JP2022508971A - 水素発生反応触媒 - Google Patents
水素発生反応触媒 Download PDFInfo
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- JP2022508971A JP2022508971A JP2021547602A JP2021547602A JP2022508971A JP 2022508971 A JP2022508971 A JP 2022508971A JP 2021547602 A JP2021547602 A JP 2021547602A JP 2021547602 A JP2021547602 A JP 2021547602A JP 2022508971 A JP2022508971 A JP 2022508971A
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- vanadium
- electrode
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
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- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8472—Vanadium
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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Abstract
Description
・活性触媒種を含む触媒金属種、及び
・バナジウム種
を含む水素発生反応(HER)触媒であって、触媒金属種及びバナジウム種がHER触媒中に組み入れられている、水素発生反応(HER)触媒を提供する。
本明細書で用いられる場合、用語「水分解」は、出発原料としての水から元素状の水素又は酸素を発生させる任意のプロセスに関する。本明細書に記載の水分解プロセスは、本質的に電気分解である。これらの電気分解プロセスは、典型的にはカソードでの水素発生反応(HER)及びアノードでの酸素発生反応(OER)を伴う。
本発明は、触媒金属種及びバナジウム種を含む水素発生反応(HER)触媒であって、触媒金属種及びバナジウム種が触媒中に組み入れられている、水素発生反応(HER)触媒を提供する。
HER触媒及びそれを含む材料は、バナジウム種が金属触媒種に組み入れられていることを条件として、当該分野で公知の任意の手段により調製されてよい。
本発明は、水分解プロセスにより水素を発生させる方法を提供する。本方法は、少なくとも2つの電極及び電解質溶液を含み、少なくとも2つの電極の少なくとも一方が本発明のHER触媒を含む、電気化学電池において実施される。一部の実施形態では、電気化学電池はアノード及び本発明のHER触媒を含むカソードを含む二電極系である。他の実施形態では、電気化学電池は本発明のHER触媒を含む作用電極、対向電極及び参照電極を含む三電極系である。本方法は、水を電気化学電池の少なくとも2つの電極と接触させる工程及び電解質溶液を通して少なくとも2つの電極間に電圧を印加する工程を含む。HER半反応は通常二電極系のカソード又は三電極系の作用電極で発生するので、カソード又は作用電極は本発明のHER触媒を含む。一部の実施形態では、電解質溶液は水性電解質溶液である。また、水性電解質溶液は水の供給源であってもよい。電解質溶液は、約7以上のpH、たとえば、pH約7~約14を有してよい。一部の実施形態では、pHがアルカリ性であるとき、電解質溶液は強塩基、たとえば、NaOH又はKOH等の水酸化塩基を含む。また、電解質溶液は、特に電解質溶液がアルカリ性pHを有するときバナジウム塩(NH4VO3等)を含んでよい。電解質溶液中のバナジウム塩の濃度は、最大約50mM、たとえば、約0.2mM~約25mMであってよい。
ニッケル系触媒
材料合成
NiCuVOx電極の調製。全電着は、標準的な三電極電気化学設定で実施された。ニッケル発泡体(NF)又はフッ素ドープされた酸化スズ(FTO)基材上へのNiCuVOx触媒の電着は、作用電極としてNF又はFTO、補助電極としてグラファイト板、及び参照電極として飽和カロメル電極(SCE)を用いて達成された。堆積に先立ち、ニッケル発泡体はまず5MのHCl溶液で20分間超音波処理されてNiO層を取り除かれ、次いで水及びエタノールですすがれ、次いで空気雰囲気中で乾燥させられた。電着及び選択的脱合金溶液は、500mMのNiSO4、8mM~32mMのCuSO4、8mMのNH4VO3及び500mMのH3BO3から構成された。電着は、CHI660D電気化学ワークステーション(CH装置)で室温で行われた。まず、NiCuVOxフィルムは-2.0V(対SCE)で600秒間NFの表面上に電着された。場合により、電着に続き、0.6Vのアノード電位を200秒間~600秒間室温で電池に印加することによりNiCuフィルムからCuの選択的溶解がなされる。
三電極系(作用電極としてNiCuVOx、参照電極としてグラファイト板、及び参照電極としてSCE)では、1MのPBS中性溶液中で50mAcm-2の一定の電流密度が20時間維持された。この実験の結果は、図10bに示される。
X線回折分光法(XRD)。XRD測定は、標準的なCuアノードを備えたPANalytical X’Pert Empyrean装置でK-α波長=1.54nmで実施された。一般的なスキャン範囲は、10°~80°であり、0.039°s-1の刻み幅で収集された。
バナジウム複合体の堆積が成功したことは、サイクリックボルタンメトリー及び電着前後に観察されるFTOの色の変化により確認される。図1に示すサイクリックボルタモグラム(CV)に示すように、バナジウム前駆体が存在しないことの結果として、明らかなレドックスピークがなく、電気化学反応が発生していないことを示唆している。しかし、バナジウムイオンの存在下で、CVにおける明らかな減少ピークが-2.0Vに現れており、これはバナジン酸イオンの減少によると考えられている(図1)。
コバルト系触媒
実施例1に記載されているものと類似した方法を用いて、酸化バナジウムでドープされたコバルト触媒が調製された。比較のために、バナジウムドーピングなしの参照材料が調製された。図18及び図19に示されている結果には、バナジウムドープされたコバルト触媒がアルカリ性及び中性条件の両方でコバルトのみの触媒よりも優れたHER触媒活性を有することが実証されている。更に、アルカリ性条件下で、CoV触媒は市販の白金触媒に競合できる活性を有する。
Claims (17)
- ・活性触媒種を含む触媒金属種、及び
・バナジウム種
を含む水素発生反応(HER)触媒であって、触媒金属種及びバナジウム種がHER触媒中に組み入れられている、水素発生反応(HER)触媒。 - 触媒金属種が地球上に豊富に存在する金属である、請求項1に記載のHER触媒。
- 触媒金属種が、ニッケル、コバルト及びそれらの組合せから選択される、請求項2に記載のHER触媒。
- バナジウム種が酸化バナジウムである、請求項1から3のいずれか一項に記載のHER触媒。
- 粒子中に触媒金属種及びバナジウム種が含有される、請求項1から4のいずれか一項に記載のHER触媒。
- 粒子が結晶構造及び非晶質成分を有する、請求項5に記載のHER触媒。
- 粒子の平均直径が約0.1nmから約15nmである、請求項5又は6に記載のHER触媒。
- 触媒金属種が金属修飾剤を更に含む、請求項1から7のいずれか一項に記載のHER触媒。
- 金属修飾剤が銅である、請求項8に記載のHER触媒。
- 金属触媒種が金属触媒種と金属修飾剤の合金を含む、請求項8又は9に記載のHER触媒。
- 金属酸化物コーティングを更に含む、請求項1から10のいずれか一項に記載のHER触媒。
- 金属酸化物コーティングが酸化クロムコーティングである、請求項11に記載のHER触媒。
- 請求項1から12のいずれか一項に記載のHER触媒及び基材を含む、触媒材料。
- 導電性基材及び請求項1から12のいずれか一項に記載のHER触媒を含む、電極。
- 請求項1から12のいずれか一項に記載のHER触媒、請求項13に記載の触媒材料又は請求項14に記載の電極を調製する方法であって、導電性基材を金属触媒種の供給源及びバナジウム種の供給源を含む溶液と接触させる工程、並びに溶液を通して基材と対向電極との間に電圧を印加して、導電性基材の表面上に金属触媒種及びバナジウム種を電着させる工程を含む、方法。
- 水素から水を発生させる方法であって、少なくとも2つの電極及び電解質溶液を含む電気化学電池を用意する工程、水を少なくとも2つの電極と接触させる工程、並びに少なくとも2つの電極間に電圧を印加する工程を含み、少なくとも2つの電極の少なくとも一方が、請求項1から12のいずれか一項に記載のHER触媒、請求項13に記載の触媒材料又は請求項14に記載の電極を含む、方法。
- 少なくとも2つの電極及び電源を含む電解槽であって、少なくとも2つの電極の少なくとも一方が請求項1から12のいずれかに記載のHER触媒、請求項13に記載の触媒材料又は請求項14に記載の電極を含む、電解槽。
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