JP7121037B2 - アルカリ水電解中の酸素発生のための耐化学性の酸化物電極触媒 - Google Patents
アルカリ水電解中の酸素発生のための耐化学性の酸化物電極触媒 Download PDFInfo
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- JP7121037B2 JP7121037B2 JP2019553861A JP2019553861A JP7121037B2 JP 7121037 B2 JP7121037 B2 JP 7121037B2 JP 2019553861 A JP2019553861 A JP 2019553861A JP 2019553861 A JP2019553861 A JP 2019553861A JP 7121037 B2 JP7121037 B2 JP 7121037B2
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Description
これらは、ルテニウムまたはイリジウム酸化物などの貴金属触媒酸化物でコーティングされたエキスパンドメタルである。しかし、ガス拡散電極にラネーニッケル触媒を使用したシステムもある。アルカリ電解槽は世界中で広く使用されている。
焼き付け後に基板上の最終的に得られる触媒層の厚さは、約50~150nm、好ましくは80~130nm、特に好ましくは100nmである。層の厚さは、上記のようにSEMによって決定される。この層の厚さは、実験室試験に特に適している。産業用途では、より大きな層厚が一般的であり、これも本発明に従って製造することができる。
酢酸バリウム0.288g、酢酸コバルト0.396g、およびビス(2,4-ペンタンジオナト)チタン(IV)オキシド0.008gを、10mlのプロピオン酸/無水プロピオン酸5:1(体積比)に溶解する。それにより、Baカチオンに基づく0.11M溶液が得られる。溶液を140℃で1時間還流撹拌する。冷却後、PTFEの0.2μmフィルタで濾過する。
シリコンウェハSi(100)には、マグネトロンスパッタリングによって塗布される、厚さ5nmの接着層(TiO2)と、厚さ50nmの多結晶Pt(111)層が設けられる。この基板は、Pt(111)の優先配向を強化するために、4sccmのO2流量で、850℃で8分間焼き付けされる。
寿命試験では、アルカリ電解の加速条件下で化学的安定性が実証された。正確な手順は、文献11の手順、特にp.157の図1に対応している。
Claims (28)
- A=BaおよびB=Coである構造ABO3を有するペロブスカイト系の導電性二相混合酸化物であって、5~45at%のCo3O4(前記ペロブスカイトABO3中のCo原子の総数に基づくCoのat%)、およびドーパントとして0.5~3at%のTi(at%は前記ペロブスカイトABO3中のCoカチオンの総数に基づく)をさらに含む、ペロブスカイト系の導電性二相混合酸化物。
- 15~30at%のCo 3 O 4 を含む、請求項1に記載の導電性二相混合酸化物。
- 1~2.5at%のTiを含む、請求項1または2に記載の導電性二相混合酸化物。
- x=0.005~0.03である式BaCo1-xTixO3-δ:Co3O4の請求項1~3のいずれか一項に記載の導電性二相混合酸化物であって、δは前記ペロブスカイト構造の酸素空孔を定義し、0.1~0.8の範囲にある、前記導電性二相混合酸化物。
- x=0.01~0.025である、請求項4に記載の導電性二相混合酸化物。
- δが0.3~0.7の範囲にある、請求項4または5に記載の導電性二相混合酸化物。
- δが0.5~0.6の範囲にある、請求項4または5に記載の導電性二相混合酸化物。
- 式BaCo0.98Ti0.02O3-δ:Co3O4を有する、請求項4~7のいずれか一項に記載の導電性二相混合酸化物。
- 請求項1~8のいずれか一項に記載の導電性二相混合酸化物を含む、アルカリ環境における酸素発生反応のための触媒。
- 請求項1~8のいずれか一項に記載の導電性ペロブスカイト系二相混合酸化物と、導電性基板材料とを含むアノード。
- 前記基板材料が、TiO2接着層および多結晶Pt(111)層を備えたシリコンウェハである、請求項10に記載のアノード。
- アルカリ水電解または金属空気電池における請求項9に記載の触媒の使用。
- アルカリ水電解用または金属空気電池用のアノードを調製するための、請求項1~8のいずれか一項に記載の導電性ペロブスカイト系二相混合酸化物の使用。
- 請求項1~8のいずれか一項に記載の導電性二相混合酸化物の前駆体の製造方法であって、
a)有機カルボン酸、ジカルボン酸、トリカルボン酸塩、および/または、他の酸化物形成塩を、BaおよびCoならびにTiの塩として、非水溶媒に溶解するステップと、
b)還流下で前記溶液を加熱するステップと、
c)必要に応じて濾過するステップと、
を含み、前記導電性混合酸化物に望まれるCo3O4の添加は、化学量論的ペロブスカイト相に関して対応して選択されたCoの過剰量によって調整されることを特徴とする、
方法。 - 前記BaおよびCoの塩が酢酸塩、プロピオン酸塩、シュウ酸塩および/またはペンタンジオナト(pentanedionates)であり、前記Tiの塩がビス(2,4-ペンタンジオナ
ト)チタン(IV)オキシドである、請求項14に記載の方法。 - 前記溶媒が、10:1~2:1の比(体積比)のプロピオン酸とプロピオン酸無水物の混合物である、請求項14または15に記載の方法。
- プロピオン酸とプロピオン酸無水物の混合物の比(体積比)が、7:1~4:1である、請求項16に記載の方法。
- アノードの製造方法であって、請求項14~17のいずれか一項に記載の方法によって得られた前駆体溶液が、
a)湿式コーティングプロセスで導電性基板に塗布され、
b)乾燥され、その後
c)焼き付けされ、
そして、所望の層厚が達成されるまで、前記ステップa)からc)が任意に複数回繰り返される、
ことを特徴とする、方法。 - 前記湿式コーティングプロセスが、スピンコーティング、スプレーコーティングまたは浸漬コーティングプロセスである、請求項18に記載の方法。
- 前記乾燥が250~400℃で実施される、請求項18または19に記載の方法。
- 前記乾燥が300~380℃で実施される、請求項20に記載の方法。
- 前記焼き付けが700~1000℃で実施される、請求項18~21のいずれか一項に記載の方法。
- 前記焼き付けが800~900℃で実施される、請求項22に記載の方法。
- 前記基板が、TiO2接着層および多結晶Pt層でコーティングされたシリコンウェハである、請求項18~23のいずれか一項に記載の方法。
- 前記基板が、Si(100)である、請求項24に記載の方法。
- 前記多結晶Pt層が、多結晶Pt(111)層である、請求項24または25に記載の方法。
- ステップc)による触媒層の厚さが、SEM法により決定される50~150nmである、請求項18~26のいずれか一項に記載の方法。
- ステップc)による前記触媒層の厚さが、80~130nmである、請求項27に記載の方法。
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DE102017205339.9A DE102017205339A1 (de) | 2017-03-29 | 2017-03-29 | Chemisch beständiger, oxidischer Elektrokatalysator für die Sauerstoffentwicklung während der alkalischen Wasserelektrolyse basierend auf BaCoO3-delta, Verfahren zu seiner Herstellung und ihn umfassende Anode sowie katalytisch aktives und chemisch stabiles Reaktionsprodukt davon |
PCT/EP2018/057880 WO2018178135A1 (de) | 2017-03-29 | 2018-03-28 | Chemisch beständiger, oxidischer elektrokatalysator für die sauerstoffentwicklung während der alkalischen wasserelektrolyse basierend auf bacooj_5, verfahren zu seiner herstellung und ihn umfassende anode sowie katalytisch aktives und chemisch stabiles reaktionsprodukt davon |
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EP3601639B1 (de) | 2021-11-10 |
CN110494595B (zh) | 2022-05-27 |
EP3601639A1 (de) | 2020-02-05 |
DE102017205339A1 (de) | 2018-10-04 |
CN110494595A (zh) | 2019-11-22 |
WO2018178135A1 (de) | 2018-10-04 |
US11111587B2 (en) | 2021-09-07 |
ES2904973T3 (es) | 2022-04-06 |
JP2020515405A (ja) | 2020-05-28 |
US20200040473A1 (en) | 2020-02-06 |
DK3601639T3 (da) | 2022-01-24 |
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