JP4077839B2 - カーボンナノチューブ−中型多孔性炭素複合体,カーボンナノチューブ−中型多孔性炭素複合体の製造方法,燃料電池用の担持触媒および燃料電池 - Google Patents
カーボンナノチューブ−中型多孔性炭素複合体,カーボンナノチューブ−中型多孔性炭素複合体の製造方法,燃料電池用の担持触媒および燃料電池 Download PDFInfo
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Classifications
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Description
(A)界面活性剤Triton X−100(Aldrich)5.0gを,水200mlに溶かした後,ここにSWNT(Single−Walled CNT)0.14gを添加し,混合した。ここに,TEOS48.4gを溶かし,水300mlと35%塩酸溶液85gとをさらに追加した後,40℃を維持しつつ,よく混ざるように2時間攪拌した。
(C)スクロース0.94gを水3.75mlに溶かし,ここに硫酸0.11gを入れてよく攪拌して,炭素前駆体ゾルを製造した。その後,炭素前駆体ゾルに上記で製造されたCNT−中型多孔性シリカ複合体1gを混合させた。上記のように製造された結果物をオーブンに入れ,160℃で2時間熱処理した。熱処理された結果物に,再び初めに入れた量の60%になるように調節して新たに製造した炭素前駆体ゾルを入れ,160℃で2時間熱処理を再び行った。
(E)上記(C)で製造したCNT−中型多孔性炭素複合体0.5gをビニールバックに入れた後,H2PtCl6を1.9232g測量して,1.5mlのアセトンに溶解させた。上記の溶液を,上記炭素担体が入っているビニールバックに入れて,混合した。この混合溶液を空気中で4時間乾燥させた後,るつぼに移し,60℃の乾燥器内で一晩乾燥させた。次いで,窒素が流れる電気炉内に上記のるつぼを入れて,窒素を10分間流した。その後,流れるガスを水素に転換した後,常温で200℃まで昇温し,この温度を2時間維持して,上記の炭素担体に担持されたPt塩を還元させた。再びガスを窒素に転換した後で,温度を250℃まで5℃/分の速度で昇温させた後,5時間維持してから常温まで冷却して,Ptの担持濃度が60質量%である炭素複合体担持触媒を得た。
(G)上記(E)で製造した中型多孔性炭素複合体の担持触媒を,イソプロピルアルコールにナフィオン115(デュポン社製)を分散させた溶液に分散させて,スラリーを製造した。その後,スプレー工程を通じて炭素電極上にコーティングし,触媒のコーティング濃度は,Pt含量を基準として3mg/cm2とした。次いで,上記の電極成形体をローリングマシンに通過させて,触媒層と炭素紙との接着力を向上させ,カソードを製造した。一方,アノード電極としては,商業的に入手可能なPt−Ru Black触媒を使用して製造されたアノード電極を使用し,これらを利用して単位電池を製造した。
Claims (17)
- カーボンナノチューブと;
中型多孔性炭素と;
を含むことを特徴とする,カーボンナノチューブ−中型多孔性炭素複合体。 - 前記カーボンナノチューブの含量は,カーボンナノチューブ−中型多孔性炭素複合体100質量部に対して0.6〜20質量部であることを特徴とする,請求項1に記載のカーボンナノチューブ−中型多孔性炭素複合体。
- 前記カーボンナノチューブ−中型多孔性炭素複合体の中型気孔の平均直径は,2〜10nmであることを特徴とする,請求項1または2に記載のカーボンナノチューブ−中型多孔性炭素複合体。
- 前記カーボンナノチューブ−中型多孔性炭素複合体の比表面積は,800〜3500m2/gであることを特徴とする,請求項1〜3のいずれかに記載のカーボンナノチューブ−中型多孔性炭素複合体。
- (a)カーボンナノチューブと中型多孔性シリカとが含まれたカーボンナノチューブ−中型多孔性シリカ複合体を製造する工程と;
(b)重合性炭素含有の化合物とキャリアとを混合して,炭素前駆体ゾルを製造する工程と;
(c)前記(b)工程で製造した前記炭素前駆体ゾルに,前記(a)工程で製造した前記カーボンナノチューブ−中型多孔性シリカ複合体を含浸させる工程と;
(d)前記(c)工程で,前記カーボンナノチューブ−中型多孔性シリカ複合体の内部に浸透した前記炭素前駆体ゾルを熱処理により重合させて,炭素前駆体を製造する工程と;
(e)前記(d)工程で重合された前記炭素前駆体を熱分解により転換させて,炭素構造体を製造する工程と;
(f)前記(e)工程で製造された前記炭素構造体を,シリカを選択的に溶解させることが可能な溶液で処理して,シリカを除去する工程と;
を含むことを特徴とするカーボンナノチューブ−中型多孔性炭素複合体の製造方法。 - 前記(b)工程で,
前記重合性炭素含有の化合物は,炭水化物またはフルフリルアルコールであり,
前記キャリアは,水または有機溶媒であることを特徴とする,請求項5に記載のカーボンナノチューブ−中型多孔性炭素複合体の製造方法。 - 前記(b)工程で,前記炭素前駆体ゾルの製造時,酸をさらに付加することを特徴とする,請求項5または6に記載のカーボンナノチューブ−中型多孔性炭素複合体の製造方法。
- 前記(d)工程で,前記炭素前駆体ゾルを50〜250℃で熱処理することを特徴とする,請求項5〜7のいずれかに記載のカーボンナノチューブ−中型多孔性炭素複合体の製造方法。
- 前記熱処理は,
50〜150℃で行われる第1次熱処理と,
前記第1次熱処理の後に150〜250℃で行われる第2次熱処理と,
を含むことを特徴とする,請求項8に記載のカーボンナノチューブ−中型多孔性炭素複合体の製造方法。 - 前記(d)工程と前記(e)工程との間に,
(g)前記(d)工程で製造した前記炭素前駆体を,前記(b)工程で製造した前記炭素前駆体ゾルに含浸させる工程と;
(h)前記(g)工程の結果物を熱処理する工程と;
を1回以上反復的に実施することを特徴とする,請求項5〜9のいずれかに記載のカーボンナノチューブ−中型多孔性炭素複合体の製造方法。 - 前記(e)工程で,前記炭素構造体を600〜1400℃で熱分解させることを特徴とする,請求項5〜10のいずれかに記載のカーボンナノチューブ−中型多孔性炭素複合体の製造方法。
- 前記(f)工程で,前記シリカを選択的に溶解させることが可能な溶液は,フッ化水素酸または水酸化ナトリウム水溶液であることを特徴とする,請求項5〜11のいずれかに記載のカーボンナノチューブ−中型多孔性炭素複合体の製造方法。
- カーボンナノチューブと中型多孔性炭素とが含まれたカーボンナノチューブ−中型多孔性炭素複合体と;
前記カーボンナノチューブ−中型多孔性炭素複合体に分散されて担持されている金属触媒粒子と;
を含むことを特徴とする,燃料電池用の担持触媒。 - 前記カーボンナノチューブ−中型多孔性炭素複合体の中型気孔の平均直径は,2〜10nmであることを特徴とする,請求項13に記載の燃料電池用の担持触媒。
- 前記カーボンナノチューブ−中型多孔性炭素複合体の比表面積は,800〜3500m2/gであることを特徴とする,請求項13または14に記載の燃料電池用の担持触媒。
- 前記金属触媒粒子の含量は,前記担持触媒の全体質量を基準として40〜80質量%であることを特徴とする,請求項13〜15のいずれかに記載の燃料電池用の担持触媒。
- カソード,アノード及び前記カソードとアノードとの間に介在された電解質膜を含み,
前記カソード及びアノードのうち少なくとも一方が,請求項13〜16のいずれか一項による担持触媒を含有していることを特徴とする,燃料電池。
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EP (1) | EP1686106B1 (ja) |
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