JP6800608B2 - 電池電極、電池電極触媒層用組成物及び電池 - Google Patents
電池電極、電池電極触媒層用組成物及び電池 Download PDFInfo
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- JP6800608B2 JP6800608B2 JP2016099056A JP2016099056A JP6800608B2 JP 6800608 B2 JP6800608 B2 JP 6800608B2 JP 2016099056 A JP2016099056 A JP 2016099056A JP 2016099056 A JP2016099056 A JP 2016099056A JP 6800608 B2 JP6800608 B2 JP 6800608B2
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- 239000000758 substrate Substances 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000005211 surface analysis Methods 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
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Description
(c)fnarrow:0.4%以上、13.0%以下;を満たすこととしてもよい。この場合、極めて優れた耐久性を有する電池電極を実現することができる。
まず、炭素化の対象となる原料を調製した。1.0gのポリアクリロニトリル−ポリメタクリル酸共重合体(PAN/PMA)を15gのジメチルホルムアミドに加えて溶解させることにより溶液(a)を調製した。また、1.0gの2−メチルイミダゾールと5.78gの塩化亜鉛(ZnCl2)とを15gのジメチルホルムアミドに加えて溶解させることにより溶液(b)を調製した。次に、溶液(a)と溶液(b)とを混合し、さらに0.187gの鉄粉末を加えて混合した。その後、得られた混合溶液を60℃で一昼夜、真空乾燥させた。
上述の炭素触媒CA−Iaの製造において、5.78gの塩化亜鉛(ZnCl2)に代えて、0.18gの塩化鉄(III)六水和物(FeCl3・6H2O)を使用し、鉄粉末を使用しなかったこと以外は同様にして、鉄を含む炭素構造を有する粉末状の炭素化材料である炭素触媒CA−IIaを得た。
まず、炭素化の対象となる原料を調製した。1.5gのポリアクリロニトリル−ポリメタクリル酸共重合体(PAN/PMA)と1.5gの2−メチルイミダゾールと1.25gの塩化鉄(III)六水和物(FeCl3・6H2O)とを30gのジメチルホルムアミドに加えて混合した。その後、得られた混合溶液を60℃で一昼夜、真空乾燥させた。
まず、炭素化の対象となる原料を調製した。3.3gのフェノール樹脂(レジトップPSK−2320、群栄化学工業株式会社製)を237gのアセトンに加えて溶解し、1.0gの鉄フタロシアニン(東京化成工業株式会社製)を加えて混合した。その後、得られた混合溶液を60℃で一昼夜、真空乾燥させた。
粉末状の炭素触媒の試料を、ガラス試料板の凹部(2cm×2cm×厚さ0.5mm)に入れるとともにスライドガラスで押さえ、当該試料をその表面と基準面とが一致するように当該凹部に均一に充填した。次いで、この充填された試料の形態が崩れないように、ガラス試料板を広角X線回折試料台に固定した。
X線光電子分光法(XPS)による炭素触媒の表面分析は、X線光電子分光装置(AXIS NOVA、KRATOS社製)にて、X線源としてAlKα線(出力10mA×15kV)を用いて行った。具体的には、XPS測定により得られたスペクトルの各ピークの面積と検出感度係数とから、炭素原子、窒素原子、酸素原子、金属原子の表面元素濃度(%)を求め、当該各元素の濃度の比として、炭素触媒の表面における窒素原子の炭素原子に対する比(N/C比)の値を算出した。なお、定量計算の際のバックグラウンドはShirley法により決定した。
昇温脱離装置(日本ベル株式会社製)に炭素触媒を設置し、高真空下で熱処理することで当該炭素触媒の表面官能基の脱離を行った後、当該炭素触媒の表面に酸素を吸着させ、キャリアガス(He)を50mL/分で流通させて当該炭素触媒を加熱し、脱離したガスを四重極質量分析計(Quadrupole Mass Spectrometer:QMS)で測定した。
炭素触媒CA−Iaに対して、2重量%の白金(Pt)を使用して白金担持処理を行った。すなわち、まず、0.055gのヘキサクロロ白金(IV)酸六水和物(H2PtCl6・6H2O)(白金を0.021g含有)を50gの蒸留水中に溶解し、白金含有溶液を調製した。次いで、この白金含有溶液に、1gの炭素触媒CA−Iaを加え、100℃で3時間還流した。その後、固形材料を蒸留水で洗浄し、吸引ろ過で回収した。さらに、真空乾燥後、水素雰囲気中で650℃にて還元処理した固形材料を、炭素触媒CA−Iaと、当該炭素触媒CA−Iaに担持された白金粒子とからなる対照触媒Pt/CA−Iaとして得た。
上述のようにして製造された炭素触媒0.2gと、炭素担体に担持された白金粒子(Pt/C)と、電解質材料としての5重量%NAFION(登録商標)溶液(Aldrich社製)2.80gと、ボール25gをポットに投入し、200rpm、50分間ボールミルで混合することにより、均一に分散された当該炭素触媒と当該Pt/Cと当該電解質材料とを含むスラリー状の触媒層用組成物を得た。
上述のようにして製造された触媒層用組成物における、白金以外の金属の含有量に対する白金の含有量の質量比を測定した。
上述した炭素触媒の昇温脱離法において、炭素触媒に代えて、触媒層用組成物を使用したこと以外は同様にして、当該触媒層用組成物の昇温脱離法を実施した。
上述の触媒用組成物の製造に使用されたPt/Cについて、当該Pt/Cに含まれる白金粒子の平均粒子径を測定した。すなわち、粉末状のPt/Cの試料を、ガラス試料板の凹部(2cm×2cm×厚さ0.5mm)に入れるとともにスライドガラスで押さえ、当該試料をその表面と基準面とが一致するように当該凹部に均一に充填した。次いで、この充填された試料の形態が崩れないように、ガラス試料板の広角X線回折試料台に固定した。
上述の触媒層用組成物の製造に使用されたPt/Cについて、当該Pt/Cに含まれる白金粒子の電気化学的有効表面積(ECA)を測定した。すなわち、白金粒子の電気化学的有効表面積(ECA)は、サイクリックボルタンメトリーにおける水素吸着量に該当する電気量から求めた。まず、次の条件で回転ディスク電極を用いて電流電圧特性波形(ボルタモグラム)を求めた:電解液:0.1mоl/L HClO4水溶液(窒素ガス飽和)、温度:25℃、対極:白金カウンター電極(コイル状)、参照極:可逆水素電極、走査範囲:1.06〜0.06V(vs.RHE)、走査速度:50mV/s、電極直径:4mm、電極の単位面積あたりのPt/Cの含有量:0.1mg/cm2。
上述のようにして製造されたスラリー状の触媒層用組成物を、3cm角のガス拡散層(SGLカーボン社製、“25BC”)上(5cm2)に、電池電極の単位面積あたりの炭素触媒の含有量が2.5mg/cm2又は1.0mg/cm2になるように塗布して乾燥させることにより、当該ガス拡散層上に触媒層を形成した。こうして、炭素担体に担持された白金粒子と、炭素触媒とを含む触媒層が形成された電池電極を得た。
上述のようにして製造された、炭素担体に担持された白金粒子と、炭素触媒とを含む触媒層の状態(主に、触媒層における、クラック(ひび割れ)の形成の程度)を目視で評価した。
上述のようにして製造された電池電極の耐久性試験を行った。すなわち、正極としては、上述のようにして製造された、炭素担体に担持された白金粒子と、炭素触媒とを含む触媒層(正極触媒層)を含む電池電極を使用した。
上述のようにして製造した炭素触媒、Pt/担体及び触媒層の一部について、透過型電子顕微鏡(TEM)による観察を行った。
図1Aには、例C1〜例C10及び例1〜例39の各々について、使用された炭素触媒(ただし、例C1では、炭素触媒に代えて、ケッチェンブラック(KB)を使用した。)及びPt/担体(例C8〜例C10では、Ptを担持していない炭素触媒を使用せず、Pt/担体として、Pt/Cに代えて、対照触媒(Pt/CA−Ia、Pt/CA−III又はPt/CA−IV)を使用した。その他の例では、Pt/担体として、Pt/Cを使用した。)の特性を示す。すなわち、図1Aには、炭素触媒について、試料名と、XRDのピーク分離により得られた3種類のピーク(fbroad、fmiddle及びfnarrow)の面積割合(%)と、XPSにより得られたN/C比(−)と、昇温脱離法(TPD)におけるCO脱離量(mmol/g)及びCO2脱離量(mmol/g)とを示し、Pt/担体について、当該Pt/担体全体に対する白金(Pt)の含有量の割合(wt%)と、当該Pt/担体に含まれるPtの電気化学的有効表面積(ECA)(m2/g)と、当該Pt/担体に含まれるPtの平均粒子径(nm)と、を示す。
Claims (16)
- 炭素触媒と、前記炭素触媒に担持されていない白金粒子とを含む触媒層を含む電池電極であって、
前記触媒層は、互いに直接接触していない前記炭素触媒及び前記白金粒子を含み、
前記電池電極の単位面積あたりの前記白金粒子の含有量が0.0010mg/cm2以上、0.1200mg/cm2以下である
ことを特徴とする電池電極。 - 炭素触媒と、前記炭素触媒に担持されていない白金粒子とを含む触媒層を含む電池電極であって、
前記触媒層は、前記白金粒子の二次粒子を含み、
前記電池電極の単位面積あたりの前記白金粒子の含有量が0.0010mg/cm 2 以上、0.1200mg/cm 2 以下である
ことを特徴とする電池電極。 - 前記白金粒子の平均粒子径は、30.0nm以下である
ことを特徴とする請求項1又は2に記載の電池電極。 - 前記炭素触媒は、含窒素炭素触媒である
ことを特徴とする請求項1乃至3のいずれかに記載の電池電極。 - 前記含窒素炭素触媒の表面の炭素原子数に対する窒素原子数の比が、0.001以上、0.600以下である
ことを特徴とする請求項4に記載の電池電極。 - 前記炭素触媒は、白金以外の金属を含む
ことを特徴とする請求項1乃至5のいずれかに記載の電池電極。 - 前記白金以外の金属の含有量に対する前記白金の含有量の質量比が0.04以上、20.00以下である
ことを特徴とする請求項6に記載の電池電極。 - 前記炭素触媒は、
粉末X線回折において、X線回折図形における回折角26°付近にピークトップを有するピークを分離することにより得られる3つのピークfbroad(回折角24.0°±4.0°付近)、fmiddle(回折角26.3°±1.5°付近)及びfnarrow(回折角26.5°±1.0°付近)の面積割合が下記条件(a)〜(c):
(a)fbroad:60.0%以上、96.0%以下;、
(b)fmiddle:3.5%以上、32.0%以下;及び
(c)fnarrow:0.4%以上、15.0%以下;
を満たす炭素構造を有する
ことを特徴とする請求項1乃至7のいずれかに記載の電池電極。 - 前記炭素触媒は、
0℃から1000℃までの一酸化炭素及び二酸化炭素の脱離量を測定する昇温脱離法において、150℃から1000℃までの一酸化炭素脱離量0.250mmol/g以上と、150℃から900℃までの二酸化炭素脱離量0.040mmol/g以上とを示す炭素構造を有する
ことを特徴とする請求項1乃至8のいずれかに記載の電池電極。 - 電池電極における触媒層の形成に使用される組成物であって、
炭素触媒と、前記炭素触媒に担持されていない白金粒子とを含み、
前記炭素触媒及び前記白金粒子は、互いに直接接触していない炭素触媒及び白金粒子を含み、
前記電池電極の単位面積あたりの前記白金粒子の含有量が0.0010mg/cm2以上、0.1200mg/cm2以下となるように使用される
ことを特徴とする電池電極触媒層用組成物。 - 電池電極における触媒層の形成に使用される組成物であって、
炭素触媒と、前記炭素触媒に担持されていない白金粒子とを含み、
前記白金粒子は、白金粒子の二次粒子を含み、
前記電池電極の単位面積あたりの前記白金粒子の含有量が0.0010mg/cm 2 以上、0.1200mg/cm 2 以下となるように使用される
ことを特徴とする電池電極触媒層用組成物。 - 前記電池電極触媒層用組成物の0℃から1000℃までの一酸化炭素及び二酸化炭素の脱離量を測定する昇温脱離法において、150℃から1000℃までの一酸化炭素脱離量が0.150mmol/g以上であり、150℃から900℃までの二酸化炭素脱離量が0.030mmol/g以上である
ことを特徴とする請求項10又は11に記載の電池電極触媒層用組成物。 - 前記炭素触媒は、白金以外の金属を含む
ことを特徴とする請求項10乃至12のいずれかに記載の電池電極触媒層用組成物。 - 前記白金以外の金属の含有量に対する前記白金の含有量の質量比が0.04以上、20.00以下である
ことを特徴とする請求項13に記載の電池電極触媒層用組成物。 - 請求項1乃至9のいずれかに記載の電池電極を含む
ことを特徴とする電池。 - 燃料電池である
ことを特徴とする請求項15に記載の電池。
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