[go: up one dir, main page]

WO2006109059A1 - Purification de nanoparticules par separation de phase - Google Patents

Purification de nanoparticules par separation de phase Download PDF

Info

Publication number
WO2006109059A1
WO2006109059A1 PCT/GB2006/001337 GB2006001337W WO2006109059A1 WO 2006109059 A1 WO2006109059 A1 WO 2006109059A1 GB 2006001337 W GB2006001337 W GB 2006001337W WO 2006109059 A1 WO2006109059 A1 WO 2006109059A1
Authority
WO
WIPO (PCT)
Prior art keywords
suspension
nanotubes
nanoparticles
nanorods
phase
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.)
Ceased
Application number
PCT/GB2006/001337
Other languages
English (en)
Inventor
Shanju Zhang
Ian Anthony Kinloch
Alan H. Windle
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.)
Cambridge University Technical Services Ltd CUTS
Cambridge Enterprise Ltd
Original Assignee
Cambridge University Technical Services Ltd CUTS
Cambridge Enterprise Ltd
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
Priority claimed from GB0507661A external-priority patent/GB0507661D0/en
Application filed by Cambridge University Technical Services Ltd CUTS, Cambridge Enterprise Ltd filed Critical Cambridge University Technical Services Ltd CUTS
Publication of WO2006109059A1 publication Critical patent/WO2006109059A1/fr
Anticipated expiration legal-status Critical
Ceased 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0547—Nanofibres or nanotubes
    • 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
    • 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
    • C01B32/17—Purification
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/0475—Purification
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/56—Treatment of carbon black ; Purification
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • 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
    • 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
    • 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
    • C01B2202/34—Length
    • 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
    • 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
    • C01P2004/13—Nanotubes
    • 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
    • C01P2004/133—Multiwall nanotubes

Definitions

  • the isotropic and nematic phases are separated by a two phase region (Flory chimney) extending over a fixed range of compositions [8] .
  • the two phase region is a part of the overall thermodynamic equilibrium, and within it the co-existing isotropic and liquid crystalline phases each have a fixed composition but change in relevant amounts, as the overall concentration of the solute (i.e. CNTs) in suspension is increased.
  • the two phase region covers a few % of the overall concentration range.
  • the suspensions are in a solvent selected from water, polar organic solvents such as alcohol (for example ethanol) , acetone, DMSO, DMS, DMF, THF and NMP, halogenated solvents such as tetrachloroethylene, DCM and chloroform, acid (for example sulphuric acid or nitric acid) and oleum.
  • polar organic solvents such as alcohol (for example ethanol) , acetone, DMSO, DMS, DMF, THF and NMP
  • halogenated solvents such as tetrachloroethylene, DCM and chloroform
  • acid for example sulphuric acid or nitric acid
  • oleum oleum
  • Figure 1 (a) shows a polarised light micrograph of nematic structures in crude 8 wt% aqueous suspension of chopped CNTs between crossed polars .
  • a Schlieren texture which can be confirmed on rotation of the crossed polars is observed, indicating a single-phase polydomain in the crude suspension.
  • Figure 2 (b) shows an electron micrograph of the continuous nematic phase in Figure 2 (a) . Significantly, the longer CNTs dominate the nematic phase.
  • Figure 9 shows a plot of individual concentrations of isotropic and anisotropic phases as a function of total nanotube suspension concentration. The lines are drawn to guide the eye only.
  • Figure 10 shows a plot of the anisotropic phase volume fraction versus the total suspension concentration for nanotube aqueous suspension with various cycles of centrifugation as indicated in the Figure.
  • phase separation is carried out by leaving the first suspension to stand for several weeks.
  • the aqueous suspensions of nanotubes were prepared by oxidising the as-synthesised nanotubes for 24 hours in a 3:1 mixture of concentrated sulphuric acid and concentrated nitric acid under ultrasonication and then extracting them with deionised water. The chopped nanotubes were then dissolved in deionised water at different concentrations.
  • a thin liquid film was prepared by placing a drop of nanotube suspensions between two glass slides to form a sandwich cell, which was subsequently sealed using epoxy glue.
  • the wet samples were left standing at room temperature for several days to develop the texture.
  • the phases were identified by characteristic textures observed under the reflected polarised optical microscopy (Olympus BX-50) .
  • the morphologies and microstructures of nanotubes in isotropic and anisotropic phases were examined using a JEOL 6340F field emission gun scanning electron microscopy at an accelerating voltage of 5 kV. This analysis method was also used as appropriate in Examples 2 and 3.
  • FIGS. 2b and 2c show typical electron micrographs for the nanotube distributions and alignments in the two phases.
  • the nematic consists of highly ordered, longer nanotubes ( Figure 2b) .
  • the liquid crystalline region, which is classified as nematic, contains topological defects or disclinations, two of which are present in Figure 2b.
  • the disclination density and the lateral separation between individual nanotubes decreased considerably compared to the crude nematic sample ( Figure Ib) .
  • Example 3 This example relates to a more detailed study of the method and product of Example 2.
  • Fig. 10 shows the volume fraction of anisotropic phase against the total concentration for different cycles of centrifugation. For each cycle of centrifugation, increasing the total concentration resulted in an increase of volume fraction of anisotropic phase, following a simple linear function. The slope of each linear curve increases with increase of cycle number. It should be noted that the value of critical concentration (ci*) of starting anisotropic is roughly same for each cycle, e.g. Ci* ⁇ 1.6 wt% .

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Composite Materials (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

Méthode de purification de nanoparticules comprenant les étapes suivantes : préparer une première suspension de nanoparticules ; causer ou permettre la séparation de phase de la première suspension pour obtenir une suspension liquide cristalline de nanoparticules purifiées et une deuxième suspension ; et séparer la suspension liquide cristalline de nanoparticules purifiées de la deuxième suspension.
PCT/GB2006/001337 2005-04-15 2006-04-12 Purification de nanoparticules par separation de phase Ceased WO2006109059A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
GB0507661A GB0507661D0 (en) 2005-04-15 2005-04-15 Nematic-induced phase separation and length fractionation of multiwall carbon nanotubes
GB0507661.7 2005-04-15
GB0512951.5 2005-06-24
GB0512951A GB0512951D0 (en) 2005-04-15 2005-06-24 Purification of nanoparticles by phase separation

Publications (1)

Publication Number Publication Date
WO2006109059A1 true WO2006109059A1 (fr) 2006-10-19

Family

ID=36660158

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB2006/001337 Ceased WO2006109059A1 (fr) 2005-04-15 2006-04-12 Purification de nanoparticules par separation de phase

Country Status (1)

Country Link
WO (1) WO2006109059A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009059017A3 (fr) * 2007-10-30 2010-04-15 Auburn University Nanocylindres inorganiques sous la forme de cristaux liquides
WO2012094072A1 (fr) * 2011-01-04 2012-07-12 Carestream Health, Inc. Procédés de récupération de nanofils, compositions, et articles
CN102653415A (zh) * 2011-03-04 2012-09-05 中国科学院金属研究所 二氧化钛纳米材料的固相制备方法
CN116873905A (zh) * 2023-07-25 2023-10-13 中国科学院物理研究所 用于分离长碳纳米管和短碳纳米管的方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004024428A1 (fr) * 2002-09-10 2004-03-25 The Trustees Of The University Pennsylvania Nanotubes de carbone: dispersions hautement solides et leurs gels nematiques

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004024428A1 (fr) * 2002-09-10 2004-03-25 The Trustees Of The University Pennsylvania Nanotubes de carbone: dispersions hautement solides et leurs gels nematiques

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
DAVIS V A ET AL: "PHASE BEHAVIOR AND RHEOLOGY OF SWNTS IN SUPERACIDS", MACROMOLECULES, ACS, WASHINGTON, DC, US, vol. 37, no. 1, 2004, pages 154 - 160, XP008054982, ISSN: 0024-9297 *
DIERKING I ET AL: "Aligning and reorienting carbon nanotubes with nematic liquid crystals", ADVANCED MATERIALS, WILEY VCH, WEINHEIM, DE, vol. 16, no. 11, 4 June 2004 (2004-06-04), pages 865 - 869, XP002381529, ISSN: 0935-9648 *
RAMESH SIVARAJAN ET AL: "Dissolution of pristine single walled carbon nanotubes in superacids by direct protonation", J PHYS CHEM B; JOURNAL OF PHYSICAL CHEMISTRY B JUL 1 2004, vol. 108, no. 26, 1 July 2004 (2004-07-01), pages 8794 - 8798, XP002391690 *
SONG WENHUI ET AL: "Isotropic-nematic phase transition of dispersions of multiwall carbon nanotubes", MACROMOLECULES; MACROMOLECULES JUL 12 2005, vol. 38, no. 14, 12 July 2005 (2005-07-12), pages 6181 - 6188, XP002391691 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009059017A3 (fr) * 2007-10-30 2010-04-15 Auburn University Nanocylindres inorganiques sous la forme de cristaux liquides
WO2012094072A1 (fr) * 2011-01-04 2012-07-12 Carestream Health, Inc. Procédés de récupération de nanofils, compositions, et articles
US8696947B2 (en) 2011-01-04 2014-04-15 Carestream Health, Inc. Nanowire recovery methods, compositions, and articles
CN102653415A (zh) * 2011-03-04 2012-09-05 中国科学院金属研究所 二氧化钛纳米材料的固相制备方法
CN116873905A (zh) * 2023-07-25 2023-10-13 中国科学院物理研究所 用于分离长碳纳米管和短碳纳米管的方法
CN116873905B (zh) * 2023-07-25 2025-06-27 中国科学院物理研究所 用于分离长碳纳米管和短碳纳米管的方法

Similar Documents

Publication Publication Date Title
Zhang et al. Mesogenicity drives fractionation in lyotropic aqueous suspensions of multiwall carbon nanotubes
US7968073B2 (en) Stable aqueous dispersions of carbon nanotubes
Davis et al. True solutions of single-walled carbon nanotubes for assembly into macroscopic materials
Doorn et al. High resolution capillary electrophoresis of carbon nanotubes
KR101210513B1 (ko) 액정성을 가지는 그래핀 조성물 및 그의 제조방법
Lagerwall et al. Carbon nanotubes in liquid crystals
Tang et al. Assembly of 1D nanostructures into sub‐micrometer diameter fibrils with controlled and variable length by dielectrophoresis
JP3676337B2 (ja) カーボンナノチューブとイオン性液体とから成るゲル状組成物とその製造方法
Huang et al. Hierarchical, interface-induced self-assembly of diphenylalanine: formation of peptidenanofibers and microvesicles
Bisoyi et al. Carbon-based liquid crystals: art and science
Ao et al. Cholesteric and nematic liquid crystalline phase behavior of double-stranded DNA stabilized single-walled carbon nanotube dispersions
Scalia Alignment of carbon nanotubes in thermotropic and lyotropic liquid crystals
AU2009204202A1 (en) Method and apparatus for identifying and characterizing material solvents and composite matrices and methods of using same
Yang et al. Role and impact of surfactants in carbon nanotube dispersions and sorting
King et al. Vacuum filtration based formation of liquid crystal films of semiconducting carbon nanotubes and high performance transistor devices
Davis Liquid crystalline assembly of nanocylinders
Shi et al. Electrospun fibers based on polyvinyl pyrrolidone/Eu-polyethylene glycol as phase change luminescence materials
Rai12 et al. Dispersions of functionalized single-walled carbon nanotubes in strong acids: Solubility and rheology
Tang et al. Study of the dispersion and electrical properties of carbon nanotubes treated by surfactants in dimethylacetamide
Seo et al. Mild acid-based surfactant-free solutions of single-walled carbon nanotubes: Highly viscous, less toxic, and humidity-insensitive solutions
WO2006109059A1 (fr) Purification de nanoparticules par separation de phase
KR102722324B1 (ko) 2차원 탄소나노물질과 탄소나노튜브를 포함하는 섬유 복합체 및 이의 제조방법
Agha et al. Interactions of carbon nanotubes in a nematic liquid crystal. II. Experiment
Scalia Liquid crystals of carbon nanotubes and carbon nanotubes in liquid crystals
CN113891853A (zh) 制备片状石墨烯的方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application
NENP Non-entry into the national phase

Ref country code: DE

WWW Wipo information: withdrawn in national office

Country of ref document: DE

NENP Non-entry into the national phase

Ref country code: RU

WWW Wipo information: withdrawn in national office

Country of ref document: RU

122 Ep: pct application non-entry in european phase

Ref document number: 06726736

Country of ref document: EP

Kind code of ref document: A1