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WO2012000741A1 - Particules magnétiques partiellement silylées et dispersions contenant ces particules - Google Patents

Particules magnétiques partiellement silylées et dispersions contenant ces particules Download PDF

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Publication number
WO2012000741A1
WO2012000741A1 PCT/EP2011/059346 EP2011059346W WO2012000741A1 WO 2012000741 A1 WO2012000741 A1 WO 2012000741A1 EP 2011059346 W EP2011059346 W EP 2011059346W WO 2012000741 A1 WO2012000741 A1 WO 2012000741A1
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WO
WIPO (PCT)
Prior art keywords
magnetic core
shell particles
shell
content
particles according
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/EP2011/059346
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German (de)
English (en)
Inventor
Harald Herzog
Friedel Schultheis
Uwe Paulmann
Stipan Katusic
Jürgen Meyer
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.)
Evonik Operations GmbH
Original Assignee
Evonik Degussa GmbH
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Filing date
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Publication of WO2012000741A1 publication Critical patent/WO2012000741A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C04B35/62802—Powder coating materials
    • C04B35/62805—Oxide ceramics
    • C04B35/62807—Silica or silicates
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/24—Heavy metals; Compounds thereof
    • A61K33/26—Iron; Compounds thereof
    • 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
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0018—Mixed oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0018—Mixed oxides or hydroxides
    • C01G49/0036—Mixed oxides or hydroxides containing one alkaline earth metal, magnesium or lead
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0018—Mixed oxides or hydroxides
    • C01G49/0054—Mixed oxides or hydroxides containing one rare earth metal, yttrium or scandium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0018—Mixed oxides or hydroxides
    • C01G49/0063—Mixed oxides or hydroxides containing zinc
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0018—Mixed oxides or hydroxides
    • C01G49/0072—Mixed oxides or hydroxides containing manganese
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/06—Ferric oxide [Fe2O3]
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/08—Ferroso-ferric oxide [Fe3O4]
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62625—Wet mixtures
    • C04B35/6263—Wet mixtures characterised by their solids loadings, i.e. the percentage of solids
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62625—Wet mixtures
    • C04B35/6264—Mixing media, e.g. organic solvents
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    • 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
    • C09C1/22—Compounds of iron
    • C09C1/24—Oxides of iron
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    • 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C09C3/063—Coating
    • 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
    • C01P2004/86—Thin layer coatings, i.e. the coating thickness being less than 0.1 time the particle radius
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
    • C01P2004/88—Thick layer coatings
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2006/42—Magnetic properties
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5409—Particle size related information expressed by specific surface values
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/72—Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
    • C04B2235/721—Carbon content

Definitions

  • An object of the invention are magnetic core-shell particles comprising a core of one or more magnetic metal oxides and a shell of silica, wherein the surface of the shell is partially silylated.
  • Partially silylated is intended to mean that the surface of the silica shell comprises silanol groups Si-OH and silylated silanol groups Si-O-Si.
  • a preferred SiOH residual content of the particles according to the invention is 0.1 to 20 l / nm 2 particle surface, particularly preferably 0.5 to 10 l / nm 2 particle surface, in each case based on the particle.
  • the silylated silanol groups are those formed by reaction of hydroxy groups on the silica surface with organosilanes,
  • the organosiloxanes are preferably selected from one or more of the following compounds:
  • Vinyldimethylchlorosilane vinyldimethylethoxysilane, vinyldimethylmethoxysilane, vinylmethyldichlorosilane, vinylmethyldiethoxysilane, vinylmethyldimethoxysilane, vinyltrichlorosilane, vinyltriethoxysilane and vinyltrimethoxysilane, with octyltriethoxysilane and octyltrimethoxysilane being most preferred.
  • the core of the particles according to the invention may contain one or more oxides of iron, cobalt, nickel, chromium, europium, yttrium, samarium, gadolinium or mixed oxides thereof.
  • the metal oxides may be present in the core in a uniform modification or in various modifications.
  • the magnetic material of the core may further comprise mixed oxides comprising these metal oxides.
  • the BET surface area of the magnetic core-shell particles is preferably 20 to 100 m 2 / g, particularly preferably 30 to 60 m 2 / g.
  • the BET surface area is determined according to DIN ISO 9277.
  • Stable foams are obtained with ethanol contents of 10 to 30 vol.%, With 20 vol.% Being best. These foams are stabilized by the adsorption of magnetic particles at the interfaces of the bubbles.
  • the formation of reinforced bubbles provides adequate protection against any type of destabilization, ie dissolving gas, coarsening and coalescing; in fact, no visible changes are detected after a period of 2 months.
  • the bubbles are polydisperse with a range of sizes between 60 and 400 ⁇ .
  • the stability of the foam is influenced by the wettability of the partially silylated powder. The wettability can be adjusted by the ethanol concentration of the dispersion. The wettability translates into the so-called wetting angle q, which forms a gas / liquid interface with the particle surface.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Nanotechnology (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Epidemiology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Dispersion Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Developing Agents For Electrophotography (AREA)

Abstract

L'invention concerne des particules magnétiques coeur-écorce, comprenant un coeur constitué d'un ou de plusieurs oxydes métalliques magnétiques et d'une écorce en dioxyde de silicium, la surface de l'écorce étant partiellement silylée. L'invention concerne également des dispersions contenant ces particules.
PCT/EP2011/059346 2010-07-01 2011-06-07 Particules magnétiques partiellement silylées et dispersions contenant ces particules Ceased WO2012000741A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE201010030822 DE102010030822A1 (de) 2010-07-01 2010-07-01 Teilsilylierte magnetische Partikel und Dispersionen davon
DE102010030822.6 2010-07-01

Publications (1)

Publication Number Publication Date
WO2012000741A1 true WO2012000741A1 (fr) 2012-01-05

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PCT/EP2011/059346 Ceased WO2012000741A1 (fr) 2010-07-01 2011-06-07 Particules magnétiques partiellement silylées et dispersions contenant ces particules

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DE (1) DE102010030822A1 (fr)
WO (1) WO2012000741A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102012216010A1 (de) * 2012-09-10 2014-03-13 Evonik Industries Ag Kautschukmischung enthaltend Eisen-Silicium-Oxidpartikel mit verbesserter Aufheizgeschwindigkeit

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19614136A1 (de) * 1996-04-10 1997-10-16 Inst Neue Mat Gemein Gmbh Verfahren zur Herstellung agglomeratfreier nanoskaliger Eisenoxidteilchen mit hydrolysebeständigem Überzug
WO2001088540A1 (fr) * 2000-05-17 2001-11-22 University Of Florida Nanoparticules enrobees
WO2007123846A2 (fr) * 2006-04-17 2007-11-01 Rensselaer Polytechnic Institute SYNTHÈSE, FONCTIONNALISATION ET ENSEMBLE DE NANOAIMANTS MONODISPERSES À BASE DE FePt À ENVELOPPE DE SILICE DE COERCITIVITÉ ÉLEVÉE DE TAILLE ACCORDABLE, COMPOSITION ET STABILITÉ THERMIQUE À PARTIR DE MICRO-ÉMULSIONS
DE102008044384A1 (de) * 2008-12-05 2010-06-10 Evonik Degussa Gmbh Eisen-Silicium-Oxidpartikel mit einer Kern-Hülle-Struktur
WO2010096203A2 (fr) * 2009-02-23 2010-08-26 The Regents Of The University Of California Assemblage de cristaux photoniques accordables magnétiquement dans des solvants non polaires
WO2010149463A1 (fr) * 2009-06-23 2010-12-29 Evonik Degussa Gmbh Initiateurs de radicaux libres pouvant être activés par de la chaleur et matériau composite qui comprend des particules magnétiques

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19614136A1 (de) * 1996-04-10 1997-10-16 Inst Neue Mat Gemein Gmbh Verfahren zur Herstellung agglomeratfreier nanoskaliger Eisenoxidteilchen mit hydrolysebeständigem Überzug
WO2001088540A1 (fr) * 2000-05-17 2001-11-22 University Of Florida Nanoparticules enrobees
WO2007123846A2 (fr) * 2006-04-17 2007-11-01 Rensselaer Polytechnic Institute SYNTHÈSE, FONCTIONNALISATION ET ENSEMBLE DE NANOAIMANTS MONODISPERSES À BASE DE FePt À ENVELOPPE DE SILICE DE COERCITIVITÉ ÉLEVÉE DE TAILLE ACCORDABLE, COMPOSITION ET STABILITÉ THERMIQUE À PARTIR DE MICRO-ÉMULSIONS
DE102008044384A1 (de) * 2008-12-05 2010-06-10 Evonik Degussa Gmbh Eisen-Silicium-Oxidpartikel mit einer Kern-Hülle-Struktur
WO2010063557A1 (fr) 2008-12-05 2010-06-10 Evonik Degussa Gmbh Particules d'oxyde de fer-silicium dotées d’une structure de type cœur-écorce
WO2010096203A2 (fr) * 2009-02-23 2010-08-26 The Regents Of The University Of California Assemblage de cristaux photoniques accordables magnétiquement dans des solvants non polaires
WO2010149463A1 (fr) * 2009-06-23 2010-12-29 Evonik Degussa Gmbh Initiateurs de radicaux libres pouvant être activés par de la chaleur et matériau composite qui comprend des particules magnétiques

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
A. C. MARTINEZ, E. RIO, G. DELON, A. SAINT-JALMES, D. LANGEVIN, B. P. BINKS, SOFT MATTER, vol. 4, no. 7, 2008, pages 1531 - 1535
A. STOCCO, W. DRENCKHAN, E. RIO, D. LANGEVIN, B. P. BINKS, SOFT MATTER, vol. 5, no. 11, 2009, pages 2215 - 2222
B. P. BINKS, T. S. HOROZOV, ANGEWANDTE CHEMIE, vol. 44, no. 24, 2005, pages 3722 - 3725
VON J. MATHIAS, G. WANNEMACHER, JOURNAL OF COLLOID AND INTERFACE SCIENCE, vol. 125, 1988

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