JP4583928B2 - カーボン・ナノチューブの合成のための方法 - Google Patents
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- JP4583928B2 JP4583928B2 JP2004555048A JP2004555048A JP4583928B2 JP 4583928 B2 JP4583928 B2 JP 4583928B2 JP 2004555048 A JP2004555048 A JP 2004555048A JP 2004555048 A JP2004555048 A JP 2004555048A JP 4583928 B2 JP4583928 B2 JP 4583928B2
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Images
Classifications
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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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/1271—Alkanes or cycloalkanes
- D01F9/1272—Methane
-
- 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
-
- 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
-
- 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
- Y10S977/89—Deposition of materials, e.g. coating, cvd, or ald
- Y10S977/891—Vapor phase deposition
Description
ここで、dは、ナノメートル単位のナノチューブの直径であり、ωは、cm−1単位のラマン励起の波数(wavenumber)である。上述のように、図8に示されているスペクトルは、カーボン・ナノチューブを識別する際に使用されるラマン・スペクトルの例を示している。所与の励起周波数は、所定のサイズのナノチューブとしか相互作用しないため、カーボン・ナノチューブのサンプルを十分に特徴付けるには、異なる励起周波数で複数のラマン・スペクトルを得る必要があろう。
Claims (23)
- 1つまたは複数の種類の金属塩、および不動態化溶剤からなる混合物を供給するステップと、
前記1つまたは複数の種類の金属塩および前記不動態化溶剤の前記混合物を、混合するステップと、
前記1つまたは複数の種類の金属塩および前記不動態化溶剤の前記混合物を、前記1つまたは複数の種類の金属塩のうちの少なくとも1つの融点よりも高い温度に加熱し、前記1つまたは複数の種類の金属塩のうちの少なくとも1つの融点よりも高い前記温度を維持して、金属ナノ粒子を形成するステップと、
多孔質の粉末酸化物を、前記金属ナノ粒子および前記不動態化溶剤の前記混合物に添加するステップと、
前記金属ナノ粒子、前記粉末酸化物、および前記不動態化溶剤の前記混合物を、混合するステップと、
前記不動態化溶剤から、前記粉末酸化物およびその孔内に定着した前記金属ナノ粒子を抽出するステップと、
前記金属ナノ粒子および前記粉末酸化物を、アニールするステップと、
前記金属ナノ粒子および前記粉末酸化物を、堆積温度よりも高い温度に加熱するステップと、
前記温度を前記堆積温度よりも高くなるように保持しながら、前記金属ナノ粒子を、炭素前駆体ガスにさらすステップと、を含む、カーボン・ナノチューブを生成する方法。 - 前記金属ナノ粒子および前記粉末酸化物の前記混合物をアニールするステップは、
前記金属ナノ粒子および前記粉末酸化物の前記混合物を、10%のH2および90%のHeからなるガス流の存在下で、400℃から550℃の範囲の温度まで加熱するステップを含む、請求項1に記載の方法。 - 前記金属ナノ粒子および前記粉末酸化物の前記混合物をアニールするステップは、
前記金属ナノ粒子および前記粉末酸化物の前記混合物を、不活性ガス流の存在下で、500℃から550℃の範囲の温度まで加熱するステップを含む、請求項1に記載の方法。 - 前記1つまたは複数の種類の金属塩は、遷移金属酢酸塩である、請求項1に記載の方法。
- 前記1つまたは複数の種類の金属塩のうち少なくとも1つは、酢酸鉄、酢酸パラジウム、酢酸ニッケル、または酢酸モリブデンからなるグループから選択された物質である、
請求項1に記載の方法。 - 前記粉末酸化物は、酸化アルミニウムおよび酸化ケイ素からなるグループから選択される、請求項1に記載の方法。
- 前記堆積温度は、680℃から900℃の範囲内である、請求項1に記載の方法。
- 前記不動態化溶剤は、グリコールエーテルである、請求項1に記載の方法。
- 前記不動態化溶剤は、2−(2−ブトキシエトキシ)エタノールである、請求項1に記載の方法。
- 前記1つまたは複数の種類の金属塩および前記不動態化溶剤の前記混合物を加熱するステップは、前記1つまたは複数の種類の金属塩および前記不動態化溶剤の前記混合物を還流するステップを含む、請求項1に記載の方法。
- 前記1つまたは複数の種類の金属塩および前記不動態化溶剤の前記混合物は、前記不動態化溶剤の沸点で還流される、請求項10に記載の方法。
- 前記1つまたは複数の種類の金属塩および前記不動態化溶剤の前記混合物のモル比は、2:1から1:45までである、請求項1に記載の方法。
- 前記1つまたは複数の種類の金属塩および前記不動態化溶剤の前記混合物を混合するステップは、前記1つまたは複数の種類の金属塩および前記不動態化溶剤の前記混合物を混合し、均質な混合物を形成するステップを含む、請求項1に記載の方法。
- 前記金属ナノ粒子、前記粉末酸化物、および前記不動態化溶剤の前記混合物を混合するステップは、前記金属ナノ粒子、前記粉末酸化物、および前記不動態化溶剤の前記混合物を混合して、均質な混合物を形成するステップを含む、請求項1に記載の方法。
- 金属と粉末酸化物のモル比は、1:10から1:15までの範囲である、請求項1に記載の方法。
- 前記1つまたは複数の種類の金属塩および前記不動態化溶剤の前記混合物の温度は、20分から2400分の範囲の時間にわたり、前記1つまたは複数の種類の金属塩のうちの少なくとも1つの前記融点よりも高い温度に保持される、請求項1に記載の方法。
- 前記炭素前駆体ガスは、メタンである、請求項1に記載の方法。
- さらに、前記さらすステップで形成された生成物から、前記カーボン・ナノチューブを抽出するステップを含む、請求項1に記載の方法。
- 前記さらすステップは、前記金属ナノ粒子を、30分から60分の間、炭素前駆体ガスにさらすことを含む、請求項1に記載の方法。
- 金属酢酸塩および不動態化溶剤を含む混合物を供給するステップと、
前記金属酢酸塩および前記不動態化溶剤の前記混合物を、混合するステップと、
前記金属酢酸塩および前記不動態化溶剤の前記混合物を還流して、金属ナノ粒子を形成するステップと、
多孔質の粉末酸化物を、前記金属ナノ粒子および前記不動態化溶剤の前記混合物に添加するステップと、
前記不動態化溶剤から、前記粉末酸化物およびその孔内に定着した前記金属ナノ粒子からなる成長触媒を抽出するステップと、
前記成長触媒を、堆積温度よりも高い温度に加熱するステップと、
温度を前記堆積温度よりも高くなるように保持しながら、前記成長触媒を炭素前駆体ガスにさらすステップと、を含む、カーボン・ナノチューブを生成する方法。 - 前記成長触媒は、前記金属ナノ粒子および粉末酸化物を含む、請求項20に記載の方法。
- 前記金属酢酸塩は、酢酸鉄、酢酸パラジウム、酢酸ニッケル、および酢酸モリブデンからなるグループから選択された物質である、請求項20に記載の方法。
- 前記堆積温度は、680℃から900℃の範囲内である、請求項20に記載の方法。
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US10/304,317 US7214361B2 (en) | 2002-11-26 | 2002-11-26 | Method for synthesis of carbon nanotubes |
PCT/JP2003/015085 WO2004048262A1 (en) | 2002-11-26 | 2003-11-26 | Method for synthesis of carbon nanotubes |
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US7431965B2 (en) * | 2002-11-01 | 2008-10-07 | Honda Motor Co., Ltd. | Continuous growth of single-wall carbon nanotubes using chemical vapor deposition |
KR100401335B1 (en) * | 2003-03-08 | 2003-10-10 | Mijitech Co Ltd | Metal nanoparticle surface-coated with silicon oxides and preparation thereof |
JP5374801B2 (ja) * | 2004-08-31 | 2013-12-25 | 富士通株式会社 | 炭素元素からなる線状構造物質の形成体及び形成方法 |
US20060078489A1 (en) * | 2004-09-09 | 2006-04-13 | Avetik Harutyunyan | Synthesis of small and narrow diameter distributed carbon single walled nanotubes |
WO2008016390A2 (en) * | 2006-01-30 | 2008-02-07 | Honda Motor Co., Ltd. | Catalyst for the growth of carbon single-walled nanotubes |
US7704553B2 (en) * | 2006-03-06 | 2010-04-27 | National Institute Of Aerospace Associates | Depositing nanometer-sized particles of metals onto carbon allotropes |
US20100239491A1 (en) * | 2006-06-28 | 2010-09-23 | Honda Motor Co., Ltd. | Method of producing carbon nanotubes |
KR100830871B1 (ko) * | 2006-10-11 | 2008-05-21 | 삼성전기주식회사 | 비분산성 금속 나노입자의 표면개질방법 및 이에 의해표면개질된 잉크젯용 금속 나노입자 |
JP5194514B2 (ja) * | 2007-03-29 | 2013-05-08 | 富士通セミコンダクター株式会社 | 基板構造及びその製造方法 |
CN101394712B (zh) * | 2007-09-21 | 2010-08-25 | 清华大学 | 黑孔化溶液及其制备方法 |
US9174847B2 (en) * | 2008-05-01 | 2015-11-03 | Honda Motor Co., Ltd. | Synthesis of high quality carbon single-walled nanotubes |
US8591858B2 (en) * | 2008-05-01 | 2013-11-26 | Honda Motor Co., Ltd. | Effect of hydrocarbon and transport gas feedstock on efficiency and quality of grown single-walled nanotubes |
WO2010014650A2 (en) * | 2008-07-29 | 2010-02-04 | Honda Motor Co., Ltd. | Preferential growth of single-walled carbon nanotubes with metallic conductivity |
EP2261402B1 (en) * | 2009-06-12 | 2013-10-16 | University of Limerick | Method for producing germanium semiconductor nanowires |
WO2015134578A1 (en) | 2014-03-04 | 2015-09-11 | University Of Florida Research Foundation, Inc. | Method for producing nanoparticles and the nanoparticles produced therefrom |
US11369929B2 (en) * | 2017-06-22 | 2022-06-28 | University Of Maryland, College Park | Nanoparticles and systems and methods for synthesizing nanoparticles through thermal shock |
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JPS5391054A (en) | 1977-01-21 | 1978-08-10 | Hitachi Maxell | Metal cobalt powder manufacturing process |
JPS56136904A (en) | 1980-03-31 | 1981-10-26 | Toshiba Corp | Production of platinum group particle |
JPS6169906A (ja) | 1984-09-13 | 1986-04-10 | Nissan Chem Ind Ltd | 超微粒子金属コバルト分散体の製造法 |
US5165909A (en) * | 1984-12-06 | 1992-11-24 | Hyperion Catalysis Int'l., Inc. | Carbon fibrils and method for producing same |
EP0706709A1 (en) * | 1993-06-30 | 1996-04-17 | Carnegie Mellon University | Metal, alloy, or metal carbide nanoparticles and a process for forming same |
US5472749A (en) * | 1994-10-27 | 1995-12-05 | Northwestern University | Graphite encapsulated nanophase particles produced by a tungsten arc method |
US5759230A (en) * | 1995-11-30 | 1998-06-02 | The United States Of America As Represented By The Secretary Of The Navy | Nanostructured metallic powders and films via an alcoholic solvent process |
US6436167B1 (en) * | 1996-05-13 | 2002-08-20 | The United States Of America As Represented By The Secretary Of The Navy | Synthesis of nanostructured composite particles using a polyol process |
JP3511128B2 (ja) | 1998-03-02 | 2004-03-29 | 日立造船株式会社 | 金属微粒子の製造方法および同微粒子の多孔質担体への担持方法 |
JP3336948B2 (ja) | 1998-04-08 | 2002-10-21 | 三菱マテリアル株式会社 | 金属微粉末の製造方法 |
EP1252360A4 (en) * | 2000-01-07 | 2006-07-26 | Univ Duke | HIGH-PERFORMANCE GAS PHASE STEAM SEPARATION METHOD FOR THE MANUFACTURE OF LARGE-FORMATED, NON-ONE-NANOPHESES |
JP2001254109A (ja) | 2000-03-10 | 2001-09-18 | Toda Kogyo Corp | 金属粒子粉末の製造法 |
GB0025989D0 (en) * | 2000-10-24 | 2000-12-13 | Shipley Co Llc | Plating catalysts |
JP3743628B2 (ja) | 2000-12-28 | 2006-02-08 | 株式会社豊田中央研究所 | 単層カーボンナノチューブの製造方法 |
US6875253B2 (en) * | 2001-02-08 | 2005-04-05 | Hitachi Maxell, Ltd. | Metal alloy fine particles and method for producing thereof |
US20020184969A1 (en) * | 2001-03-29 | 2002-12-12 | Kodas Toivo T. | Combinatorial synthesis of particulate materials |
US7288238B2 (en) * | 2001-07-06 | 2007-10-30 | William Marsh Rice University | Single-wall carbon nanotube alewives, process for making, and compositions thereof |
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EP1565403B1 (en) | 2015-07-15 |
US7214361B2 (en) | 2007-05-08 |
US20040101467A1 (en) | 2004-05-27 |
EP1565403A1 (en) | 2005-08-24 |
AU2003283835A1 (en) | 2004-06-18 |
EP1565403A4 (en) | 2008-12-24 |
WO2004048262A1 (en) | 2004-06-10 |
JP2006507207A (ja) | 2006-03-02 |
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