JP6220337B2 - ガス拡散電極、当該ガス拡散電極の製造方法、当該ガス拡散電極を用いたセル - Google Patents
ガス拡散電極、当該ガス拡散電極の製造方法、当該ガス拡散電極を用いたセル Download PDFInfo
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- 238000009792 diffusion process Methods 0.000 title claims description 73
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 238000000034 method Methods 0.000 claims description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 239000003054 catalyst Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 17
- 239000011230 binding agent Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- 230000002787 reinforcement Effects 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 230000003014 reinforcing effect Effects 0.000 claims description 8
- 239000004744 fabric Substances 0.000 claims description 7
- 239000006229 carbon black Substances 0.000 claims description 5
- 238000003490 calendering Methods 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims description 4
- 229920000554 ionomer Polymers 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000006262 metallic foam Substances 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 238000010030 laminating Methods 0.000 claims description 2
- -1 wire mesh Substances 0.000 claims description 2
- FGRBYDKOBBBPOI-UHFFFAOYSA-N 10,10-dioxo-2-[4-(N-phenylanilino)phenyl]thioxanthen-9-one Chemical compound O=C1c2ccccc2S(=O)(=O)c2ccc(cc12)-c1ccc(cc1)N(c1ccccc1)c1ccccc1 FGRBYDKOBBBPOI-UHFFFAOYSA-N 0.000 claims 1
- 239000007789 gas Substances 0.000 description 69
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 230000008901 benefit Effects 0.000 description 7
- 238000005868 electrolysis reaction Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 238000005363 electrowinning Methods 0.000 description 5
- 239000012528 membrane Substances 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012080 ambient air Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000003518 caustics Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 238000003475 lamination Methods 0.000 description 3
- 230000028161 membrane depolarization Effects 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 125000006850 spacer group Chemical group 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 239000003570 air Substances 0.000 description 2
- 239000007900 aqueous suspension Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- LWUVWAREOOAHDW-UHFFFAOYSA-N lead silver Chemical compound [Ag].[Pb] LWUVWAREOOAHDW-UHFFFAOYSA-N 0.000 description 2
- 239000011244 liquid electrolyte Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
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- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
- C25B11/032—Gas diffusion electrodes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/44—Ion-selective electrodialysis
- B01D61/46—Apparatus therefor
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- C25B11/069—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of at least one single element and at least one compound; consisting of two or more compounds
- C25B11/071—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of at least one single element and at least one compound; consisting of two or more compounds comprising metal or alloy powder and non-metallic binders
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- 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
- C25B11/095—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 at least one of the compounds being organic
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- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
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Description
フッ素化バインダーおよび伝導性粉末をペースト中に混入するステップであって、たとえば、フッ素化バインダー水性懸濁液またはエマルジョンから開始して、バインダーを軽質アルコールなどの好適な物質で沈殿させ、沈殿させたバインダーをカーボンブラックなどの伝導性粉末と混合するステップと;
たとえば2mm未満、一実施形態においては0.2mm未満の厚さの薄層までペーストをカレンダー加工するステップと;
積層構造が得られるまで、加熱プレス下、100〜150℃および12〜24kPaの圧力で各層を補強部材上に積層するステップと(一実施形態では15〜60分を要しうる);
水相が除去されるまで、温度を300〜400℃まで上昇させ、圧力を25〜50kPaにするステップと(一実施形態では15〜60分を要しうる);
緩和条件下で完全に焼結するまで、圧力を大気圧まで開放するステップと(これは、ガス拡散層を補強材に密接に結合させる利点を有し、一実施形態では1〜15分を要しうる);
ゴム状ガス拡散層がキャストされ、高い長手方向弾性率が組立体に付与されるまで、加熱プレス下、300〜400℃において30〜60kPaの圧力下で焼結した構造をキャストするステップと(一実施形態においては15〜60分を要しうる)
を含む方法に関する。
DuPont,USAより市販されるPTFE水性懸濁液を体積比50:50の2−プロパノールと脱イオン水との混合物中に沈殿させた。沈殿したPTFEを、Cabot Corp.,USAより市販されるShawinigan Acetylene Black(SAB)粉末と、炭素対PTFEの重量比60:40で機械的に混合した。パン生地のコンシステンシーを有する材料が得られ、カレンダーロールを使用する押出機で直ちに加工して10cm×10cm×0.1mmの層を得た。開口幅0.50mm、ワイヤ直径0.14mm、および比重量0.53kg/m2の銀メッシュ織物の異なるサンプル上に加熱プレスによって各層を積層し;このプロセスは複数のステップで行い、最初に組立体を17.9kPa、120℃において30分間プレスし、次にさらに30分間温度を335℃および圧力を44.8kPaにして、圧力を開放し、積層構造を周囲空気に5分間曝露し、最後に組立体を34.5kPaおよび335℃でさらに30分間再びプレスした。
日本のTorayより市販される厚さ280μmのTGP−H−090カーボンペーパーを補強部材として使用して、実施例1の手順を繰り返した。実施例1のようにカレンダー加工することによってSAB/PTFE層を得て、カーボンペーパーの各サンプル上に積層し;このプロセスは複数のステップで行い、最初に組立体を13.7kPa、120℃において30分間プレスし、次にさらに30分間温度を335℃および圧力を27.5kPにして、圧力を開放し、積層構造を周囲空気に5分間曝露し、最後に組立体を34.5kPaおよび335℃でさらに30分間再びプレスした。
Textron Systems Corporation,USAより市販される厚さ0.75mmのAvCarb(商標)1243炭素布を補強部材として使用して、実施例1および2の手順を繰り返した。上記実施例のようにカレンダー加工することによってSAB/PTFE層を得て、カーボンペーパーの各サンプル上に積層し;このプロセスは複数のステップで行い、最初に組立体を20kPaおよび120℃において30分間プレスし、次にさらに30分間温度を335℃および圧力を45.5kPaにして、圧力を開放し、積層構造を周囲空気に5分間曝露し、最後に組立体を55kPaおよび335℃でさらに30分間再びプレスした。
実施例1において銀メッシュ補強部材上に得られた1つのガス拡散電極サンプル、および実施例3において炭素布補強部材上に得られた1つのガス拡散電極サンプルについて、加圧領域として使用される直径8cmの開口部を有するビーカーから得られる、実験室設備における加圧下での透過率を試験した。
従来の鉛−銀(Pb0.75Ag)アノード板と、50cm2の活性領域のアルミニウムカソード板とが取り付けられた間隙が1cmの実験室用電解採取セルについて、以下の反応:
2ZnSO4+2H2O→2H2SO4+2Zn+O2
による、高純度ZnOおよび試薬グレードの硫酸を脱イオン水に溶解させることで得た50g/lのZnおよび170g/lのH2SO4を含有する硫酸塩電解質からの亜鉛の堆積について試験した。試験は、500A/m2において3.1Vの全セル電圧において行った。
同じPTFE水性懸濁液を体積比50:50の2−プロパノールおよび脱イオン水の混合物中に沈殿させ、沈殿したPTFEと、5重量%の白金粉末が機械的に合金化された銀粉末とを、80:20のAg−Pt対PTFEの重量比で機械的に混合し、得られたペーストをカレンダーロールを用いて押し出すことによって得られた厚さ1mmの触媒層を、ガス拡散層の、銀メッシュ部材の反対側の面に同時積層したことを除けば、実施例1と同様にして、ガス拡散電極を得た。積層、焼結、およびキャスティングのステップを実施例1に記載のように行うと、長手方向(面内)弾性率が41,000MPaのガス拡散電極が得られた。
Claims (10)
- 補強部材上に積層されたガス拡散層を含むガス拡散電極の製造方法であって、前記ガス拡散層が、焼結およびキャストされた組成物からなり、前記組成物は伝導性粉末とフッ素化バインダーとからなり、そして前記ガス拡散層/補強部材組立体の長手方向弾性率が少なくとも10,000MPaであり、そして
前記方法が、
a.フッ素化バインダーおよび伝導性粉末を含むペーストを得るステップと、
b.前記ペーストを2mm未満の厚さの層にカレンダー加工するステップと、
c.加熱プレス下、100〜150℃の温度および12〜24kPaの圧力において前記層を補強部材上に積層して、積層構造を得るステップと、
d.温度を300〜400℃にして、圧力を25〜50kPaにするステップと、
e.圧力を大気圧まで開放し、積層構造を空気に曝露して焼結を誘導するステップと、
f.前記焼結した構造を加熱プレスした300〜400℃の温度および30〜60kPaの圧力でキャストするステップと
を含む方法。 - 前記ガス拡散層/補強部材組立体の長手方向弾性率が15,000〜120,000MPaの間の範囲である、請求項1に記載の方法。
- 前記補強部材が、エキスパンドメタル、金網、金属フォーム、炭素または金属の布またはフェルト材料からなる群から選択される、請求項1または2に記載の方法。
- 前記組成物中の前記伝導性粉末がカーボンブラックである、請求項1〜3のいずれか一項に記載の方法。
- 前記組成物中の前記フッ素化バインダーがPTFE、PFA、またはFEPである、請求項1〜4のいずれか一項に記載の方法。
- 前記組成物中の伝導性粉末:フッ素化バインダーの重量比が1:1〜2:1の間の範囲である、請求項4または5に記載の方法。
- 前記ガス拡散電極が、前記補強部材とは反対側の前記ガス拡散層の上に堆積された触媒層をさらに含む、請求項1〜6のいずれか一項に記載の方法。
- 前記触媒層が、アイオノマーと触媒粉末からなる、請求項7に記載の方法。
- 前記触媒層が、前記ガス拡散層上に積層された、焼結およびキャストされた組成物からなり、前記組成物は炭素担持触媒粉末とフッ素化バインダーとからなる、請求項7に記載の方法。
- 前記ステップc、d、およびfの持続時間が15〜60分であり、ステップeの大気圧での空気への曝露の持続時間が1〜15分である、請求項1〜9のいずれか一項に記載の方法。
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