WO2010059070A1 - Ceramic powders coated with a nanoparticle layer and process for obtaining thereof - Google Patents

Ceramic powders coated with a nanoparticle layer and process for obtaining thereof Download PDF

Info

Publication number
WO2010059070A1
WO2010059070A1 PCT/PT2008/000040 PT2008000040W WO2010059070A1 WO 2010059070 A1 WO2010059070 A1 WO 2010059070A1 PT 2008000040 W PT2008000040 W PT 2008000040W WO 2010059070 A1 WO2010059070 A1 WO 2010059070A1
Authority
WO
WIPO (PCT)
Prior art keywords
emulsion
detonation
coated
nanoparticles
ceramic
Prior art date
Application number
PCT/PT2008/000040
Other languages
English (en)
French (fr)
Inventor
João Manuel CALADO DA SILVA
Elsa Marisa Dos Santos Antunes
Original Assignee
Cuf-Companhia União Fabril, Sgps, S.A.
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 to PCT/PT2008/000040 priority Critical patent/WO2010059070A1/en
Priority to PT88130554T priority patent/PT2337821E/pt
Priority to US13/120,036 priority patent/US9512043B2/en
Priority to BRPI0823165-6A priority patent/BRPI0823165A2/pt
Priority to JP2011530979A priority patent/JP5836124B2/ja
Priority to ES08813055.4T priority patent/ES2460574T3/es
Priority to EP08813055.4A priority patent/EP2337821B1/en
Priority to PL08813055T priority patent/PL2337821T3/pl
Application filed by Cuf-Companhia União Fabril, Sgps, S.A. filed Critical Cuf-Companhia União Fabril, Sgps, S.A.
Priority to CA2739991A priority patent/CA2739991A1/en
Priority to EA201100396A priority patent/EA019292B1/ru
Priority to CN2008801312234A priority patent/CN102165021B/zh
Priority to AU2008364348A priority patent/AU2008364348B2/en
Priority to DK08813055.4T priority patent/DK2337821T3/da
Priority to KR1020117008282A priority patent/KR20110084500A/ko
Publication of WO2010059070A1 publication Critical patent/WO2010059070A1/en
Priority to EG2011040555A priority patent/EG26472A/en
Priority to ZA2011/02811A priority patent/ZA201102811B/en

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4584—Coating or impregnating of particulate or fibrous ceramic material
    • 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
    • C09C3/06—Treatment with inorganic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00—Compounds of copper
    • C01G3/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C04B35/62802—Powder coating materials
    • C04B35/62805—Oxide ceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C04B35/62886—Coating the powders or the macroscopic reinforcing agents by wet chemical techniques
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C04B35/62889—Coating the powders or the macroscopic reinforcing agents with a discontinuous coating layer
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C04B35/62892—Coating the powders or the macroscopic reinforcing agents with a coating layer consisting of particles
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C04B35/62897—Coatings characterised by their thickness
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63432—Polystyrenes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • 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
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • 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
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/40—Compounds of aluminium
    • 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
    • C09C3/06—Treatment with inorganic compounds
    • C09C3/063—Coating
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • 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
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/448—Sulphates or sulphites
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]

Definitions

  • the present invention concerns ceramic powders coated with nanoparticle layers of multiple crystalline structures, thickness, adhesion grade and crystallite size and process for obtaining these coated powders.
  • the ceramic powders according to the present invention present optical, mechanical, electrical, magnetic, catalytic and of reactive prOpei'ties substantially different from those of non-coated particles, which makes them particularly attractive for a set of applications in the nanotechnology field, such as electronics - for instance in semiconductor prodtiction, the biomedicine - for instance, in cancer treatments with magnetic nanoparticles surface-coated with functionality- enhanced nanoparticles in order to adhere to specific antibodies, chemistry - for instance in photocatalysis, in the ceramics industry - such as for obtaining sintering additives, in energy applications - such as in the nanographite material deposition. onto the surface of certain materials, in order to increase its electrical conductivity.
  • the methods usually used to prepare ceramic coatings are generally divided into four categories:
  • the micro emulsion, and sol-gel deposition, techniques are examples in this process.
  • the four main steps are the following: a) The colloidal particles intended to coat form a stable dispersion in a liquid, which also comprises the coating precursors; b) These precursor deposition onto the particle surfaces by spraying, immersion or rotation; c) The particles are polymerized during the removal of stabilizers, thus producing a gel in a. continuous net ; d) The final thermal handling results in the pyrolysis removal of the organic materials, leaving a crystalline or amorphous coating.
  • the main difficulty in coating processes via wet chemistry consists of controlling de reaction speed of the coating particle formation, making it difficult to obtain uniform coatings, with high adhesions.
  • CVD chemical vapor deposition
  • the coating thickness is high, typically between 5 and 12 microns, and there is no individual particle coating, but rather a substrate that might, have several geometrical forms .
  • a gas usually a gaseous organometalic precursor, is absorbed at the substrate surface;
  • Reaction of the first gaseous precursor with a second gas forming a monolayer, the number of reaction cycles between both precursors being the factor that controls the film's final thickness.
  • Another more elaborated technique consists of the synthesis of the base particles and of the coating particles from two gaseous precursors injected at different times in a hot- wall aerosol flow reactor.
  • a key example of this technique is the coating of tita ⁇ ia particles (TiO2) with silica (SiO2) .
  • TiO2 tita ⁇ ia particles
  • SiO2 silica
  • This approach starts from a suspension of particles intended to coat, to which a cation set is added, the cations being afterwards electrochemically reduced, forming a set of nanoparticles set which are deposited at the surface of the base particle.
  • the formation and deposition of copper oxide (CuO) nanoparticles onto silica particles (SiO2) is a classical example of the implementation of this technique .
  • the projection technique wherein a dense DC'amic-tax'get comprising the coating material, is sputtered by electrons, thus depositing it almost atom by atom in a substrate, thus forming a film.
  • a dense DC'amic-tax'get comprising the coating material
  • the method proposed by the present invention consisting of the detonation of an (W/0) emulsion, to which at least a solid precursor was previously added, which decomposes during the emulsion detonation, forming the nanoparticles comprising the desired composition, quantity and crystalline structure for the coating.
  • This method presents an enormous versatility, given that it promptly allows two different preparation means of the ceramic powders coated by a nanoparticle layer: a) Synthesizing in the same (W/0) emulsion detonation step, both the ceramic powders intended to coat, as the nanoparticles that form the coating layer.
  • two reaction kinetics are used differently for the precursors thereof, the formation reaction being extremely fast for the ceramic powders and slower in the case of decomposition of the precursors, which derive the nanoparticles that compose the coating layer .
  • the process allows: a. coating ceramic powders such as oxides, carbides, nitrides, inert metals, among others, from nanometric dimension to about 500 microns; b. From the addition of different precursors to the (W/O) emulsion in stechiometric proportions and of the combination among them during the detonation reaction, obtaining coatings with oxide nanoparticles in a multiplicity of crystalline structures (binary, ternary or superior), nitrides, inert metals, carbides, sulphides, etc; c.
  • ceramic powders such as oxides, carbides, nitrides, inert metals, among others, from nanometric dimension to about 500 microns
  • the document US5855827 in its turn, describes a cyclic process of detonation for the production of micrometric and nanometric powders and their projection at high-speed in different substrates, thus obtaining coated surfaces.
  • the detonation happens in a gaseous mixture to which metals of fine granulometry are added, a suspension, being formed.
  • the process of the present invention stands out from the later due to the use of an (W/0) emulsion, in the liquid phase, to which solid precursors are added or dissolved, or still inert ceramic particles, making it possible to obtain individual particles coated with a nanoparticle layer.
  • this emulsion is added with new types of precursors, the inert ceramic particles, intended to coat and solid nanoparticle precursors, that are critical elements for its final result, the ceramic powders coated by a nanoparticle layer.
  • the document PT 104085 discloses a method for obtaining nanomaterials at low temperature (inferior to 2000 0 C), from the detonation of two (W/0) emulsions, wherein the first is to stabilize the detonation front and the second has in its composition three types of precursors: dissolved oxidants in the internal phase, miscible fuels in the external phase and metals or alloys in the solid state, that combine during detonation in order to synthesize materials of nanometric dimension.
  • the (W/0) emulsion additionally to the types of precursors already disclosed in the said document, comprises at least a precursor added to the (W/0) emulsion, in the solid state, in way to guarantee sufficiently-differentiated formation kinetics of the base particle and nanoparticles, in order to obtain a ceramic powder coated with nanoparticles.
  • the. inert ceramic particle intended to coat is directly added to the (W/O) emulsion and, unlike the precursors in the quoted document, it does not take part in the (W/0) emulsion detonation reaction, allowing the nanoparticles to deposit on its surface.
  • the (W/0) emulsion with the precursors of the nanoparticles dissolved in the (W/0) emulsion sensitized by a military explosive (RDX) .
  • RDX military explosive
  • the (W/0) emulsion besides the oxidants dissolved in its internal phase, equally referred in the sais document, requires at least a precursor added to the
  • the inert ceramic particle intended to coat is directly added to (W/0) emulsion and, unlike the precursors in the said document, it does not take part in the (W/0) emulsion detonation reaction, allowing the nanoparticles to deposit on its surface .
  • the present invention relates to ceramic powders coated with a. nanoparticle layer with different compositions and process for obtaining the same.
  • the coatings of the pi ⁇ esent invention present a multiplicity of crystalline structures, thickness of the coating layer between 5 and 150 nm, a percentage of coated surface area, among 50 to 9b%, a high adhesiveness to the support base particle, changing their properties and functionalizing the base ceramic powders, for a multiple set of applications.
  • the process for coating the ceramic powders surface with a nanoparticles layer of different crystalline structures is based on the introduction of at least: a. precursor, in the solid state or dissolved in an (W/0) emulsion that, by decomposing during detonation result in nanoparticles, that are deposited onto the base particle that is intend to coat .
  • the said emulsion intended to detonate is of the (W/O) type, being broadly used, for instance, in the production of explosive emulsions.
  • This emulsion comprises two intimately linked phases, under the action of a surfactant: the internal (aqueous) and the external (insoluble) phase.
  • the process of the present invention can comprise two different embodiments, differing not only in the formation of the base particle (A) intended to coat, but also in the introduction of the precursor (s) that originate the nanoparticles (b) , of the coating layer (Pig.l).
  • both the base ceramic particles and the coating nanoparticles are formed during the detonation of the (W/0) emulsion
  • the ceramic particles intended to coat are directly placed and homogenized in the (W/0) emulsion.
  • the precursors of the coating nanoparticles are, in the first case, added in the solid state whereas, in the second case, they are generally dissolved in the internal structure of the (W/0) emulsion.
  • both the base ceramic particle (A) and the coating nanoparticles (b) are synthesized during the (W/0) emulsion detonation step.
  • the key aspect of this variant is that the ceramic powder (A) precursors intended for coating and the nanoparticle Cb) precursors, which constitute the coating layer, present very different reaction kinetics, during the (W/0) emulsion detonation.
  • the precursors of the base ceramic particle A are part of the emulsion internal structure, being dissolved in its internal p>hase, homogeneously mixed in the external phase, or being high reactivity metals, which allows them to present an extremely fast reaction kinetics, reacting inside or immediately behind the reaction zone, which is the zone that precedes and supports the advance of the shock wave, in the classical detonation model .
  • nanoparticle solid precursors are in the form of nitrides, sulphates, carbides, chlorides etc., for they are in the solid state and the respective decomposition reactions are highly endothermic, they do not react in the reaction zone, but in a very subsequent phase of the designated Taylor zone (or gas expansion) , zone where the base particles A are already formed, once the temperatures are inferior to their melting points, thus resulting in the fact that its coalescence-based growth no longer occurs. So being, the nanoparticles (b) are deposited and coat the surface of the base particles (A) .
  • This variant presents an enormous advantage for during the stage of (W/0) emulsion detonation, both the base particles (A) , and the coating layer nanoparticles (b) are formed.
  • the appropriate control of the process variables allows obtaining not only an enormous multiplicity of base particles of different dimensions and structures, but also base nanoparticles coatings, not only of binary structures (two elements from a single precursor) , but also ternary (from two solid precursors which combine during its decomposition, reaction) .
  • a base ceramic particle with a spynel- type structure such as MgAl204, coated by nanoparticles also of MgAl204, being for such sufficient that the (W/0) emulsion contains, in its internal phase, the stechiometric quantities of salts of magnesium and aluminium dissolved and, at the same time, be also added and mixed a certain quantity of solid precursors of the same elements (magnesium and aluminium) , depending on the coating thickness intended, the precursor quantity being larger as the thickness and the percentage of coated area increase .
  • the MgAl204 base particles are formed from the reaction of the salts dissolved in the (W/0) emulsion.
  • the coalescence and growth process of the formed particles occurs, in a subsequent phase, the external solid precursors decompose and combine, thus forming the MgAl204 nanoparticles, which project and coat the MgA12O4 base particle.
  • this variant of the process for preparing ceramic powders coated with a nanoparticle layer is constituted by the following steps:
  • the components of the (W/0) emulsion are selected from the group of soluble oxidant precursors, soluble fuels, mi ⁇ cible fuels, the choice of its nature and relative ratio depending on the empiric formula, structure type and dimension of the ceramic powder (A) intended to coat .
  • Starting from the stechiometry of the chemical reaction it is possible to calculate the necessary quantity of each precursor for the formation of a given compound, and it is equally possible to estimate from the enthalpy of the chemical reaction the detonation temperature and the coalescence time of the particles. With these data it is possible to estimate the dimension of the formed particles,
  • the step for the formation of a (W/0) emulsion begins, consisting of two intimately-linked phases, under the action of a surfactant: discontinuous internal phase (aqueous) and continuous external phase (insoluble) .
  • a surfactant discontinuous internal phase (aqueous) and continuous external phase (insoluble) .
  • the internal phase of the (W./'O) emulsion is a result of the dissolution of the precursors in water, according to the composition of the emulsion selected in 1.1.1. This phase is heated up to a. temperature between (35-105 0 C) above the crystallization point of all components, in order to allow its complete dissolution, which is important to obtain a good homogeneity of the formed products.
  • the external phase of the (w/0) emulsion is obtained by mixing of the hydrocarbons or organic materials, that compose it with a surfactant appropriate to low pH values (between 2 and 5) , soft heating between 35-85°C, in order to guarantee the appropriate viscosity of the mixture at a close temperature of the internal phase, which is important to guarantee a good emulsification of the two phases required. for carrying out stable and repi'oducible detonations .
  • the (W/0) emulsion according to the present invention is obtained, by emulsification of both internal and external phases formerly prepared according to the previously described, in an emulsified matrix, and subsequently refined at about 60-150 psi, in order to obtain micelles of 1 to 10 microns so as to produce a stable emulsion, that is, a non-degradable emulsion during the mixture of the remaining precursors .
  • an organic sensibiliser such as expanded polystyrene or plastic spheres without contaminants
  • an organic sensibiliser such as expanded polystyrene or plastic spheres without contaminants
  • the addition of metals in the solid state is endorsed, with subsequent homogenization in the (W/O) emulsion.
  • the homogenization of the emulsion is fundamental to guarantee that the parameters of the detonation reaction remain stable through time and space.
  • the dimension of particle A depends on reaction temperature and coalescence time, and. latter two parameters vary according to quantity of precursors and final material produced, the reaction/detonation temperature is the result of the difference between formation enthalpies of reagents and final products.
  • the (W/O) emulsion is subsequently placed in a cartridge of cylindrical geometry, for instance, in an appropriate material for detonation, such as paper, polyethylene or other material that it is selected in order not to introduce contaminants in the synthesized materials, with a diameter which is largei" than its critical diameter (the critical diameter is the diameter from which it is possible to sustain a. detonation, being usually experimentally determined) the detonation being then started inside an appropriate chamber from a detonation system, such as a detonator, a capacitive discharge system, laser system, among others .
  • a detonation system such as a detonator, a capacitive discharge system, laser system, among others .
  • the powders are dragged by the gases resulting from the detonation reaction, inside the expansion chamber, where they are cooled and collected in. dry or wet means.
  • the first aspect refers to the placement of the ceramic powder (A) intended to coat directly in the (W/O) emulsion, instead of being synthesized according to the previously described embodiment of the invention.
  • the second aspect refers to the nanoparticle (b) precursors, which in this case are already part of the internal structure of the (W/O) emulsion and are not subsequently added in the solid state, unlike the previously described embodiment of the invention, thus allowing not only the reduction of the quantity of total solids in the final composition, but also the improvement of the (w/0) emulsion' s rhe ⁇ logy, processability and detonability.
  • the incorporation of solids in the emulsion significantly increases its viscosity, which, limits the solids % considered as possible to introduce and difficult its homogenization, this way being preferable to dissolve them in the internal phase .
  • the key step of the coating process includes the control of the system' s atmosphere type (oxidant/reducing/inert ), mainly the (W/0) emulsion detonation temperature, in order to assure two essential aspects: a) the base particle A does not decompose, for instance the carbides decompose at high temperatures into a solid oxide and they release gaseous CO 2 ; and b) no reaction in the solid state takes place between the base particle (A) and the nanoparticles (b) which compose the coating, such as for example, when one intends to coat base alumina particles, with MgO nanoparticles, the (W/0) emulsion detonation temperature should be inferior to 800 0 C, taken that a temperature above such value will result in an undesired side reaction in the solid state between the alumina and magnesium oxide, leading to the formation of another structure (spinel Mg ⁇ 12O4), in the form of a single uncoated particle.
  • the system' s atmosphere type mainly the (W
  • this embodiment of the process of the present invention in which the ceramic powder intended to coat is directly placed in the (W/0) emulsion, has a drawback in as much as the particle intended to coat has to be previously synthesized by any process, but in compensation it allows that, both the particles intended to coat and the coating nanoparticles can be more diversified including, for instance, oxides, nitrides, carbides, siilphides, noble/inert metals. It compi'ises essentially the following stages :
  • the components of the (W/O) emulsion are selected from the group of soluble oxidant precursors, soluble fuels - such as the hydrazine and urea, for the synthesis of nitrides, miscible fuels, its relative ratio being dependent on empiric formula, on the structure type, and on the desired nanocoating (b) properties (thickness, percentage of base particle coated area, adhesiveness) .
  • the selection of the precursors is accomplished as described in 1.1.1.
  • the preparation of the (W/O) emulsion is carried out as described in 1.1.2.
  • the preparation of the (W/O) emulsion external phase is carried out as described in 1.1.2.2.
  • the emulsification of the phases, for obtaining the (W/O) emulsion, is carried out as described in 1.1.2.3. 1.2.2.4-additiori of an organic sensitizer
  • the detonation of the (W/0) emulsion is carried out as described in 1.1.4.
  • the collection and treatment of the reaction products is carried out as described in 1.1.5.
  • the coatings according to the present invention intended for ceramic particles comprise a nanoparticles layer, and are based on the detonation of a (W/0) emulsion, according to the process of the present invention. Since they are obtained at simultaneously high temperatures and pressures, they pi'esent a set of peculiax ⁇ properties.
  • These particles present the following as main characteristics : a.) they are constituted by a multiplicity of chemical compound families, such as oxides, nitrides, carbides, sulphides, noble metals;
  • the X-ray diffraction is an indispensable analysis in coating characterization, once it allows identifying the compounds present in a given sample, when a particle A (base particle) is coated by a particle (B) , it means that two different compounds are identified by the X-ray diffraction. technique; when a single compound is identified, it means that the detonation reaction conditions were not the ideal for a coating formation, except when the compound of the base particle is similar to the coating compound.
  • the X-ray diffraction technique it is possible to quantify the percentage of each compound in a given sample.
  • the size value of the crystallite is determined from Scherrer equation and with the width values at half height of the most intense pick of the X-ray diffractogram . However, this technique should be complemented with the scanning electron microscopy.
  • microscopy plays a fundamental role in coating characterization, given that it allows the morphology observation of a given compound, giving way to asses whether there are individual particles or coated particles with particles of nanometric dimension. This technique further allows quantifying the dimension of the base particle as well as dimension/thickness of the nanoparticles responsible for the coating.
  • the preparation of a suspension for determining the particle size distribution can be decisive to evaluate qualitatively the adhesiveness of the nanoparticles to the base particle. If the particle size distribution is not sensitive to the intensity and time of Bonification (application of ultrasound in a. sample) , it means that the adhesion of the coating is quite intense.
  • the results of the particle size distribution should be conjugated with the SEM images, once in the SEM it is possible to evaluate the size of the base particles and coating nanoparticles, if in the particle size distribution particles with the characteristic dimension of the coating nanoparticles appear, it means that its adhesiveness to the base particle is weak, given that such link was broken with ultrasound application during the preparation of the sample suspension. For instance, in the case of an excellent adhesion of the coating to the base particle, the result of the particle size distribution shall reflect only the base particle size that should be coherent with the size observed, in the SEM.
  • FIG 1 illustrates the three steps that are part of the two processes of the present invention:
  • step 1 consists of the preparation of the (W/O) emulsion, comprising the precursors, such as dissolved salts or metals of the base ceramic particle (A) .
  • step 2 the nanoparticles solid precursor is added, which presents a slower reaction kinetics.
  • step 3 the (W/0) emulsion detonation occurs, of which a ceramic particle (A) results being coated by a nanoparticles layer (b) .
  • the first step is constituted by the preparation of the emulsion (W/0) , comprising the nanoparticles precursors (b) , as salts or soluble fuels.
  • the base ceramic particles are added (A), which are intended to coat.
  • the third step such as process I, consists of the detonation of the (W/0) emulsion of the first step, of which ceramic particles (A) coated with nanoparticles (b) result .
  • Figure 2 illustrates the subdivision of the process II, wherein depending on the temperature of the (W/0) emulsion detonation, different situations in terms of products are obtained, namely for: a) - Temperature of (W/0) emulsion detonation inferior to the reaction temperature in the solid state (Trs) , among the particles (A) and the nanoparticles (b) , resulting in base particles (A) coated by nanoparticles (b) ; b) - Temperature of (W/0) emulsion detonation superior to the reaction temperature in the solid state, among the base ceramic particles (A) and the nanoparticles (b) , it give rise to an uniform ceramic powder (non coated) , with binary, ternary or superior crystalline structure.
  • the process for obtaining ceramic powders, coated with a nanoparticle layer depends in the first place on the powder type that is intended to be coated:
  • the preparation of the internal phase the precursors are dissolved in water, according to the composition previously selected. Subsequently, the solution is heated up to a temperature (35-105 0 C) superior to the crystallisation point of the different reagents.
  • the preparation of the emulsion external phase takes place by mixing the hydrocarbons or organic materials that compose it, with a surfactant appropriate to the mixture's pH values.
  • the mixture is heated up to a temperature among
  • an organic sensitizer occurs (0,2 to 2%), such as expanded polystyrene or plastic spheres without contaminants, which is consumed in the detonation reaction and is responsible for regulating the density to a value inferior to 1,25 g/cm3 f in. order to assure the sensibility level requested, to reach a stable detonation speed.
  • the last phase for preparing the detonation composition is mixing the sensitized (W/'O) emulsion with the two precursors in the previously defined i ⁇ atios.
  • This mixture, the detonable composition is made in a mechanical stirred tank, at a very slow speed to avoid precursor friction or degradation.
  • the (W/0) emulsion is subsequently placed in a cylindrical cartridge ⁇ or presenting a different geometry, such as spherical or of plane faces) made of paper, polyethylene or any other material, with a diameter which is superior to its critical diameter and it is initiated inside an appropriate chamber from a detonator, or any other system with similar effects, such as, capacitive discharge, laser, etc .
  • the precursors are dissolved in water, according to the composition previously selected. Subsequently, the solution is heated up to a temperature (35-105 0 C) superior to the crystallization point of the different reagents.
  • the preparation of the emulsion external phase takes place through the mixture of hydrocarbons or organic materials that compose it, with a. surfactant appropriate to the mixture pH values.
  • the merge is heated up to a temperature between 35 -85 0 C.
  • an oi ⁇ ganic sensitizer is promoted (0,2 to 2%), such as expanded polystyrene or plastic spheres without contaminants .
  • the (W/0) emulsion is subsequently placed in a cylindrical cartridge (or any other geometry such as a sphere or plane faces) made of paper, polyethylene or any other material, with a diameter which is superior to its critical diameter and initiated inside an appropriate chamber starting from a detonator, or any other system with similar effects, such as capacitive discharge, laser etc.
  • the first two examples herein presented illustrate two different ways of carrying out coatings according to the method of detonating an (W/0) emulsion.
  • the preparation of the detonable composition was carried out according to the following stages: 1.1.1. Preparation of the oxidant solution. Internal phase: dissolution of 90% ammonium nitrate in 10% deraineralised water in a stirred tank at 100 0 C. 1.1.2. Preparation of the external phase: homogeneous mixture of 80% vegetable oil with 20% surfactant.
  • Emulsification of external and internal phases emulsifying in an eraulsifier appropriate to the viscosity range, the two phases obtaining an emulsified matrix.
  • sensitized W./O emulsion homogeneous mixture, in a mechanical stirred tank, 99,7% of the emulsified matrix with 0,3% expanded polystyrene, the final product being designated sensitized W/O emulsion.
  • the last phase of the composition preparation intended for detonation consists of mixing the sensitized W/0 emulsion with both precursors in the above-mentioned ratios.
  • This mixture designated detonable composition, is carried out in a mechanical stirred tank, at a very slow speed in oi'der to avoid metal friction.
  • the detonable composition was put in a paper cartridge with a 35 mm diameter and 200mm long. Subsequently detonation was carried out,. by using the electrical detonator as detonation ignition source.
  • composition comprising the following components :
  • Titania particle size inferior to 500 nanometres
  • Emulsification of the external and internal phases in an emulsifier adequate to the viscosity range, emulsifying the two phases obtaining an emulsified matrix.
  • sensitized W/O emulsion homogenous mixture, in a mechanically stirred tank, 99,5% emulsified matrix with 0,5% expanded polystyrene, the final product being designated, sensitized W/O emulsion. l.l.b.
  • the last phase for the preparation of the composition intended for detonation is mixing of the sensitized W/0 emulsion with the two precursors in the above mentioned ratios. This mixture, designated detonable composition, is carried out in a mechanically stirred tank.
  • the detonable composition was placed in a paper cartridge with a 35 mm diameter and 200mm long. Subsequently, its detonation followed, under application of the electrical detonator as a detonation ignition source.
  • Example 3 Previous Placement of the base particle in the emulsion (W/O) )
  • composition comprising the following components :
  • Emulsifying the external phase and internal phase in an emulsifier appropriate to the viscosity range, emulsifying both phases thus obtaining an emulsified matrix.
  • the last phase for preparing the composition intended, for detonation consists of mixing the sensitized W/O emulsion with both precursors following the above- mentioned ratios.
  • This mixture, designated detonable composition is carried out in a mechanically stirred tank.
  • the composition intended for detonation was placed in a paper cartridge with a 35 mm diameter and approximately 200mm long. Subsequently, its detonation followed, under application of the electrical detonator as a detonation ignition source. 3. Collecting, treating and characterizing the products The magnesium aluminate powder was collected in wet state and was dried at 100° C. Subsequently, a representative sample was subject to the following analyses: observation in SEM, X-ray diffraction and particle size analysis.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geology (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Glanulating (AREA)
  • Paints Or Removers (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Dispersion Chemistry (AREA)
  • Colloid Chemistry (AREA)
PCT/PT2008/000040 2008-10-13 2008-10-13 Ceramic powders coated with a nanoparticle layer and process for obtaining thereof WO2010059070A1 (en)

Priority Applications (16)

Application Number Priority Date Filing Date Title
CA2739991A CA2739991A1 (en) 2008-10-13 2008-10-13 Ceramic powders coated with a nanoparticle layer and process for obtaining thereof
PT88130554T PT2337821E (pt) 2008-10-13 2008-10-13 Pós cerâmicos revestidos com uma camada de nanopartículas e respectivo processo para a sua obtenção
EA201100396A EA019292B1 (ru) 2008-10-13 2008-10-13 Керамические порошки, покрытые слоем наночастиц, и способ их получения
JP2011530979A JP5836124B2 (ja) 2008-10-13 2008-10-13 ナノ粒子層で被覆されたセラミック粉末及びその調製方法
ES08813055.4T ES2460574T3 (es) 2008-10-13 2008-10-13 Polvos cer�micos recubiertos con una capa de nanopart�culas y proceso para obtenci�n de los mismos
EP08813055.4A EP2337821B1 (en) 2008-10-13 2008-10-13 Ceramic powders coated with a nanoparticle layer and process for obtaining thereof
PL08813055T PL2337821T3 (pl) 2008-10-13 2008-10-13 Ceramiczne proszki powleczone warstwą nanocząstek oraz sposób ich otrzymywania
PCT/PT2008/000040 WO2010059070A1 (en) 2008-10-13 2008-10-13 Ceramic powders coated with a nanoparticle layer and process for obtaining thereof
US13/120,036 US9512043B2 (en) 2008-10-13 2008-10-13 Ceramic powders coated with a nanoparticle layer and process for obtaining thereof
BRPI0823165-6A BRPI0823165A2 (pt) 2008-10-13 2008-10-13 Pós cerâmicos revestidos com uma camada de nanopartículas e respectivo processo para a sua obtenção
CN2008801312234A CN102165021B (zh) 2008-10-13 2008-10-13 涂覆有纳米颗粒层的陶瓷粉末及其获得方法
AU2008364348A AU2008364348B2 (en) 2008-10-13 2008-10-13 Ceramic powders coated with a nanoparticle layer and process for obtaining thereof
DK08813055.4T DK2337821T3 (da) 2008-10-13 2008-10-13 Keramiske pulvere overtrukket med et nanopartikellag og fremgangsmåde til opnåelse heraf
KR1020117008282A KR20110084500A (ko) 2008-10-13 2008-10-13 나노입자 층으로 코팅된 세라믹 분말, 및 이를 제조하는 방법
EG2011040555A EG26472A (en) 2008-10-13 2011-04-11 Ceramic powders coated with a layer of fine particles and practical to obtain
ZA2011/02811A ZA201102811B (en) 2008-10-13 2011-04-14 Ceramic powders coated with a nanoparticle layer and process for obtaining thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/PT2008/000040 WO2010059070A1 (en) 2008-10-13 2008-10-13 Ceramic powders coated with a nanoparticle layer and process for obtaining thereof

Publications (1)

Publication Number Publication Date
WO2010059070A1 true WO2010059070A1 (en) 2010-05-27

Family

ID=40788925

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/PT2008/000040 WO2010059070A1 (en) 2008-10-13 2008-10-13 Ceramic powders coated with a nanoparticle layer and process for obtaining thereof

Country Status (16)

Country Link
US (1) US9512043B2 (da)
EP (1) EP2337821B1 (da)
JP (1) JP5836124B2 (da)
KR (1) KR20110084500A (da)
CN (1) CN102165021B (da)
AU (1) AU2008364348B2 (da)
BR (1) BRPI0823165A2 (da)
CA (1) CA2739991A1 (da)
DK (1) DK2337821T3 (da)
EA (1) EA019292B1 (da)
EG (1) EG26472A (da)
ES (1) ES2460574T3 (da)
PL (1) PL2337821T3 (da)
PT (1) PT2337821E (da)
WO (1) WO2010059070A1 (da)
ZA (1) ZA201102811B (da)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012049660A1 (en) * 2010-10-15 2012-04-19 Innovnano - Materiais Avançados, S.A. Process for nanomaterial synthesis from the preparation and detonation of an emulsion, products and emulsions thereof
WO2012052923A1 (en) * 2010-10-18 2012-04-26 Innovnano - Materiais Avançados, S.A. Continuous process for nanomaterial synthesis from simultaneous emulsification and detonation of an emulsion
WO2012147449A1 (ja) * 2011-04-28 2012-11-01 第一稀元素化学工業株式会社 スピネル粉末およびその製造方法、ならびに溶射膜およびガスセンサ素子の製造方法
CN106045526A (zh) * 2016-08-22 2016-10-26 中国科学院力学研究所 一种液态co2制备陶瓷粉体的方法

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102212373B1 (ko) 2012-12-13 2021-02-03 어플라이드 머티어리얼스, 인코포레이티드 배터리 분리막들 상의 세라믹 코팅
US9343315B2 (en) 2013-11-27 2016-05-17 Taiwan Semiconductor Manufacturing Co., Ltd. Method for fabricating semiconductor structure, and solid precursor delivery system
US9796019B2 (en) 2015-03-27 2017-10-24 United Technologies Corporation Powder metal with attached ceramic nanoparticles
KR102140728B1 (ko) 2017-12-18 2020-08-05 (주)무진오토 세라믹에 폴리머가 코팅된 파우더를 함유하는 펠렛 및 사출성형용 펠렛의 제조방법
CN109608911A (zh) * 2018-11-23 2019-04-12 华南理工大学 一种用于纸张加填的粉煤灰基碳化修饰复合填料制备方法
LU101177B1 (en) 2019-04-16 2020-10-16 Delmee Maxime Functionalized metal powders by small particles made by non-thermal plasma glow discharge for additive manufacturing applications
CN110935394B (zh) * 2019-11-05 2021-07-30 南京清大迈特新材料有限公司 一种微纳粉体精细加工方法及装置
WO2021116531A1 (en) * 2019-12-13 2021-06-17 Oulun Yliopisto Electroceramic composite material and method of manufacturing it
CN113292355A (zh) * 2021-04-20 2021-08-24 广西壮族自治区环境保护科学研究院 一种利用污水处理厂污泥制备陶粒的方法
CN116496650B (zh) * 2023-04-27 2024-04-09 西安交通大学 一种管廊壁面抑爆涂料及其制备方法和应用

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5855827A (en) 1993-04-14 1999-01-05 Adroit Systems, Inc. Pulse detonation synthesis
PT103838A (pt) 2007-09-28 2008-02-19 Cuf Companhia Uniao Fabril Sgp Óxidos cerâmicos esféricos nanocristalinos, processo para a sua síntese e respectivas utilizações
PT104085A (pt) 2008-05-27 2008-09-24 Cuf Companhia Uniao Fabril Sgps S A Materiais cerâmicos de dimensão nanométrica, processo para a sua síntese e respectivas utilizações

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0779957B2 (ja) * 1991-06-11 1995-08-30 株式会社椿本チエイン 粉，粒体状材料の合成装置
US6652967B2 (en) * 2001-08-08 2003-11-25 Nanoproducts Corporation Nano-dispersed powders and methods for their manufacture
KR0173445B1 (ko) * 1996-09-17 1999-02-01 이능희 화장료용 이중캡슐 및 이를 함유하는 화장료 조성물
JPH1149502A (ja) * 1997-08-01 1999-02-23 Toyota Central Res & Dev Lab Inc 酸化物粉末の製造方法
JP3984383B2 (ja) * 1998-12-16 2007-10-03 日本工機株式会社 油中水滴型エマルション爆薬組成物の製造方法
DE102004004147A1 (de) * 2004-01-28 2005-08-18 Degussa Ag Oberflächenmodifizierte, mit Siliziumdioxid umhüllte Metalloid/Metalloxide
WO2006082844A1 (ja) * 2005-02-02 2006-08-10 National Institute For Materials Science ナノサイズ粉体の製造方法
KR100691908B1 (ko) * 2005-09-08 2007-03-09 한화석유화학 주식회사 금속산화물 표면에 금속산화물 초미립자를 코팅하는 방법및 이로부터 제조된 코팅체
CN101104567B (zh) * 2007-07-25 2010-09-15 浙江亚通金属陶瓷有限公司 氧化铝陶瓷表面金属复合层及复合工艺

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5855827A (en) 1993-04-14 1999-01-05 Adroit Systems, Inc. Pulse detonation synthesis
PT103838A (pt) 2007-09-28 2008-02-19 Cuf Companhia Uniao Fabril Sgp Óxidos cerâmicos esféricos nanocristalinos, processo para a sua síntese e respectivas utilizações
PT104085A (pt) 2008-05-27 2008-09-24 Cuf Companhia Uniao Fabril Sgps S A Materiais cerâmicos de dimensão nanométrica, processo para a sua síntese e respectivas utilizações

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
TAKOA TAMI; KAZUMASA TAKATARI; NAOYSASHI WATANABLE; NABUO KANIYA: "Metal oxidize powder synthesis by the Combustion Method", JOURNAL OF MATERIALS RESEARCH, 1997
XIAO HONG WANG ET AL: "Nano-MnFe2O4 powder synthesis by detonation of emulsion explosive", APPLIED PHYSICS A; MATERIALS SCIENCE & PROCESSING, SPRINGER, BERLIN, DE, vol. 90, no. 3, 1 March 2008 (2008-03-01), pages 417 - 422, XP019588101, ISSN: 1432-0630, [retrieved on 20071106] *

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2011315099B2 (en) * 2010-10-15 2015-07-16 Innovnano - Materiais Avancados, S.A. Process for nanomaterial synthesis from the preparation and detonation of an emulsion, products and emulsions thereof
WO2012049660A1 (en) * 2010-10-15 2012-04-19 Innovnano - Materiais Avançados, S.A. Process for nanomaterial synthesis from the preparation and detonation of an emulsion, products and emulsions thereof
JP2014501601A (ja) * 2010-10-15 2014-01-23 イノブナノ−マテリアイス アバンサドス，ソシエダッド アノニマ エマルジョンの調製及び爆発によるナノ物質の合成方法、そのナノ物質及びエマルジョン
US9115001B2 (en) 2010-10-15 2015-08-25 Innovnano—Materiais A vançados, S.A. Process for nanomaterial synthesis from the preparation and detonation of an emulsion, products and emulsions thereof
CN103201027A (zh) * 2010-10-15 2013-07-10 创新纳米材料先进股份有限公司 通过乳液的制备和爆轰合成纳米材料的方法及其产品和乳液
CN103201027B (zh) * 2010-10-15 2015-08-19 创新纳米材料先进股份有限公司 通过乳液的制备和爆轰合成纳米材料的方法及其产品和乳液
US20130224488A1 (en) * 2010-10-15 2013-08-29 Innovnano - Materiais Avancados, S.A. Process for nanomaterial synthesis from the preparation and detonation of an emulsion, products and emulsions thereof
CN103201212A (zh) * 2010-10-18 2013-07-10 创新纳米材料先进股份有限公司 通过乳液的同时乳化和爆轰连续合成纳米材料的方法
AU2011319509B2 (en) * 2010-10-18 2015-01-22 Innovnano - Materiais Avancados, S.A. Continuous process for nanomaterial synthesis from simultaneous emulsification and detonation of an emulsion
US20130251623A1 (en) * 2010-10-18 2013-09-26 Innovnano-Materiais Avançados, S.A. Continuous process for nanomaterial synthesis from simultaneous emulsification and detonation of an emulsion
WO2012052923A1 (en) * 2010-10-18 2012-04-26 Innovnano - Materiais Avançados, S.A. Continuous process for nanomaterial synthesis from simultaneous emulsification and detonation of an emulsion
US9327257B2 (en) 2010-10-18 2016-05-03 Innovnano—Materiais Avancados, S.A. Continuous process for nanomaterial synthesis from simultaneous emulsification and detonation of an emulsion
CN103201212B (zh) * 2010-10-18 2016-08-24 创新纳米材料先进股份有限公司 通过乳液的同时乳化和爆轰连续合成纳米材料的方法
JP2014500785A (ja) * 2010-10-18 2014-01-16 イノブナノ−マテリアイス アバンサドス，ソシエダッド アノニマ エマルジョンの乳化及び爆発が同時に行われるナノ物質の連続合成方法
WO2012147449A1 (ja) * 2011-04-28 2012-11-01 第一稀元素化学工業株式会社 スピネル粉末およびその製造方法、ならびに溶射膜およびガスセンサ素子の製造方法
CN103562133A (zh) * 2011-04-28 2014-02-05 第一稀元素化学工业株式会社 尖晶石粉末及其制备方法以及喷镀膜及气体传感器元件的制备方法
JP2012232871A (ja) * 2011-04-28 2012-11-29 Daiichi Kigensokagaku Kogyo Co Ltd スピネル粉末およびその製造方法、溶射膜の製造方法、ならびにガスセンサ素子の製造方法
US9340680B2 (en) 2011-04-28 2016-05-17 Daiichi Kigenso Kagaku Kogyo Co., Ltd. Spinel powder and manufacturing process therefor, and processes for producing thermal spraying film and gas sensor elements
CN106045526A (zh) * 2016-08-22 2016-10-26 中国科学院力学研究所 一种液态co2制备陶瓷粉体的方法

Also Published As

Publication number Publication date
CN102165021B (zh) 2013-08-21
KR20110084500A (ko) 2011-07-25
US20110183833A1 (en) 2011-07-28
EA201100396A1 (ru) 2011-10-31
AU2008364348A1 (en) 2010-05-27
EG26472A (en) 2013-11-17
PL2337821T3 (pl) 2015-05-29
EA019292B1 (ru) 2014-02-28
JP5836124B2 (ja) 2015-12-24
AU2008364348B2 (en) 2015-05-14
BRPI0823165A2 (pt) 2015-06-23
JP2012505075A (ja) 2012-03-01
ES2460574T3 (es) 2014-05-13
ZA201102811B (en) 2012-06-27
EP2337821B1 (en) 2014-02-19
EP2337821A1 (en) 2011-06-29
CA2739991A1 (en) 2010-05-27
US9512043B2 (en) 2016-12-06
PT2337821E (pt) 2014-05-07
CN102165021A (zh) 2011-08-24
DK2337821T3 (da) 2014-05-26

Similar Documents

Publication Publication Date Title
EP2337821B1 (en) Ceramic powders coated with a nanoparticle layer and process for obtaining thereof
CN103201027B (zh) 通过乳液的制备和爆轰合成纳米材料的方法及其产品和乳液
US20160145117A1 (en) Nanocrystaline spherical ceramic oxides, process for the synthesis and use thereof
JP5731376B2 (ja) ナノメートルサイズのセラミック材料、その合成法及びその使用
DE112006000294B4 (de) Verfahren zur Herstellung von Pulverteilchen mit Nanogröße
Ojha et al. Combustion characteristics of jet a-1 droplet loaded with aluminum/magnesium-decorated boron particles
Keshmiri et al. Colloidal formation of monodisperse YSZ spheres: Kinetics of nucleation and growth
Ravi et al. Liquid precursor plasma spraying of functional materials: A case study for yttrium aluminum garnet (YAG)
CN1569617A (zh) 氧化物粉末的爆轰合成方法
Qian et al. Characterization and synthesis mechanism of Co3O4 nanoparticles synthesized by the emulsion detonation method
Liang et al. Preparation and combustion performance of molecular perovskite energetic material DAP-4-based composite with Titanium powder
Li et al. Design and preparation of core–shell AP@ HNS composites with high safety and excellent thermal decomposition performance
Mangalaraja et al. Synthesis of nanocrystalline yttria through in-situ sulphated-combustion technique
AU2008303156B2 (en) Nanocrystaline spherical ceramic oxides, process for the synthesis and use thereof
Mursalat Effect of Process Control Agents Used in Mechanochemical Synthesis on Properties of the Prepared Composite Reactive Materials
Wang et al. Synthesis and oxidation behavior of Ti-Zr-Ta (Hf) high entropy carbide nanopowders by sol-gel method
Singh Rare earth oxide coating with controlled chemistry using thermal spray
Helmich Aerosol Synthesis of Energetic Materials

Legal Events

Date Code Title Description
WWE Wipo information: entry into national phase

Ref document number: 200880131223.4

Country of ref document: CN

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 08813055

Country of ref document: EP

Kind code of ref document: A1

WWE Wipo information: entry into national phase

Ref document number: 1374/DELNP/2011

Country of ref document: IN

WWE Wipo information: entry into national phase

Ref document number: 2008813055

Country of ref document: EP

WWE Wipo information: entry into national phase

Ref document number: 2008364348

Country of ref document: AU

WWE Wipo information: entry into national phase

Ref document number: 13120036

Country of ref document: US

WWE Wipo information: entry into national phase

Ref document number: 201100396

Country of ref document: EA

ENP Entry into the national phase

Ref document number: 2008364348

Country of ref document: AU

Date of ref document: 20081013

Kind code of ref document: A

WWE Wipo information: entry into national phase

Ref document number: 2739991

Country of ref document: CA

ENP Entry into the national phase

Ref document number: 20117008282

Country of ref document: KR

Kind code of ref document: A

WWE Wipo information: entry into national phase

Ref document number: 2011530979

Country of ref document: JP

NENP Non-entry into the national phase

Ref country code: DE

ENP Entry into the national phase

Ref document number: PI0823165

Country of ref document: BR

Kind code of ref document: A2

Effective date: 20110413