JPWO2012102066A1 - 有機光電変換層材料組成物、有機光電変換素子、有機光電変換素子の製造方法及び太陽電池 - Google Patents
有機光電変換層材料組成物、有機光電変換素子、有機光電変換素子の製造方法及び太陽電池 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- H10K85/10—Organic polymers or oligomers
- H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
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- H—ELECTRICITY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
Description
2.前記一般式(1)で表される溶剤が、Cl原子またはBr原子で置換されたトルエンまたはキシレンであることを特徴とする前記1に記載の有機光電変換層材料組成物。
図1は、順層型のバルクヘテロジャンクション型の有機光電変換素子の一例を示す断面図である。図1において、バルクヘテロジャンクション型の有機光電変換素子10は、基板11の面上に、透明電極(一般に陽極)12、正孔輸送層17、光電変換層14、電子輸送層18及び対極(一般に陰極)13が順次積層されている。
本発明の有機光電変換層材料組成物においては、本発明に係る前記一般式(1)で表される溶剤を含むことを特徴とする。該溶剤を含有することにより、短時間の乾燥においても高い変換効率と耐久性が向上することができ、安定な相分離構造を早期に形成することができる。
本発明に係る有機光電変換層(以下、バルクヘテロジャンクション層ともいう)に用いられるp型共役高分子半導体材料としては、主鎖に電子供与性基(ドナー性ユニット)と電子吸引性基(アクセプター性ユニット)とを有する共重合体であるバンドギャップを小さくしたp型共役高分子半導体材料を用いる。このような共重合体は、太陽光スペクトルの広い範囲にわたる放射エネルギーを効率よく吸収させることができる。このような共重合体としては公知の共役高分子材料が使用できる。
本発明に係るバルクヘテロジャンクション層に用いられる電子受容性を有するn型有機半導体材料としては、特に限定されないが、例えば、フラーレン、オクタアザポルフィリン等、p型半導体の水素原子をフッ素原子に置換したパーフルオロ体(パーフルオロペンタセンやパーフルオロフタロシアニン等)、ナフタレンテトラカルボン酸無水物、ナフタレンテトラカルボン酸ジイミド、ペリレンテトラカルボン酸無水物、ペリレンテトラカルボン酸ジイミド等の芳香族カルボン酸無水物やそのイミド化物を骨格として含む高分子化合物等を挙げることができる。
本発明に係る有機光電変換層は、p型有機半導体材料とn型有機半導体材料と本発明に係る一般式(1)で表される溶剤を含有する有機光電変換層材料組成物を塗布することにより形成されることが好ましい。
本発明の有機光電変換素子においては、バルクヘテロジャンクション層と陰極との中間に電子輸送層を形成することで、バルクヘテロジャンクション層で発生した電荷をより効率的に取り出すことが可能となるため、電子輸送層あるいは正孔ブロック層を有していることが好ましい。
本発明の有機光電変換素子は、バルクヘテロジャンクション層と陽極との中間には正孔輸送層を設けることにより、バルクヘテロジャンクション層で発生した電荷をより効率的に取り出すことができるため、これらの層を有していることが好ましい。
エネルギー変換効率の向上や、素子寿命の向上を目的に、各種中間層を素子内に有する構成としてもよい。中間層の例としては、正孔注入層、電子注入層、励起子ブロック層、UV吸収層、光反射層、波長変換層等を挙げることができる。また、上層に偏在した金属酸化物微粒子をより安定にするため、シランカップリング剤等を含有する層を設けてもよい。更に、本発明に係るバルクヘテロジャンクション型の有機光電変換層に隣接して金属酸化物含有層を積層してもよい。
本発明の有機光電変換素子においては、少なくとも陽極と陰極(第1の電極、第2の電極)を有する。また、タンデム構成をとる場合には、中間電極を用いることでタンデム構成を達成することができる。なお、本発明においては、主に正孔が流れる電極を陽極と呼び、主に電子が流れる電極を陰極と呼ぶ。
本発明に係る陽極は、好ましくは380〜800nmの光を透過する電極である。陽極を構成する材料としては、例えば、インジウムチンオキシド(ITO)、SnO2、ZnO等の透明導電性金属酸化物、金、銀、白金等の金属薄膜、金属ナノワイヤー、カーボンナノチューブ等を用いることができる。
陰極は導電材料のみから構成される単独層であってもよいが、導電性を有する材料に加えて、これらを保持する樹脂を併用してもよい。陰極の導電材としては、仕事関数の小さい(4eV以下)金属、合金、電気伝導性化合物及びこれらの混合物を、電極物質として用いられる。このような電極物質の具体例としては、ナトリウム、ナトリウム−カリウム合金、マグネシウム、リチウム、マグネシウム/銅混合物、マグネシウム/銀混合物、マグネシウム/アルミニウム混合物、マグネシウム/インジウム混合物、アルミニウム/酸化アルミニウム(Al2O3)混合物、インジウム、リチウム/アルミニウム混合物、希土類金属等が挙げられる。これらの中で、電子の取り出し性能及び酸化等に対する耐久性の点から、これら第1金属と、この第1金属より仕事関数の値が大きく安定な金属である第2金属との混合物、例えば、マグネシウム/銀混合物、マグネシウム/アルミニウム混合物、マグネシウム/インジウム混合物、アルミニウム/酸化アルミニウム(Al2O3)混合物、リチウム/アルミニウム混合物、アルミニウム等が好適である。陰極はこれらの電極物質を蒸着やスパッタリング等の方法により薄膜を形成させることにより、作製することができる。また、膜厚は通常10nm〜5μm、好ましくは50〜200nmの範囲で選ばれる。
また、図3で示したようなタンデム構成の場合に必要となる中間電極(電荷再結合層)の材料としては、透明性と導電性を併せ持つ化合物を用いた層であることが好ましく、上記説明した陽極で用いたような材料(例えば、ITO、AZO、FTO、酸化チタン等の透明金属酸化物、Ag、Al、Au等の非常に薄い金属層またはナノ粒子・ナノワイヤーを含有する層、PEDOT:PSS(ポリエチレンジオキシチオフェン:ポリスチレンスルホネート)、ポリアニリン等の導電性高分子材料等)を用いることができる。
基板側から光電変換される光が入射する場合、基板はこの光電変換される光を透過させることが可能な、即ちこの光電変換すべき光の波長に対して透明な部材であることが好ましい。基板は、例えば、ガラス基板や樹脂基板等が好適に挙げられるが、軽量性と柔軟性の観点から透明樹脂フィルムを用いることが望ましい。
本発明の有機光電変換素子は、太陽光のより効率的な受光を目的として、各種の光学機能層を有していてよい。光学機能層としては、例えば、反射防止膜、マイクロレンズアレイ等の集光層、陰極で反射した光を散乱させて再度発電層に入射させることができるような光拡散層等を設けてもよい。
本発明に係る電極、発電層、正孔輸送層、電子輸送層等をパターニングする方法やプロセスには、特に制限はなく、公知のパターニング方法を適宜適用することができる。
また、作製した有機光電変換素子が環境中の酸素、水分等で劣化しないために、有機光電変換素子だけでなく有機エレクトロルミネッセンス素子等で公知の手法によって封止することが好ましい。例えば、アルミまたはガラスでできたキャップを接着剤によって接着することによって封止する手法、アルミニウム、酸化ケイ素、酸化アルミニウム等のガスバリア層が形成されたプラスチックフィルムと有機光電変換素子上を接着剤で貼合する手法、ガスバリア性の高い有機高分子材料(ポリビニルアルコール等)をスピンコートする方法、ガスバリア性の高い無機薄膜(酸化ケイ素、酸化アルミニウム等)または有機膜(パリレン等)を真空下で堆積する方法、及びこれらを複合的に積層する方法等を挙げることができる。
〔有機光電変換素子の作製〕
(有機光電変換素子101の作製)
ポリエチレンテレフタレート(PET)基板上に、インジウム・スズ酸化物(ITO)透明導電膜を150nm堆積した(シート抵抗12Ω/□)薄膜を形成した後、通常のフォトリソグラフィ技術と湿式エッチングとを用いて10mm幅にパターニングし、第1電極を形成した。パターン形成した第1電極を、界面活性剤と超純水による超音波洗浄、超純水による超音波洗浄の順で洗浄後、窒素ブローで乾燥させ、最後に紫外線オゾン洗浄を行った。これ以降は、透明基板をグローブボックス内に持ち込み、窒素雰囲気下で作業した。
上記有機光電変換素子101の作製において、有機光電変換層101に代えて、表1に記載のp型有機半導体材料の種類、溶剤の種類、塗布時の各有機光電変換層材料組成物の液温度、乾燥温度、乾燥時間をそれぞれ表1に記載の組み合わせに変更した有機光電変換層102〜132をそれぞれ用いた以外は同様にして、有機光電変換素子102〜132を作製した。
(光電変換効率の評価)
上記作製した封止済みの各有機光電変換素子に、ソーラーシミュレーター(AM1.5Gフィルタ)を用いて、100mW/cm2の強度の光を照射し、有効面積を4.0mm2にしたマスクを受光部に重ね、短絡電流密度Jsc(mA/cm2)及び開放電圧Voc(V)、曲線因子(フィルファクター)FFを、同素子上に形成した4箇所の受光部についてそれぞれ測定し、平均値を求めた。また、Jsc、Voc、FFから、下式(1)に従ってエネルギー変換効率η(%)を求めた。
η(%)=Jsc(mA/cm2)×Voc(V)×FF
以上により得られた結果を、表1に示す。なお、η(%)の数字が大きい程、エネルギー変換効率(光電変換効率)に優れていることを示す。
〔有機光電変換素子の作製〕
(有機光電変換素子201の作製)
実施例1に記載の有機光電変換素子103の作製において、作製に用いた有機光電変換層103を、下記の方法に従って形成した有機光電変換層201に変更した以外は同様にして、有機光電変換素子201を作製した。
溶剤として2−ブロモトルエンと、p型有機半導体材料として下記PCPDTBTを0.6質量%と、n型半導体材料としてPC71BM(フロンティアカーボン製nanom spectra E110)を1.2質量%で混合した溶液を調製し、オーブンで70℃に加熱しながら撹拌(60分)し、2−ブロモトルエンに、PCPDTBTとPC71BMとを溶解した後、0.45μmのフィルタでろ過して、有機光電変換層材料組成物201を調製した。次いで、この有機光電変換層材料組成物201の液温度を50℃に保ちながら、乾燥膜厚が約100nmになるようにブレードコーターを用いて,電子輸送層上に塗布した後、乾燥温度50℃で3分間の乾燥を行い、有機光電変換層201を製膜した。
上記有機光電変換素子201の作製において、有機光電変換層201の形成に用いた有機光電変換層材料組成物201の溶剤の種類(一部、2種組み合わせ)を、表2、表3に記載の溶剤に変更した以外は同様にして、有機光電変換素子202〜239を作製した。
(光電変換効率の評価)
実施例1に記載の方法と同様にして、光電変換効率の評価を行った。得られた結果を、表2、表3に示す。
各有機光電変換素子に対し、ソーラシミュレーター(AM1.5G)の光を100mW/cm2の照射強度で照射して、電圧−電流特性を測定し、暴露前の光電変換効率を測定した。次いで、陽極と陰極の間に抵抗を接続したまま、各有機光電変換素子を80℃に加熱し、ソーラシミュレーター(AM1.5G)の光を10倍の1000mW/cm2の照射強度で100時間照射し続けた後、有機光電変換素子を室温まで冷却した後、ソーラシミュレーター(AM1.5G)の光を100mW/cm2の照射強度で照射して、電圧−電流特性を測定し、暴露後の光電変換効率を測定した。次いで、下式(2)により光電変換効率の相対低下率(%)を算出し、これを光電変換効率の耐久性の尺度とした。
光電変換効率の相対低下率(%)=(1−暴露後の光電変換効率/暴露前の光電変換効率)×100
以上により得られた評価結果を表2、表3に示す。なお、光電変換効率の相対低下率(%)が小さい程、エネルギー変換効率の耐久性(光電変換効率の耐久性)が良好であることを示す。
〔有機光電変換素子の作製〕
(有機光電変換素子301〜339の作製)
実施例2に記載の有機光電変換素子201〜239の作製において、各有機光電変換層形成時の有機光電変換層材料組成物の塗布液温度を50℃から70℃に変更し、塗膜乾燥時の乾燥温度を50℃から70℃に変更し、かつ乾燥時間を3分から1分に変更した以外は同様にして各有機光電変換層を形成して、有機光電変換素子301〜339を作製した。
次いで、実施例2に記載の方法と同様にして、光電変換効率の評価と、光電変換効率の耐久性評価(光電変換効率の相対低下率の測定)を行い、得られた結果を表4、表5に示す。
11 基板
12 透明電極
13 対極
14 光電変換層
15 電荷再結合層
16 第2の光電変換層
17 正孔輸送層
18 電子輸送層
19 第1の光電変換層
Claims (7)
- 前記一般式(1)で表される溶剤が、Cl原子またはBr原子で置換されたトルエンまたはキシレンであることを特徴とする請求項1に記載の有機光電変換層材料組成物。
- 前記一般式(1)で表される溶剤が、Cl原子またはBr原子で置換されたチオフェンまたはフランであることを特徴とする請求項1に記載の有機光電変換層材料組成物。
- 少なくとも、基板上に第1の電極、請求項1から3のいずれか一項に記載の有機光電変換層材料組成物を塗布、乾燥して得られる有機光電変換層、及び第2の電極を有することを特徴とする有機光電変換素子。
- 第1電極を有する基材上に、50℃以上に加温した請求項1から3のいずれか一項に記載の有機光電変換層材料組成物を塗布し、90℃以上で乾燥することにより有機光電変換層を形成することを特徴とする有機光電変換素子の製造方法。
- 請求項4に記載の有機光電変換素子を具備することを特徴とする太陽電池。
- 請求項5に記載の有機光電変換素子の製造方法により得られた有機光電変換素子を具備することを特徴とする太陽電池。
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