JP2012018957A - 有機光電変換素子、その製造方法及び太陽電池 - Google Patents
有機光電変換素子、その製造方法及び太陽電池 Download PDFInfo
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- JP2012018957A JP2012018957A JP2010153689A JP2010153689A JP2012018957A JP 2012018957 A JP2012018957 A JP 2012018957A JP 2010153689 A JP2010153689 A JP 2010153689A JP 2010153689 A JP2010153689 A JP 2010153689A JP 2012018957 A JP2012018957 A JP 2012018957A
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- photoelectric conversion
- organic photoelectric
- conversion element
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Abstract
【解決手段】少なくとも一方が光透過性を有する第1電極と第2電極の間に、p型半導体材料とn型半導体材料を含有する発電層と、正孔または電子を主に輸送する電荷輸送層を少なくとも有する有機光電変換素子の製造方法において、1)発電層、電荷輸送層、第2電極の順に形成し、2)電荷輸送層は、架橋構造を形成し得る化合物を含有する塗布液を用いたウエットプロセスで形成し、3)第2電極は、有機金属錯体の熱分解もしくは還元反応で形成された、表面保護基が表面に吸着した金属微粒子の分散物を含有する塗布液を用いたウエットプロセスで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。
【選択図】なし
Description
1)発電層、電荷輸送層、第2電極の順に形成し、
2)電荷輸送層は、架橋構造を形成し得る化合物を含有する塗布液を用いたウエットプロセスで形成し、
3)第2電極は、有機金属錯体の熱分解もしくは還元反応で形成された、表面保護基が表面に吸着した金属微粒子の分散物を含有する塗布液を用いたウエットプロセスで形成する
ことを特徴とする有機光電変換素子の製造方法。
6.前記電荷輸送層の塗布液が、さらにπ共役系高分子及びポリアニオンを含有することを特徴とする前記5記載の有機光電変換素子の製造方法。
本発明の有機光電変換素子は、第1電極と第2電極と、両者に挟まれた発電層(p型半導体とn型半導体が混合された層であり、バルクヘテロジャンクション層、またはBHJ層、i層とも言う)が少なくとも1層以上あり、光を照射すると電流を発生する素子である。
本発明の第2電極は、有機金属錯体の熱分解もしくは還元反応で形成された金属微粒子を含む塗布液を用いた塗布プロセスで形成されることが特徴である。
本発明の金属微粒子は、表面保護基が表面に吸着した金属微粒子である。その表面保護基となる化合物の炭素数は、1〜18のものを選定することが好ましい。このような化合物の選定によって、160℃以下のベーク処理での蒸発反応を促進することができ、成膜された第2電極層中に、当該表面保護基となる化合物はほとんど存在することなく形成できる他、金属微粒子の融着が促進され、鏡面反射を有す導電性の高い電極を形成することができる。
金属微粒子の原料としては、銀アルキルアミン錯体やシュウ酸アルキルアミン錯体を用いることができる。
本発明の電荷輸送層は、発電層と第2電極の間に、架橋構造を形成し得る化合物を含有する塗布液を用いたウエットプロセスで形成されることが必要である。
本発明の電荷輸送層には、上述の水酸基含有非導電性ポリマーとして、下記一般式で示される単位構造を少なくとも分子内に有するポリマー(A)を含むことが好ましい。
本発明に好ましく用いられるπ共役系高分子としては、特に限定されないが、所謂導電性高分子であることが好ましい。さらには、π共役系高分子とポリアニオンとを有してなることがより好ましい。こうした高分子は、後述するπ共役系高分子を形成する前駆体モノマーを、適切な酸化剤と酸化触媒と後述のポリアニオンの存在下で化学酸化重合することによって容易に製造できる。
本発明で好ましく用いられるポリアニオンは特に限定されないが、アニオン性基として、スルホ基を有することがより好ましい。本発明においては、電荷輸送層の塗布液が第2電極塗布液中の金属微粒子の表面保護基と相互作用する官能基を有する化合物を含有することが好ましいが、金属微粒子の表面保護基が上述のオレイルアミン等の場合にはポリアニオンが相互作用する化合物となる。
本発明において前記電荷輸送層が、前記ポリマー(A)と、π共役系高分子とポリアニオンとを少なくとも含むことがより好ましい。例えば、ポリマー(A)を含む親水性のポリマーバインダー成分と、π共役系高分子成分と、ポリアニオン成分と、溶媒とを少なくとも含んでなる塗布液を塗布、乾燥することで形成することができる。
本発明者らの鋭意検討の結果、本発明の電荷輸送層において、ポリアニオンとしてスルホ基を有するポリマーと、上記ポリマー(A)を含む場合、水酸基の脱水反応による製膜後の架橋反応によって、膜強度が大幅に高くなることが分かり、電極形成時の有機層へのダメージを低減する効果が期待できより好ましい構成である。
本発明の架橋反応による膜強度の向上は、ナノインデンテーション法を用いた弾性率により評価することができる。本発明におけるナノインデンテーション弾性率とは、特殊なSPMのカンチレバーを一定荷重で対象膜に押し付け、カンチレバーのへこみ具合から、弾性率を算出する手法である。
電荷輸送層の本来の機能として、発電層で発生した正孔または電子のみを電極まで輸送し、反対のキャリアの輸送を阻止する阻止層としての役割がある。この場合、正孔輸送層を電子阻止層、電子輸送層を正孔阻止層と言い換えることができる。
本発明の発電層(バルクへテロジャンクション層)に用いられるp型半導体材料としては、種々の縮合多環芳香族低分子化合物や共役系ポリマーが挙げられる。
本発明のバルクへテロジャンクション層に用いられるn型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。
有機光電変換素子における第1電極(透明電極)としては、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するものが好ましく用いられる。電荷輸送層との接合構成に応じて最適な仕事関数の材料組成を選択できる。仕事関数が浅い組成としては、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、希土類金属等の極薄膜が挙げられる。また、仕事関数の深い組成としては、金、銀、白金等の極薄膜、またはそれらのナノ粒子・ナノワイヤー層、インジウムチンオキシド(ITO)、SnO2、ZnO等の導電性金属酸化物材料、及び導電性ポリマー等が挙げられる。また、IDIXO(In2O3−ZnO)等非晶質で光透過性の導電膜を作製可能な材料を用いてもよい。
太陽光利用率(光電変換効率)の向上を目的として、図1に示すような第1電極及び第2電極間でサンドイッチした構造に替わり、一対の櫛歯状電極上に素子を形成させたバックコンタクト型の有機光電変換素子が構成とすることもできる。
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、たとえば、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。
電子受容体と電子供与体とが混合された光電変換層、及び輸送層・電極の形成方法としては、蒸着法、塗布法(キャスト法、スピンコート法を含む)等を例示することができる。このうち、光電変換層の形成方法としては、蒸着法、塗布法(キャスト法、スピンコート法を含む)等を例示することができる。このうち、前述の正孔と電子が電荷分離する界面の面積を増大させ、高い光電変換効率を有する素子を作製するためには、塗布法が好ましい。また塗布法は、製造速度にも優れている。
本発明に係る電極、発電層、正孔輸送層、電子輸送層、ブロック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、公知の手法を適宜適用することができる。
作製した有機光電変換素子が大気中の酸素、水分等で劣化しないために、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。
〔銀微粒子塗布液AG−101の調製〕
特開2009−270146号公報,p9,実施例8に記載の方法で銀ナノ粒子を作製した。
特開2009−270146公報,p9,実施例9に記載の方法で銀ナノ粒子を作製した。
ポリマー(A)として、PHEA(ポリ(2−ヒドロキシエチルアクリレート))を合成した。
前記ポリ(2−ヒドロキシエチルアクリレート)の合成において、モノマーとしてヒドロキシエチルビニルエーテルを用いた以外は同様にして、ポリヒドロキシエチルビニルエーテル(数平均分子量約2万、数平均分子量<1000の含量0%)を得た。
装置:Wagers2695(Separations Module)
検出器:Waters 2414 (Refractive Index Detector)
カラム:Shodex Asahipak GF−7M HQ
溶離液:ジメチルホルムアミド(20mM LiBr)
流速:1.0ml/min
温度:40℃
〔架橋構造による弾性率向上確認〕
ナノインデンテーション法による弾性率の測定を以下に従って行った。
〔有機光電変換素子SC−101の作製〕
PEN基板上に、インジウム・スズ酸化物(ITO)透明導電膜を150nm堆積したもの(シート抵抗12Ω/□)を、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。
有機光電変換素子SC−101の作製において、発電層まで同様にして機能層を製膜した。続けて、導電性高分子及びポリアニオンからなるPEDOT−PSS(Baytron P4083、スタルクヴィテック社製、IP(HOMO):−5.0eV)、花王ケミカル株式会社製エマルゲン、イソプロパノールに加え、上記合成したPHEA(ポリ(2−ヒドロキシエチルアクリレート))を乾燥膜の固形分で5質量%含むよう調液し、乾燥膜厚が約100nmになるように塗布乾燥した。その後、150℃で10分間加熱処理し正孔輸送層を製膜した。
有機光電変換素子SC−102の作製において、正孔輸送層にPHEA(ポリ(2−ヒドロキシエチルアクリレート))を乾燥膜の固形分で30質量%含むようにした以外は同様にして有機光電変換素子SC−103を作製した。
有機光電変換素子SC−102の作製において、正孔輸送層にPHEA(ポリ(2−ヒドロキシエチルアクリレート))を乾燥膜の固形分で50質量%含むようにした以外は同様にして有機光電変換素子SC−104を作製した。
PEN基板上に、インジウム・スズ酸化物(ITO)透明導電膜を150nm堆積したもの(シート抵抗12Ω/□)を、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。
有機光電変換素子SC−104の作製において、銀微粒子塗布液AG−101を銀微粒子塗布液AG−102に変更し、第2電極AG102を形成した以外は同様にして、有機光電変換素子SC−106を作製した。
有機光電変換素子SC−106の作製において、電荷輸送層の塗布液に用いるPHEAをP−1に変更し、電荷輸送層を形成した以外は同様にして、有機光電変換素子SC−107を作製した。
上記作製した有機光電変換素子について、ソーラーシミュレーター(AM1.5Gフィルタ)の100mW/cm2の強度の光を照射し、有効面積を1cm2にしたマスクを受光部に重ね、IV特性を評価することで、短絡電流密度Jsc(mA/cm2)、開放電圧Voc(V)及びフィルファクターFFを、同素子上に形成した4箇所の受光部をそれぞれ測定した。ここで、Jsc及びFFは有機光電変換素子SC−101のJsc及びFFを100とした相対値で表す。
〔銀微粒子塗布液AG−201の調製〕
特開2010−500475号公報、p23、実施例17に記載の方法で銀ナノ粒子を作製した。
〔有機光電変換素子SC−201の作製〕
実施例1の有機光電変換素子SC−101の作製において、銀微粒子塗布液AG−101を銀微粒子塗布液AG−201に変更し、第2電極AG201を形成した以外は同様にして有機光電変換素子SC−201を作製した。
実施例1の有機光電変換素子SC−104の作製において、銀微粒子塗布液AG−101を銀微粒子塗布液AG−201に変更し、第2電極AG201を形成した以外は同様にして有機光電変換素子SC−202を作製した。
得られた有機光電変換素子を実施例1と同様に評価した。ここで、Jsc及びFFは有機光電変換素子SC−201のJsc及びFFを100とした相対値で表す。
101 第1の電極
102 正孔阻止層(または電子輸送層)
103 発電層
103a p型半導体材料
103b n型半導体材料
104 電子阻止層(正孔輸送層)
105 第2の電極
Claims (8)
- 少なくとも一方が光透過性を有する第1電極と第2電極の間に、p型半導体材料とn型半導体材料を含有する発電層と、正孔または電子のどちらかを主に輸送する電荷輸送層を少なくとも有する有機光電変換素子の製造方法において、
1)発電層、電荷輸送層、第2電極の順に形成し、
2)電荷輸送層は、架橋構造を形成し得る化合物を含有する塗布液を用いたウエットプロセスで形成し、
3)第2電極は、有機金属錯体の熱分解もしくは還元反応で形成された、表面保護基が表面に吸着した金属微粒子の分散物を含有する塗布液を用いたウエットプロセスで形成する
ことを特徴とする有機光電変換素子の製造方法。 - 前記電荷輸送層の塗布液が、前記第2電極の塗布液中の金属微粒子の表面保護基と相互作用する官能基を有する化合物を含有することを特徴とする請求項1記載の有機光電変換素子の製造方法。
- 前記有機金属錯体が、シュウ酸架橋アルキルアミン金属錯体からなることを特徴とする請求項1または2記載の有機光電変換素子の製造方法。
- 前記金属微粒子が銀微粒子であることを特徴とする請求項1〜3のいずれか1項記載の有機光電変換素子の製造方法。
- 前記電荷輸送層の塗布液が、さらにπ共役系高分子及びポリアニオンを含有することを特徴とする請求項5記載の有機光電変換素子の製造方法。
- 請求項1〜6のいずれか1項記載の有機光電変換素子の製造方法により得られたことを特徴とする有機光電変換素子。
- 請求項7に記載の有機光電変換素子を用いたことを特徴とする太陽電池。
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