EP1516345A1 - Monodisperse, magnetische nanokolloide einstellbarer grösse und verfahren zu deren herstellung - Google Patents

Monodisperse, magnetische nanokolloide einstellbarer grösse und verfahren zu deren herstellung

Info

Publication number
EP1516345A1
EP1516345A1 EP03722460A EP03722460A EP1516345A1 EP 1516345 A1 EP1516345 A1 EP 1516345A1 EP 03722460 A EP03722460 A EP 03722460A EP 03722460 A EP03722460 A EP 03722460A EP 1516345 A1 EP1516345 A1 EP 1516345A1
Authority
EP
European Patent Office
Prior art keywords
magnetic
magnetic particles
particle size
cobalt
nickel
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Withdrawn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
EP03722460A
Other languages
German (de)
English (en)
French (fr)
Inventor
Helmut Bönnemann
Werner Brijoux
Rainer Brinkmann
Nina Matoussevitch
Norbert WALDÖFNER
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.)
Studiengesellschaft Kohle gGmbH
Original Assignee
Studiengesellschaft Kohle gGmbH
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 Studiengesellschaft Kohle gGmbH filed Critical Studiengesellschaft Kohle gGmbH
Publication of EP1516345A1 publication Critical patent/EP1516345A1/de
Withdrawn legal-status Critical Current

Links

Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16CSHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C33/00Parts of bearings; Special methods for making bearings or parts thereof
    • F16C33/02Parts of sliding-contact bearings
    • F16C33/04Brasses; Bushes; Linings
    • F16C33/06Sliding surface mainly made of metal
    • F16C33/10Construction relative to lubrication
    • F16C33/1025Construction relative to lubrication with liquid, e.g. oil, as lubricant
    • F16C33/103Construction relative to lubrication with liquid, e.g. oil, as lubricant retained in or near the bearing
    • F16C33/1035Construction relative to lubrication with liquid, e.g. oil, as lubricant retained in or near the bearing by a magnetic field acting on a magnetic liquid
    • 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
    • B22F9/30Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
    • 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
    • B22F9/30Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
    • B22F9/305Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis of metal carbonyls
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y25/00Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16CSHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C32/00Bearings not otherwise provided for
    • F16C32/04Bearings not otherwise provided for using magnetic or electric supporting means
    • F16C32/0406Magnetic bearings
    • F16C32/044Active magnetic bearings
    • GPHYSICS
    • G11INFORMATION STORAGE
    • G11BINFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B11/00Recording on or reproducing from the same record carrier wherein for these two operations the methods are covered by different main groups of groups G11B3/00 - G11B7/00 or by different subgroups of group G11B9/00; Record carriers therefor
    • G11B11/10Recording on or reproducing from the same record carrier wherein for these two operations the methods are covered by different main groups of groups G11B3/00 - G11B7/00 or by different subgroups of group G11B9/00; Record carriers therefor using recording by magnetic means or other means for magnetisation or demagnetisation of a record carrier, e.g. light induced spin magnetisation; Demagnetisation by thermal or stress means in the presence or not of an orienting magnetic field
    • G11B11/105Recording on or reproducing from the same record carrier wherein for these two operations the methods are covered by different main groups of groups G11B3/00 - G11B7/00 or by different subgroups of group G11B9/00; Record carriers therefor using recording by magnetic means or other means for magnetisation or demagnetisation of a record carrier, e.g. light induced spin magnetisation; Demagnetisation by thermal or stress means in the presence or not of an orienting magnetic field using a beam of light or a magnetic field for recording by change of magnetisation and a beam of light for reproducing, i.e. magneto-optical, e.g. light-induced thermomagnetic recording, spin magnetisation recording, Kerr or Faraday effect reproducing
    • G11B11/10582Record carriers characterised by the selection of the material or by the structure or form
    • GPHYSICS
    • G11INFORMATION STORAGE
    • G11BINFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B11/00Recording on or reproducing from the same record carrier wherein for these two operations the methods are covered by different main groups of groups G11B3/00 - G11B7/00 or by different subgroups of group G11B9/00; Record carriers therefor
    • G11B11/10Recording on or reproducing from the same record carrier wherein for these two operations the methods are covered by different main groups of groups G11B3/00 - G11B7/00 or by different subgroups of group G11B9/00; Record carriers therefor using recording by magnetic means or other means for magnetisation or demagnetisation of a record carrier, e.g. light induced spin magnetisation; Demagnetisation by thermal or stress means in the presence or not of an orienting magnetic field
    • G11B11/105Recording on or reproducing from the same record carrier wherein for these two operations the methods are covered by different main groups of groups G11B3/00 - G11B7/00 or by different subgroups of group G11B9/00; Record carriers therefor using recording by magnetic means or other means for magnetisation or demagnetisation of a record carrier, e.g. light induced spin magnetisation; Demagnetisation by thermal or stress means in the presence or not of an orienting magnetic field using a beam of light or a magnetic field for recording by change of magnetisation and a beam of light for reproducing, i.e. magneto-optical, e.g. light-induced thermomagnetic recording, spin magnetisation recording, Kerr or Faraday effect reproducing
    • G11B11/10582Record carriers characterised by the selection of the material or by the structure or form
    • G11B11/10586Record carriers characterised by the selection of the material or by the structure or form characterised by the selection of the material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/0036Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
    • H01F1/0045Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
    • H01F1/0054Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
    • 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
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy

Definitions

  • the present invention relates to new, single- and multi-metallic, magnetic colloid particles (for example Fe, Co, Fe / Co) with an average particle size which can be set between 2 nm and approx. 15 nm and a narrow distribution without a separation step (such as magnetic separation) the particle sizes (standard deviation maximum 1.6 nm) and a process for their production.
  • the advantage of the new materials is their high saturation magnetization and their special suitability for the production of highly efficient ferrofluids with a low metal concentration and low viscosity.
  • Magnetic nanocolloids are sought-after materials for the production of magnetic fluids. These are used in technology as a sealing medium against dust and gases in magnetic fluid seals (liquid O-ring), for the lubrication and bearing of rotating shafts (magnetic levitation bearings) and for magneto-optical information storage. Applications in the medical-pharmaceutical field are, for example, magnetic markers of sick cells and the magnetic cell separation in biological samples, as well as the local application of drugs.
  • Giersig (Aust. J. Chem. 2001, 54, pp. 497 - 501) went another way to obtain monodisperse Co-particles with a narrow size distribution from dispersions with high saturation magnetization, using magnetic separation. According to this method, co-colloids with a wide size distribution are first obtained, from which a certain area has to be filtered out by magnetic separation. As a result, the yield of the desired material was very low. According to C. Petit, A. Taleb and MP Pileni (J. Phys. Chem. B, Vol. 103 (11), 1999, pp.
  • the magnetization curve (A in FIG. 3) of a dispersion of 10 nm cobalt particles produced according to the invention shows a magnetization of 11.6 T at a concentration of only 0.6 vol.% Cobalt.
  • the setting of the average particle size is controlled by the alkyl radical and the concentration of the organometallic compound. Become mixtures When low-valent compounds of different metals are used, multi-metallic magnetic particles (alloy particles) are formed.
  • the isolated, monodisperse, magnetic nanocolloids produced by this process are not long-term stable in air, but can easily be protected against total oxidation by an aftertreatment. If the magnetic particles in the organic solvent are subsequently treated by passing air through them or passing them through, magnetic particles are obtained which are resistant to oxidation after drying.
  • Cobalt particles which were prepared from CO 2 (CO) s in the presence of Al (C8H-
  • the unprotected or post-protected magnetic nanoparticles of either 2 nm to 15 nm, but at least up to 10.5 nm in size can be used in isolated form or with the aid of dispersants (eg Korantin SH from BASF or Sarcosyl from Merck) Bring colloidal into solution and continue to use in the form of magnetic fluids.
  • dispersants eg Korantin SH from BASF or Sarcosyl from Merck
  • the following examples may be mentioned: sealing medium against dust and gases in magnetic fluid seals (liquid O-ring), lubrication and bearing of rotating shafts (magnetic levitation bearings) as well as magneto-optical information storage, for example in compact and mini disks.
  • a cell-compatible layer e.g. gold, cf.
  • WO 99/41758 on the particle surface are also suitable for the magnetic in-vitro labeling of cells and can be used for the magnetic separation of labeled cells in biological samples or for the local application of medicaments.
  • the monodispersity of the magnetic nanoparticles produced according to the invention is of decisive advantage for all areas of application.
  • Example 1 Co-colloids of uniform size (10 nm) by thermolysis of CO 2 (CO) s in the presence of AI (CgH-
  • 7) 3 (atomic ratio Co: AI 12: 1)
  • Example 4 Co-colloids of uniform size (5.4 nm) from CO 2 (CO) 8 by thermolysis in the presence of Al (C8H-
  • 7) 3 (atomic ratio Co: AI 1: 2)
  • Example 6 Monodisperse Co-Colloid (3.4 nm) by thermolysis of CO 2 (CO) s in the presence of (C ⁇ Hg ⁇ AIH
  • Example 7 Comparative example: Co-colloids according to the conventional method
  • Example 8 Monodisperse Ni colloid (2.5 nm) by thermolysis of Ni (COD) 2 in the presence of (C2Hs) 3 AI
  • Ni particles is mixed with 2 ml (1.77 g, 5 mmol) of the dispersant KorantinSH (BASF) in 50 ml of Toiuol, a deep black-brown colored Ni magnetic fluid with a particle size of 2.5 nm ⁇ 0.8 nm is obtained.
  • KorantinSH dispersantinSH
  • Example 9 Co-colloids of uniform size (10 nm) from CO 2 (CO) s in the presence of Al (C8H-
  • 7) 3 (atomic ratio Co: Al 10: 1) and post-treatment with air
  • reaction mixture was stirred for a further 16 h while cooling to room temperature.
  • the reaction mixture was then oxidized by passing air through (approx. 5 h) and stirred for approx. 16 h. After the precipitate had settled for 3 h, the supernatant solution was decanted from the precipitate.
  • Example 10 Co-colloids of uniform size (8 nm) from CO 2 (CO) 8 in the presence of Al (C8H-
  • 7) 3 (atomic ratio Co: Al 5: 1) and post-treatment with air

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • General Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Biomedical Technology (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Power Engineering (AREA)
  • Soft Magnetic Materials (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Colloid Chemistry (AREA)
EP03722460A 2002-06-21 2003-04-12 Monodisperse, magnetische nanokolloide einstellbarer grösse und verfahren zu deren herstellung Withdrawn EP1516345A1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10227779A DE10227779A1 (de) 2002-06-21 2002-06-21 Monodisperse, magnetische Nanokolloide einstellbarer Größe und Verfahren zu deren Herstellung
DE10227779 2002-06-21
PCT/EP2003/003814 WO2004001776A1 (de) 2002-06-21 2003-04-12 Monodisperse, magnetische nanokolloide einstellbarer grösse und verfahren zu deren herstellung

Publications (1)

Publication Number Publication Date
EP1516345A1 true EP1516345A1 (de) 2005-03-23

Family

ID=29719339

Family Applications (1)

Application Number Title Priority Date Filing Date
EP03722460A Withdrawn EP1516345A1 (de) 2002-06-21 2003-04-12 Monodisperse, magnetische nanokolloide einstellbarer grösse und verfahren zu deren herstellung

Country Status (7)

Country Link
US (1) US20060037434A1 (ja)
EP (1) EP1516345A1 (ja)
JP (1) JP2005530354A (ja)
AU (1) AU2003229654A1 (ja)
CA (1) CA2489975A1 (ja)
DE (1) DE10227779A1 (ja)
WO (1) WO2004001776A1 (ja)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3930495B2 (ja) 2004-06-16 2007-06-13 三菱重工業株式会社 ニッケル超微粒子分散液体ナトリウムの製造方法、装置、液体ナトリウムの漏洩検出方法
CA2500077A1 (en) * 2005-03-09 2006-09-09 Chemical Vapour Metal Refining Inc. Production of ultra fine transition metal powders
WO2008034062A2 (en) * 2006-09-15 2008-03-20 Board Of Supervisors Of Louisiana State University And Agricultural And Mechanical College Method for making cobalt nanomaterials
BRPI0800207B1 (pt) * 2008-01-24 2018-01-09 Petroleo Brasileiro S.A. - Petrobras Catalisador metálico e método para a produção de catalisador metálico
US9384862B2 (en) 2012-06-22 2016-07-05 Ge-Hitachi Nuclear Energy Americas Llc Method of fabricating liquid-metal coolants for nuclear reactors

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE977064C (de) * 1950-05-12 1965-01-07 Gen Aniline & Film Corp Verfahren zur Herstellung von Metallen gleichmaessiger, sehr kleiner Teilchengroesse durch thermische Zersetzung von Metallcarbonylen
US2744040A (en) * 1952-03-25 1956-05-01 Gen Aniline & Film Corp Process of preparing iron powder for magnetic cores
DE1084395B (de) * 1952-12-03 1960-06-30 Gen Aniline & Film Corp Verfahren zur Verbesserung der elektromagnetischen Eigenschaften von Carbonyl-Eisenpulver
US3856580A (en) * 1973-06-22 1974-12-24 Gen Electric Air-stable magnetic materials and method
DE3934351A1 (de) * 1989-10-14 1991-04-18 Studiengesellschaft Kohle Mbh Verfahren zur herstellung von mikrokristallinen bis amorphen metall- bzw. legierungspulvern und ohne schutzkolloid in organischen solventien geloesten metallen bzw. legierungen
EP0672765B1 (en) * 1994-03-14 1999-06-30 Studiengesellschaft Kohle mbH Electrochemical reduction of metal salts as a method of preparing highly dispersed metal colloids and substrate fixed metal clusters by electrochemical reduction of metal salts
DE19654864A1 (de) * 1996-02-27 1997-08-28 Thomas Dipl Ing Haehndel Magnetofluid mit einer Sättigungsmagnetisierung von 150 bis 450 mT
DE19821968A1 (de) * 1998-05-18 1999-11-25 Studiengesellschaft Kohle Mbh Verfahren zur Modifizierung der Dispergiereigenschaften von metallorganisch-prästabilisierten bzw. -vorbehandelten Nanometallkolloiden

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2004001776A1 *

Also Published As

Publication number Publication date
AU2003229654A1 (en) 2004-01-06
US20060037434A1 (en) 2006-02-23
WO2004001776A1 (de) 2003-12-31
CA2489975A1 (en) 2003-12-31
JP2005530354A (ja) 2005-10-06
DE10227779A1 (de) 2004-01-08

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