JPWO2017164191A1 - 光電極、水分解用光電気化学システム及び光電極の製造方法 - Google Patents
光電極、水分解用光電気化学システム及び光電極の製造方法 Download PDFInfo
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- 239000010935 stainless steel Substances 0.000 claims abstract description 37
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 36
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- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
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- 239000008096 xylene Substances 0.000 description 2
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- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
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- 238000000354 decomposition reaction Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
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- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
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- 229910052710 silicon Inorganic materials 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000003115 supporting electrolyte Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
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Abstract
Description
ステンレス系材料からなる金属基板の少なくともいずれか一方の面上にスズ酸化物からなる中間層を形成して、前記金属基板と前記中間層とを備える積層体を得る第1の工程と、
前記中間層の前記金属基板と反対の面上に、V及びBiを含有するバナジン酸ビスマス前駆体溶液を用いてバナジン酸ビスマスからなる光触媒層を形成して、前記金属基板と、前記金属基板の少なくともいずれか一方の面上に積層された前記中間層と、前記中間層の前記金属基板と反対の面上に積層された前記光触媒層と、を備える光電極を得る第2の工程と、
を含むものである。
ステンレス系材料からなる金属基板の少なくともいずれか一方の面上にスズ酸化物からなる中間層を形成して、前記金属基板と前記中間層とを備える積層体を得る第1の工程と、
前記中間層の前記金属基板と反対の面上に、V及びBiを含有するバナジン酸ビスマス前駆体溶液を用いてバナジン酸ビスマスからなる光触媒層を形成して、前記金属基板と、前記金属基板の少なくともいずれか一方の面上に積層された前記中間層と、前記中間層の前記金属基板と反対の面上に積層された前記光触媒層と、を備える光電極を得る第2の工程と、
を含む。ステンレス系材料からなる金属基板、スズ酸化物からなる中間層、バナジン酸ビスマスからなる光触媒層、及びこれらを備える光電極としては、前述の本発明の光電極で述べたとおりである。
先ず、SUS304からなる厚さ1.0mmの金属基板の一方の面(3.1cm2)をアセトン洗浄した後、その面に、スパッタリング装置(株式会社パスカル製)を用いて、アルゴンガス雰囲気下(酸素濃度約0容量%)、ターゲット酸化第二スズ(SnO2)、圧力2.0Pa、温度500℃の条件で、酸化第二スズからなる中間層を形成し、前記金属基板と前記中間層とを備える積層体を得た。前記中間層の厚さは100nmとなるようにした。また、中間層の単位面積あたりの質量は0.2mg/cm2であった。次いで、前記積層体を、空気中において、500℃で1.0時間焼成し、前記金属基板の前記中間層に覆われていない面上全てに酸化被膜を形成させた。
先ず、SUS304からなる厚さ1.0mmの金属基板の一方の面(3.1cm2)をアセトン洗浄した後、その面にITOをスパッタ法で成膜して中間層を形成し、前記金属基板と前記中間層とを備える積層体を得た。前記中間層の厚さは300nmとなるようにした。実施例1の積層体に代えてこの積層体を用いたこと以外は、実施例1と同様にして金属基板/中間層/光触媒層が順に積層された光電極を得た。
中間層を形成しなかったこと以外は実施例1と同様にして、金属基板/光触媒層が順に積層された光電極を得た。
実施例1〜2及び比較例1で得られた各光電極の金属基板に導線を介してポテンショスタットを接続し、ポテンショスタットには導線を介して参照電極(銀−塩化銀電極)及び前記光電極の対極(白金電極)を接続した。前記光電極、前記参照電極及び前記対極がホールスカベンジャー(亜硫酸ナトリウム)含有アルカリ金属ホウ酸塩水溶液(ホウ酸ナトリウム緩衝溶液、pH8.5)に浸るように設置し、前記光電極の光触媒層面にソーラーシュミレータで光(擬似太陽光、強さ:100mW/cm2)を照射し、電流密度−対銀−塩化銀電極電圧曲線を得た。また、対銀−塩化銀電極電圧を対RHE(可逆水素電極)電圧に換算して、電流密度−対RHE電圧曲線(電流−電圧特性曲線)を得た。実施例1及び比較例1の光電極を用いて得られた電流−電圧特性曲線を図5に、実施例2及び比較例1の光電極を用いて得られた電流−電圧特性曲線を図6に、それぞれ示す。
先ず、SUS304からなる厚さ1.0mmの金属基板の一方の面(3.1cm2)をアセトン洗浄した後、その面に、スパッタリング装置(株式会社パスカル製)を用いて、アルゴンガス雰囲気下(酸素濃度約0容量%)、ターゲット酸化第二スズ(SnO2)、圧力2.0Pa、温度500℃の条件で、酸化第二スズからなる第1の中間層を形成し、前記金属基板と前記第1の中間層とを備える積層体を得た。前記第1の中間層の厚さは65nmとなるようにした。
実施例3で得られた光電極について、実施例1と同様にして電流測定を実施し、電流−電圧特性曲線を得た。実施例1において得られた電流−電圧特性曲線(光照射有り)と、実施例3において得られた電流−電圧特性曲線(光照射有り)とから、それぞれ、対RHE電圧が0.55Vのときの電流密度(A/cm2)を求め、次式:
性能比=(実施例3で求められた電流密度)/(実施例1で求められた電流密度)
より、実施例1で得られた光電極に対する実施例3で得られた光電極の性能比を求めた。得られた結果を図11に示す。
Claims (10)
- ステンレス系材料からなる金属基板と、前記金属基板の少なくともいずれか一方の面上に積層されたスズ酸化物からなる中間層と、前記中間層の前記金属基板と反対の面上に積層されたバナジン酸ビスマスからなる光触媒層と、を備える光電極。
- 前記中間層の前記光触媒層と接する側の面が凹凸形状を有する請求項1に記載の光電極。
- 前記中間層の厚さが5〜1000nmである請求項1又は2に記載の光電極。
- 前記ステンレス系材料が、オーステナイト系ステンレス、フェライト系ステンレス及びマルテンサイト系ステンレスからなる群から選択されるいずれか1種である請求項1〜3のうちのいずれか一項に記載の光電極。
- 前記スズ酸化物が酸化第二スズである請求項1〜4のうちのいずれか一項に記載の光電極。
- 前記金属基板の前記中間層に覆われていない面上に酸化被膜をさらに備える請求項1〜5のうちのいずれか一項に記載の光電極。
- 請求項1〜6のうちのいずれか一項に記載の光電極を作用電極として備える水分解用光電気化学システム。
- ステンレス系材料からなる金属基板の少なくともいずれか一方の面上にスズ酸化物からなる中間層を形成して、前記金属基板と前記中間層とを備える積層体を得る第1の工程と、
前記中間層の前記金属基板と反対の面上に、V及びBiを含有するバナジン酸ビスマス前駆体溶液を用いてバナジン酸ビスマスからなる光触媒層を形成して、前記金属基板と、前記金属基板の少なくともいずれか一方の面上に積層された前記中間層と、前記中間層の前記金属基板と反対の面上に積層された前記光触媒層と、を備える光電極を得る第2の工程と、
を含むことを特徴とする光電極の製造方法。 - 第1の工程において、真空蒸着法、スパッタ法、イオンプレーティング法、メッキ法、電解紡糸法及び熱負荷スプレー法からなる群から選択される少なくとも一つの成膜法により不活性ガス雰囲気下で前記中間層を形成することを特徴とする請求項8に記載の光電極の製造方法。
- 第1の工程の後、かつ、第2の工程の前に、前記積層体を焼成する工程をさらに含むことを特徴とする請求項8又は9に記載の光電極の製造方法。
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