JPWO2006064760A1 - 単層カーボンナノチューブの製造方法 - Google Patents
単層カーボンナノチューブの製造方法 Download PDFInfo
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- JPWO2006064760A1 JPWO2006064760A1 JP2006548824A JP2006548824A JPWO2006064760A1 JP WO2006064760 A1 JPWO2006064760 A1 JP WO2006064760A1 JP 2006548824 A JP2006548824 A JP 2006548824A JP 2006548824 A JP2006548824 A JP 2006548824A JP WO2006064760 A1 JPWO2006064760 A1 JP WO2006064760A1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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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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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C01B2202/06—Multi-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
- C01B2202/30—Purity
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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
- 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
- Y10S977/843—Gas phase catalytic growth, i.e. chemical vapor deposition
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Abstract
Description
請求項1は、1〜50m/secの流通線速度で水素ガスが流通する導出帯域に、原料炭化水素、メタロセン及び硫黄化合物を含有する原料混合物を、前記水素ガス及び前記原料混合物の合計質量に対して、前記原料炭化水素の濃度が0.01〜2.0質量%、前記メタロセンの濃度が0.001〜0.2質量%、及び、前記硫黄化合物の濃度が前記メタロセンに対して質量比で1/8〜4倍となる割合で、煙霧状に導出し、次いで、前記水素ガス及び導出された前記原料混合物を800〜1000℃に設定された反応帯域に流通させることを特徴とする単層カーボンナノチューブの製造方法であり、
請求項2は、前記導出帯域は、前記原料炭化水素の沸点以下の温度であることを特徴とする請求項1に記載の単層カーボンナノチューブの製造方法であり、
請求項3は、前記原料混合物は、前記反応帯域を0.1〜10秒で流通することを特徴とする請求項1又は2に記載の単層カーボンナノチューブの製造方法であり、
請求項4は、単層カーボンナノチューブの平均直径が0.5〜2nmである請求項1〜3のいずれか1項に記載の単層カーボンナノチューブの製造方法である。
2 反応管
10 導出帯域
11 反応帯域
12 水素ガス導入手段
13 原料混合物導出手段
14 加熱手段
15 冷却手段
16 分離手段
17 原料混合物温度調節装置
18 整流板
19 ノズル先端部
30 原料混合物
31 メタロセン
32 原料炭化水素
33 硫黄化合物
34 炭素原子
35 メタルカーバイド
36 凝集した金属微粒子
37 凝集したメタルカーバイド
40 単層カーボンナノチューブ
41 多層カーボンナノチューブ
図1に示される装置1を用いた。この装置1における反応管2の全長(導出帯域10と反応帯域11との合計長さ)は2mであり、反応管2の上部(ノズル先端部19)から反応管2の約1/6の位置までの領域を導出帯域10とし、導出帯域10に連続する帯域を反応帯域11とした。装置1における水素ガス導入手段12から1m/secの流通線速度となるように反応管2に水素ガスを導入し、反応管2の内壁面に沿って流通させた。一方、トルエン、フェロセン及びチオフェンを含有する原料混合物を1.1気圧の供給圧で、原料混合物導出手段13に供給し、表1に示す「原料混合物の供給温度」に調節し、表1に示す「反応温度」となるように、加熱手段14により反応帯域11を加熱した。このとき、ノズル先端部19近傍の温度を光高温計等によって測定したところ、トルエンの沸点以下の温度であった。
ラマンスペクトルにおける単層カーボンナノチューブ固有のラマンブリージングモード(the radical breathing mode(RBM))の有無によって、検体が単層カーボンナノチューブであるか否かを確認し、次いで、ラマンスペクトルにおける1590cm−1近辺に現れるGバンドと、1350cm−1近辺に表れる欠陥由来又は多層カーボンナノチューブ由来のDバンドとの強度比によって、検体中に、多層カーボンナノチューブが含まれているか否かを確認した。また、透過型電子顕微鏡(TEM)及び走査型電子顕微鏡(SEM)によって得られた画像から同様に検体を確認した。得られたカーボンナノチューブの層厚さ(層数)及び直径の結果を表2に示した。
Claims (4)
- 1〜50m/sの流通線速度で水素ガスが流通する導出帯域に、原料炭化水素、メタロセン及び硫黄化合物を含有する原料混合物を、前記水素ガス及び前記原料混合物の合計質量に対して、前記原料炭化水素の濃度が0.01〜2.0質量%、前記メタロセンの濃度が0.001〜0.2質量%、及び、前記硫黄化合物の濃度が前記メタロセンに対して質量比で1/8〜4倍となる割合で、煙霧状に導出し、次いで、前記水素ガス及び導出された前記原料混合物を800〜1000℃に設定された反応帯域に流通させることを特徴とする単層カーボンナノチューブの製造方法。
- 前記導出帯域は、前記原料炭化水素の沸点以下の温度であることを特徴とする請求項1に記載の単層カーボンナノチューブの製造方法。
- 前記原料混合物は、前記反応帯域を0.1〜10秒で流通することを特徴とする請求項1又は2に記載の単層カーボンナノチューブの製造方法。
- 単層カーボンナノチューブの平均直径が0.5〜2nmである請求項1〜3のいずれか1項に記載の単層カーボンナノチューブの製造方法。
Priority Applications (1)
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JP2006548824A JP4968643B2 (ja) | 2004-12-13 | 2005-12-12 | 単層カーボンナノチューブの製造方法 |
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JP2004360009 | 2004-12-13 | ||
JP2004360009 | 2004-12-13 | ||
PCT/JP2005/022768 WO2006064760A1 (ja) | 2004-12-13 | 2005-12-12 | 単層カーボンナノチューブの製造方法 |
JP2006548824A JP4968643B2 (ja) | 2004-12-13 | 2005-12-12 | 単層カーボンナノチューブの製造方法 |
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JPWO2006064760A1 true JPWO2006064760A1 (ja) | 2008-06-12 |
JP4968643B2 JP4968643B2 (ja) | 2012-07-04 |
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JP2006548824A Expired - Fee Related JP4968643B2 (ja) | 2004-12-13 | 2005-12-12 | 単層カーボンナノチューブの製造方法 |
Country Status (6)
Country | Link |
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US (1) | US8048396B2 (ja) |
JP (1) | JP4968643B2 (ja) |
KR (1) | KR101274492B1 (ja) |
CN (1) | CN100579900C (ja) |
TW (1) | TWI374857B (ja) |
WO (1) | WO2006064760A1 (ja) |
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CN204455392U (zh) * | 2015-02-12 | 2015-07-08 | 新永裕应用科技材料股份有限公司 | 气相成长石墨纤维组成物的生产系统 |
CN107614426B (zh) | 2015-07-16 | 2020-09-25 | 东丽株式会社 | 含碳纳米管组合物的制造方法 |
JP6479202B2 (ja) * | 2015-10-01 | 2019-03-06 | 株式会社名城ナノカーボン | カーボンナノチューブの製造装置および製造方法 |
CN106082174B (zh) * | 2016-06-20 | 2019-06-28 | 青岛科技大学 | 一种碳纳米管分散装置 |
KR20210035201A (ko) | 2018-07-31 | 2021-03-31 | 가부시키가이샤 오사카소다 | 탄소 나노 튜브의 제조 방법 |
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KR102283427B1 (ko) * | 2020-12-15 | 2021-07-29 | 한밭대학교 산학협력단 | 산화그래핀을 혼합하여 혼합용액을 제조하는 혼합용액 제조시스템 |
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- 2005-12-12 JP JP2006548824A patent/JP4968643B2/ja not_active Expired - Fee Related
- 2005-12-12 KR KR1020077015953A patent/KR101274492B1/ko not_active IP Right Cessation
- 2005-12-12 TW TW094143832A patent/TWI374857B/zh not_active IP Right Cessation
- 2005-12-12 US US11/792,962 patent/US8048396B2/en not_active Expired - Fee Related
- 2005-12-12 CN CN200580042697A patent/CN100579900C/zh not_active Expired - Fee Related
- 2005-12-12 WO PCT/JP2005/022768 patent/WO2006064760A1/ja not_active Application Discontinuation
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JP2003146633A (ja) * | 2001-11-16 | 2003-05-21 | National Institute Of Advanced Industrial & Technology | カーボンナノチューブの製造方法 |
JP2003201630A (ja) * | 2001-12-26 | 2003-07-18 | Nikkiso Co Ltd | カーボンナノファイバーの後処理方法及び黒鉛化カーボンナノファイバーの製造方法 |
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Publication number | Publication date |
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CN101087730A (zh) | 2007-12-12 |
JP4968643B2 (ja) | 2012-07-04 |
CN100579900C (zh) | 2010-01-13 |
KR20070104351A (ko) | 2007-10-25 |
US8048396B2 (en) | 2011-11-01 |
TWI374857B (en) | 2012-10-21 |
TW200626495A (en) | 2006-08-01 |
US20080107587A1 (en) | 2008-05-08 |
KR101274492B1 (ko) | 2013-06-14 |
WO2006064760A1 (ja) | 2006-06-22 |
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