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WO2005023923A2 - Procedes de traitement de nanocristaux et compositions, dispositifs et systemes comprenant ces nanocristaux - Google Patents

Procedes de traitement de nanocristaux et compositions, dispositifs et systemes comprenant ces nanocristaux Download PDF

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Publication number
WO2005023923A2
WO2005023923A2 PCT/US2004/028966 US2004028966W WO2005023923A2 WO 2005023923 A2 WO2005023923 A2 WO 2005023923A2 US 2004028966 W US2004028966 W US 2004028966W WO 2005023923 A2 WO2005023923 A2 WO 2005023923A2
Authority
WO
WIPO (PCT)
Prior art keywords
nanocrystals
solvent
surfactant
less
mixture
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/US2004/028966
Other languages
English (en)
Other versions
WO2005023923A3 (fr
Inventor
Erik Scher
Mihai Buretea
Jeffery A. Whiteford
Andreas Meisel
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.)
Nanosys Inc
Original Assignee
Nanosys Inc
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 US10/656,802 external-priority patent/US6878871B2/en
Priority claimed from US10/656,910 external-priority patent/US6949206B2/en
Application filed by Nanosys Inc filed Critical Nanosys Inc
Priority to JP2006526216A priority Critical patent/JP2007505991A/ja
Publication of WO2005023923A2 publication Critical patent/WO2005023923A2/fr
Publication of WO2005023923A3 publication Critical patent/WO2005023923A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/02—Crystallisation from solutions
    • 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

Definitions

  • a first general class of embodiments provides methods of processing nanocrystals.
  • the nanocrystals are provided in a first solvent in which they are soluble.
  • the nanocrystals have a total amount of surfactant associated therewith, the total amount of surfactant including an amount of free surfactant and an amount of nanocrystal bound surfactant.
  • the nanocrystals are precipitated by adding a second solvent of higher polarity to the first solvent, producing a precipitating solvent mixture in which the nanocrystals are insoluble, to provide precipitated nanocrystals.
  • the precipitated nanocrystals are separated from the precipitating solvent mixture and are then redissolved by addition of a third solvent in which they are soluble.
  • the surfactant is typically soluble in at least the second solvent and the precipitating solvent mixture.
  • This process is optionally repeated to yield a desired level of purity.
  • Such repeated processing may be carried out a selected number of iterations, e.g., as are known to yield the desired purity.
  • the steps can be repeated two or more, three or more, four or more, five or more, or even six or more times.
  • the dissolved nanocrystals are checked for purity, e.g., to determine whether the surfactant level in the composition is sufficiently low.
  • the combination, phase formation, and separation steps are then optionally repeated as necessary until the amount of free surfactant in the nanocrystal mixture is less than 10% or less than 5% of the total surfactant concentration (free and bound), preferably less than 1%, and more preferably less than 0.1% of the total amount of surfactant.
  • Figure 1 is a flow chart that schematically illustrates nanocrystal synthesis using a surfactant mediated synthesis process.
  • a nanostructure includes a plurality of nanostructures
  • a solvent includes mixtures of solvents
  • a surfactant includes mixtures of surfactants, and the like.
  • a “nanocrystal” is a nanostructure that is substantially monocrystalline.
  • a nanocrystal thus has at least one region or characteristic dimension with a dimension of less than about 500 nm, e.g., less than about 200 nm, less than about 100 nm, less than about 50 nm, or even less than about 20 nm.
  • Nanocrystals can be substantially homogeneous in material properties, or in certain embodiments can be heterogeneous (e.g. heterostructures).
  • the term “nanocrystal” is intended to encompass substantially monocrystalline nanostructures comprising various defects, stacking faults, atomic substitutions, and the like, as well as substantially monocrystalline nanostructures without such defects, faults, or substitutions.
  • reduction of the amount of free surfactant in the nanocrystal containing solution is optionally carried out by an iterative washing process that involves selectively precipitating out the nanocrystal portion of the solution away from a majority of the contaminating free surfactant, redissolving the nanocrystals, and repeating the precipitation and redissolving steps until the level of free surfactant in solution is reduced to a desired level.
  • Heating of the reaction mixture (106) then permits annealing and growth of nanocrystallites, e.g., as a substantially monodisperse particle size population.
  • the growth process is then stopped by reducing the temperature of the reaction mixture (108).
  • Further refining of size distribution of the particles may optionally be accomplished by size selective precipitation (110) of the nanocrystals from the solvent mixture (see, e.g., U.S. Patent No. 6,322,901) using, e.g., low molecular weight alcohols, e.g., during one of the subsequent processing steps described below, to change the polarity of the reaction mixture and thus precipitate out nanocrystals.
  • the resulting nanocrystals are then subject to further processing (112).
  • the washing of the nanocrystal populations is carried out using a mixed solvent process that employs a solvent mixture that includes at least two different solvents of differing polarity whereby the nanocrystals are soluble in a sufficient concentration of a nonpolar or less polar first solvent and the surfactant portion is soluble in a sufficient concentration of the more polar second solvent.
  • a mixed solvent process that employs a solvent mixture that includes at least two different solvents of differing polarity whereby the nanocrystals are soluble in a sufficient concentration of a nonpolar or less polar first solvent and the surfactant portion is soluble in a sufficient concentration of the more polar second solvent.
  • both the more polar and less polar solvents are present at such permissive concentrations, e.g., both crystals and surfactants are soluble in the first mixture.
  • Subsequent precipitation steps typically add more polar solvent at the ratios described previously, e.g., between 2: 1 and 1:2 less polar to more polar solvent. This may be at the same level as used in the first precipitation step, or alternatively, it may be at a level greater than used in the first step.
  • the first precipitation step may also be used as a size selection process necessitating closer control over the added more polar solvent, e.g., to precipitate some, but not all nanocrystals in solution.
  • Subsequent precipitation steps are focused on recovering most if not all of the nanocrystals, rather than on such size selection. Accordingly, in many instances, the amount of more polar solvent added in such subsequent precipitation steps will be higher than in the initial precipitation.
  • the nanocrystals are combined with a first solvent in which the nanocrystals are soluble and a second solvent in which the nanocrystals are less soluble (e.g., insoluble).
  • the first and second solvents are permitted to form a first liquid phase comprising the first solvent and the nanocrystals and a second liquid phase comprising the second solvent, and the phases are then separated (e.g., one phase is pipetted, decanted, etc. away from the other).
  • the nanocrystals Once the nanocrystals have reached the desired level of purity, either by having been iteratively extracted a prescribed number of times or by having been analyzed to determine purity, they are optionally then subjected to additional processing steps, e.g., as described in greater detail below (see, e.g., the following section, entitled "Reduction of Bound Surfactant”).
  • additional processing steps e.g., as described in greater detail below (see, e.g., the following section, entitled "Reduction of Bound Surfactant”).
  • C. Reduction of Bound Surfactant Once the excess free surfactant is removed from the nanocrystals, e.g., following the last precipitation and separation step, the resulting nanocrystals may then be further processed to reduce the level of bound surfactant on the surfaces of the nanocrystals.
  • the nanocrystals that have been purified away from excess free surfactant are once again precipitated (step 216), and then redissolved in a combination of less polar solvent and a base, e.g., pyridine (step 218) and optionally incubated at elevated temperature (step 220).
  • a base e.g., pyridine
  • compositions including a population of nanocrystals and a surfactant bound thereto, wherein the surfactant comprises less than a bilayer.
  • the surfactant preferably comprises about a monolayer or less.
  • PEDOT layer processing [0114] PEDOT/PSS Poly(3,4-ethylenedioxythiophene) poly(styrenesulfonate) (e.g.,

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Photovoltaic Devices (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention concerne des procédés de traitement de nanocristaux destinés à éliminer l'excédent de matière organique libre et liée et en particulier des tensioactifs utilisés au cours du processus de synthèse. L'invention concerne également des compositions, des dispositifs et des systèmes comprenant des nanocristaux traités par ce procédé, ces compositions, dispositifs et systèmes pouvant être intégrés physiquement, électriquement et chimiquement dans une application finale.
PCT/US2004/028966 2003-09-04 2004-09-02 Procedes de traitement de nanocristaux et compositions, dispositifs et systemes comprenant ces nanocristaux Ceased WO2005023923A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2006526216A JP2007505991A (ja) 2003-09-04 2004-09-02 ナノ結晶の処理方法、並びに前記ナノ結晶を含む組成物、装置及びシステム

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
US10/656,802 US6878871B2 (en) 2002-09-05 2003-09-04 Nanostructure and nanocomposite based compositions and photovoltaic devices
US10/656,802 2003-09-04
US10/656,910 US6949206B2 (en) 2002-09-05 2003-09-04 Organic species that facilitate charge transfer to or from nanostructures
US10/656,910 2003-09-04
US54428504P 2004-02-11 2004-02-11
US60/544,285 2004-02-11

Publications (2)

Publication Number Publication Date
WO2005023923A2 true WO2005023923A2 (fr) 2005-03-17
WO2005023923A3 WO2005023923A3 (fr) 2005-06-16

Family

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Family Applications (1)

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PCT/US2004/028966 Ceased WO2005023923A2 (fr) 2003-09-04 2004-09-02 Procedes de traitement de nanocristaux et compositions, dispositifs et systemes comprenant ces nanocristaux

Country Status (3)

Country Link
JP (1) JP2007505991A (fr)
KR (1) KR20060079209A (fr)
WO (1) WO2005023923A2 (fr)

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US7057881B2 (en) 2004-03-18 2006-06-06 Nanosys, Inc Nanofiber surface based capacitors
US7105428B2 (en) 2004-04-30 2006-09-12 Nanosys, Inc. Systems and methods for nanowire growth and harvesting
US7267875B2 (en) 2004-06-08 2007-09-11 Nanosys, Inc. Post-deposition encapsulation of nanostructures: compositions, devices and systems incorporating same
WO2008013199A1 (fr) * 2006-07-28 2008-01-31 The Furukawa Electric Co., Ltd. DISPERSION DE FINES PARTICULES ET procédé de fabrication de DISPERSION DE FINES PARTICULES
WO2008013198A1 (fr) * 2006-07-28 2008-01-31 The Furukawa Electric Co., Ltd. procédé de fabrication de dispersion de fines particules et dispersion de fines particules
US7339184B2 (en) 2004-07-07 2008-03-04 Nanosys, Inc Systems and methods for harvesting and integrating nanowires
US7365395B2 (en) 2004-09-16 2008-04-29 Nanosys, Inc. Artificial dielectrics using nanostructures
US7501315B2 (en) 2004-06-08 2009-03-10 Nanosys, Inc. Methods and devices for forming nanostructure monolayers and devices including such monolayers
US7557028B1 (en) 2004-07-28 2009-07-07 Nanosys, Inc. Process for group III-V semiconductor nanostructure synthesis and compositions made using same
US7776760B2 (en) 2006-11-07 2010-08-17 Nanosys, Inc. Systems and methods for nanowire growth
US7776758B2 (en) 2004-06-08 2010-08-17 Nanosys, Inc. Methods and devices for forming nanostructure monolayers and devices including such monolayers
US7794600B1 (en) 2004-08-27 2010-09-14 Nanosys, Inc. Purification of nanocrystal solutions by chromatography
US7968273B2 (en) 2004-06-08 2011-06-28 Nanosys, Inc. Methods and devices for forming nanostructure monolayers and devices including such monolayers
US7976646B1 (en) 2005-08-19 2011-07-12 Nanosys, Inc. Electronic grade metal nanostructures
US7985454B2 (en) 2004-04-30 2011-07-26 Nanosys, Inc. Systems and methods for nanowire growth and manufacturing
US8558311B2 (en) 2004-09-16 2013-10-15 Nanosys, Inc. Dielectrics using substantially longitudinally oriented insulated conductive wires
US9005480B2 (en) 2013-03-14 2015-04-14 Nanosys, Inc. Method for solventless quantum dot exchange
US9139770B2 (en) 2012-06-22 2015-09-22 Nanosys, Inc. Silicone ligands for stabilizing quantum dot films
US9169435B2 (en) 2012-07-02 2015-10-27 Nanosys, Inc. Highly luminescent nanostructures and methods of producing same
US9695482B2 (en) 2007-10-12 2017-07-04 Fio Coporation Flow focusing method and system for forming concentrated volumes of microbeads, and microbeads formed further thereto
US9792809B2 (en) 2008-06-25 2017-10-17 Fio Corporation Bio-threat alert system
US9805165B2 (en) 2009-01-13 2017-10-31 Fio Corporation Handheld diagnostic test device and method for use with an electronic device and a test cartridge in a rapid diagnostic test
US9945837B2 (en) 2008-08-29 2018-04-17 Fio Corporation Single-use handheld diagnostic test device, and an associated system and method for testing biological and environmental test samples
US10279341B2 (en) 2004-02-02 2019-05-07 Oned Material Llc Porous substrates, articles, systems and compositions comprising nanofibers and methods of their use and production
CN110038350A (zh) * 2019-04-18 2019-07-23 苏州星烁纳米科技有限公司 纯化纳米晶溶液的装置及纯化方法
US10490817B2 (en) 2009-05-19 2019-11-26 Oned Material Llc Nanostructured materials for battery applications

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US7553371B2 (en) 2004-02-02 2009-06-30 Nanosys, Inc. Porous substrates, articles, systems and compositions comprising nanofibers and methods of their use and production
US8563133B2 (en) 2004-06-08 2013-10-22 Sandisk Corporation Compositions and methods for modulation of nanostructure energy levels
CA2580589C (fr) 2006-12-19 2016-08-09 Fio Corporation Systeme de detection microfluidique
US8623288B1 (en) 2009-06-29 2014-01-07 Nanosys, Inc. Apparatus and methods for high density nanowire growth
JP5868751B2 (ja) * 2012-03-26 2016-02-24 富士フイルム株式会社 銀ナノワイヤ分散液の製造方法
JP6958323B2 (ja) * 2017-12-18 2021-11-02 東洋インキＳｃホールディングス株式会社 量子ドット、量子ドット含有組成物、およびインクジェットインキ

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JP4404489B2 (ja) * 1998-09-18 2010-01-27 マサチューセッツ インスティテュート オブ テクノロジー 水溶性蛍光半導体ナノ結晶
US6251303B1 (en) * 1998-09-18 2001-06-26 Massachusetts Institute Of Technology Water-soluble fluorescent nanocrystals
AU6392399A (en) * 1998-09-18 2000-04-10 Massachusetts Institute Of Technology Biological applications of semiconductor nanocrystals
US6440213B1 (en) * 1999-10-28 2002-08-27 The Regents Of The University Of California Process for making surfactant capped nanocrystals
KR100867281B1 (ko) * 2001-10-12 2008-11-06 재단법인서울대학교산학협력재단 크기분리 과정 없이 균일하고 결정성이 우수한 금속,합금, 금속 산화물, 및 복합금속 산화물 나노입자를제조하는 방법
JP3900414B2 (ja) * 2002-02-18 2007-04-04 富士フイルム株式会社 ナノ粒子およびナノ粒子の製造方法、並びに、磁気記録媒体

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US10279341B2 (en) 2004-02-02 2019-05-07 Oned Material Llc Porous substrates, articles, systems and compositions comprising nanofibers and methods of their use and production
US7466533B2 (en) 2004-03-18 2008-12-16 Nanosys, Inc Nanofiber surface based capacitors
US7116546B2 (en) 2004-03-18 2006-10-03 Nanosys, Inc. Nanofiber surface based capacitors
US7057881B2 (en) 2004-03-18 2006-06-06 Nanosys, Inc Nanofiber surface based capacitors
US7295419B2 (en) 2004-03-18 2007-11-13 Nanosys, Inc. Nanofiber surface based capacitors
US7105428B2 (en) 2004-04-30 2006-09-12 Nanosys, Inc. Systems and methods for nanowire growth and harvesting
US7273732B2 (en) 2004-04-30 2007-09-25 Nanosys, Inc. Systems and methods for nanowire growth and harvesting
US7985454B2 (en) 2004-04-30 2011-07-26 Nanosys, Inc. Systems and methods for nanowire growth and manufacturing
US7666791B2 (en) 2004-04-30 2010-02-23 Nanosys, Inc. Systems and methods for nanowire growth and harvesting
US7501315B2 (en) 2004-06-08 2009-03-10 Nanosys, Inc. Methods and devices for forming nanostructure monolayers and devices including such monolayers
US7776758B2 (en) 2004-06-08 2010-08-17 Nanosys, Inc. Methods and devices for forming nanostructure monolayers and devices including such monolayers
US7267875B2 (en) 2004-06-08 2007-09-11 Nanosys, Inc. Post-deposition encapsulation of nanostructures: compositions, devices and systems incorporating same
US8143703B2 (en) 2004-06-08 2012-03-27 Nanosys, Inc. Methods and devices for forming nanostructure monolayers and devices including such monolayers
US7585564B2 (en) 2004-06-08 2009-09-08 Nanosys, Inc. Post-deposition encapsulation of nanostructures: compositions, devices and systems incorporating same
US7968273B2 (en) 2004-06-08 2011-06-28 Nanosys, Inc. Methods and devices for forming nanostructure monolayers and devices including such monolayers
US7344961B2 (en) 2004-07-07 2008-03-18 Nanosys, Inc. Methods for nanowire growth
US7339184B2 (en) 2004-07-07 2008-03-04 Nanosys, Inc Systems and methods for harvesting and integrating nanowires
US7557028B1 (en) 2004-07-28 2009-07-07 Nanosys, Inc. Process for group III-V semiconductor nanostructure synthesis and compositions made using same
US9688534B1 (en) 2004-07-28 2017-06-27 Nanosys, Inc. Process for group III-V semiconductor nanostructure synthesis and compositions made using same
US9469538B1 (en) 2004-07-28 2016-10-18 Nanosys, Inc. Process for group III-IV semiconductor nanostructure synthesis and compositions made using same
US10266409B1 (en) 2004-07-28 2019-04-23 Nanosys, Inc. Process for group III-V semiconductor nanostructure synthesis and compositions made using same
US8062967B1 (en) 2004-07-28 2011-11-22 Nanosys, Inc. Process for group III-V semiconductor nanostructure synthesis and compositions made using same
US9884763B1 (en) 2004-07-28 2018-02-06 Nanosys, Inc. Process for group III-V semiconductor nanostructure synthesis and compositions made using same
US8884273B1 (en) 2004-07-28 2014-11-11 Nanosys, Inc. Process for group III-V semiconductor nanostructure synthesis and compositions made using same
US7794600B1 (en) 2004-08-27 2010-09-14 Nanosys, Inc. Purification of nanocrystal solutions by chromatography
US8558311B2 (en) 2004-09-16 2013-10-15 Nanosys, Inc. Dielectrics using substantially longitudinally oriented insulated conductive wires
US7365395B2 (en) 2004-09-16 2008-04-29 Nanosys, Inc. Artificial dielectrics using nanostructures
US7976646B1 (en) 2005-08-19 2011-07-12 Nanosys, Inc. Electronic grade metal nanostructures
WO2008013199A1 (fr) * 2006-07-28 2008-01-31 The Furukawa Electric Co., Ltd. DISPERSION DE FINES PARTICULES ET procédé de fabrication de DISPERSION DE FINES PARTICULES
WO2008013198A1 (fr) * 2006-07-28 2008-01-31 The Furukawa Electric Co., Ltd. procédé de fabrication de dispersion de fines particules et dispersion de fines particules
US7776760B2 (en) 2006-11-07 2010-08-17 Nanosys, Inc. Systems and methods for nanowire growth
US9695482B2 (en) 2007-10-12 2017-07-04 Fio Coporation Flow focusing method and system for forming concentrated volumes of microbeads, and microbeads formed further thereto
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US11600821B2 (en) 2009-05-19 2023-03-07 Oned Material, Inc. Nanostructured materials for battery applications
US12224441B2 (en) 2009-05-19 2025-02-11 Oned Material, Inc. Nanostructured materials for battery
US10490817B2 (en) 2009-05-19 2019-11-26 Oned Material Llc Nanostructured materials for battery applications
US12469849B2 (en) 2009-05-19 2025-11-11 Oned Material, Inc. Nanostructured materials for battery applications
US11233240B2 (en) 2009-05-19 2022-01-25 Oned Material, Inc. Nanostructured materials for battery applications
US9139770B2 (en) 2012-06-22 2015-09-22 Nanosys, Inc. Silicone ligands for stabilizing quantum dot films
US9884993B2 (en) 2012-07-02 2018-02-06 Nanosys, Inc. Highly luminescent nanostructures and methods of producing same
US10707371B2 (en) 2012-07-02 2020-07-07 Nanosys, Inc. Highly luminescent nanostructures and methods of producing same
US9685583B2 (en) 2012-07-02 2017-06-20 Nanosys, Inc. Highly luminescent nanostructures and methods of producing same
US9631141B2 (en) 2012-07-02 2017-04-25 Nanosys, Inc. Highly luminescent nanostructures and methods of producing same
US9169435B2 (en) 2012-07-02 2015-10-27 Nanosys, Inc. Highly luminescent nanostructures and methods of producing same
US9005480B2 (en) 2013-03-14 2015-04-14 Nanosys, Inc. Method for solventless quantum dot exchange
CN110038350A (zh) * 2019-04-18 2019-07-23 苏州星烁纳米科技有限公司 纯化纳米晶溶液的装置及纯化方法

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Publication number Publication date
WO2005023923A3 (fr) 2005-06-16
JP2007505991A (ja) 2007-03-15
KR20060079209A (ko) 2006-07-05

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