JP2016536248A - 酸素還元電極触媒用の窒素ドープカーボンナノホーンの製造方法 - Google Patents
酸素還元電極触媒用の窒素ドープカーボンナノホーンの製造方法 Download PDFInfo
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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
- H01M4/90—Selection of catalytic material
- H01M4/9091—Unsupported catalytic particles; loose particulate catalytic materials, e.g. in fluidised state
-
- 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
- C01B32/15—Nano-sized carbon materials
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- 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
- C01B32/15—Nano-sized carbon materials
- C01B32/18—Nanoonions; Nanoscrolls; Nanohorns; Nanocones; Nanowalls
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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
- H01M4/8878—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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
Description
(a)カーボンナノホーンを前処理する工程;
(b)工程(a)のカーボンナノホーンを、窒素源の存在下、500〜1200℃で1〜3時間アニールする工程
を含む、導電率を高め、表面積を向上した窒素ドープカーボンナノホーンの製造方法を提供する。
CNH:カーボンナノホーン
SWCNH:単層カーボンナノホーン
FCNH:官能基化カーボンナノホーン
ORR:酸素還元反応
(a)カーボンナノホーンを前処理する工程;
(b)工程(a)のカーボンナノホーンを、窒素源の存在下、および任意に金属の存在下、500〜1200℃で1〜3時間アニールする工程
を含む、導電率を高め、表面積を向上した窒素ドープカーボンナノホーンの製造方法を提供する。
膨らんだ性質を取り除くため、2gのSWCNHを100mLのメタノール溶液と十分に混合した。この混合物を濾過した後、メタノールを完全に除去するために、黒色粉末を真空下、80℃で乾燥し、得られたナノホーンを純粋なSWCNHとして処理した。2gの得られたSWCNHを丸底フラスコ中で250mLの30%過酸化水素と混合し、60℃で5時間環流した。官能基化の後、過酸化水素を完全に除去するために、得られた溶液を濾過し、脱イオン水で数回洗浄した。得られたカーボンナノホーンケーキを真空下、80℃で12時間乾燥した。この材料を、官能基化単層カーボンナノホーン(FCNH)として処理した。
乳鉢と乳棒を使用して、50mgのFCNHを250mgの尿素と混合し、次いで、アルゴン雰囲気中、600℃で1時間アニールした。得られた材料を、精製することなく、N‐600と呼ばれるNCNHsとして使用した。
乳鉢と乳棒を使用して、50mgのFCNHを250mgの尿素と混合し、次いで、アルゴン雰囲気中、800℃で1時間アニールした。得られた材料を、精製することなく、N‐800と呼ばれるNCNHsとして使用した。
乳鉢と乳棒を使用して、50mgのFCNHを250mgの尿素と混合し、次いで、アルゴン雰囲気中、1000℃で1時間アニールした。得られた材料を、精製することなく、N‐1000と呼ばれるNCNHsとして使用した。
比較のため、FCNHを尿素なしで800℃で1時間アニールし、C‐800と呼んだ。
まず、15分間超音波処理することによって、900mgのメラミン粉末を蒸留水30mL中に溶解させ、続いて室温(25℃)で300mgの官能基化単層カーボンナノホーンを加えた。メラミンおよび単層カーボンナノホーンの完全混合の後、溶媒を70℃で蒸発させた。得られた粉末を、アルゴン雰囲気中、高温(900℃)で3時間アニールして、窒素ドープ単層カーボンナノホーンを得た。高温アニール後のナノホーンの形態は損傷がなく、60〜90nmのサイズを有する球状の形態を有した。NCNHの表面積は、FCNHおよび尿素混合物を用いて作製したNCNHに比べて小さく、1327[m2/g]であった。表面積のこの減少は、高温アニール時のメラミン由来の炭素のNCNHへの
沈着に主に起因する。ナノホーン中の全窒素含有量は、尿素を用いて作製されるNCNHと比較される、2.2重量%である。しかしながら、窒素源としてメラミンを用いて作製したNCNHのORR活性は、市販の40%Pt/Cと比較可能な開始電位を示す。
まず、15分間超音波処理することによって、900mgのメラミン粉末を蒸留水30mL中に溶解させ、続いて室温(25℃)で300mgの官能基化単層カーボンナノホーンを加えた。次いで、18mgのFeCl3を加えた。反応物が十分に溶液中に分散されるように、連続的な超音波処理が好ましい。全体の水分含量が蒸発してしまうまで、得られた混合物を70℃で連続的に撹拌しながら保持した。乾燥した混合物を、アルゴン雰囲気下、900℃で3時間アニールした。アニールした混合物を、濃HClで30分間超音波処理し、次いで濾過することによって、酸洗浄を行った。濾液を、乾燥するために、60℃の加熱炉中で保持した。表面積は、1315[m2/g]であった。FeNCNH‐900とNCNHの表面積はほぼ同等であるが、SWCNHのそれよりも4倍高いものであった。しかしながら、NCNHとFeNCNHの表面積は、低くなることがわかったが、これはメラミンの分解時にナノホーンの表面に炭素の堆積によるものであると推測される。
SWCNHの形態を、図2に示すように、高分解能透過電子顕微鏡(HR‐TEM)を用いて分析した。図2aから、SWCNHは、集められ、束ねられて、約60〜80nmのサイズを有する、「ダリア」のような形態を形成する。官能基化の後、たとえ顕著でなくても、いくつかの形態の変化が、ミクロ細孔とメソ細孔の発生だけでなく官能基の形成によって発生する(図2b)。官能基化後に合体は観察されず、FCNHの個々の管束およびそのバンドルと花びらは、未処理のSWCNHのように損傷のないままである。これは明らかに、アルゴン雰囲気の存在下、高温でのアニールは、そのような形態において実質的な変形をしないことを示している。
1.バルクレベルでNCNHsを合成する容易な方法。
2.潜在的コスト効果のある、高分子電解質膜燃料電池用の金属不含カソード触媒。
3.高耐久性。
4.広く使用されているプラチナ触媒を超える経済的優位性を有すること。
Claims (10)
- (a)カーボンナノホーンを前処理する工程;
(b)工程(a)のカーボンナノホーンを、窒素源の存在下、500〜1200℃で1〜3時間アニールする工程
を含む、導電率を高め、表面積を向上した窒素ドープカーボンナノホーンの製造方法。 - 前記カーボンナノホーンが、好ましくは単層カーボンナノホーンである、請求項1記載の方法。
- 前記窒素源が、尿素、メラミンから選択される、請求項1記載の方法。
- 前記窒素ドープカーボンナノホーンが、FeおよびCoから選択された金属で、任意にコドープされている、請求項1記載の方法。
- カーボンナノホーンの前処理によって、カーボンナノホーンを官能基化する、請求項1記載の方法。
- 官能基化が、過酸化水素を用いて行われる、請求項5記載の方法。
- 窒素ドープカーボンナノホーンの表面積が、300〜1500[m2/g]である、請求項1〜6のいずれか1項記載の方法。
- 窒素ドープカーボンナノホーンの導電率が、5〜9[S/cm]である、請求項1〜7のいずれか1項記載の方法。
- 請求項1〜8のいずれか1項記載の方法によって製造した、300〜1500[m2/g]の表面積および5〜9[S/cm]の導電率を有する窒素ドープカーボンナノホーン。
- 酸素還元反応(ORR)に使用するための、請求項9記載の窒素ドープカーボンナノホーン。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IN3169DE2013 | 2013-10-25 | ||
IN3169/DEL/2013 | 2013-10-25 | ||
PCT/IN2014/000675 WO2015059718A1 (en) | 2013-10-25 | 2014-10-22 | A process for the preparation of nitrogen doped carbon nanohorns for oxygen reduction electrocatalysis |
Publications (2)
Publication Number | Publication Date |
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JP2016536248A true JP2016536248A (ja) | 2016-11-24 |
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US20160087148A1 (en) | 2014-09-19 | 2016-03-24 | National Cheng Kung University | Non-metallic semiconductor quantum dot and method of carrying out chemical reaction or photoluminescence reaction by using the same |
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CN105161728A (zh) * | 2015-08-11 | 2015-12-16 | 东南大学 | 尿素改性硼碳中空球的制备及其在燃料电池中的应用 |
CN105195183B (zh) * | 2015-10-19 | 2017-07-21 | 太原理工大学 | 一种Co3O4@ACSs/BiOCl球形吸附‑光催化复合催化剂的制备方法 |
US10446852B2 (en) * | 2016-03-14 | 2019-10-15 | Iowa State University Research Foundation, Inc. | Fuel-cell system and method of generating energy from crude fuel |
US10730752B2 (en) | 2016-05-03 | 2020-08-04 | Virginia Commonwealth University | Heteroatom-doped porous carbons for clean energy applications and methods for their synthesis |
US11264630B2 (en) | 2017-02-28 | 2022-03-01 | Okinawa Institute Of Science And Technology School Corporation | Process for preparing a supported catalytic material, and supported catalytic material |
CN107039660B (zh) * | 2017-06-07 | 2019-09-20 | 北京化工大学常州先进材料研究院 | Fe-NPS共掺杂的多孔碳微球的制备及其作为ORR催化剂的应用 |
CN109665525B (zh) * | 2019-01-30 | 2020-04-28 | 河南工程学院 | 一种“哑铃型”铁氮双掺杂多孔碳的制备方法 |
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US20230278864A1 (en) * | 2022-03-04 | 2023-09-07 | Nabors Energy Transition Solutions Llc | Nitrogen doped carbon-based nanomaterial and methods of forming the same |
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