JP5066916B2 - 燃料電池用電極触媒、燃料電池用電極及び燃料電池 - Google Patents
燃料電池用電極触媒、燃料電池用電極及び燃料電池 Download PDFInfo
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- JP5066916B2 JP5066916B2 JP2006547739A JP2006547739A JP5066916B2 JP 5066916 B2 JP5066916 B2 JP 5066916B2 JP 2006547739 A JP2006547739 A JP 2006547739A JP 2006547739 A JP2006547739 A JP 2006547739A JP 5066916 B2 JP5066916 B2 JP 5066916B2
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- fuel cell
- catalyst
- cell electrode
- electrode catalyst
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- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 1
- 125000001559 cyclopropyl group Chemical group [H]C1([H])C([H])([H])C1([H])* 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- WJJMNDUMQPNECX-UHFFFAOYSA-N dipicolinic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=N1 WJJMNDUMQPNECX-UHFFFAOYSA-N 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 125000002228 disulfide group Chemical group 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 125000003754 ethoxycarbonyl group Chemical group C(=O)(OCC)* 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 239000006232 furnace black Substances 0.000 description 1
- 125000002541 furyl group Chemical group 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 1
- 125000001072 heteroaryl group Chemical group 0.000 description 1
- DOUHZFSGSXMPIE-UHFFFAOYSA-N hydroxidooxidosulfur(.) Chemical compound [O]SO DOUHZFSGSXMPIE-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 125000001041 indolyl group Chemical group 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- ZBKFYXZXZJPWNQ-UHFFFAOYSA-N isothiocyanate group Chemical group [N-]=C=S ZBKFYXZXZJPWNQ-UHFFFAOYSA-N 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 125000004170 methylsulfonyl group Chemical group [H]C([H])([H])S(*)(=O)=O 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 125000002950 monocyclic group Chemical group 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- MINYDRINCIJYOG-UHFFFAOYSA-N naphtho[1,2-e][1,3]benzoselenazole Chemical compound C1=CC=CC2=C3C(N=C[se]4)=C4C=CC3=CC=C21 MINYDRINCIJYOG-UHFFFAOYSA-N 0.000 description 1
- YASDDKMNKPXQKA-UHFFFAOYSA-N naphtho[1,2-e][1,3]benzothiazole Chemical compound C1=CC=CC2=C3C(N=CS4)=C4C=CC3=CC=C21 YASDDKMNKPXQKA-UHFFFAOYSA-N 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 125000003261 o-tolyl group Chemical group [H]C1=C([H])C(*)=C(C([H])=C1[H])C([H])([H])[H] 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 1
- 125000003356 phenylsulfanyl group Chemical group [*]SC1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 125000003367 polycyclic group Chemical group 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920005596 polymer binder Polymers 0.000 description 1
- 239000002491 polymer binding agent Substances 0.000 description 1
- 229920005597 polymer membrane Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 125000000168 pyrrolyl group Chemical group 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- CTDQAGUNKPRERK-UHFFFAOYSA-N spirodecane Chemical compound C1CCCC21CCCCC2 CTDQAGUNKPRERK-UHFFFAOYSA-N 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 125000005504 styryl group Chemical group 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 125000000475 sulfinyl group Chemical group [*:2]S([*:1])=O 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- 125000004354 sulfur functional group Chemical group 0.000 description 1
- 125000003718 tetrahydrofuranyl group Chemical group 0.000 description 1
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 1
- 150000003536 tetrazoles Chemical class 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- VLLMWSRANPNYQX-UHFFFAOYSA-N thiadiazole Chemical compound C1=CSN=N1.C1=CSN=N1 VLLMWSRANPNYQX-UHFFFAOYSA-N 0.000 description 1
- RBRCCWBAMGPRSN-UHFFFAOYSA-N thieno[2,3-d][1,3]thiazole Chemical compound S1C=NC2=C1C=CS2 RBRCCWBAMGPRSN-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 125000001391 thioamide group Chemical group 0.000 description 1
- 125000002813 thiocarbonyl group Chemical group *C(*)=S 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 150000007944 thiolates Chemical class 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Classifications
-
- 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
- H01M4/90—Selection of catalytic material
-
- 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
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
-
- 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
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/923—Compounds thereof with non-metallic elements
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M2008/1095—Fuel cells with polymeric electrolytes
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inert Electrodes (AREA)
- Fuel Cell (AREA)
Description
3.前記一部あるいは全てが硫黄元素あるいは窒素元素を構成原子とする官能基を少なくとも一つと、少なくとも一つのプロトン受容性の基とを分子内に有する化合物が、下記一般式(2)または(3)で表される化合物であることを特徴とする前記1に記載の燃料電池用電極触媒。
4.前記一部あるいは全てが硫黄元素あるいは窒素元素を構成原子とする官能基を少なくとも一つと、少なくとも一つのプロトン受容性の基とを分子内に有する化合物が、下記一般式(4)または(5)で表される化合物であることを特徴とする前記1に記載の燃料電池用電極触媒。
5.前記一般式(1)〜(5)におけるZが、Ra−S−基、Ra−S−S−基、HS−基または(Rb)(Rc)N−基(Raはアルキル基、シクロアルキル基、アラルキル基、アリール基または複素環基を表し、Rb及びRcは各々水素原子、アルキル基、シクロアルキル基、アラルキル基、アリール基または複素環基を表す。)であることを特徴とする前記2〜4のいずれか1項に記載の燃料電池用電極触媒。
1 固体高分子電解質膜
2 アノード極側触媒層
3 カソード極側触媒層
4、5 拡散層
6、7 セパレータ
(触媒1の作製:白金黒に金粒子を吸着、還元)
白金ルテニウム黒(TEC090110 田中貴金属社製)0.5gを純水1000ml中に混合した。その後、1mol/Lの塩化金酸水溶液40mlを添加した。還元剤として100mmolとなるように、2mol/Lのクエン酸ナトリウム水溶液を添加した。この溶液を95℃で7時間、撹拌、混合した。その後、濾過乾燥を行い、金を白金ルテニウム黒上に析出させた。
白金ルテニウム担持カーボン触媒(TEC81E81 田中貴金属社製)を白金量換算として0.5gを純水1000ml中に混合した。その後、1mol/Lの塩化金酸水溶液40mlを添加した。還元剤として100mmolとなるように、2mol/Lのクエン酸ナトリウム水溶液を添加した。この溶液を、95℃で7時間、撹拌、混合した。その後、濾過、乾燥を行い、金を触媒上に析出させた。
白金担持カーボン触媒(TEC10E60E 田中貴金属社製)を白金量換算として0.5gを純水1000ml中に混合した。その後、1mol/Lの塩化金酸水溶液40mlを添加した。還元剤として100%エタノールを100ml添加した。この溶液を、95℃で7時間、撹拌、混合した。その後、濾過、乾燥を行い、金を触媒上に析出させた。
それぞれ上記作製した触媒1、2、3の0.4gを、純水1000ml中に分散させ、表1に示した本発明に係る化合物を1×10-4mol/L添加し、金属触媒近傍に本発明に係る化合物を吸着させた。未吸着分子はデカンテーションにより除去し、濾過により本発明に係る化合物が吸着した触媒を取り出した。
(負極用ペーストの作製)
表1に示すように、触媒1、2及びその本発明に係る化合物による修飾触媒のいずれかと、蒸留水、60質量%のテフロン(登録商標)分散液、5質量%のナフィオン溶液(アルドリッチ社製)を、固形分としてテフロン(登録商標)量が12質量%となるように混合し、超音波で均一に分散させて、負極用ペーストを作製した。
表1に示すように、負極用ペーストの作製において、触媒を3及びその本発明に係る化合物による修飾触媒に変更した以外は同様の操作を行い、正極用ペーストを作製した。
空隙率75%、厚み0.40mmのカーボンペーパーをテフロン(登録商標)分散液(三井デュポンフロロケミカル社製)に浸漬し、表面に0.5mg/cm2のテフロン(登録商標)をとりつけ、撥水処理カーボンペーパーを作製した。
表1に示す負極、正極で、上記作製の撥水処理カーボンペーパーの表面に負極用ペーストを、白金量が3.0mg/cm2となるように均一に塗布し、窒素雰囲気下80℃で1時間乾燥し、負極を作製した。同様に撥水処理カーボンペーパーの表面に、正極用ペーストを白金量が3.0mg/cm2となるように塗布し、正極を作製した。次いで、これらの正極及び負極でナフィオン112膜(デュポン社製)を挟み、ホットプレスを行い、電解質膜/電極接合体を作製した。
白金表面に本発明に係る化合物のスルホン酸基が局在している状態は、電界放出型電子銃を備えた分析透過電子顕微鏡(ATEM:Analytical Transmission Electron Microscope)のスポット分析で確認することができる。具体的には、マイクログリッドを貼ったグリッドメッシュ上に載せた試料について透過像で確認した後、1nm程度に絞った電子線を分析位置に照射し、そこから発生する特性X線をエネルギー分散型X線分析装置(EDS:Energy Dispersive X−ray Spectrometer)で、スペクトルのS(硫黄)強度を比較した。
作製した電解質膜/電極接合体を用いて、直接メタノール型燃料電池の単電池を組み立て、温度を60℃、大気圧下における燃料の流速を30ml/分、空気の流速を100ml/分とした条件で、負極側に燃料組成物を正極側に空気を供給し、電流−電圧特性を測定した。測定水準及び0.6Vでの電流値を表1に示す。
Claims (9)
- 一部あるいは全てが硫黄元素あるいは窒素元素を構成原子とする官能基を少なくとも一つと少なくとも一つのプロトン受容性の基とを分子内に有する化合物が金属触媒に吸着しており、前記一部あるいは全てが硫黄元素あるいは窒素元素を構成原子とする官能基を少なくとも一つと少なくとも一つのプロトン受容性の基とを分子内に有する化合物が、下記一般式(1)〜(5)のいずれか一つで表される化合物であることを特徴とする燃料電池用電極触媒。
- 前記一般式(1)乃至(5)におけるZが、Ra−S−基、Ra−S−S−基、HS−基または(Rb)(Rc)N−基(Raはアルキル基、シクロアルキル基、アラルキル基、アリール基または複素環基を表し、Rb及びRcは各々水素原子、アルキル基、シクロアルキル基、アラルキル基、アリール基または複素環基を表す。)であることを特徴とする請求項1に記載の燃料電池用電極触媒。
- 前記一般式(1)乃至(5)におけるAが、カルボキシル基、リン酸基、亜リン酸基またはスルホン酸基であることを特徴とする請求項1または2に記載の燃料電池用電極触媒。
- 前記金属触媒が、白金、金、銀、銅及びルテニウムから選ばれる少なくとも一つの元素を含有することを特徴とする請求項1〜3のいずれか1項に記載の燃料電池用電極触媒。
- 前記金属触媒が、白金と、金、銀及び銅から選ばれる少なくとも一つの元素とを含有することを特徴とする請求項1〜3のいずれか1項に記載の燃料電池用電極触媒。
- 前記金属触媒が、白金と、ルテニウムと、金、銀及び銅から選ばれる少なくとも一つの元素とを含有することを特徴とする請求項1〜3のいずれか1項に記載の燃料電池用電極触媒。
- 前記金属触媒が、金または他の金属に金を吸着させたものであることを特徴とする請求項1〜3のいずれか1項に記載の燃料電池用電極触媒。
- 請求項1〜7のいずれか1項に記載の燃料電池用電極触媒を用いることを特徴とする燃料電池用電極。
- 請求項8に記載の燃料電池用電極を用いることを特徴とする燃料電池。
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WO2007046239A1 (ja) * | 2005-10-17 | 2007-04-26 | Kaneka Corporation | 燃料電池用電解質組成物、及びにそれを用いた燃料電池用膜-電極接合体、並びに燃料電池 |
KR20140039382A (ko) * | 2012-09-20 | 2014-04-02 | 삼성전자주식회사 | 연료전지용 전극 및 이를 채용한 연료전지 |
JP6313764B2 (ja) * | 2013-08-08 | 2018-04-18 | 田中貴金属工業株式会社 | 固体高分子形燃料電池用の触媒及びその製造方法 |
CN108704670B (zh) * | 2018-06-07 | 2021-02-19 | 中国科学技术大学先进技术研究院 | 一种Pt1@MIL纳米催化剂及其制备方法和应用 |
CN114014788B (zh) * | 2021-10-12 | 2023-10-10 | 科之杰新材料集团(贵州)有限公司 | 一种聚羧酸减水剂用链转移剂及其用途和制备方法 |
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WO2006059485A1 (ja) | 2006-06-08 |
US7666809B2 (en) | 2010-02-23 |
JPWO2006059485A1 (ja) | 2008-06-05 |
US20080081760A1 (en) | 2008-04-03 |
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