JP6049986B2 - 酸素消費電極およびその製造方法 - Google Patents
酸素消費電極およびその製造方法 Download PDFInfo
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims description 45
- 239000001301 oxygen Substances 0.000 title claims description 45
- 229910052760 oxygen Inorganic materials 0.000 title claims description 45
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 239000003054 catalyst Substances 0.000 claims description 59
- 239000007789 gas Substances 0.000 claims description 52
- 239000000725 suspension Substances 0.000 claims description 37
- 239000003792 electrolyte Substances 0.000 claims description 35
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 31
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 29
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 29
- 229910052709 silver Inorganic materials 0.000 claims description 27
- 239000004332 silver Substances 0.000 claims description 27
- 238000005868 electrolysis reaction Methods 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 20
- 230000002209 hydrophobic effect Effects 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 17
- 239000003513 alkali Substances 0.000 claims description 13
- 239000000446 fuel Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 239000002612 dispersion medium Substances 0.000 claims description 8
- 229920001600 hydrophobic polymer Polymers 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 239000011149 active material Substances 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002759 woven fabric Substances 0.000 claims description 3
- 238000004438 BET method Methods 0.000 claims description 2
- 239000006260 foam Substances 0.000 claims description 2
- 229920001002 functional polymer Polymers 0.000 claims description 2
- 239000004745 nonwoven fabric Substances 0.000 claims description 2
- 230000036284 oxygen consumption Effects 0.000 claims 1
- 239000010410 layer Substances 0.000 description 62
- 239000007788 liquid Substances 0.000 description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- 239000011780 sodium chloride Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 239000002356 single layer Substances 0.000 description 6
- 239000003014 ion exchange membrane Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 239000002562 thickening agent Substances 0.000 description 5
- 230000002706 hydrostatic effect Effects 0.000 description 4
- 229920000609 methyl cellulose Polymers 0.000 description 4
- 239000001923 methylcellulose Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 230000005518 electrochemistry Effects 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- -1 hydroxide ions Chemical class 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 239000012459 cleaning agent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 229920002113 octoxynol Polymers 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229920001479 Hydroxyethyl methyl cellulose Polymers 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910001514 alkali metal chloride Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000011552 falling film Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 239000002563 ionic surfactant Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
-
- C—CHEMISTRY; METALLURGY
- 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
- C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
- C25B1/46—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis in diaphragm cells
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/04—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type
-
- 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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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
- H01M4/662—Alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8636—Inert electrodes with catalytic activity, e.g. for fuel cells with a gradient in another property than porosity
- H01M4/8642—Gradient in composition
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
- H01M4/8668—Binders
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8846—Impregnation
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- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/886—Powder spraying, e.g. wet or dry powder spraying, plasma spraying
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- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8882—Heat treatment, e.g. drying, baking
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- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8896—Pressing, rolling, calendering
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- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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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
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- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Inert Electrodes (AREA)
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- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
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Description
a)触媒活性物質の粒子、分散媒および疎水性ポリマーの粒子を含む成分を分散または混合することにより少なくとも2つの懸濁液を製造する工程であって、該少なくとも2つの懸濁液は、疎水性ポリマーの異なった割合を有する、工程
b)少なくとも2つの懸濁液を、1以上の工程において支持体に噴霧して、触媒を異なった割合で含む少なくとも2つの層を製造する工程であって、該支持体を100℃〜160℃の範囲の温度に加熱し、それにより、少なくとも部分的に分散媒を除去する、工程、
c)工程b)後に得られた電極を、0.04〜0.4t/cm2の圧力下で、60〜200℃の温度にて加熱プレスする工程、
d)次いで、電極を少なくとも200℃の温度で焼結する工程
を含む、酸素消費電極を製造するための方法である。
1.触媒およびPTFE、必要に応じて増粘剤、安定剤および界面活性剤の懸濁液/ペーストの製造工程、
2.懸濁液/ペーストの支持体への適用工程、
3.乾燥、任意の焼結工程、
4.任意の、工程2および3を繰り返す工程、
5.任意の、工程4からのOCCの任意に高温での圧縮工程、
6.焼結工程
により製造することができる。
a)少なくとも触媒活性物質の粒子、好ましくは銀粒子、および分散媒、好ましくは有機溶媒または水、特に好ましくは水、疎水性ポリマーの異なった割合を有する疎水性ポリマーの粒子からなる成分を分散または混合することにより少なくとも少なくとも2つの懸濁液を製造する工程、
b)該懸濁液を、1以上の工程において支持体に噴霧して、変動層、好ましくはニッケル支持体を製造する工程であって、該支持体を、100℃〜160℃、好ましくは100〜145℃の範囲の温度に加熱し、分散媒を少なくとも部分的に除去する工程、
c)工程b)後に得られた電極を、特に、0.1〜3t/cm2の範囲の圧力下で、好ましくは0.1〜0.25t/cm2の範囲で、110℃〜140℃の範囲の温度で、特に好ましくは130℃にて加熱プレスする工程、
d)次いで、少なくとも200℃の温度で、好ましくは少なくとも250℃で、特に好ましくは少なくとも300℃の温度で、電極を焼結する工程
により新規な酸素消費電極を製造するための方法をさらに提供する。
種々の銀含有量を有する酸素消費カソード単一層:a)93重量%、b)97重量%、c)98重量%(比較例)
3つの単一層酸素消費カソードを、実施例1に記載の方法により製造した。しかしながら、残存固体を基準としてa)93重量%、b)97重量%またはc)98重量%の銀含有量を有する1つだけの分散体を用いた。全ての3つの電極は、塩化ナトリウム溶液の電解において、実施例1に記載の条件下で、100mV増加したセル電圧を示し、酸素の200ミリバールで重大な気体の貫流を示し、液体の貫流を1mの静水高さにて示した。
酸素消費カソード、2層、触媒含有量:第1層(電解質に面する)99%、第2層(気体側に面する)88%(比較例)
2層酸素消費カソードを、実施例1に記載の方法により製造したが、電解質に面する層に99重量%および気体に面する層に88重量%の触媒含有量を生じさせる異なった触媒の割合を有する2つの分散体のみを用いた。120mV高いセル電圧を、塩化ナトリウム溶液の電解において、実施例1に記載の条件下で得た。
Claims (18)
- 酸素含有気体に面する側およびアルカリ性電解質に面する側を有し、
少なくとも1つの支持体、および
触媒および疎水性物質を含む少なくとも2つの層であって、気体側に面する最外層が、電解質側に面する最外層より低い触媒の割合を有し、疎水性物質の割合が、触媒および疎水性物質の全量を基準として8重量%を越えない層
を含んでなり、
前記気体側に面する最外層が、92〜98重量%の触媒を含み、前記電解質側に面する最外層が、95〜99.9重量%の触媒を含み、100%に対する残部は、疎水性物質に基づく、
多層酸素消費電極。 - 触媒は、触媒活性成分として銀を含む、請求項1に記載の酸素消費電極。
- 触媒を含む少なくとも2の層は、銀粒子を含む懸濁液を支持体に適用し、該懸濁液を乾燥し、該層をプレスし、次いで形成した電極を焼結することにより製造される、請求項1に記載の酸素消費電極。
- 銀粒子は、懸濁液のための粉末形態であり、8μm未満のD90および1μm未満のD10の粒度分布を有する、請求項3に記載の酸素消費電極。
- 銀粒子は、2〜6g/cm3のタップ密度を有する、請求項3に記載の酸素消費電極。
- 銀粉末は、BET法により決定された平均表面0.3〜2.5m2/gを有する、請求項4に記載の酸素消費電極。
- 触媒を含む少なくとも3つの層が存在し、気体側に面する最外層は92〜98重量%の触媒を含み、電解質側に面する最外層は95〜99.9%の触媒を含み、中間層は、気体側に面する最外層の触媒含有量を越え、かつ電解質側に面する最外層の触媒含有量未満の触媒含有量を含む、請求項1に記載の酸素消費電極。
- 疎水性物質は、疎水性ポリマーを含む、請求項1に記載の酸素消費電極。
- 疎水性物質は、PTFEである、請求項1に記載の酸素消費電極。
- 電極は、100〜300mg/cm2の触媒活性成分の全充填を有する、請求項3に記載の酸素消費電極。
- 支持体は、ニッケル、銀およびこれらの混合物からなる群から選択される物質に基づく、請求項1に記載の酸素消費電極。
- 支持体は、ガーゼ、編織布、形成ループニット、引張ループニット、不織布およびフォームからなる群から選択される、請求項1に記載の酸素消費電極。
- 電極は、厚み0.2〜0.8mmを有する、請求項1に記載の酸素消費電極。
- 触媒を含む少なくとも2つの層は、0.4mm以下の厚みを有する、請求項1に記載の酸素消費電極。
- 請求項1〜14のいずれか1に記載の酸素消費電極を製造するための方法であって、
a)触媒活性物質の粒子、分散媒および疎水性ポリマーの粒子を含む成分を分散または混合することにより少なくとも2つの懸濁液を製造する工程であって、該少なくとも2つの懸濁液は、疎水性ポリマーの異なった割合を有する、工程、
b)前記少なくとも2つの懸濁液を、1以上の工程において支持体に噴霧して、触媒を異なった割合で含む少なくとも2つの層を製造する工程であって、該支持体を100℃〜160℃の範囲の温度に加熱し、それにより、少なくとも部分的に分散媒を除去する工程、
c)工程b)後に得られた電極を、0.04〜0.4t/cm2の圧力下で、60〜200℃の温度にて加熱プレスする工程、
d)次いで、電極を少なくとも200℃の温度で焼結する工程
を含む、方法。 - 請求項1に記載の酸素消費電極を含む、燃料電池。
- 請求項1に記載の酸素消費電極を含む、金属/空気電池。
- 請求項1に記載の酸素消費電極を、酸素消費カソードとして含む、塩素アルカリ電解装置。
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