WO2012152740A3 - Synthesis of nanoparticles comprising oxidation sensitive metals with tuned particle size and high oxidation stability - Google Patents

Synthesis of nanoparticles comprising oxidation sensitive metals with tuned particle size and high oxidation stability Download PDF

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Publication number
WO2012152740A3
WO2012152740A3 PCT/EP2012/058339 EP2012058339W WO2012152740A3 WO 2012152740 A3 WO2012152740 A3 WO 2012152740A3 EP 2012058339 W EP2012058339 W EP 2012058339W WO 2012152740 A3 WO2012152740 A3 WO 2012152740A3
Authority
WO
WIPO (PCT)
Prior art keywords
nanoparticles
citrate
capped
thin
synthesis
Prior art date
Application number
PCT/EP2012/058339
Other languages
French (fr)
Other versions
WO2012152740A2 (en
Inventor
Frank Rauscher
Claus Feldmann
Christian Kind
Huachang Lu
Karen KÖHLER
Leslaw Mleczko
Original Assignee
Bayer Intellectual Property Gmbh
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 EP11165705A external-priority patent/EP2522445A1/en
Priority claimed from EP11168094A external-priority patent/EP2529861A1/en
Application filed by Bayer Intellectual Property Gmbh filed Critical Bayer Intellectual Property Gmbh
Publication of WO2012152740A2 publication Critical patent/WO2012152740A2/en
Publication of WO2012152740A3 publication Critical patent/WO2012152740A3/en

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • B22F1/056Submicron particles having a size above 100 nm up to 300 nm
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

Process for the synthesis of nanoparticles comprising oxidation sensitive metals, in particular copper comprising the following steps: Preparation and nucleation of citrate-capped Metal-hydroxide nanoparticles, reduction of the intermediate citrate-capped Metal-hydroxide nanoparticles to Metal0 by reduction via NaBH4 Cu0 nanoparticles with narrow size distribution are obtained by NaBH4 Li-induced reduction of CUCI2 2H2O in diethylene glycol. The course of the reaction essentially involves an intermediate formation of Cu(OH)2 nanoparticles as well as the presence of citrate to control the nucleation of almost monodisperse and non-agglomerated Cu0 nanoparticles. The citrate-capped Cu0 nanoparticles of the invention are surprisingly stable against air oxidation. Via simple solvent evaporation, porous Cu0 thin-films are prepared on glass substrates that exhibit bulk-like sheet resistances of 0.23 - 0.42 Ωϛ after vacuum sintering at 250 °C (bulk-Cu sheet under similar conditions with: 0.3 Ωϛ). With these features the as-prepared, citrate-capped Cu0 nanoparticles become highly relevant to electronic devices in particular thin-film electronics, thin-film sensors and high-power batteries.
PCT/EP2012/058339 2011-05-11 2012-05-07 Synthesis of nanoparticles comprising oxidation sensitive metals with tuned particle size and high oxidation stability WO2012152740A2 (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
EP11165705A EP2522445A1 (en) 2011-05-11 2011-05-11 Synthesis of nanoparticles comprising oxidation sensitive metals with tuned particle size and high oxidation stability
EP11168094.8 2011-05-11
EP11165705.2 2011-05-11
EP11168094A EP2529861A1 (en) 2011-05-30 2011-05-30 Synthesis of Nanoparticles comprising oxidation sensitive metals with Tuned Particle Size and High Oxidation Stability

Publications (2)

Publication Number Publication Date
WO2012152740A2 WO2012152740A2 (en) 2012-11-15
WO2012152740A3 true WO2012152740A3 (en) 2013-01-10

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2012/058339 WO2012152740A2 (en) 2011-05-11 2012-05-07 Synthesis of nanoparticles comprising oxidation sensitive metals with tuned particle size and high oxidation stability

Country Status (2)

Country Link
TW (1) TW201306974A (en)
WO (1) WO2012152740A2 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9700940B2 (en) * 2012-09-27 2017-07-11 Lockheed Martin Corporation Metal nanoparticles formed around a nucleus and scalable processes for producing same
CN103408896B (en) * 2013-05-21 2016-01-27 中国科学院深圳先进技术研究院 A kind of epoxy resin composite material containing Nanometer Copper and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070190323A1 (en) * 2006-02-15 2007-08-16 Samsung Electro-Mechanics Co., Ltd. Method of producing metal nanoparticles
JP2010189681A (en) * 2009-02-17 2010-09-02 Hitachi Ltd Method for producing oxidation resistant copper nanoparticle, and joining method using the same

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE112005003693T5 (en) 2005-09-30 2008-08-07 Inspire AG für mechatronische Produktionssysteme und Fertigungstechnik Pressure cell and printhead for printing molten metals
JP2008190020A (en) 2007-02-07 2008-08-21 Osaka Univ Method for forming metal nanoparticle in medium

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070190323A1 (en) * 2006-02-15 2007-08-16 Samsung Electro-Mechanics Co., Ltd. Method of producing metal nanoparticles
JP2010189681A (en) * 2009-02-17 2010-09-02 Hitachi Ltd Method for producing oxidation resistant copper nanoparticle, and joining method using the same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
KYLER J. CARROLL ET AL: "Preparation of Elemental Cu and Ni Nanoparticles by the Polyol Method: An Experimental and Theoretical Approach", JOURNAL OF PHYSICAL CHEMISTRY C, vol. 115, no. 6, 17 February 2011 (2011-02-17), pages 2656 - 2664, XP055044673, ISSN: 1932-7447, DOI: 10.1021/jp1104196 *

Also Published As

Publication number Publication date
TW201306974A (en) 2013-02-16
WO2012152740A2 (en) 2012-11-15

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