EP1230147A2 - Verfahren zur herstellung von aus übergangsmetalloxiden bestehenden nanotubes - Google Patents

Verfahren zur herstellung von aus übergangsmetalloxiden bestehenden nanotubes

Info

Publication number
EP1230147A2
EP1230147A2 EP00967492A EP00967492A EP1230147A2 EP 1230147 A2 EP1230147 A2 EP 1230147A2 EP 00967492 A EP00967492 A EP 00967492A EP 00967492 A EP00967492 A EP 00967492A EP 1230147 A2 EP1230147 A2 EP 1230147A2
Authority
EP
European Patent Office
Prior art keywords
template
suspension
transition metal
layers
nanotubes
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP00967492A
Other languages
German (de)
English (en)
French (fr)
Inventor
Reinhard Nesper
Hans-Joachim Muhr
Markus Josef Niederberger
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Eidgenoessische Technische Hochschule Zurich ETHZ
Original Assignee
Eidgenoessische Technische Hochschule Zurich ETHZ
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Eidgenoessische Technische Hochschule Zurich ETHZ filed Critical Eidgenoessische Technische Hochschule Zurich ETHZ
Publication of EP1230147A2 publication Critical patent/EP1230147A2/de
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/36—Methods for preparing oxides or hydroxides in general by precipitation reactions in aqueous solutions
    • C01B13/366—Methods for preparing oxides or hydroxides in general by precipitation reactions in aqueous solutions by hydrothermal processing
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/12—Particle morphology extending in one dimension, e.g. needle-like with a cylindrical shape
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/13—Nanotubes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • the invention relates to a method for producing nanotubes consisting of transition metal oxides using a template.
  • Applicant's WO 98/26871 discloses a method for direct chemical synthesis of nanotubes consisting of transition metal oxides.
  • a solution is made from a neutral surfactant molecule and a metal alkoxide.
  • the solution is hydrolyzed and the precipitate aged.
  • the precipitate is then heated.
  • the neutral surfactant molecule is, for example, hexadecylamine and the metal alkoxide is a Vanadiu al- koxic or molybdenum alkoxide.
  • the nanotubes produced by this process are significantly more stable to oxidation than carbon nanotubes and show clear redox activators. They are also suitable as an active material for. -Atalytic reactions. This manufacturing process enables the production of larger quantities of transition metal oxide nanotubes, but the manufacturing costs are still comparatively high.
  • the invention proposes a further and even more cost-effective method for the direct production of nanotubes consisting of transition metal oxides.
  • V 2 0 5 is particularly suitable as a precursor and can be produced many times more cost-effectively than the metal alkoxides used hitherto.
  • the invention therefore makes it possible to reduce the manufacturing costs by a multiple. As before, larger quantities can be produced, for example in the kilogram range.
  • V 2 0 5's insensitivity to water and air makes it easy to work without an inert atmosphere.
  • FIG. 2 shows an X-ray diagram of dodecylamine-containing nanotubes and produced according to the invention from V 2 Os
  • FIG. 3 shows an overview and an individual image of nanotubes produced from V 2 Os and dodecylamine
  • FIG. 4 electron diffraction patterns of nanotubes produced from V 2 Os and containing dodecylamine
  • FIG. 5 schematically shows the essential steps of the inventive method.
  • a transition metal oxide with the layer structure is reacted with a template and the layers are thus widened.
  • the templates are stored between the layers.
  • the transition metal oxide with the layer structure forms the precursor.
  • the expanded layer structure is heated.
  • the layers convert topochemically to nanotubes.
  • FIG. 5 schematically shows these process steps.
  • the transition metal oxide with the layer structure is designated by A here.
  • B schematically shows the expanded layers S, between which the template D is stored.
  • C schematically represents a nanotube, with layers S typically being arranged in a roll shape. A reduction takes place at the transition from B to C.
  • transition metal oxides with a layer structure are suitable as precursors.
  • V 2 Os has proven to be particularly suitable.
  • the template is preferably a neutral amine.
  • FIG. 1 shows the infrared spectrum of the nanotubes produced by this method.
  • FIG. 2 shows the powder diagram, which gives a layer spacing of 27.4 ⁇ .
  • FIG. 3 shows an overview of nanotubes that were produced by this method.
  • FIG. 4 shows electron diffraction reflections of such nanotubes, these reflections resulting in a " layer spacing of 21.8 ⁇ .
  • the difference in the layer spacing is due to the ultra-high vacuum conditions and the thermal stress on the material in the electron microscope.
  • the order structure of the template molecules is changed.
  • Dodecylamine can be replaced by another neutral amine or terminal diamine.
  • the ratio of vanadium oxide to template is, for example, 2: 1.
  • V 2 Os in ethanolic dodecylamine solution resulted in a brown-yellow lamellar structured composite of surfactant (amine) and vanadium (V) oxide after adding water and subsequent aging.
  • the regular layer spacing in this material is around 2.9 nm.
  • a subsequent treatment under hydrothermal conditions yielded a product of overgrown and individual nanorums with a gross composition of V0 2 , 4 [C ⁇ 2 H 2 sN] 0 , 3 .
  • the neutral template molecules are converted into ammonium cations.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Composite Materials (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)
EP00967492A 1999-10-27 2000-10-25 Verfahren zur herstellung von aus übergangsmetalloxiden bestehenden nanotubes Withdrawn EP1230147A2 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
CH195899 1999-10-27
CH195899 1999-10-27
PCT/CH2000/000570 WO2001030690A2 (de) 1999-10-27 2000-10-25 Verfahren zur herstellung von aus übergangsmetalloxiden bestehenden nanotubes

Publications (1)

Publication Number Publication Date
EP1230147A2 true EP1230147A2 (de) 2002-08-14

Family

ID=4222584

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00967492A Withdrawn EP1230147A2 (de) 1999-10-27 2000-10-25 Verfahren zur herstellung von aus übergangsmetalloxiden bestehenden nanotubes

Country Status (4)

Country Link
EP (1) EP1230147A2 (ja)
JP (1) JP2003512284A (ja)
AU (1) AU7767700A (ja)
WO (1) WO2001030690A2 (ja)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004011375A1 (de) * 2002-07-26 2004-02-05 Eidgenössische Technische Hochschule Zürich Verfahren zur herstellung von übergangsmetalloxid-nanotubes und nach diesem verfahren hergestellte nanotubes
KR100453820B1 (ko) * 2002-08-12 2004-10-20 학교법인 포항공과대학교 알루미나 나노튜브의 제조방법 및 제조된 알루미나나노튜브의수소저장체로서의 용도
DK1394115T3 (da) 2002-08-24 2010-01-04 Haldor Topsoe As Rhenium (iv) sulfid-nanorörmateriale og fremgangsmåde til fremstilling
WO2005071702A1 (ja) * 2004-01-21 2005-08-04 Kyushu University, National University Corporation レドックスキャパシタ用電極材料及びその製造方法
JP4505635B2 (ja) * 2004-09-16 2010-07-21 国立大学法人 香川大学 ナノスケール物質およびその製造方法
CN109775758A (zh) * 2018-12-26 2019-05-21 中国电子科技集团公司第十八研究所 一种大层距五氧化二钒的制备方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH690720A5 (de) * 1996-12-18 2000-12-29 Eidgenoess Tech Hochschule Nanotubes, Verwendung solcher Nanotubes sowie Verfahren zu deren Herstellung.

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO0130690A3 *

Also Published As

Publication number Publication date
AU7767700A (en) 2001-05-08
JP2003512284A (ja) 2003-04-02
WO2001030690A3 (de) 2001-09-20
WO2001030690A2 (de) 2001-05-03

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