JP2006321712A - メソ細孔性炭素体とその製造方法、担持触媒および燃料電池 - Google Patents
メソ細孔性炭素体とその製造方法、担持触媒および燃料電池 Download PDFInfo
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- JP2006321712A JP2006321712A JP2006132211A JP2006132211A JP2006321712A JP 2006321712 A JP2006321712 A JP 2006321712A JP 2006132211 A JP2006132211 A JP 2006132211A JP 2006132211 A JP2006132211 A JP 2006132211A JP 2006321712 A JP2006321712 A JP 2006321712A
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- carbon body
- mesoporous carbon
- acid
- mesoporous
- body according
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 59
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims description 48
- 239000000203 mixture Substances 0.000 claims description 29
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- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 claims 1
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- 229910002849 PtRu Inorganic materials 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
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- 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
- H01M4/8605—Porous electrodes
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- 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
- H01M4/8803—Supports for the deposition of the catalytic active composition
- H01M4/8807—Gas diffusion layers
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- 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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- H01M4/86—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
- H01M4/885—Impregnation followed by reduction of the catalyst salt precursor
-
- 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
- H01M4/8878—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
-
- 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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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
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Abstract
【解決手段】本発明によれば、75.4kgf/cm2の圧力下で測定した面抵抗が250mΩ/cm2以下であり、メソ細孔性炭素体のメソ細孔の平均直径が2〜20nmであることを特徴とするメソ細孔性炭素体とその製造方法、担持触媒および燃料電池が提供される。これにより、他の物性の犠牲なしに面抵抗を顕著に低下させて、電気エネルギーを効率的に伝達できる。したがって、燃料電池電極の導電材料に応用する場合、高効率の燃料電池電極及び燃料電池の製造が可能である。その他にも、多様な電気化学装置などの導電素材として活用が可能である。
【選択図】図1
Description
このメソ細孔性炭素体に分散されて担持されている金属触媒粒子と、を含む担持触媒が提供される。
以下に示す実施例及び比較例において、面抵抗は、4点試験方式(四端子法)で測定した。以下の実施例および比較例において製造されたメソ細孔性炭素体を、図2に示したような面抵抗測定器に50mg入れ、圧力を75.4kgf/cm2及び150.7kgf/cm2に加えつつ、それぞれの場合について面抵抗を測定した。面抵抗測定器は、被測定物質を収容するチャンバーの底部に、電圧を測定できる一対の電極と、電流を測定できる一対の電極(したがって、電極は計4個)とが設けられているものである。
(実施例1)
フェナントレン0.9gとパラトルエン硫酸2.7gとをアセトン7.5gに完全に溶解させて、均一な前駆体混合物を製造した。この前駆体混合物を41.0(i):29.5(ii):23.0(iii):6.5(iv)の割合に分けて、(i)溶液をSBA−15の1gに含浸させた。このように含浸させたSBA−15を、常温のフードで30分間乾燥させた後、160℃の温度で10分間乾燥させた。
フェナントレンを0.7g使用し、パラトルエン硫酸を2.1g使用した点を除いては、実施例1と同じ方法でメソ細孔性炭素体を製造した。このように製造したメソ細孔性炭素体の面抵抗の測定結果を、以下の表1に示した。
炭化する際に、900℃の代わりに1100℃まで昇温させた点を除いては、実施例2と同じ方法でメソ細孔性炭素体を製造した。このように製造したメソ細孔性炭素体の面抵抗の測定結果を、以下の表1に示した。
フェナントレンを0.9g使用し、パラトルエン硫酸を2.7g使用した点を除いては、実施例3と同じ方法でメソ細孔性炭素体を製造した。このように製造したメソ細孔性炭素体の面抵抗の測定結果を、以下の表1に示した。
フェナントレンを0.7g使用し、硫酸を1.1g使用した点を除いては、実施例1と同じ方法でメソ細孔性炭素体を製造した。このように製造したメソ細孔性炭素体の面抵抗の測定結果を、以下の表1に示した。
フェナントレンの代わりにサッカロース1.5gを使用し、酸として硫酸0.18gを使用した点を除いては、実施例1と同じ方法でメソ細孔性炭素体を製造した。このように製造したメソ細孔性炭素体の面抵抗の測定結果を、以下の表1に示した。
(実施例6)
上記のようにして製造したメソ細孔性炭素体0.5gをビニルバックに入れた後、0.9616gのH2PtCl6を1.5mlのアセトンに溶解させた。この溶液をメソ細孔性炭素体が入っているビニルバックに入れて混合した。この混合溶液を空気中で4時間に乾燥させた後、るつぼに移し、60℃の乾燥器内で一晩乾燥させた。次いで、窒素が流れる電気ファーネス内に上記るつぼを入れ、窒素を10分間流した後、流すガスを水素に転換した。そして、温度を常温から200℃まで昇温して2時間一定に維持しつつ、メソ細孔性炭素体に担持されたPt塩を還元させた。ガスを再び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徐々に冷却させた。次いで、再び0.9616gのH2PtCl6を1.5mlのアセトンに溶解させた溶液にもう一度含浸した後で、再び還元過程を経て、Ptの担持濃度が60質量%である担持触媒を得た。
上記の比較例1で製造した結果物について、実施例6と同じ方法でPtを担持させて担持触媒を製造した。
(実施例7)
実施例6で製造した担持触媒を、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を製造した後、スプレー工程を通じて炭素電極上にコーティングした。触媒のコーティング濃度は、Ptの含量を基準として3mg/cm2にした。次いで、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間の接着力を増大させてカソードを製造した。一方、アノード電極としては、常用のPtRuブラック触媒を使用して製造されたアノード電極を使用し、それらを利用して単位電池を製造した。
比較例2で製造した担持触媒について、実施例7と同じ方法を適用して単位電池を製造した。
Claims (19)
- 75.4kgf/cm2の圧力下で測定した面抵抗が250mΩ/cm2以下であり、
メソ細孔の平均直径が2〜20nmであることを特徴とする、メソ細孔性炭素体。 - 前記メソ細孔性炭素体の比表面積は、500〜2000m2/gであることを特徴とする、請求項1に記載のメソ細孔性炭素体。
- 前記メソ細孔性炭素体の1次粒子の大きさは、100〜500nmであることを特徴とする、請求項1または2に記載のメソ細孔性炭素体。
- 前記メソ細孔性炭素体のX線回折分析において、0.5〜1.5°の2θ範囲に主ピークが観測され、5°以下の2θ範囲に一つ以上のピークが観測されることを特徴とする、請求項1〜3のいずれかに記載のメソ細孔性炭素体。
- (a)フェナントレンを5〜15質量部と、酸を10〜35質量部と、溶媒を55〜80質量部と、を含む前駆体混合物を100質量部製造する工程と、
(b)メソ細孔性シリカに前記前駆体混合物を含浸させる工程と、
(c)前記(b)工程の結果物を熱処理する工程と、
(d)前記(c)工程の結果物を炭化させる工程と、
(e)シリカのみを選択的に溶解させることができる溶液を用いて、前記メソ細孔性シリカを除去する工程と、
を含むことを特徴とする、メソ細孔性炭素体の製造方法。 - 前記酸は、有機酸または無機酸であることを特徴とする、請求項5に記載のメソ細孔性炭素体の製造方法。
- 前記酸は、硫酸、硝酸、リン酸、これらの有機酸、または塩酸であることを特徴とする、請求項5または6に記載のメソ細孔性炭素体の製造方法。
- 前記溶媒は、水、アセトン、メタノール、エタノール、イソプロピルアルコール、n−プロピルアルコール、ブチルアルコール、ジメチルアセトアミド、ジメチルホルムアミド、ジメチルスルホキシド、N−メチル−2−ピロリドン、テトラヒドロフラン、テトラブチルアセテート、酢酸ブチル、m−クレゾール、トルエン、エチレングリコール、γ−ブチロラクトンまたはヘキサフルオロイソプロパノールであることを特徴とする、請求項5〜7のいずれかに記載のメソ細孔性炭素体の製造方法。
- 前記フェナントレンと前記酸との質量比は、1:2.5〜1:3.5であることを特徴とする、請求項5〜8のいずれかに記載のメソ細孔性炭素体の製造方法。
- 前記メソ細孔性シリカの含量は、前駆体混合物100質量部に対して、5〜15質量部であることを特徴とする、請求項5〜9のいずれかに記載のメソ細孔性炭素体の製造方法。
- 前記(b)工程と前記(c)工程との間に、前記(b)工程の結果物を乾燥させる工程を更に含むことを特徴とする、請求項5〜10のいずれかに記載のメソ細孔性炭素体の製造方法。
- 前記熱処理は、50〜250℃の温度で行われることを特徴とする、請求項5〜11のいずれかに記載のメソ細孔性炭素体の製造方法。
- 前記熱処理では、50〜150℃で行われる第1次熱処理と150〜250℃で行われる第2次熱処理とを順次行うことを特徴とする、請求項12に記載のメソ細孔性炭素体の製造方法。
- 前記(c)工程の結果物を、前記(a)工程で使用した混合物に添加して、前記(a)工程〜前記(c)工程を2回〜10回繰り返した後に、前記(d)工程を行うことを特徴とする、請求項5〜13のいずれかに記載のメソ細孔性炭素体の製造方法。
- 前記炭化は、600〜1400℃の温度で行われることを特徴とする、請求項5〜14のいずれかに記載のメソ細孔性炭素体の製造方法。
- 前記メソ細孔性シリカを、HFまたはNaOHを用いて除去することを特徴とする、請求項5〜15のいずれかに記載のメソ細孔性炭素体の製造方法。
- 請求項1〜4のいずれか一項に記載のメソ細孔性炭素体と、
前記メソ細孔性炭素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、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17に記載の担持触媒。
- カソードと、
アノードと、
前記カソードと前記アノードとの間に介在された電解質膜と、
を備え、
前記カソード及び前記アノードのうち少なくとも一つは、請求項17に記載の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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2006
- 2006-04-30 CN CN2006100772178A patent/CN1865132B/zh not_active Expired - Fee Related
- 2006-05-11 JP JP2006132211A patent/JP4471174B2/ja not_active Expired - Fee Related
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WO2008093731A1 (ja) | 2007-02-01 | 2008-08-07 | National Institute Of Advanced Industrial Science And Technology | 燃料電池用電極触媒およびこれを用いた燃料電池 |
JPWO2008093731A1 (ja) * | 2007-02-01 | 2010-05-20 | 独立行政法人産業技術総合研究所 | 燃料電池用電極触媒およびこれを用いた燃料電池 |
JP2012074234A (ja) * | 2010-09-28 | 2012-04-12 | Toppan Printing Co Ltd | 固体高分子形燃料電池用の炭素被覆触媒物質、その製造方法、電極触媒層、及び膜電極接合体 |
JP2015513449A (ja) * | 2012-02-08 | 2015-05-14 | シュトゥディエンゲゼルシャフト・コーレ・ミット・ベシュレンクテル・ハフツングStudiengesellschaft Kohle mbH | メソ多孔性黒鉛粒子上に担持された、高度に焼結安定性の金属ナノ粒子およびその使用 |
WO2014175106A1 (ja) * | 2013-04-25 | 2014-10-30 | 日産自動車株式会社 | 電極、並びにこれを含む燃料電池用電極触媒層 |
WO2019163396A1 (ja) | 2018-02-21 | 2019-08-29 | デクセリアルズ株式会社 | 多孔質炭素材料、及びその製造方法、並びに合成反応用触媒 |
US11338271B2 (en) | 2018-02-21 | 2022-05-24 | Dexerials Corporation | Porous carbon material, method for producing same, and catalyst for synthesis reaction |
JP2021084852A (ja) * | 2019-11-29 | 2021-06-03 | 株式会社豊田中央研究所 | メソ多孔カーボン及びその製造方法、並びに、固体高分子形燃料電池 |
JP7153005B2 (ja) | 2019-11-29 | 2022-10-13 | 株式会社豊田中央研究所 | メソ多孔カーボン及びその製造方法、並びに、固体高分子形燃料電池 |
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US20060263288A1 (en) | 2006-11-23 |
CN1865132B (zh) | 2010-06-09 |
KR100612896B1 (ko) | 2006-08-14 |
US7670582B2 (en) | 2010-03-02 |
CN1865132A (zh) | 2006-11-22 |
JP4471174B2 (ja) | 2010-06-02 |
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