Ga−O)、ITZO(In−Sn−Zn−O)、IZO(In−Zn−O)、およびIHZO(In−Hf−Zn−O)等であってもよい。
発光層150は、有機EL素子用の発光材料として知られる材料で構成されてもよい。
電子ブロック層155は、電子ブロック性を有する材料から選定される。
ホール輸送層160は、ホール輸送性を有する材料から選定される。
ホール注入層170は、ホール注入性を有する材料から選定される。
なお、ホール注入層170は、省略してもよい。
陽極180としては、通常、金属または金属酸化物が使用される。使用材料は、仕事関数が4eV以上であるものが好ましい。有機EL素子100の光取り出し面を陽極180側とする場合、陽極180は、透明である必要がある。
(1)基板、陰極、および陽極をこの順に有し、基板側を光取出し面とする構成;
(2)基板、陰極、および陽極をこの順に有し、陽極側を光取出し面とする構成;
(3)基板、陽極、および陰極をこの順に有し、基板側を光取出し面とする構成;
(4)基板、陽極、および陰極をこの順に有し、陰極側を光取出し面とする構成。
本発明の有機EL素子は、開口率の観点から、上記(2)および(4)の構成をとるのが好ましい。また、有機EL素子の輝度安定性の観点から、上記(1)または(2)の構成をとるのが好ましい。
前述した本発明の「金属酸化物の薄膜」は、太陽電池の層部材として用いることができる。太陽電池は、一対の電極と、一対の電極の間に光電変換層とを有する。一対の電極は、電子を取り出す側の電極およびホールを取り出す側の電極からなる。本発明の太陽電池では、光電変換層と電子を取り出す側の電極の間に、「金属酸化物の薄膜」が配置される。
(スパッタリング条件)
成膜装置には、RFマグネトロンスパッタ装置(エイコー社製)を使用した。スパッタリングターゲットには、直径3インチで、酸化物換算のモル%表記で、ZnOを45%、SnO2を45%、SiO2を10%含む焼結体ターゲットを使用した。
得られた薄膜について、ゼーマンボーリン法によりX線回折スペクトルを測定した。ゼーマンボーリン法については、日本金属学会会報第27巻第6号461〜465頁(1988)に示されている。ここでは、加速電圧45kV、放電電流200mAの条件で電子線をCuに照射し、発生したCuKα線を入射角0.5°に固定してサンプルに照射し、回折パターンを得た。
(評価 光吸収特性)
得られた薄膜について反射率および透過率を測定し、光吸収特性を評価した。
成型したZnO−SnO2−SiO2の混合粉末を焼結(1300℃,5時間、空気中)して、ターゲットを作製した。ターゲットには、組成の異なる2種類のものを使用した。
得られた薄膜について反射率および透過率を測定し、光吸収特性を評価した。
得られた薄膜(Zn:Sn:Si=45:45:10の組成を有する薄膜)について、ホール効果測定法により、電子濃度および電子移動度を測定した。金属酸化物の薄膜上に、6mm間隔で厚み10nmのTiと厚み100nmのAuを積層した電極をEB蒸着によって成膜し、電極とした。測定の結果、薄膜の電子密度は1.6×1016cm−3、電子移動度は3.8cm2V−1s−1であった。
成型したZnO−SnO2の混合粉末を、空気中で1300℃にて5時間焼結して、ターゲットを作製した。ターゲットには、組成の異なる6種類のものを使用した。
ここで、「金属酸化物であって、錫(Sn)、ケイ素(Si)および酸素(O)を含み、酸化物換算で、前記非晶質金属酸化物の合計100mol%に対して、SnO2が15mol%以上、95mol%以下である非晶質金属酸化物」を、特に「TSO」と称する。
110 基板
120 陰極
130 電子注入層
140 電子輸送層
145 ホールブロック層
150 発光層
155 電子ブロック層
160 ホール輸送層
170 ホール注入層
180 陽極
Claims (5)
- 有機エレクトロルミネッセンス素子の製造方法であって、
前記有機エレクトロルミネッセンス素子は、電子注入層および/またはホールブロック層としての薄膜を有し、
前記薄膜は、亜鉛(Zn)、錫(Sn)、ケイ素(Si)および酸素(O)を含み、
酸化物換算で、前記薄膜の酸化物の合計100mol%に対して、SnO 2 が15mol%超、95mol%以下の金属酸化物の薄膜であり、
当該製造方法は、
スパッタリング法によりチャンバー内で電子注入層および/またはホールブロック層としての薄膜を形成する前に前記チャンバー内の圧力を8.0×10−4Pa以下とした後にスパッタリングガスを導入し、その後に前記チャンバー内の圧力を0.1Pa〜5.0Paとし成膜する工程を含み、
前記スパッタリングガスは、NO(一酸化窒素)およびCO(一酸化炭素)からなる群から選ばれるガスである、製造方法。 - 前記薄膜は、酸化物換算で、前記薄膜の酸化物の合計100mol%に対して、SnO 2 が35mol%以上、60mol%以下である、請求項1に記載の製造方法。
- 前記薄膜は、酸化物換算で、前記薄膜の酸化物の合計100mol%に対して、SiO2が7mol%以上、30mol%以下である、請求項1または2に記載の製造方法。
- 前記薄膜は、厚さが10nm〜2000nmである、請求項1乃至3のいずれか一項に記載の製造方法。
- 前記スパッタリング法で使用するターゲットは、Zn、Sn、およびSiを含み、前記ターゲットにおけるSi/(Zn+Sn+Si)の原子数比は、0.01〜0.70である、請求項1乃至4のいずれか一項に記載の製造方法。
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JP6813982B2 (ja) * | 2016-08-01 | 2021-01-13 | 株式会社日本マイクロニクス | 二次電池 |
JP6431940B2 (ja) | 2017-02-22 | 2018-11-28 | 株式会社神戸製鋼所 | 誘電体層、光記録媒体、スパッタリングターゲット及び酸化物 |
JP6844845B2 (ja) | 2017-05-31 | 2021-03-17 | 三国電子有限会社 | 表示装置 |
KR102057963B1 (ko) * | 2017-11-15 | 2019-12-20 | 성균관대학교 산학협력단 | 전자화물 박막 및 이를 포함하는 유/무기 발광소자 |
JP7190729B2 (ja) * | 2018-08-31 | 2022-12-16 | 三国電子有限会社 | キャリア注入量制御電極を有する有機エレクトロルミネセンス素子 |
JP7246681B2 (ja) | 2018-09-26 | 2023-03-28 | 三国電子有限会社 | トランジスタ及びトランジスタの製造方法、並びにトランジスタを含む表示装置 |
KR102233853B1 (ko) * | 2018-11-21 | 2021-03-30 | 성균관대학교 산학협력단 | 이차원 페리자성 전자화물 및 이의 제조방법 |
JP7190740B2 (ja) | 2019-02-22 | 2022-12-16 | 三国電子有限会社 | エレクトロルミネセンス素子を有する表示装置 |
CN113711378A (zh) * | 2019-04-25 | 2021-11-26 | Agc株式会社 | 纳米粒子的集合体、纳米粒子的分散液、油墨、薄膜、有机发光二极管和纳米粒子的集合体的制造方法 |
KR20200132537A (ko) | 2019-05-17 | 2020-11-25 | 삼성전자주식회사 | 광전 변환 소자, 유기 센서 및 전자 장치 |
KR102304839B1 (ko) * | 2019-06-11 | 2021-09-24 | 경북대학교 산학협력단 | 발광소자 및 이의 제조 방법 |
JPWO2021090877A1 (ja) | 2019-11-06 | 2021-05-14 | ||
AU2021215857A1 (en) * | 2020-02-04 | 2022-08-25 | Ubiquitous Energy, Inc. | Compound charge transport layer for organic photovoltaic devices |
JP7444436B2 (ja) | 2020-02-05 | 2024-03-06 | 三国電子有限会社 | 液晶表示装置 |
KR102385038B1 (ko) * | 2020-03-16 | 2022-04-12 | 티오에스주식회사 | 단결정 금속산화물 반도체 에피 성장 장치 |
KR102336228B1 (ko) * | 2020-04-06 | 2021-12-09 | 티오에스주식회사 | 챔버 분리형 에피 성장 장치 |
KR102706471B1 (ko) * | 2020-06-25 | 2024-09-11 | 주식회사 엘지화학 | 전자 수송층, 이를 포함하는 양자점 발광 소자, 이러한 전자 수송층 평가를 위한 단일 전하 소자 및 그 제조 방법 |
US11997936B2 (en) | 2020-09-02 | 2024-05-28 | Applied Materials, Inc. | Optimized selector and memory element with electron barrier |
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JP2001176667A (ja) | 1999-12-21 | 2001-06-29 | Toyota Motor Corp | 有機el素子 |
JP4552950B2 (ja) * | 2006-03-15 | 2010-09-29 | 住友金属鉱山株式会社 | ターゲット用酸化物焼結体、その製造方法、それを用いた透明導電膜の製造方法、及び得られる透明導電膜 |
JP4730204B2 (ja) * | 2006-05-24 | 2011-07-20 | 住友金属鉱山株式会社 | 酸化物焼結体ターゲット、及びそれを用いた酸化物透明導電膜の製造方法 |
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CN102762518A (zh) * | 2010-02-18 | 2012-10-31 | 住友化学株式会社 | 氧化物烧结体、氧化物混合物、它们的制造方法以及使用它们的靶 |
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JP5718072B2 (ja) * | 2010-07-30 | 2015-05-13 | 三星ディスプレイ株式會社Samsung Display Co.,Ltd. | 薄膜トランジスタの半導体層用酸化物およびスパッタリングターゲット、並びに薄膜トランジスタ |
JP5814843B2 (ja) * | 2011-09-02 | 2015-11-17 | 富士フイルム株式会社 | フレキシブル有機電子デバイス |
WO2013103440A1 (en) * | 2012-01-06 | 2013-07-11 | Qd Vision, Inc. | Light emitting device including blue emitting quantum dots and method |
WO2013191212A1 (ja) * | 2012-06-20 | 2013-12-27 | 国立大学法人東京工業大学 | 有機エレクトロルミネッセンス素子 |
JP2014055324A (ja) * | 2012-09-12 | 2014-03-27 | Idemitsu Kosan Co Ltd | 酸化物半導体膜の製造方法 |
US8941111B2 (en) | 2012-12-21 | 2015-01-27 | Invensas Corporation | Non-crystalline inorganic light emitting diode |
CN103346221A (zh) * | 2013-05-25 | 2013-10-09 | 浙江大学 | 一种无机金属氧化物作为电子传输层的量子点发光二极管及其制备方法 |
KR102281399B1 (ko) | 2013-12-26 | 2021-07-23 | 고쿠리츠다이가쿠호진 토쿄고교 다이가꾸 | 금속 산화물의 박막, 그 박막을 구비한 유기 일렉트로 루미네선스 소자, 태양전지, 및 유기 태양전지 |
JP6114710B2 (ja) * | 2014-03-27 | 2017-04-12 | 富士フイルム株式会社 | 太陽電池 |
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KR102363274B1 (ko) | 2022-02-16 |
TWI716360B (zh) | 2021-01-21 |
WO2016043234A1 (ja) | 2016-03-24 |
JPWO2016043234A1 (ja) | 2017-07-06 |
US20170186984A1 (en) | 2017-06-29 |
US20210343961A1 (en) | 2021-11-04 |
US11871590B2 (en) | 2024-01-09 |
JP2019201231A (ja) | 2019-11-21 |
US20190058142A1 (en) | 2019-02-21 |
TW201618121A (zh) | 2016-05-16 |
KR20170059996A (ko) | 2017-05-31 |
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