JP4466549B2 - 大径化された単層カーボンナノチューブを製造する方法 - Google Patents
大径化された単層カーボンナノチューブを製造する方法 Download PDFInfo
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- JP4466549B2 JP4466549B2 JP2005352117A JP2005352117A JP4466549B2 JP 4466549 B2 JP4466549 B2 JP 4466549B2 JP 2005352117 A JP2005352117 A JP 2005352117A JP 2005352117 A JP2005352117 A JP 2005352117A JP 4466549 B2 JP4466549 B2 JP 4466549B2
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
- C01B3/0021—Carbon, e.g. active carbon, carbon nanotubes, fullerenes; Treatment thereof
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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
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
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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
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C11/00—Use of gas-solvents or gas-sorbents in vessels
- F17C11/005—Use of gas-solvents or gas-sorbents in vessels for hydrogen
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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
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/02—Single-walled nanotubes
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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
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/36—Diameter
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- 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
- Y02E60/32—Hydrogen storage
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- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/70—Nanostructure
- Y10S977/734—Fullerenes, i.e. graphene-based structures, such as nanohorns, nanococoons, nanoscrolls or fullerene-like structures, e.g. WS2 or MoS2 chalcogenide nanotubes, planar C3N4, etc.
- Y10S977/742—Carbon nanotubes, CNTs
- Y10S977/75—Single-walled
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- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/84—Manufacture, treatment, or detection of nanostructure
- Y10S977/842—Manufacture, treatment, or detection of nanostructure for carbon nanotubes or fullerenes
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- Combustion & Propulsion (AREA)
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Description
大径化された高純度の単層カーボンナノチューブを得るため、種々の処理条件によって試験を行った。原料の単層カーボンナノチューブとしては、カーボン・ナノテクノロジーズ社(CNI)のHiPco法により合成された約1.1nmの平均チューブ径を有する単層カーボンナノチューブを使用した。この原料カーボンナノチューブ中に本質的に含まれる合成用金属触媒、具体的にはFeの量は20〜30wt%であり、グラファイトは含まれていなかった。
・チューブ径分布測定:透過型電子顕微鏡(TEM)
・触媒量測定: 熱重量分析(TGA)(空気中、室温〜800℃)
・グラファイト量測定:TGA、TEM
実施例1において、触媒量及びグラファイト量の低減並びにカーボンナノチューブの大径化それぞれに効果のあったB領域に関し、大径化処理の前により低温で前処理を行った場合についてその効果を評価した。原料としては、実施例1と同じ単層カーボンナノチューブを使用し酸処理は行わなかった。原料カーボンナノチューブの初期触媒量は18wt%であった。
実施例1において、触媒量及びグラファイト量の低減並びにカーボンナノチューブの大径化それぞれに効果のあったB領域における温度1800℃、真空度1.3×10-5Paの処理条件に関し、大径化処理の前により低温の種々の温度で前処理を行った場合についてその効果を評価した。原料としては、実施例1と同様の酸処理を行った単層カーボンナノチューブを使用した。前処理として、所定の温度及び真空度1.3×10-5Paで8時間保持し、次いで、大径化処理として、温度1800℃及び真空度1.3×10-5Paで10時間保持した。大径化処理後のカーボンナノチューブについて、触媒量(wt%)、グラファイト量(wt%)及び平均チューブ径(nm)を評価した。その結果を表1に示す。
実施例3において、触媒量及びグラファイト量の低減並びにカーボンナノチューブの大径化それぞれに高い効果の得られた試料1に関し、それを約450℃で空気酸化してキャップ構造を開放し、そのガス吸蔵特性について評価した。その結果、本試料のBET法による比表面積は1850m2/g、35MPa及び室温(25℃)での水素吸蔵量は1.45mass%であった。比較として、実施例1〜3の原料カーボンナノチューブ(平均チューブ径:約1.1nm)についても同様にキャップ開放処理を行い、そのガス吸蔵特性を評価した。その結果、BET法による比表面積は840m2/g、35MPa及び室温(25℃)での水素吸蔵量は0.4mass%であった。
Claims (3)
- 原料カーボンナノチューブを1.3×10-2Pa以下の真空度でかつ1400〜1600℃の温度範囲で加熱する前処理工程、及び
前処理された原料カーボンナノチューブを1.3×10-2Pa以下の真空度でかつ1700〜2000℃の温度範囲で加熱する大径化処理工程
を含むことを特徴とする、大径化された単層カーボンナノチューブを製造する方法。 - 前記前処理工程の後、温度を1200℃以下に低下させることなく前記大径化処理工程が実施されることを特徴とする、請求項1に記載の方法。
- 前記原料カーボンナノチューブが、HiPco法によって合成された単層カーボンナノチューブであることを特徴とする、請求項1又は2に記載の方法。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2005352117A JP4466549B2 (ja) | 2005-12-06 | 2005-12-06 | 大径化された単層カーボンナノチューブを製造する方法 |
PCT/JP2006/324602 WO2007066780A1 (ja) | 2005-12-06 | 2006-12-04 | 大径化された単層カーボンナノチューブを製造する方法 |
EP06834357.3A EP1958922B1 (en) | 2005-12-06 | 2006-12-04 | Process for producing single-layer carbon nanotube with increased diameter |
CN2006800455462A CN101321694B (zh) | 2005-12-06 | 2006-12-04 | 制造大径化了的单层碳纳米管的方法 |
CA2632147A CA2632147C (en) | 2005-12-06 | 2006-12-04 | Process for producing single-walled carbon nanotubes with increased diameter |
US12/096,247 US8029758B2 (en) | 2005-12-06 | 2006-12-04 | Process for producing single-walled carbon nanotubes with increased diameter |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2005352117A JP4466549B2 (ja) | 2005-12-06 | 2005-12-06 | 大径化された単層カーボンナノチューブを製造する方法 |
Publications (2)
Publication Number | Publication Date |
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JP2007153688A JP2007153688A (ja) | 2007-06-21 |
JP4466549B2 true JP4466549B2 (ja) | 2010-05-26 |
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JP2005352117A Expired - Fee Related JP4466549B2 (ja) | 2005-12-06 | 2005-12-06 | 大径化された単層カーボンナノチューブを製造する方法 |
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Country | Link |
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US (1) | US8029758B2 (ja) |
EP (1) | EP1958922B1 (ja) |
JP (1) | JP4466549B2 (ja) |
CN (1) | CN101321694B (ja) |
CA (1) | CA2632147C (ja) |
WO (1) | WO2007066780A1 (ja) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101898759B (zh) * | 2010-06-29 | 2012-07-18 | 清华大学 | 碳纳米管结构的制备方法 |
BR112013022568B1 (pt) | 2011-03-11 | 2021-01-12 | Fenwal, Inc. | método para umedecer uma membrana em um separador de membrana |
JP5679939B2 (ja) * | 2011-09-28 | 2015-03-04 | 日立造船株式会社 | 触媒金属の除去方法 |
Family Cites Families (8)
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JP2003154260A (ja) | 2001-11-21 | 2003-05-27 | National Institute Of Advanced Industrial & Technology | ガス吸蔵材 |
JP3962773B2 (ja) | 2002-12-05 | 2007-08-22 | 独立行政法人科学技術振興機構 | 原料吹き付け式カーボンナノ構造物の製造方法及び装置 |
JP4532913B2 (ja) | 2003-01-23 | 2010-08-25 | キヤノン株式会社 | ナノカーボン材料の製造方法 |
CN100473601C (zh) | 2003-01-23 | 2009-04-01 | 佳能株式会社 | 制造纳米碳材料的方法 |
JP2004344775A (ja) * | 2003-05-22 | 2004-12-09 | Ishikawajima Harima Heavy Ind Co Ltd | 水素吸蔵材料及びそれを備えた燃料電池 |
JP2005306681A (ja) * | 2004-04-22 | 2005-11-04 | Toyota Motor Corp | 触媒金属の除去方法 |
JP2005343746A (ja) * | 2004-06-03 | 2005-12-15 | Toyota Motor Corp | 単層カーボンナノチューブの製造方法およびそれにより製造された単層カーボンナノチューブ |
JP4815783B2 (ja) | 2004-10-28 | 2011-11-16 | トヨタ自動車株式会社 | カーボンナノチューブ、カーボンナノチューブの製造方法及び電子放出材料 |
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2005
- 2005-12-06 JP JP2005352117A patent/JP4466549B2/ja not_active Expired - Fee Related
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2006
- 2006-12-04 WO PCT/JP2006/324602 patent/WO2007066780A1/ja active Application Filing
- 2006-12-04 US US12/096,247 patent/US8029758B2/en not_active Expired - Fee Related
- 2006-12-04 EP EP06834357.3A patent/EP1958922B1/en not_active Not-in-force
- 2006-12-04 CA CA2632147A patent/CA2632147C/en not_active Expired - Fee Related
- 2006-12-04 CN CN2006800455462A patent/CN101321694B/zh not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
CA2632147A1 (en) | 2007-06-14 |
CN101321694B (zh) | 2011-06-22 |
EP1958922A4 (en) | 2013-06-05 |
JP2007153688A (ja) | 2007-06-21 |
US20100061918A1 (en) | 2010-03-11 |
US8029758B2 (en) | 2011-10-04 |
EP1958922B1 (en) | 2016-08-31 |
CN101321694A (zh) | 2008-12-10 |
EP1958922A1 (en) | 2008-08-20 |
CA2632147C (en) | 2011-08-02 |
WO2007066780A1 (ja) | 2007-06-14 |
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