WO2012036010A1 - 電解質組成物用添加剤及びこの添加剤を用いた電解質組成物並びに色素増感太陽電池 - Google Patents
電解質組成物用添加剤及びこの添加剤を用いた電解質組成物並びに色素増感太陽電池 Download PDFInfo
- Publication number
- WO2012036010A1 WO2012036010A1 PCT/JP2011/070142 JP2011070142W WO2012036010A1 WO 2012036010 A1 WO2012036010 A1 WO 2012036010A1 JP 2011070142 W JP2011070142 W JP 2011070142W WO 2012036010 A1 WO2012036010 A1 WO 2012036010A1
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- WIPO (PCT)
- Prior art keywords
- dye
- additive
- electrolyte composition
- tio
- pyridine
- Prior art date
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Classifications
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- H—ELECTRICITY
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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
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
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- H—ELECTRICITY
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- 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
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- H01G9/022—Electrolytes; Absorbents
- H01G9/035—Liquid electrolytes, e.g. impregnating materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01G9/20—Light-sensitive 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
- H01G9/2004—Light-sensitive devices characterised by the electrolyte, e.g. comprising an organic electrolyte
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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
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
Definitions
- the pyridine derivative having an alkylsilyl group introduced into the pyridine ring has reasons such as an increase in electric dipole moment, an increase in molecular size, and an increase in HOMO level due to the introduction of the alkylsilyl group into the pyridine ring. Therefore, compared with the case where conventional 4-TBpy is used as an additive for an electrolyte composition, it is possible to suppress a decrease in short-circuit current and improve an open circuit voltage, resulting in high photoelectric conversion efficiency.
- the TiO 2 nanoparticle dispersed paste is applied to the conductive film 14b of the base material 14a by a squeegee method, screen printing method, electrodeposition method, spray method, DJP (Direct jet printing). After applying by a method or the like and press-molding as necessary, a porous TiO 2 thin film 15b is formed on the conductive film 14b by microwave irradiation or the like.
- Electrolyte composition 7 types of electrolyte compositions A to G having different electrolyte composition additives were prepared.
- the blending components and ratios of the electrolyte compositions A to G are shown in Table 1 below.
- the pyridines shown by the following structural formula were used for the additive for electrolyte compositions.
- a sandwich type open cell 20 shown in FIG. 4 was produced.
- the photoelectrode 21 is formed by forming a dye adsorbing porous TiO 2 thin film 25 of 1.2 cm ⁇ 1.2 cm and a thickness of 16.5 ⁇ m at the center of the glass 24 with FTO film, and the counter electrode 22 is made of platinum.
- a glass 26 with an FTO film sputtered to a thickness of about 30 nm was used.
- a 30 ⁇ m-thick polyethylene film was used as the spacer 27, and a 15 mm ⁇ 40 mm window portion 27 a for injecting the electrolyte composition 23 was provided at the center.
- conductive copper foil tapes 28 and 29 having a width of 3 mm were attached to the edges of the photoelectrode 21 and the counter electrode 22.
- 4-TMSpy is considered an ideal additive for electrolyte compositions that can greatly increase the open-circuit voltage V oc and fill factor FF without substantially reducing the short-circuit current density J sc. It became clear that it has the following characteristics. This high photoelectric conversion efficiency is based on the elemental characteristics of silicon. (1) Increase in electric dipole moment, (2) Increase in molecular size, (3) HOMO level by introducing an alkylsilyl group into a specific part of the pyridine ring It is interpreted as the rise of
- Short circuit in the case of using an electrolyte composition (electrolyte composition A, H, K, and N) to which no pyridine-based additive (4-TBpy or 4-TMSpy) is added to express a short circuit current reduction deterrent
- the current value is 1, and the short-circuit current value when the pyridine-based additive is added is shown in Table 5 as a relative ratio.
- the parentheses in the table represent the type of electrolyte composition.
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Abstract
Description
<電解質組成物及びその添加剤>
色素増感太陽電池における電解質組成物としては、通常、有機溶媒中にヨウ素レドックス(I3 -/I-)を含有させた組成物が用いられる。この組成物中に、塩基性化合物を添加することにより、光電変換効率の改善を試みた研究が数多くなされている。例えば、ピリジン誘導体、ピリミジン誘導体、アミノピリジン誘導体、キノリン誘導体、イミダゾール誘導体、ベンズイミダゾール誘導体、ピラゾール誘導体、アミノトリアゾール誘導体、アミノチアゾール誘導体などのヘテロ環式化合物がこれまでに検討され、現在までのところ、4-TBpyが最も色素増感太陽電池の変換効率改善に有効な電解質組成物用添加剤としてよく知られている。
(1) 4-TBpyがTiO2ナノ粒子表面に吸着した結果、TiO2表面と電子受容電解質(I3 -)との接触が物理的に阻止され、電荷再結合(TiO2からI3 -への逆電子移動;リーク電流)が抑制される。
(2) 4-TBpyがTiO2ナノ粒子表面に吸着した結果、4-TBpyの塩基性により、TiO2の伝導帯端(Conduction Band Edge;CBE)のポテンシャルが負側ヘシフトする。また、電解質組成物中にカウンターカチオンとしてLi+イオンが含まれる場合(LiIとして電解質組成物中に添加)、Li+がTiO2に吸着又はインターカレートし、TiO2のCBEポテンシャルを正側にシフトさせるが、4-TBpyはLi+とTiO2との相互作用を妨害すると考えられている。この結果として、4-TBpyの添加によりTiO2のCBE準位(正確にはフェルミレベル;Vf)とレドックスメディエーターの酸化還元電位(Vred)との差で規定される開放電圧(Voc=|Vf-Vred|)は向上する。
(3) 4-TBpyとヨウ素分子とが1:1の電荷移動錯体を形成する。この錯体においては、密度汎関数計算により、ヨウ素のσ*軌道とピリジン環窒素の孤立電子対が相互作用していることが明らかになっている。ここで、電荷移動錯体(4-TBpy)I2を形成した結果、以下の式(2)で示すように、TiO2表面における電子受容電解質(I3 -)濃度が減少し、TiO2からI3 -への逆電子移動が抑制される。この結果、開放電圧が向上する。
<色素増感太陽電池の製造方法>
続いて、上記電解質組成物用添加剤を用いた色素増感太陽電池の製造方法を説明する。
<TiO2ナノ粒子分散ペーストの調製>
・ スピンコート用ぺースト(SCぺースト)の調製
先ず、TiO2ナノ粒子として、高い分散性が報告されているP-25(日本アエロジル社製)を選択した。なお、P-25は、結晶構造割合がアナターゼ:ルチル=8:2、平均粒径が21nm、BET表面積が50m2/gである。次に、イオン交換水70mL、硝酸0.2mL、TiO2ナノ粒子31g、アセチルアセトン1.5mL、非イオン性界面活性剤(Triton X-100)0.5gを成分とする混合液に対して、ホモジナイザーを用いて分散操作を行うことにより、TiO2ナノ粒子を分散させたSCぺーストを調製した。
先ず、TiO2ナノ粒子として、高い分散性が報告されているP-25(日本アエロジル社製)、上記P-25に比べて若干の凝集性を有するST-21(石原産業社製)及びAMT-600(テイカ社製)、また、100nm以上の比較的大きな粒径を有するTITANIX JA-1(テイカ社製)を所定の割合で混合した混合粒子を選択した。なお、ST-21は、結晶構造割合がアナターゼ100%、平均粒径が20nm、BET表面積が50m2/gである。また、AMT-600は、結晶構造割合がアナターゼ100%、平均粒径が30nm、BET表面積が52m2/gである。また、TITANIX JA-1は、結晶構造割合がアナターゼ100%、平均粒径が180nm、BET表面積が9m2/gである。次に、イオン交換水300mL、硝酸1.0mL、TiO2ナノ粒子(ST-21)4.0g、TiO2ナノ粒子(P-25)3.0g、TiO2ナノ粒子(AMT-600)2.0g、TiO2ナノ粒子(TITANIX JA-1)1.0gを成分とする混合液に対して、ホモジナイザーを用いて分散操作を行うことにより、TiO2ナノ粒子分散液を作製した。更に、このTiO2ナノ粒子分散液にポリエチレングリコール2000 10.0gを加え、水の量を8.0gに調節することにより、TiO2ナノ粒子を分散させたSPぺーストを調製した。
先ず、酸化錫にフッ素をドープした膜を有するFTOガラス(旭ガラス社製;A110U80)を用意した。次いで、このFTOガラスを中性洗剤水溶液、イオン交換水、メタノール中で順次超音波洗浄し、乾燥後、UV-O3洗浄装置を用いたFTOガラス表面の清浄処理を行った。そして清浄処理後すぐに、TiCl4処理を行った。TiCl4処理は、40mmol/LのTiCl4水溶液中にFTOガラスを浸漬して70℃で30分間保持し、その後、イオン交換水及びエタノールで洗浄することにより行われる。このTiCl4処理を施すことで、TiO2ナノ粒子とFTOとの密着性を向上させる、及びFTOから電解質組成物への逆電子移動を防ぐ効果が得られる。
増感色素には、以下の構造式で示され、N3色素として知られている標準的な増感色素シス-ジ(チオシアナト)-ビス(2,2'-ビピリジル-4,4'-ジカルボン酸)ルテニウム(II)(cis-di(thiocyanato)-bis(2,2'-bipyridyl-4,4'-dicarboxylic acid)ruthenium(II)、Ruthenium 535;SOLARONIX)を使用した。
次に、電解質組成物用添加剤の異なる7種類の電解質組成物A~Gを用意した。電解質組成物A~Gの配合成分及びその割合を次の表1に示す。また、電解質組成物用添加剤は次の構造式で示されるピリジン類を使用した。
色素増感太陽電池の光発電特性を評価するために、図4に示すサンドイッチ型オープンセル20を作製した。光電極21には、FTO膜付きガラス24の中央部に1.2cm×1.2cm、厚さ16.5μmの色素吸着多孔質TiO2薄膜25を形成したものを、対電極22には白金を約30nm厚にスパッタしたFTO膜付きガラス26を使用した。スペーサー27には厚さ30μmのポリエチレンフィルムを使用し、その中央部には電解質組成物23を注入するための15mm×40mmの窓部分27aを設けた。また、光電極21及び対電極22の縁部には、3mm幅で導電性銅箔テープ28,29を貼り付けた。
電解質組成物A~Gを用いて作製したセルの光発電特性は、遮光マスクを用いてセルのアパーチャ面積を12.0mm角の1.44cm2とし、光照射下におけるI-V曲線により評価した。I-V曲線は、色素増感太陽電池測定における標準試験条件(Standard Test Conditions:STC)に基づき、25±2℃において、擬似太陽光(Global-1 sun;AM-1.5G,100mWcm-2)をセルに垂直照射することにより測定した。
<光電極の作製(TiO2)>
先ず、FTOガラス基板(2.5×5cm)の表面をベンコット(旭化成せんい株式会社製)で拭き、マスキングテープ(厚さ58μm)で2.5×1.5cmのサイズにマスキングした。次に、10重量%となるように酸化チタン粉末(Ti-NanoxideD、ソーラロニクス社製)を、水に懸濁したものを用いて、スキージ法にて塗布した。マスキングテープを剥がし取り、この基板を電気炉により450℃で焼成し、厚さ5μmの金属酸化物半導体層を形成した。続いて、表3に記載の色素及び溶媒を3×10-4Mに調製した色素溶液に、上記作製した金属酸化物半導体層を10時間浸漬して色素吸着させた。吸着後、表面の余分な色素をエタノールで洗い流し、ドライヤーで乾燥させた。
上記光電極の作製(TiO2)と同様に、マスキングした基板に酸化チタン粉末を用いたスキージ法の代わりに、酸化亜鉛ペースト(ソーラー社製)をスピンコート(300rpm、1分)法にて塗布し、120℃、10分乾燥の工程を6回繰り返した。マスキングテープを剥がし取り、この基板を電気炉により450℃で焼成し、厚さ5μmの金属酸化物半導体層を形成した。続いて、表3に記載の色素及び溶媒を3×10-4Mに調製した色素溶液に、上記作製した金属酸化物半導体層を10時間浸漬して色素吸着させた。吸着後、表面の余分な色素をエタノールで洗い流し、ドライヤーで乾燥させた。
電解質濃度、電解質組成物用添加剤及び溶媒の異なる電解質組成物A、C、D及びH~Yを用意した。電解質組成物の配合成分及びその割合を次の表4に示す。
表3の光電極及び表4の電解液組成物を下記表5の組み合わせで用いて、実施例1の<オープンセルの組み上げ>と同様に、図4に示すサンドイッチ型オープンセル20を作製した。
組み上げたオープンセルの光発電特性は、遮光マスクを用いてセルのアパーチャ面積を1cm2とし、光照射下におけるI-V曲線により評価した。I-V曲線は、色素増感太陽電池測定における標準試験条件(STC)に基づき実施例1と同様に測定した。短絡電流の低下抑止力を表すために、ピリジン系添加剤(4-TBpy又は4-TMSpy)を加えない電解液組成物(電解液組成物A、H、K及びN)を用いた場合の短絡電流値を1として、ピリジン系添加剤を添加した場合の短絡電流値を相対比として表5に示す。尚、表中の括弧内は電解質組成物の種類を表す。
11 光電極
12 対電極
13 電解質組成物
Claims (9)
- ピリジン環にアルキルシリル基を導入したピリジン誘導体を含むことを特徴とする色素増感太陽電池に用いる電解質組成物用添加剤。
- 前記ピリジン誘導体が、ピリジン環の4位にアルキルシリル基を有する請求項1記載の電解質組成物用添加剤。
- 前記ピリジン誘導体が4-(トリメチルシリル)ピリジンである請求項1又は2記載の電解質組成物用添加剤。
- ピリジン環にアルキルシリル基を導入したピリジン誘導体を含む電解質組成物用添加剤を添加したことを特徴とする色素増感太陽電池に用いる電解質組成物。
- 前記ピリジン誘導体が、ピリジン環の4位にアルキルシリル基を有する請求項4記載の電解質組成物。
- 前記ピリジン誘導体が4-(トリメチルシリル)ピリジンである請求項4又は5記載の電解質組成物。
- ピリジン環にアルキルシリル基を導入したピリジン誘導体を含む電解質組成物用添加剤を添加した電解質組成物を用いたことを特徴とする色素増感太陽電池。
- 前記ピリジン誘導体が、ピリジン環の4位にアルキルシリル基を有する請求項7記載の色素増感太陽電池。
- 前記ピリジン誘導体が4-(トリメチルシリル)ピリジンである請求項7又は8記載の色素増感太陽電池。
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CN201180039877.6A CN103069645B (zh) | 2010-09-16 | 2011-09-05 | 电解质组合物用添加剂及使用了该添加剂的电解质组合物以及染料敏化太阳能电池 |
US13/819,595 US9818551B2 (en) | 2010-09-16 | 2011-09-05 | Additive for electrolytic composition, electrolytic composition using this additive, and dye-sensitized solar cell |
JP2012533945A JP5702394B2 (ja) | 2010-09-16 | 2011-09-05 | 電解質組成物用添加剤及びこの添加剤を用いた電解質組成物並びに色素増感太陽電池 |
KR1020137004017A KR20140009967A (ko) | 2010-09-16 | 2011-09-05 | 전해질 조성물용 첨가제 및 이 첨가제를 사용한 전해질 조성물 및 색소 증감 태양전지 |
EP11825016.6A EP2618420B1 (en) | 2010-09-16 | 2011-09-05 | Additive for use in dye-sensitized solar cell |
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JP2015520509A (ja) * | 2012-05-08 | 2015-07-16 | エルジー・ケム・リミテッド | 色素増感太陽電池およびその製造方法{dye−sensitizedsolarcellandmethodformanufacturingsame} |
JP2015201569A (ja) * | 2014-04-09 | 2015-11-12 | 株式会社フジコー | 色素増感太陽電池用アノードの製造方法及び色素増感太陽電池の製造方法 |
JP2019009240A (ja) * | 2017-06-22 | 2019-01-17 | 石川県 | 色素増感太陽電池および色素増感太陽電池の製造方法 |
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US20180025849A1 (en) * | 2015-02-13 | 2018-01-25 | Rensselaer Polytechnic Institute | Solar cell employing phosphorescent materials |
TWI671933B (zh) * | 2017-11-03 | 2019-09-11 | 長興材料工業股份有限公司 | 電解質組合物及其應用 |
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JP2015520509A (ja) * | 2012-05-08 | 2015-07-16 | エルジー・ケム・リミテッド | 色素増感太陽電池およびその製造方法{dye−sensitizedsolarcellandmethodformanufacturingsame} |
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JP2019009240A (ja) * | 2017-06-22 | 2019-01-17 | 石川県 | 色素増感太陽電池および色素増感太陽電池の製造方法 |
Also Published As
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TWI510497B (zh) | 2015-12-01 |
KR20140009967A (ko) | 2014-01-23 |
CN103069645B (zh) | 2016-01-20 |
EP2618420A4 (en) | 2014-10-22 |
US9818551B2 (en) | 2017-11-14 |
US20130161555A1 (en) | 2013-06-27 |
EP2618420B1 (en) | 2016-12-07 |
EP2618420A1 (en) | 2013-07-24 |
CN103069645A (zh) | 2013-04-24 |
JP5702394B2 (ja) | 2015-04-15 |
TW201217391A (en) | 2012-05-01 |
JPWO2012036010A1 (ja) | 2014-02-03 |
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