JPWO2015146012A1 - 光電気化学セル、光電気化学セルの製造方法、および光電気化学反応装置 - Google Patents
光電気化学セル、光電気化学セルの製造方法、および光電気化学反応装置 Download PDFInfo
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- JPWO2015146012A1 JPWO2015146012A1 JP2016509971A JP2016509971A JPWO2015146012A1 JP WO2015146012 A1 JPWO2015146012 A1 JP WO2015146012A1 JP 2016509971 A JP2016509971 A JP 2016509971A JP 2016509971 A JP2016509971 A JP 2016509971A JP WO2015146012 A1 JPWO2015146012 A1 JP WO2015146012A1
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Images
Classifications
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- H01G9/20—Light-sensitive devices
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Abstract
Description
図1Aおよび図1Bは実施形態による光電気化学セルの第1の例を示す図である。図1Aは光電気化学セルの平面図、図1Bは図1AのX−X線に沿った断面図である。図1Aおよび図1Bに示す光電気化学セル1は、光電変換層2と、光電変換層2の第1の面上に設けられた第1の電極3と、光電変換層2の第2の面上に設けられた第2の電極4とを具備している。第1の電極3上には、第1の触媒層5が設けられている。第2の電極4上には、導電性支持体6を介して第2の触媒層7が設けられている。光電気化学セル1の側面は、光電変換層2のリーク電流および電解液による浸食を防ぐために、絶縁層8で覆われている。第1および第2の電極3、4は、光電変換層2に対してオーミック接触を形成しており、第1の電極3から第2の電極4まで直列に接続されている。ここでは、光電変換層2の第1の面(第1の電極3の形成面)が受光面である場合について説明する。
次に、実施形態の光電気化学反応装置について、図8および図9を参照して説明する。図8は実施形態による光電気化学反応装置の第1の例を示す断面図である。図8に示す光電気化学反応装置21は、前述した実施形態の光電気化学セル1が配置された電解槽22を備えている。光電気化学反応装置21は、電解液23が収容された電解槽22と、電解槽22内に配置され、電解液23に浸漬された光電気化学セル1とを備えている。電解槽22は、光電気化学セル1により二室に分離されている。電解槽22は、第1の電解液23Aが充填され、第1の電解液23Aに第1の触媒層5を浸漬させる第1の液室22Aと、第2の電解液23Bが充填され、第2の電解液23Bに第2の触媒層7を浸漬させる第2の液室22Bとに分離されている。
2H2O → 4H++O2+4e− …(1)
2CO2+4H++4e− → 2CO+2H2O …(2)
実施例1では、三接合型光電変換層の光入射面側に複数の触媒部9とそれらの間隙に配置された透明誘電体部10とで構成された第1の触媒層5を配置した光電気化学セル1を作製し、その特性を評価した。図11は三接合型光電気化学セルの構造を示している。
セルのITO層全面に薄膜状のNi(OH)2触媒のみを形成する以外は、実施例1と同一の構造を有するセルを準備した。Ni(OH)2触媒の厚さは15nmであった。
Ni(OH)2触媒層の厚さを30nmにする以外は、比較例1−1と同一の構造を有するセルを準備した。
Ni(OH)2触媒層の厚さを45nmにする以外は、比較例1−1と同一の構造を有するセルを準備した。
実施例2では、触媒/透明誘電体の複合構造における触媒部の面積率が異なる8種類の光電気化学セルを作製して評価した。セルの作製方法は、実施例1と同様とした。この際、感光性エポキシ樹脂の露光時に用いるマスクパターンを任意に変えることによって、実施例2−1〜2−8のセルで径の異なる開口部パターンを有する透明誘電体部を形成した。その後、開口部に500nmのNi(OH)2触媒層を形成した。触媒/透明誘電体の複合構造は、三角格子状とした。触媒部間の平均距離は、100μmであった。触媒部の径を変えることにより面積率を制御した。還元触媒は、実施例1と同様とした。
実施例3では、触媒/透明誘電体の複合構造において触媒層の高さの異なる光電気化学セルを作製して評価した。実施例1と同様の構造体を準備し、実施例1と同様に、感光性エポキシ樹脂をITO層上に塗布し、露光・現像処理により感光性エポキシ樹脂層にライン状の開口部を設けた。感光性エポキシ樹脂の厚さは1μmとした。その後、開口部に電着法により水酸化触媒として酸化コバルト層を形成した。1μmより厚い触媒層を形成する場合は、感光性エポキシ樹脂層を形成する触媒層の厚さより十分に厚い膜厚に塗布した後、露光・現像処理による開口パターンの形成および電着による触媒層の形成を行った。最後に、酸素と四フッ化炭素(CF4)の混合ガスを用いた反応性イオンエッチング(RIE)により感光性エポキシ樹脂層のみを厚さ1μmになるまでエッチングした。
セルのITO面上に薄膜状の酸化コバルト触媒のみを形成する以外は、実施例3と同一の構造を有するセルを準備した。酸化コバルト触媒の厚さは10nmであった。
酸化コバルト触媒層の厚さを50nmにする以外は、比較例3−1と同一の構造を有するセルを準備した。
実施例4では、触媒部間の距離が異なる触媒/透明誘電体の複合構造を有する光電気化学セルを作製して評価した。実施例1と同様の構造体を準備した。次に、ITO層上に触媒/透明誘電体の複合構造を形成した。ITO層上にレジスト層をスピンコートにより塗布した。次に、i線または電子線による露光処理を行い、続いて現像処理を行うことによって、レジスト層に開口パターンを形成した。続いて、レジスト層の開口部に電着により水酸化触媒として1μmの酸化コバルトを形成した。その後、レジスト層のみを有機溶剤を用いて剥離し、透明誘電体層としてフッ素樹脂(サイトップ(商品名、旭硝子社製))を触媒層上に塗布した。最後に、酸素とCF4の混合ガスを用いたRIE処理を行うことによって、触媒層が露出するまで透明誘電体層を選択エッチングし、触媒/透明誘電体の複合構造をITO層上に形成した。
セルのITO面上に薄膜状の酸化コバルト触媒のみを形成する以外は、実施例4と同一の構造を有するセルを準備した。酸化コバルト触媒の厚さは10nmであった。
酸化コバルト触媒層の厚さを50nmにする以外は、比較例4−1と同一の構造を有するセルを準備した。
実施例5では、光電気化学セルの光入射面に還元触媒層が配置されるセルを作製して評価した。まず、InGaP層、InGaAs層、およびGe層からなるpn接合型の三接合光電変換層、光電変換層の入射面上に形成されたITO透明導電膜、光電変換層の裏面上に形成されたAu電極を有する構造体を準備した。
セルのITO面上に薄膜状のAu触媒のみを形成する以外は、実施例5と同一の構造を有するセルを準備した。Au触媒の厚さは5nmであった。
Au触媒層の厚さを10nmにする以外は、比較例5−1と同一の構造を有するセルを準備した。
光電変換層として実施例1と同様の構造体を準備した。次に、SUS基板の裏面にスパッタ法により厚さ1μmの水素発生触媒として白金膜を形成した。続いて、厚さ50μmの感光性エポキシ樹脂をITO層上に塗布し、露光・現像処理により感光性エポキシ樹脂層にドット状の開口部を設けた。その後、開口部に電解めっきにより導電層としてニッケルを50μmの厚さで形成した。続いて、O2とCF4の混合ガスを用いたRIE処理により感光性エポキシ樹脂層のみを厚さ5μmになるまでエッチングした。この際、ニッケル層は円柱状の形をしていた。
実施例6−2においては、ニッケル層を電解めっきで形成するまでは実施例6−1と同様とし、その後のO2とCF4の混合ガスを用いたRIE処理で感光性エポキシ樹脂層が5.5μmになるまでエッチングした。次いで、アルゴンプラズマのみを用いたRIE処理を行うことで、ニッケルピラー部を先鋭化してテーパー状にした。次いで、O2とCF4の混合ガスを用いたRIE処理を再度行い、感光性エポキシ樹脂層が厚さ5μmになるまでエッチングした。その後、ニッケル層表面に電着により厚さ20nmの水酸化コバルト触媒を形成し、実施例6−1と同様にして1cm2のセルを作製した。
実施例7では、透明誘電体層として無機材料の陽極酸化アルミニウム膜を有する光電気化学セルを作製して評価した。まず、光電変換層として実施例1と同様のpin型のa−Si/a−SiGe/a−SiGeからなる三接合型の光電変換層(厚さ500nm)、光電変換層上の透明導電膜としてITO電極(厚さ100nm)、光電変換層下面の電極層としてZnO電極(厚さ300nm)を有し、電極層下面にAg反射層(厚さ200nm)および支持基板としてSUS基板(厚さ1.5μm)を有する構造体を準備した。
セルのITO層上に薄膜状の酸化コバルト触媒のみを形成する以外は、実施例7と同一の構造を有するセルを準備した。酸化コバルト触媒の厚さは10nmであった。
酸化コバルト触媒層の厚さを50nmにする以外は、比較例7−1と同一の構造を有するセルを準備した。
実施例8では、導電部と触媒部との積層部間の間隙に透明誘電体部を配置した触媒層を有する光電気化学セルを作製して評価した。まず、実施例1と同様に、ITO電極(厚さ100nm)、pin型のa−Si/a−SiGe/a−SiGeからなる三接合型の光電変換層(厚さ500nm)、ZnO電極(厚さ300nm)、Ag反射層(厚さ200nm)、およびSUS基板(厚さ1.5μm)を有する構造体を準備した。
TiN膜およびTiNの酸化被膜を形成することなく、セルのITO層全面に薄膜状のNi(OH)2触媒のみを形成する以外は、実施例8と同一の構造を有するセルを準備した。Ni(OH)2触媒の厚さは15nmであった。
Ni(OH)2触媒層の厚さを30nmにする以外は、比較例8−1と同一の構造を有するセルを準備した。
Ni(OH)2触媒層の厚さを45nmにする以外は、比較例8−1と同一の構造を有するセルを準備した。
TiN膜およびTiNの酸化被膜を形成することなく、セルのITO層上に実施例8と同様な間隙を有するNi(OH)2触媒を形成する以外は、実施例8と同一の構造を有するセルを準備した。
実施例9では、光電気化学セルの光入射面にライン状の還元触媒層を配置したセルを作製して評価した。まず、InGaP層、InGaAs層、およびGe層からなるpn接合型の三接合光電変換層、光電変換層の入射面上に形成されたITO透明導電膜、光電変換層の裏面上に形成されたAu電極を有する構造体を準備した。三接合光電変換層の詳細な構成は、実施例5と同様とした。
セルのITO面上に薄膜状のAu触媒層のみを形成する以外は、実施例9と同一の構造を有するセルを準備した。Au触媒層の厚さは5nmであった。
Au触媒層の厚さを10nmにする以外は、比較例9−1と同一の構造を有するセルを準備した。
Al膜を形成することなく、セルのITO層上に実施例9と同様な間隙を有するAu触媒層を形成する以外は、実施例9と同一の構造を有するセルを準備した。
Claims (15)
- 第1の面と第2の面とを有する光電変換層と、
前記光電変換層の前記第1の面上に設けられた第1の電極と、
前記第1の電極上に配置された複数の触媒部と、前記複数の触媒部間の間隙に配置された透明誘電体部とを備える第1の触媒層と、
前記光電変換層の前記第2の面上に設けられた第2の電極と、
前記第2の電極と電気的に接続された第2の触媒層と
を具備する光電気化学セル。 - 前記第1の触媒層は、さらに前記第1の電極上に配置された導電部を備え、前記触媒部は前記導電部上に設けられている、請求項1に記載の光電気化学セル。
- 前記導電部はテーパー形状を有し、前記触媒部は前記テーパー形状の導電部の表面に沿って設けられている、請求項2に記載の光電気化学セル。
- 前記導電部は、金属、前記金属を含む合金、および前記金属を含む導電性化合物からなる群より選ばれる少なくとも1つを含有し、
前記触媒部は、前記導電部上に設けられており、
前記透明誘電体部は、前記金属を含む絶縁性化合物を含有する、請求項2に記載の光電気化学セル。 - 前記導電部は、前記金属または前記金属の窒化物からなり、
前記透明誘電体部は、前記金属の酸化物からなる、請求項4に記載の光電気化学セル。 - 前記透明誘電体部は、10nm以上1mm以下の厚さを有する、請求項1に記載の光電気化学セル。
- 前記触媒部は、金属および金属酸化物の少なくとも一方を含む、請求項1に記載の光電気化学セル。
- 前記第1の電極は、透光性を有する導電膜を備える、請求項1に記載の光電気化学セル。
- 前記触媒部は、ドット状または線状の平面形状を有する、請求項1に記載の光電気化学セル。
- 前記複数の触媒部は、前記間隙が10nm以上2mm以下となるように配置されている、請求項1に記載の光電気化学セル。
- 前記第1および第2の触媒層の一方で酸化反応が生起され、前記第1および第2の触媒層の他方で還元反応が生起される、請求項1に記載の光電気化学セル。
- 第1の面と第2の面とを有する光電変換層と、前記光電変換層の前記第1の面上に設けられた第1の電極と、前記光電変換層の前記第2の面上に設けられた第2の電極とを備える積層体を用意する工程と、
前記第1の電極上に複数の触媒部を配置すると共に、前記複数の触媒部間の間隙に透明誘電体部を配置することにより、前記触媒部と前記透明誘電体部とを備える第1の触媒層を形成する工程と、
前記第2の電極と電気的に接続された第2の触媒層を形成する工程と
を具備する光電気化学セルの製造方法。 - 前記第1の触媒層の形成工程は、
金属、前記金属を含む合金、および前記金属を含む導電性化合物からなる群より選ばれる少なくとも1つを含有する導電膜を形成する工程と、
前記導電膜上に複数の触媒部を配置する工程と、
前記導電膜の前記複数の触媒部間に露出する部分を選択的に酸化することにより、前記透明誘電体部を形成する工程と
を具備する、請求項12に記載の光電気化学セルの製造方法。 - 電解液が収容された電解槽と、
前記電解槽内に配置され、前記電解液中に浸漬された、請求項1に記載の光電気化学セルと
を具備する光電気化学反応装置。 - 前記電解槽は、前記光電気化学セルにより二室に分離されており、かつイオン交換膜を含むイオン移動経路を備える、請求項14に記載の光電気化学反応装置。
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
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JP2014059594 | 2014-03-24 | ||
JP2014059594 | 2014-03-24 | ||
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JP2003288955A (ja) * | 2002-03-27 | 2003-10-10 | Research Institute Of Innovative Technology For The Earth | 太陽光を利用した水素の製造方法及び太陽光を利用した水素の製造装置 |
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