JP5924514B2 - 太陽電池用電極体の製造方法 - Google Patents
太陽電池用電極体の製造方法 Download PDFInfo
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- JP5924514B2 JP5924514B2 JP2011080676A JP2011080676A JP5924514B2 JP 5924514 B2 JP5924514 B2 JP 5924514B2 JP 2011080676 A JP2011080676 A JP 2011080676A JP 2011080676 A JP2011080676 A JP 2011080676A JP 5924514 B2 JP5924514 B2 JP 5924514B2
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- RBTKNAXYKSUFRK-UHFFFAOYSA-N heliogen blue Chemical compound [Cu].[N-]1C2=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=NC([N-]1)=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=N2 RBTKNAXYKSUFRK-UHFFFAOYSA-N 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 150000004698 iron complex Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- DZVCFNFOPIZQKX-LTHRDKTGSA-M merocyanine Chemical compound [Na+].O=C1N(CCCC)C(=O)N(CCCC)C(=O)C1=C\C=C\C=C/1N(CCCS([O-])(=O)=O)C2=CC=CC=C2O\1 DZVCFNFOPIZQKX-LTHRDKTGSA-M 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 1
- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 description 1
- 229920000553 poly(phenylenevinylene) Polymers 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 229920002098 polyfluorene Chemical class 0.000 description 1
- 229960002796 polystyrene sulfonate Drugs 0.000 description 1
- 239000011970 polystyrene sulfonate Substances 0.000 description 1
- 229940005642 polystyrene sulfonic acid Drugs 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 150000004033 porphyrin derivatives Chemical class 0.000 description 1
- 150000004032 porphyrins Chemical class 0.000 description 1
- 229910001487 potassium perchlorate Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- KVCGISUBCHHTDD-UHFFFAOYSA-M sodium;4-methylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1 KVCGISUBCHHTDD-UHFFFAOYSA-M 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 125000005463 sulfonylimide group Chemical group 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 150000005621 tetraalkylammonium salts Chemical class 0.000 description 1
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical class CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical class CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- PFZLGKHSYILJTH-UHFFFAOYSA-N thieno[2,3-c]thiophene Chemical compound S1C=C2SC=CC2=C1 PFZLGKHSYILJTH-UHFFFAOYSA-N 0.000 description 1
- AVBCFBRGFCGJKX-UHFFFAOYSA-N thieno[3,4-d][1,3]dioxole Chemical compound S1C=C2OCOC2=C1 AVBCFBRGFCGJKX-UHFFFAOYSA-N 0.000 description 1
- 125000005208 trialkylammonium group Chemical group 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical class CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Description
(A)以下の(a1)〜(a4)のステップにより、溶媒としての水と、水に油滴として分散したモノマーとしての置換チオフェンと、上記非スルホン酸系有機化合物と、を含み、且つ透明である重合液を得る調製工程、
(a1)水に置換チオフェンを添加し、水と置換チオフェンとが相分離した相分離液を得るステップ、
(a2)上記相分離液に超音波を照射することにより、置換チオフェンを油滴として分散させ、乳濁分散液を得るステップ、
(a3)上記乳濁分散液に、(a2)ステップにおける超音波の周波数より高い周波数の超音波を照射することにより、置換チオフェンの油滴のサイズを減少させ、透明分散液を得るステップ、
(a4)上記非スルホン酸系有機化合物を、支持電解質として、上記相分離液、上記乳濁分散液、又は、上記透明分散液に添加するステップ、
及び、
(B)上記調製工程で得られた重合液に上記基体を導入し、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上記基体の導電性部分の上に形成する重合工程、
を含むことを特徴とする、太陽電池用電極体の製造方法に関する。
少なくとも表面に導電性部分を有する基体と、該基体の導電性部分の上に積層された導電性ポリマー層と、を備えた本発明の太陽電池用電極体は、上記導電性ポリマー層が、モノマーとしての置換チオフェン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、を含むことを特徴とする。
(A)以下の(a1)〜(a4)のステップにより、溶媒としての水と、水に油滴として分散したモノマーとしての置換チオフェンと、上記非スルホン酸系有機化合物と、を含み、且つ透明である重合液を得る調製工程、
(a1)水に置換チオフェンを添加し、水と置換チオフェンとが相分離した相分離液を得るステップ、
(a2)上記相分離液に超音波を照射することにより、置換チオフェンを油滴として分散させ、乳濁分散液を得るステップ、
(a3)上記乳濁分散液に、(a2)ステップにおける超音波の周波数より高い周波数の超音波を照射することにより、置換チオフェンの油滴のサイズを減少させ、透明分散液を得るステップ、
(a4)上記非スルホン酸系有機化合物を、支持電解質として、上記相分離液、上記乳濁分散液、又は、上記透明分散液に添加するステップ、
及び、
(B)上記調製工程で得られた重合液に上記基体を導入し、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、
を含む方法により好適に得ることができる。以下、各工程について詳細に説明する。
(a1)ステップ
(a1)ステップでは、水にモノマーを添加し、水とモノマーとが相分離した相分離液を得る。重合液には、環境負荷が小さく、経済的にも優れる水を溶媒として使用し、モノマーとしては、水に難溶である置換チオフェン、すなわち、3位と4位に置換基を有するチオフェンを使用する。
(a2)ステップでは、(a1)ステップで得られた相分離液に超音波処理を施こすことにより置換チオフェンを油滴として分散させ、乳濁分散液を得る。乳濁分散液中では、数μm以下の直径を有する置換チオフェンの油滴が水中に高分散状態で分散しているものの、全数の10%を超える油滴が250nmを超える直径を有しており、油滴による光散乱により液全体が乳濁して見える。
(a2)ステップに続いて、乳濁分散液に(a2)ステップにおける超音波の周波数より高い周波数の超音波を照射し、置換チオフェンの油滴の平均サイズを減少させることにより、透明な分散液、すなわち、置換チオフェンの油滴数の90%以上の油滴が250nm以下の直径を有している分散液を得ることができる。非スルホン酸系有機支持電解質を相分離液に添加しなかった場合には、(a3)ステップの前に乳濁分散液に添加することもできる((a4)ステップ)。但し、この段階でボロジサリチル酸及び/又はボロジサリチル酸塩を使用する場合には、p−ニトロフェノールと併用する。
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、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作用極の導電性部分の上に形成し、太陽電池用電極体を得る。作用極の種類は、太陽電池用電極体の用途に応じて選択される。
本発明の太陽電池用電極体により、色素増感太陽電池或いは有機薄膜太陽電池を得ることができる。
実施例1
ガラス容器に蒸留水50mLを導入し、この液にEDOTを0.140g(濃度0.02M)添加し、EDOTが水と相分離した液を得た。この液に、周波数20kHz、出力22.6W/cm2の超音波を5分間照射したところ、水にEDOTが油滴として分散した乳濁分散液が得られた。この乳濁分散液に、周波数1.6MHz、出力22W/cm2の超音波を5分間、次いで周波数2.4MHz、出力7.1W/cm2の超音波を5分間照射したところ、透明分散液が得られた。この液のEDOT油滴のサイズを25℃で動的光散乱法により測定したところ、油滴の平均直径は数平均で52.2nmであり、全数の99.9%の油滴が250nm以下の直径を有しており、全数の95.2%が100nm以下の直径を有していた。この液は、常温で2日間放置しても、透明な状態を保っていた。この液に、ビス(ペンタフルオロエタンスルホニル)イミド酸ナトリウムを0.08Mの濃度で溶解させ、重合液を得た。
ビス(ペンタフルオロエタンスルホニル)イミド酸ナトリウムの代わりに、ボロジサリチル酸アンモニウムを使用し、実施例1の手順を繰り返した。
1cm2の面積を有するITO電極上に、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、150℃で30分間乾燥し、ITO電極上に導電性ポリマー層が形成された電極体を得た。
ガラス容器に蒸留水50mLを導入し、この液にEDOT0.14g(濃度0.02M)と、スルホン酸塩基を有する界面活性剤であるブチルナフタレンスルホン酸ナトリウム1.08g(濃度0.08M)とを添加し、25℃で60分間攪拌して重合液を得た。得られた重合液に、作用極としての1cm2の面積を有するITO電極、対極としての4cm2の面積を有する白金メッシュ、及び参照電極としての銀−塩化銀電極を導入し、10μA/cm2の条件で定電流電解重合を60秒間行った。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、ITO電極上に導電性ポリマー層が形成された電極体を得た。
ビス(ペンタフルオロエタンスルホニル)イミド酸ナトリウムの代わりに、p−トルエンスルホン酸ナトリウムを使用し、実施例1の手順を繰り返した。
ビス(ペンタフルオロエタンスルホニル)イミド酸ナトリウムの代わりに、クエン酸を使用し、実施例1の手順を繰り返した。
ビス(ペンタフルオロエタンスルホニル)イミド酸ナトリウムの代わりに、硝酸カリウムを使用し、実施例1の手順を繰り返した。
ビス(ペンタフルオロエタンスルホニル)イミド酸ナトリウムの代わりに、過塩素酸カリウムを使用し、実施例1の手順を繰り返した。
実施例1,2及び比較例1〜6の電極体の正孔輸送能をサイクリックボルタモグラムにより評価した。電解液としての1Mの硫酸ナトリウムを溶解した水溶液に、作用極としての実施例1,2及び比較例1〜6のいずれかの電極体、対極としての4cm2の面積を有する白金メッシュ、及び参照電極としての銀−塩化銀電極を導入し、走査電位範囲を−0.5〜+0.5Vとし、走査速度を10mV/sとして評価した。比較例3,4の電極体については、安定なサイクリックボルタモグラムを得ることができなかった。
実施例1及び比較例1の電極体の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。
実施例3
ガラス容器に蒸留水50mLを導入し、この液にEDOTを0.140g(濃度0.02M)添加し、EDOTが水と相分離した液を得た。この液に、p−ニトロフェノールを0.02M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、それぞれ添加し、周波数20kHz、出力22.6W/cm2の超音波を5分間照射したところ、水にEDOTが油滴として分散した乳濁分散液が得られた。この乳濁分散液に、周波数1.6MHz、出力22W/cm2の超音波を5分間、次いで周波数2.4MHz、出力7.1W/cm2の超音波を5分間照射したところ、透明分散液が得られた。
実施例3において得られた陰極と、鋼の基体の上にスパッタ法により1cm2の面積のPt層を設けたPt電極から成る陽極を、酸化チタン多孔質層とPt層とが対向するように張り合わせ、間隙に電解液を含浸させることにより電解質層を形成した。電解液としては、0.5Mのヨウ化リチウム、0.05Mのヨウ素、及び0.5Mの4−t−ブチルピリジンをアセトニトリルに溶解させた液を用いた。最後にエポキシ樹脂を用いて封口し、色素増感太陽電池を得た。
Claims (6)
- 少なくとも表面に導電性部分を有する基体と、該基体の導電性部分の上に積層された導電性ポリマー層と、を備え、
前記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、
を含む太陽電池用電極体の製造方法であって、
(A)以下の(a1)〜(a4)のステップにより、溶媒としての水と、水に油滴として分散した前記モノマーと、前記非スルホン酸系有機化合物としての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と、を含み、且つ透明である重合液を得る調製工程、
(a1)水に前記モノマーを添加し、水と前記モノマーとが相分離した相分離液を得るステップ、
(a2)前記相分離液に超音波を照射することにより、前記モノマーを油滴として分散させ、乳濁分散液を得るステップ、
(a3)前記乳濁分散液に、(a2)ステップにおける超音波の周波数より高い周波数の超音波を照射することにより、前記モノマーの油滴のサイズを減少させ、透明分散液を得るステップ、
(a4)前記非スルホン酸系有機化合物としての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を、支持電解質として、前記相分離液、前記乳濁分散液、又は、前記透明分散液に添加するステップ、
及び、
(B)前記調製工程で得られた重合液に前記基体を導入し、電解重合を行うことにより、前記モノマーの重合により得られた導電性ポリマー層を前記基体の導電性部分の上に形成する重合工程、
を含むことを特徴とする、太陽電池用電極体の製造方法。 - (a2)ステップにおける超音波が15〜200kHzの範囲の周波数及び4W/cm2以上の出力を有する、請求項1に記載の太陽電池用電極体の製造方法。
- (a3)ステップにおける超音波が1〜4MHzの範囲の周波数及び5W/cm2以上の出力を有する、請求項1又は2に記載の太陽電池用電極体の製造方法。
- (a2)ステップにおける超音波照射時間が2〜10分の範囲であり、(a3)ステップにおける超音波照射時間が2〜10分の範囲である、請求項1〜3のいずれか1項に記載の太陽電池用電極体の製造方法。
- 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1〜4のいずれか1項に記載の太陽電池用電極体の製造方法。
- 前記基体が透明である、請求項1〜5のいずれか1項に記載の太陽電池用電極体の製造方法。
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