JP6218046B2 - 色素増感太陽電池 - Google Patents
色素増感太陽電池 Download PDFInfo
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- JP6218046B2 JP6218046B2 JP2014522650A JP2014522650A JP6218046B2 JP 6218046 B2 JP6218046 B2 JP 6218046B2 JP 2014522650 A JP2014522650 A JP 2014522650A JP 2014522650 A JP2014522650 A JP 2014522650A JP 6218046 B2 JP6218046 B2 JP 6218046B2
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- Prior art keywords
- dye
- layer
- solar cell
- sensitized solar
- anode
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- -1 sulfonic acid organic compound Chemical class 0.000 claims description 51
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Images
Classifications
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- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2022—Light-sensitive devices characterized by he counter electrode
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2059—Light-sensitive devices comprising an organic dye as the active light absorbing material, e.g. adsorbed on an electrode or dissolved in solution
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
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Description
本発明の色素増感太陽電池のための陽極は、置換チオフェンから選択された少なくとも一種のモノマーから構成されたポリマーと、該ポリマーに対するドーパントとしての、非スルホン酸系有機化合物であって該化合物のアニオンの分子量が200以上である少なくとも一種の化合物から発生したアニオンと、を含み、且つ、100〜10000nmの範囲の厚みを有する導電性ポリマー層を備えている。そして、この導電性ポリマー層は、上記モノマーと上記非スルホン酸系有機化合物とを含む電解重合用の重合液を得る調製工程、及び、得られた重合液に導電性部分を有する基体を導入し、電解重合を行うことにより、上記モノマーの重合により得られた導電性ポリマー層を上記基体の導電性部分の上に形成する重合工程、を含む方法により製造することができる。以下、各工程について説明する。
この工程で調製する電解重合用の重合液は、水リッチ溶媒と、モノマーとしての置換チオフェンと、上述した特定範囲の非スルホン酸系有機化合物と、を必須成分として含む。
上述の調製工程により得られた重合液に、少なくとも表面に導電性部分を有する作用極(導電性ポリマー層の基体)と対極とを導入し、電解重合を行うことにより、置換チオフェンの重合により得られた導電性ポリマー層を作用極の導電性部分の上に形成し、色素増感太陽電池のための陽極を得る。
色素増感太陽電池は、光増感剤としての色素を含む半導体層を有する陰極と、該陰極の半導体層上に積層された対を成す酸化種と還元種とを含む電解質層と、上述した陽極と、を備えている。上述した陽極の導電性ポリマー層は、電解質層中で酸化還元対を構成する酸化種を還元種に変換させるのに十分な触媒能を有している。
(a)陽極の製造
陽極A
ガラス容器に蒸留水50mLを導入し、この液にp−ニトロフェノールを0.10Mの濃度で、EDOTを0.0148Mの濃度で、ボロジサリチル酸アンモニウムを0.08Mの濃度で、この順番に添加して攪拌し、全てのEDOTが溶解した重合液を得た。得られた重合液に、1cm2の面積を有するFTO電極(FTO層表面抵抗:10Ω/□)を作用極として、5cm2の面積を有するSUSメッシュを対極として、それぞれ導入し、100μA/cm2の条件で定電流電解重合を10分間行った。重合後の作用極をメタノールで洗浄した後、160℃で30分間乾燥し、FTO電極上に350nmの厚みのPEDOT層(ドーパント:ボロジサリチル酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
ガラス容器に蒸留水50mLを導入し、この液に、EDOTを0.0148Mの濃度で、ビス(トリフルオロメタンスルホニル)イミド酸ナトリウムを0.08Mの濃度で、添加して攪拌し、全てのEDOTが溶解した重合液を得た。得られた重合液に、1cm2の面積を有するFTO電極(FTO層表面抵抗:10Ω/□)を作用極として、5cm2の面積を有するSUSメッシュを対極として、それぞれ導入し、100μA/cm2の条件で定電流電解重合を10分間行った。重合後の作用極をメタノールで洗浄した後、160℃で30分間乾燥し、FTO電極上に350nmの厚みのPEDOT層(ドーパント:ビス(トリフルオロメタンスルホニル)イミド酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
0.08Mの濃度のビス(トリフルオロメタンスルホニル)イミド酸ナトリウムの代わりに、ビス(ノナフルオロブタンスルホニル)イミド酸アンモニウムを0.08Mの濃度で用いて、陽極Bの製造手順を繰り返し、FTO電極上に350nmの厚みのPEDOT層(ドーパント:ビス(ノナフルオロブタンスルホニル)イミド酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
0.08Mの濃度のビス(トリフルオロメタンスルホニル)イミド酸ナトリウムの代わりに、1,1,2,2,3,3−ヘキサフルオロ−1,3−ジスルホニルイミド酸アンモニウムを0.08Mの濃度で用いて、陽極Bの製造手順を繰り返し、FTO電極上に350nmの厚みのPEDOT層(ドーパント:1,1,2,2,3,3−ヘキサフルオロ−1,3−ジスルホニルイミド酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
1cm2の面積を有するFTO電極(FTO層表面抵抗:10Ω/□)上に、市販のPEDOT:PSS水性分散液(商品名バイトロンP:スタルク社製)の100μLをキャストし、5000rpmの回転数で30秒間スピンコートを行った。次いで、160℃で30分間乾燥し、非特許文献1と同様の、PEDOT:PSS層を有する陽極を得た。
1cm2の面積を有するFTO電極(FTO層表面抵抗:10Ω/□)上に、EDOT(0.48M)、トリス−P−トルエンスルホン酸鉄(III)、ジメチルスルホキシドを1:8:1の質量比でn−ブタノールに溶解させた反応液の100μLをキャストし、2000rpmの回転数で30秒間スピンコートを行った。この反応液を保持したFTO電極を110℃にて5分間加熱して化学重合を進行させた後、メタノールで洗浄し、160℃で30分間乾燥することにより、特許文献1と同様の、p−トルエンスルホン酸アニオンをドーパントとして含むPEDOTの化学重合層を有する陽極を得た。
陽極A〜Fについて、I−/I3 −電解液における電気化学的応答をサイクリックボルタモグラムにより評価した。
(i)PEDOT層の厚みの影響
(a)色素増感太陽電池の製造
実施例1
ガラス容器に蒸留水50mLを導入し、この液にp−ニトロフェノール0.70g(0.10M)、EDOT0.105g(濃度0.0148M)、及びボロジサリチル酸アンモニウム1.4g(濃度0.08M)をこの順番で添加して攪拌し、全てのEDOTが溶解した重合液を得た。得られた重合液に、厚さ100μmのTi箔で構成された2.25cm2の面積を有するTi電極を作用極として、5cm2の面積を有するSUSメッシュを対極として、それぞれ導入し、100μA/cm2の条件で定電流電解重合を3分間行った。重合後の作用極をメタノールで洗浄した後、150℃で30分間乾燥し、Ti電極上に105nmの厚みのPEDOT層(ドーパント:ボロジサリチル酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
実施例1で用いた重合液に、厚さ100μmのTi箔で構成された2.25cm2の面積を有するTi電極を作用極として、5cm2の面積を有するSUSメッシュを対極として、それぞれ導入し、100μA/cm2の条件で定電流電解重合を10分間行った。重合後の作用極をメタノールで洗浄した後、150℃で30分間乾燥し、Ti電極上に350nmの厚みのPEDOT層(ドーパント:ボロジサリチル酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
実施例1で得られた重合液に、厚さ100μmのTi箔で構成された2.25cm2の面積を有するTi電極を作用極として、5cm2の面積を有するSUSメッシュを対極として、それぞれ導入し、500μA/cm2の条件で定電流電解重合を6分間行った。重合後の作用極をメタノールで洗浄した後、150℃で30分間乾燥し、Ti電極上に1050nmの厚みのPEDOT層(ドーパント:ボロジサリチル酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
実施例1で得られた重合液に、厚さ100μmのTi箔で構成された2.25cm2の面積を有するTi電極を作用極として、5cm2の面積を有するSUSメッシュを対極として、それぞれ導入し、500μA/cm2の条件で定電流電解重合を9分間行った。重合後の作用極をメタノールで洗浄した後、150℃で30分間乾燥し、Ti電極上に1575nmの厚みのPEDOT層(ドーパント:ボロジサリチル酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
実施例1で得られた重合液に、厚さ100μmのTi箔で構成された2.25cm2の面積を有するTi電極を作用極として、5cm2の面積を有するSUSメッシュを対極として、それぞれ導入し、500μA/cm2の条件で定電流電解重合を12分間行った。重合後の作用極をメタノールで洗浄した後、150℃で30分間乾燥し、Ti電極上に2100nmの厚みのPEDOT層(ドーパント:ボロジサリチル酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
実施例1で得られた重合液に、厚さ100μmのTi箔で構成された2.25cm2の面積を有するTi電極を作用極として、5cm2の面積を有するSUSメッシュを対極として、それぞれ導入し、500μA/cm2の条件で定電流電解重合を24分間行った。重合後の作用極をメタノールで洗浄した後、150℃で30分間乾燥し、Ti電極上に4200nmの厚みのPEDOT層(ドーパント:ボロジサリチル酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
0.25cm2の表面積を有するFTO電極の表面に酸化チタンペースト(日揮触媒化成株式会社製)をスクリーン印刷法によりに異なる厚みで塗布し、60℃で30分間予備乾燥し、さらに450℃で15分間焼成することにより、3〜25μmの厚みの酸化チタン多孔質層をFTO電極上に形成した。さらに、色素N719を0.5mMの濃度で含むブタノール/アセトニトリル1:1溶液に酸化チタン多孔質層を24時間浸漬した後、室温にて乾燥することにより、酸化チタン多孔質層に色素N719を添着させ、色素増感太陽電池の陰極を得た。
実施例1で用いた重合液に、1cm2の面積を有するFTO電極(FTO層表面抵抗:10Ω/□)を作用極として、5cm2の面積を有するSUSメッシュを対極として、それぞれ導入し、100μA/cm2の条件で定電流電解重合を10分間行った。重合後の作用極をメタノールで洗浄した後、160℃で30分間乾燥し、FTO電極上に350nmの厚みのPEDOT層(ドーパント:ボロジサリチル酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
実施例1で用いた重合液に、厚さ200μmのポリエチレンナフタレート/ITOスパッタ膜で構成された2.25cm2の面積を有する電極を作用極として、5cm2の面積を有するSUSメッシュを対極として、それぞれ導入し、100μA/cm2の条件で定電流電解重合を10分間行った。重合後の作用極をメタノールで洗浄した後、160℃で30分間乾燥し、ポリエチレンナフタレート/ITO電極上に350nmの厚みのPEDOT層(ドーパント:ボロジサリチル酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
実施例1で用いた重合液に、2.25cm2の面積を有するFTO電極(FTO層表面抵抗:10Ω/□)を作用極として、5cm2の面積を有するSUSメッシュを対極として、それぞれ導入し、100μA/cm2の条件で定電流電解重合を10分間行った。重合後の作用極をメタノールで洗浄した後、160℃で30分間乾燥し、FTO電極上に350nmの厚みのPEDOT層(ドーパント:ボロジサリチル酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
厚さ100μmのTi箔で構成された2.25cm2の面積を有するTi電極上に、スパッタ法によりPtを約100nmの厚みになるように蒸着し、Ti電極上にPt層が形成された陽極を得た。
厚さ100μmのTi箔で構成された2.25cm2の面積を有するTi電極に、市販のPEDOT:PSS水性分散液(商品名バイトロンP:スタルク社製)の225μLをキャストし、5000rpmの回転数で30秒間スピンコートを行った。次いで、150℃で30分間乾燥し、Ti電極上にPEDOT:PSS層が形成された陽極を得た。
1cm2の面積を有するFTO電極(FTO層表面抵抗:10Ω/□)上に、市販のPEDOT:PSS水性分散液(商品名バイトロンP:スタルク社製)の100μLをキャストし、3000rpmの回転数で30秒間スピンコートを行った。次いで、160℃で30分間乾燥し、非特許文献1と同様の、PEDOT:PSS層を有する陽極を得た。
厚さ200μmのポリエチレンナフタレート/ITOスパッタ膜で構成された2.25cm2の面積を有する電極上にPt塗布層が形成されている市販品(商品名白金膜付き導電性フィルム:ベクセルテクノロジーズ社製)を陽極として用いた。この陽極と実施例1で得られた色素を添着させた酸化チタン多孔質層を有する陰極と組み合わせ、実施例1と同じ手順で色素増感太陽電池を得た。
2.25cm2の面積を有するFTO電極(FTO層表面抵抗:10Ω/□)上に、スパッタ法によりPtを約350nmの厚みになるように蒸着し、FTO電極上にPt層が形成された陽極を得た。次いで、実施例1で得られた色素を添着させた酸化チタン多孔質層を有する陰極と組み合わせ、実施例1と同じ手順で色素増感太陽電池を得た。
実施例1〜7及び比較例1,2の色素増感太陽電池について、ソーラシュミレータによる100mW/cm2、AM1.5Gの照射条件下での電流−電圧特性を評価した。測定は、20℃で、電圧を10mV/sの速度で変化させながら行った。
(a)色素増感太陽電池の製造
実施例11
ガラス容器に蒸留水50mLを導入し、この液にp−ニトロフェノール0.70g(0.10M)、EDOT0.105g(濃度0.0148M)、及びボロジサリチル酸アンモニウム1.4g(濃度0.08M)をこの順番で添加して攪拌し、全てのEDOTが溶解した重合液を得た。得られた重合液に、2.25cm2の面積を有するFTO電極を作用極として、5cm2の面積を有するSUSメッシュを対極として、それぞれ導入し、100μA/cm2の条件で定電流電解重合を3分間又は10分間行った。重合後の作用極を水・メタノールで洗浄した後、150℃で30分間乾燥し、FTO電極上に105nm及び350nmの厚みのPEDOT層(ドーパント:ボロジサリチル酸アニオン)が形成された陽極を得た。PEDOT層の密度は、約1.6g/cm3であった。
実施例11の色素増感太陽電池について、ソーラシュミレータによる100mW/cm2、AM1.5Gの照射条件下での電流−電圧特性を評価した。測定は、20℃で、電圧を10mV/sの速度で変化させながら行った。
Claims (4)
- 光増感剤としての色素を含む半導体層を有する陰極と、
該陰極の半導体層上に積層された、対を成す酸化種と還元種とを含む電解質層と、
該電解質層上に積層された、前記酸化種を前記還元種に変換する触媒として作用する導電性ポリマー層を有する陽極と、
を備えた色素増感太陽電池であって、
前記陽極における導電性ポリマー層が、
3位と4位に置換基を有するチオフェンから成る群から選択された少なくとも一種のモノマーから構成されたポリマーと、
該ポリマーに対するドーパントとしての、非スルホン酸系有機化合物であって該化合物のアニオンの分子量が200以上である少なくとも一種の化合物から発生したアニオンと、
を含み、
前記非スルホン酸系有機化合物が、ボロジサリチル酸及びボロジサリチル酸塩から成る群から選択された少なくとも一種の化合物、又は、式(I)又は式(II)
前記導電性ポリマー層が、1.15〜1.80g/cm 3 の範囲の密度を有しており、且つ、100〜10000nmの範囲の厚みを有している
ことを特徴とする色素増感太陽電池。 - 前記陰極における半導体層が酸化チタンにより形成されている、請求項1に記載の色素増感太陽電池。
- 前記半導体層の厚みが3〜20μmの範囲である、請求項1又は2に記載の色素増感太陽電池。
- 前記モノマーが3,4−エチレンジオキシチオフェンである、請求項1〜3のいずれか1項に記載の色素増感太陽電池。
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