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WO1997024224A1 - Nanocristaux de metal monodisperses organiquement fonctionnalises - Google Patents

Nanocristaux de metal monodisperses organiquement fonctionnalises Download PDF

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Publication number
WO1997024224A1
WO1997024224A1 PCT/US1996/020402 US9620402W WO9724224A1 WO 1997024224 A1 WO1997024224 A1 WO 1997024224A1 US 9620402 W US9620402 W US 9620402W WO 9724224 A1 WO9724224 A1 WO 9724224A1
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WO
WIPO (PCT)
Prior art keywords
metal
solution
particles
organic
group
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/US1996/020402
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English (en)
Inventor
James R. Heath
Daniel V. Leff
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Individual
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Individual
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Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to AU17433/97A priority Critical patent/AU1743397A/en
Priority to JP09523908A priority patent/JP2000504374A/ja
Priority to US09/091,389 priority patent/US6103868A/en
Priority to EP96945950A priority patent/EP0914244A1/fr
Publication of WO1997024224A1 publication Critical patent/WO1997024224A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/031—Precipitation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
    • B01J35/45—Nanoparticles
    • 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
    • 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
    • B22F1/0545—Dispersions or suspensions of nanosized particles
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy

Definitions

  • the nanocrystal products of the present invention avoid the previously discussed problems.
  • the "as prepared" spherical nanoparticles are crystalline and are characterized by narrow relative size distributions (as low as ⁇ 10 %). More importantly, however, is the fact that they are functionalized with well-defined organic groups covalently bound to the particle surface. These organic functional groups may be altered both chemically and with respect to percent coverage on the surface. Such chemistry is tremendously useful in the following ways: 1) the organic functional groups, coupled with the size-dependent curvature of a particle surface, yield varying solubilities as a function of particle size.
  • the present invention provides techniques for the synthesis of various metallic nanocrystal materials in which the resultant particles are characterized by the following properties: (1) they are soluble and resoluble in various organic media, including organic solutions containing dissolved polymers; (2) they are stable as powders or monodisperse (non-aggregated) colloids under ambient conditions for at least several days; (3) they are stable for months when stored under low temperature conditions as powders or monodisperse (non-aggregated) colloids in solution; (4) they can exist as monodisperse entities (when prepared as organic colloids) which can be readily separated into arbitrarily narrow size distributions via various chemical and chromatographic techniques; (5) they can be prepared in at least gram quantities; (6) they may consist of a host of metallic elements prepared as either pure metal particles or alloys, synthesized from the combination of a host of specific metal-containing inorganic compounds, phase transfer catalysts, surface passivants, and reducing agents; (7) they are readily dispersed into various matrices or onto various substrates (gels,
  • a second example of a potential application of these materials deals with using silver particles in reprography.
  • reprographic processes which have stages that intimately depend on the nucleation and growth of small silver particles.
  • small silver particles form the amplification (latent image) center in conventional photographic processes.
  • This latent image center formed by the action of light on silver halide crystals, acquires catalytic properties that enable it to trigger the reduction of the entire silver halide crystal to metallic silver by the reducing agent of the developer.
  • uniform particle size distributions lead to uniform film quality, and small particle sizes lead to enhanced film resolution.
  • gold since gold is frequently used in small quantities as a sensitizer for photographic emulsions, the Au particles may be applicable here as well.
  • nanocrystals as functional units in innovative micro and nanoelectronic devices. These applications are based on the idea that two- and three-dimensional close-packed ordered arrays (superlattices) of these nanocrystals will exhibit novel electronic properties dominated by single electron phenomena, due to the quantum confined electronic properties of the individual particles as well as their collective coherence effects.
  • UV/vis UV-visible spectroscopy
  • IR infrared spectroscopy
  • Particle composition, size, and properties may be varied by means of the following changes: the variation of the metal precursor used, the variation of phase transfer reagents used or their omission from the synthetic procedure, the variation of one or more surface passivants used, the variation of the reducing agent used, or the variation of some of the reactant molar ratios, or any combination thereof.
  • the peak positions, line shapes, and peak-to-peak distance of the Au 4f doublet are the standard measure of the gold oxidation state.
  • the binding energies for the Au 4f doublet are 83.5(3) and 87.2(3) eV (peak-to-peak distance of 3.7 eV). These measurements are consistent with the Au oxidation state.
  • a separate solution consisting of 20 g of sodium dodecylsulfate (SDS) dissolved in 300 ml of deionized H 2 O was prepared. This yielded a 6.25 weight percent solution of SDS in H 2 O;
  • 1 ml of the 6 mg/ml Ag particle/hexane solution was added to 20 ml of the 6.25 weight percent solution of SDS in H 2 O resulting in a two-layer mixture (organic layer on top and aqueous layer on the bottom). This mixture was stirred vigorously for a period of 6 hours.
  • the film thickness was measured by profilometry to be 20 ⁇ m.
  • the dielectric measurements of the metal nanocrystal-doped polymer thin film yielded unique dielectric values as copared to the 'pure' or un-doped polymer.
  • the dielectric characteristics for the metal nanocrystal-doped polymer thin film were: a) dielectric constant - 15; b) breadown voltate - 1.2 kv/mm. As can be seen, the dielectric constant of the doped film increases by about a factor of 10.
  • dodecylamine-capped Pt nanocrystals were prepared and characterized according to the procedure of Example 7.
  • the particles used here for catalysis had an average domain size of approximately 25 A;

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

La présente invention concerne la production de nanoparticules de métal organiquement fonctionnalisées. On procède pour cela en mélangeant un précurseur métallique avec un agent organique de passivation de surface, puis en faisant réagir le mélange résultant avec un réducteur de façon à générer un métal libre tout en liant l'agent de passivation à la surface du métal libre jusqu'à produire des particules de métal organiquement fonctionnalisées.
PCT/US1996/020402 1995-12-28 1996-12-27 Nanocristaux de metal monodisperses organiquement fonctionnalises Ceased WO1997024224A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
AU17433/97A AU1743397A (en) 1995-12-28 1996-12-27 Organically-functionalized monodisperse nanocrystals of metals
JP09523908A JP2000504374A (ja) 1995-12-28 1996-12-27 有機的に官能価された金属の単分散微小結晶
US09/091,389 US6103868A (en) 1996-12-27 1996-12-27 Organically-functionalized monodisperse nanocrystals of metals
EP96945950A EP0914244A1 (fr) 1995-12-28 1996-12-27 Nanocristaux de metal monodisperses organiquement fonctionnalises

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US972195P 1995-12-28 1995-12-28
US60/009,721 1995-12-28

Publications (1)

Publication Number Publication Date
WO1997024224A1 true WO1997024224A1 (fr) 1997-07-10

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US1996/020402 Ceased WO1997024224A1 (fr) 1995-12-28 1996-12-27 Nanocristaux de metal monodisperses organiquement fonctionnalises

Country Status (5)

Country Link
EP (1) EP0914244A1 (fr)
JP (1) JP2000504374A (fr)
AU (1) AU1743397A (fr)
CA (1) CA2241183A1 (fr)
WO (1) WO1997024224A1 (fr)

Cited By (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0920912A1 (fr) * 1997-12-02 1999-06-09 Basf Aktiengesellschaft Agglomérats de palladium et leur utilisation comme catalyseurs
WO1999038615A1 (fr) * 1998-01-31 1999-08-05 Bayer Aktiengesellschaft Colloides aqueux de metal precieux et leur utilisation
WO1999043427A1 (fr) * 1998-02-26 1999-09-02 Yissum Research Development Company Of The Hebrew University Of Jerusalem Procedes de preparation de particules de matiere de nano-taille
WO2000004593A1 (fr) * 1998-07-14 2000-01-27 Cambridge Display Technology Ltd Dispositifs optiques
WO2000003950A1 (fr) * 1998-07-14 2000-01-27 Cambridge Display Technology Ltd. Dispositifs optiques
WO2002030600A1 (fr) * 2000-10-13 2002-04-18 Ulvac, Inc. Dispersion de particules metalliques ultrafines et procede de fabrication
WO2003025260A1 (fr) * 2001-09-19 2003-03-27 Evergreen Solar, Inc. Procede a haut rendement permettant de preparer des nanocristaux de silicium a surface chimiquement accessibles
WO2002041826A3 (fr) * 2000-11-24 2003-04-03 Nanosolutions Gmbh Transfert de phase de nanoparticules
US6710091B1 (en) * 1999-02-23 2004-03-23 Bayer Aktiengesellschaft Nanoparticulate, redispersible zinc oxide gels
EP1349135A4 (fr) * 2000-12-04 2005-01-12 Ulvac Inc Procede de formation d'une electrode destinee a un panneau d'affichage plat
WO2005088652A1 (fr) * 2004-03-10 2005-09-22 Asahi Glass Company, Limited Particule fine contenant un métal, dispersion liquide de particules fines contenant un métal et matériau conducteur contenant un métal
WO2005121222A1 (fr) * 2004-06-07 2005-12-22 Battelle Memorial Institute Synthese de nanoparticules dans des solutions polymeres non aqueuses et produit
US6984265B1 (en) 1999-10-05 2006-01-10 Commonwealth Scientific And Industrial Research Organisation Three dimensional array films
US7001455B2 (en) 2001-08-10 2006-02-21 Evergreen Solar, Inc. Method and apparatus for doping semiconductors
EP1698413A3 (fr) * 2005-03-01 2006-09-13 Dowa Mining Co., Ltd. Particules d'argent et procédé de sa fabrication
EP1579935A4 (fr) * 2002-08-01 2007-08-01 Masami Nakamoto Nanoparticule metallique et son procede de fabrication
US7267721B2 (en) 2001-09-19 2007-09-11 Evergreen Solar, Inc. Method for preparing group IV nanocrystals with chemically accessible surfaces
WO2007120756A3 (fr) * 2006-04-12 2008-01-31 Nanomas Technologies Inc Nanoparticules, leurs procédés de formation et applications les utilisant
EP1579506A4 (fr) * 2002-08-15 2009-06-17 Univ Rockefeller Metal soluble dans l'eau et complexes de nanoparticules semi-condutrices
WO2009048983A3 (fr) * 2007-10-09 2009-07-02 Nanomas Technologies Inc Encres et pâtes à nanoparticules conductrices et applications les utilisant
US7708910B2 (en) * 2000-10-13 2010-05-04 Ulvac, Inc. Ink for ink jet printing and method for preparing the same
EP1857205A4 (fr) * 2005-03-02 2010-12-01 Japan Science & Tech Agency Nanoparticules de film ultramince de métal noble monocristallin formées en utilisant comme champ de réaction un film micelle adsorbé formé au niveau de l interface solide/liquide et procédé de fabrication idoine
JP2011052326A (ja) * 1999-06-15 2011-03-17 Akio Komatsu 金属複合超微粒子及びその製造方法
US7960025B2 (en) 2004-03-25 2011-06-14 Consejo Superior De Investigaciones Cientificas Magnetic nanoparticles comprising a core formed from noble metals
US8557607B2 (en) 2003-06-09 2013-10-15 Consejo Superior De Investigacione Cientificas Magnetic nanoparticles
WO2016039662A1 (fr) * 2014-09-12 2016-03-17 федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский национальный исследовательский университет информационных технологий, механики и оптики" (Университет ИТМО) Procédé de transfert interphase de nano-cristaux inorganiques minéraux colloïdes semi-conducteurs
US9296622B2 (en) 2012-08-22 2016-03-29 Hy-Power Coatings Limited Method for continuous preparation of indium-tin coprecipitates and indium-tin-oxide nanopowders with substantially homogeneous indium/tin composition, controllable shape and particle size
CN112893859A (zh) * 2019-11-19 2021-06-04 中国科学院大连化学物理研究所 一种AuPd合金纳米簇及其合成方法
CN113319275A (zh) * 2021-04-14 2021-08-31 深圳大学 一种Au@AgNRs纳米棒及其制备方法和应用
CN115609001A (zh) * 2022-07-15 2023-01-17 西北工业大学 一种以炔类化合物制备功能化金纳米颗粒的方法

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KR101166001B1 (ko) 2004-03-10 2012-07-18 아사히 가라스 가부시키가이샤 금속 함유 미립자, 금속 함유 미립자 분산액 및 도전성금속 함유 재료
JP4623981B2 (ja) * 2004-03-12 2011-02-02 大研化学工業株式会社 金属超微粒子の製造方法
JP2006089786A (ja) * 2004-09-22 2006-04-06 Mitsuboshi Belting Ltd 極性溶媒に分散した金属ナノ粒子の製造方法
EP1818123B1 (fr) * 2004-12-03 2012-01-11 Japan Science and Technology Agency Procédé de production de nanoparticules d'or stabilisées, nanoparticules d'or stabilisées obtenues par le procédé et l'utilisation des nanoparticules d'or stabilisées
JP4973645B2 (ja) * 2005-03-18 2012-07-11 セイコーエプソン株式会社 金属粒子分散液、金属粒子分散液の製造方法、導電膜形成基板の製造方法、電子デバイスおよび電子機器
JP4293181B2 (ja) 2005-03-18 2009-07-08 セイコーエプソン株式会社 金属粒子分散液、金属粒子分散液の製造方法、導電膜形成基板の製造方法、電子デバイスおよび電子機器
JP5753338B2 (ja) * 2005-07-01 2015-07-22 ナショナル ユニヴァーシティー オブ シンガポール 導電性複合材料
JP5272225B2 (ja) * 2009-03-31 2013-08-28 石原薬品株式会社 低融点金属粉末およびその製造方法
JP5197518B2 (ja) * 2009-07-16 2013-05-15 株式会社ノリタケカンパニーリミテド 白金微粒子およびその製造方法

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Cited By (52)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6197720B1 (en) 1997-12-02 2001-03-06 Basf Aktiengesellschaft Palladium clusters and their use as catalysts
EP0920912A1 (fr) * 1997-12-02 1999-06-09 Basf Aktiengesellschaft Agglomérats de palladium et leur utilisation comme catalyseurs
WO1999038615A1 (fr) * 1998-01-31 1999-08-05 Bayer Aktiengesellschaft Colloides aqueux de metal precieux et leur utilisation
WO1999043427A1 (fr) * 1998-02-26 1999-09-02 Yissum Research Development Company Of The Hebrew University Of Jerusalem Procedes de preparation de particules de matiere de nano-taille
US6706795B1 (en) * 1998-02-26 2004-03-16 Yissum Research Development Company Of The Hebrew University Of Jerusalem Methods for the preparation of nanosized material particles
KR100714386B1 (ko) * 1998-07-14 2007-05-07 캠브리지 디스플레이 테크놀로지 리미티드 광전자 디바이스
CN1314137C (zh) * 1998-07-14 2007-05-02 剑桥显示技术有限公司 光学器件及形成方法
WO2000003950A1 (fr) * 1998-07-14 2000-01-27 Cambridge Display Technology Ltd. Dispositifs optiques
US6777706B1 (en) 1998-07-14 2004-08-17 Cambridge Display Technologies Optical devices
WO2000004593A1 (fr) * 1998-07-14 2000-01-27 Cambridge Display Technology Ltd Dispositifs optiques
US6710091B1 (en) * 1999-02-23 2004-03-23 Bayer Aktiengesellschaft Nanoparticulate, redispersible zinc oxide gels
JP4732645B2 (ja) * 1999-06-15 2011-07-27 丸山 稔 金属複合超微粒子の製造方法
JP2011052326A (ja) * 1999-06-15 2011-03-17 Akio Komatsu 金属複合超微粒子及びその製造方法
US6984265B1 (en) 1999-10-05 2006-01-10 Commonwealth Scientific And Industrial Research Organisation Three dimensional array films
WO2002030600A1 (fr) * 2000-10-13 2002-04-18 Ulvac, Inc. Dispersion de particules metalliques ultrafines et procede de fabrication
JP2002121606A (ja) * 2000-10-13 2002-04-26 Ulvac Corporate Center:Kk 金属超微粒子分散液及びその製造方法
US7708910B2 (en) * 2000-10-13 2010-05-04 Ulvac, Inc. Ink for ink jet printing and method for preparing the same
WO2002041826A3 (fr) * 2000-11-24 2003-04-03 Nanosolutions Gmbh Transfert de phase de nanoparticules
EP1349135A4 (fr) * 2000-12-04 2005-01-12 Ulvac Inc Procede de formation d'une electrode destinee a un panneau d'affichage plat
US7001455B2 (en) 2001-08-10 2006-02-21 Evergreen Solar, Inc. Method and apparatus for doping semiconductors
US7232484B2 (en) 2001-08-10 2007-06-19 Evergreen Solar Inc. Method and apparatus for doping semiconductors
US6855204B2 (en) 2001-09-19 2005-02-15 Evergreen Solar Inc. High yield method for preparing silicon nanocrystals with chemically accessible surfaces
WO2003025260A1 (fr) * 2001-09-19 2003-03-27 Evergreen Solar, Inc. Procede a haut rendement permettant de preparer des nanocristaux de silicium a surface chimiquement accessibles
US7214599B2 (en) 2001-09-19 2007-05-08 Evergreen Solar Inc. High yield method for preparing silicon nanocrystal with chemically accessible surfaces
US7267721B2 (en) 2001-09-19 2007-09-11 Evergreen Solar, Inc. Method for preparing group IV nanocrystals with chemically accessible surfaces
US7648554B2 (en) 2002-08-01 2010-01-19 Daiken Chemical Co., Ltd. Metal nanoparticles and method for manufacturing same
EP1579935A4 (fr) * 2002-08-01 2007-08-01 Masami Nakamoto Nanoparticule metallique et son procede de fabrication
US7951453B2 (en) 2002-08-15 2011-05-31 The Rockefeller University Water soluble metal and semiconductor nanoparticle complexes
EP2469285A1 (fr) * 2002-08-15 2012-06-27 The Rockefeller University Métal soluble dans l'eau et complexes de nanoparticules de semi-conducteur
EP1579506A4 (fr) * 2002-08-15 2009-06-17 Univ Rockefeller Metal soluble dans l'eau et complexes de nanoparticules semi-condutrices
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