WO1999047726A1 - Procede permettant de recouvrir des particules hotes avec un revetement de particules atomiques ou nanometriques - Google Patents

Procede permettant de recouvrir des particules hotes avec un revetement de particules atomiques ou nanometriques Download PDF

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Publication number
WO1999047726A1
WO1999047726A1 PCT/US1998/005431 US9805431W WO9947726A1 WO 1999047726 A1 WO1999047726 A1 WO 1999047726A1 US 9805431 W US9805431 W US 9805431W WO 9947726 A1 WO9947726 A1 WO 9947726A1
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WO
WIPO (PCT)
Prior art keywords
particles
coating
host
host particles
particle
Prior art date
Application number
PCT/US1998/005431
Other languages
English (en)
Inventor
Rajiv K. Singh
James Fitzgerald
Original Assignee
The University Of Florida
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 The University Of Florida filed Critical The University Of Florida
Priority to AU64727/98A priority Critical patent/AU6472798A/en
Priority to PCT/US1998/005431 priority patent/WO1999047726A1/fr
Publication of WO1999047726A1 publication Critical patent/WO1999047726A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/223—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating specially adapted for coating particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/18—Non-metallic particles coated with metal
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation

Definitions

  • This invention relates in general to the field of coating a substrate where physical vapor deposition (PVD) techniques for creating extremely small or atomic size species in a flux, such as laser ablation, thermal evaporation or sputtering, are used to deposit coating material onto the substrate More particularly, the invention relates to the field of material coating where the substrate consists ot individual host particles rather than a film or bulk substrate. Even more particularly, the invention relates to depositing a number of discrete particles on the host particles to form generally uniform discontinuous or continuous coatings on the individual host particles, where the coating particles vary in size from atomic to nanometer scale particles A well known technique tor coating a bulk or thin film substrate with a separate material, known as physical vapor deposition (PVD).
  • PVD physical vapor deposition
  • the coating particles produced by laser ablation may agglomerate prior to adhesion to the host particles to form coating particles of greater than desired size.
  • the aggregation strength ot the agglomerated coating particles is expected to be very high, the usefulness of these particles as coatings on the host particles is significantly reduced. Additionally, this and other coating techniques often result in the individual host p.articles agglomerating into a unified mass.
  • nano-particle coatings on host particulates can increase surface area, produce higher catalytic activity, increase adhesion and lower sintering temperatures.
  • Surface properties of the host particles relating to heat transfer, electrical, adsorption, desorption, and reflectivity can be altered.
  • the size of the coating particles and the coating parameters can be controlled such that a number of individual host particles can have a controlled number or amount of discrete coating particles, sized from atomic size to a few nanometers, adhered in a well dispersed pattern onto the surface of the host particles.
  • Host particles which may range in size for example from several nanometers to several millimeters in diameter, are provided with a relatively uniformly dispersed discontinuous or continuous coating of discrete individual coating particles sized from atomic scale to a few nanometers.
  • the coating particles are created by a PVD process, and preferably by laser ablation, where a pulsed laser beam is aimed at a target composed of the coating material under conditions sufficient to release individual particles from the target in a generally perpendicular ablation flux.
  • the laser ablation technique is especially suited for multi-elemental deposition in which the stoichiometry of the ablated species is maintained.
  • the size of the coating particles can be varied from atomic species to nanometer species by controlling the gas pressure in the system.
  • the chamber pressure can be dynamically varied with time to control the agglomeration zones.
  • the host particles are kept agitated or fluidized such that there is continual relative movement between all the host particles.
  • the fluidization of the host particles can be accomplished by various means, such as mechanical vibration or impaction of a container designed to provide exposure of the host particles to the coating particles.
  • the degree of coating is controlled by varying the laser parameters, energy density and number of pulses, gas pressure within the treatment chamber, and the treatment time.
  • the invention in general comprises a method or process, and the articles produced by this method, for creating host or core particles with discrete particles adhered generally uniformly to the surface of the host particles to form continuous or discontinuous coatings where the individual host particles remain non-agglomerated after the deposition step.
  • the coating particles are extremely small, being sized from atomic to a few nanometers in diameter, relative to the host particles, which are sized from several nanometers to several millimeters in diameter.
  • the method utilizes physical vapor deposition (PVD) such as thermal evaporation, sputtering, or preferably laser ablation of a target material to produce a flux of coating particles, and fluidization means to agitate the host particles during the coating process to prevent agglomeration.
  • PVD physical vapor deposition
  • Laser ablation of a target material to produce free particles of the target material which adhere to a substrate is a well known technique.
  • a sealable chamber is provided so that the atmosphere within the chamber may be controlled as to the particular gases present and as to the partial pressure within the system using common technology.
  • a target composed of the desired coating material is mounted, preferably rotatably, within the chamber and a UV transparent quartz window is provided through which a laser beam can be directed to strike the target.
  • a typical laser which has been used experimentally for the methodology of this application is a Lambda Physik model 305i pulsed excimer gas laser with an operating wavelength of 248 nanometers. Many other suitable lasers may be substituted therefore.
  • the laser beam will produce a particle flux generally perpendicular to the surface of the target.
  • Laser ablation is preferred since under optimized conditions the removal of species from the target takes place in a stoichiometric manner.
  • Other well known PVD techniques which produce atomic to nanometer scale ablated species in a flux, such as thermal evaporation and sputtering, may also be utilized.
  • the host or core particles are generally large relative to the size of the coating particles, with the method proven to be very applicable to host particles sized from 0.5 to 100 microns. It is understood that the host particles can be smaller, down to several nanometers in diameter, or larger, up to several millimeters in diameter, than this range if so desired.
  • the host particles are retained within a processing container which has a large enough volume to permit movement of the particles within the container.
  • the top of the container is open and the container maintained in a vertical position during fluidization, or a portion of the processing container, such as a part or all of a side or bottom, is provided with openings or apertures to retain the host particles within the processing container, if the particle deposition is to occur laterally or from below.
  • a suitable construction for the processing container has been found to be a cylindrical glass vial with one open end, the open end being covered, if necessary, by a wire mesh or screen with apertures slightly smaller than the size of the host particles.
  • the processing container is mounted within the treatment chamber with the open end facing the target at a distance of from approximately 3 to 10 centimeters such that the majority of particles in the perpendicular flux from the target will enter the processing container and contact the host particles.
  • the system may also be constructed with continuous or incremental transport means for the host particles, such as a conveyor system, whereby the host particles can be moved relative to the ablation flux during the coating process so that coating may occur in a continuous manner.
  • the host particles must be agitated or fluidized in some manner to expose the entire surface of each host particle to the coating particles entering the processing container to insure general uniformity of coating and to assist in the prevention of agglomeration of individual host particles.
  • This fluidization may be accomplished in a number of equivalent manners, such as by mechanical agitation by vibration, rotation or movement of the processing container, by providing a stirring device within the container, or by pneumatic agitation by passing gas flow through the host particles.
  • Another means to accomplish the required fluidization is to intermix magnetic particles, such as iron, with the host particles and then to apply an alternating magnetic field to the processing container during the deposition of the coating particles. The magnetic particles are separated from the host particles after the treatment process.
  • the percentage of deposition or coverage of the coating particles on the host particles is controlled by controlling the size of the coating particles and the treatment time. The longer the treatment time, the more coating particles will be adhered to the surface of the host particles, increasing both the percentage of coverage and the thickness of the coating layer. Surface coverage can be adjusted from below 1 percent up to 100 percent.
  • the size of the coating particles is controlled by the atmospheric composition and partial pressure within the treatment chamber. By dynamically controlling the gas pressure the reaction zone for forming the coating particles can be controlled. Reactive gases such as oxygen, ammonia or nitrous oxide produce higher concentrations of molecular, as opposed to atomic, species within the ablated particle flux, and are used if deposition of oxide, nitride or similar particles is desired.
  • Pressure within the chamber determines the number of collisions between ablated coating particles, with higher pressure causing more collisions and therefore larger coating particles in the ablated flux.
  • Pressure within the system may vary greatly, from 10 "6 to 10 Torr for example, but production of 1 to 10 nanometer or smaller coating particles typically occurs at approximately 400 mTorr or higher, and production of atomic particles occurs at below approximately 300 mTorr.
  • Atomic scale titanium dioxide coating particles were deposited onto silicon dioxide host particles under the following conditions: laser focal lens at 7.5 cm, laser pulse rate at 35 hz for 8 minutes at 600 mJ and energy density of 3 to 6 J/cm 2 , argon atmosphere,
  • the host particles were retained in a cylindrical glass vial approximately 1 inch in diameter and 2 inches in length with an open end covered by a wire mesh. The host particles were agitated using magnetic stirring. SEM (scanning electron microscope) photomicrography of the host particles and wavelength dispersive x-ray maps of the titanium on the surface of the host particles show a generally uniform but discontinuous deposition of discrete particles of titanium dioxide. EXAMPLE 2
  • Nano-scale silver coating particles were deposited onto silica host particles under the following conditions: laser local lens at 7.5 cm, laser pulse rate at 30 hz for 9 minutes at 450 mJ and energy density ot 3 to 6 J/cnr. 17 mTorr starting partial pressure and 10 mTorr ending partial pressure.
  • the host particles were retained in a cylindrical glass vial approximately 1 inch in diameter and 2 inches in length with an open end covered by a wire mesh.
  • the host particles were agitated using magnetic stirring.
  • SEM photomicrography of the host particles and wavelength dispersive x-ray maps of the silver on the surface on the silica host particles show a generally uniform but discontinuous deposition of discrete particles ot silver.
  • Nano-scale silver coating particles were deposited onto silica host particles under the following conditions: laser local lens at 7 5 cm, laser pulse rate at 15 hz for 40 minutes at 450 mJ and energy density ot 3 to 6 J7cm , 19 mTorr starting partial pressure and 21 mTorr ending partial pressure
  • the host particles were retained in a cylindrical glass vial approximately 1 inch in diameter and 2 inches in length with an open end covered by a wire mesh.
  • the host particles were agitated using magnetic stirring.
  • SEM photomicrography ot the host particles and wavelength dispersive x-ray maps of the silver on the surface on the silica host particles, showing a generally uniform but discontinuous deposition of discrete particles ol silver.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Structural Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

L'invention se rapporte à un procédé permettant de recouvrir des particules hôtes de diamètre compris entre quelques nanomètres et quelques millimètres avec des particules de revêtement de taille comprise entre la taille d'un atome et 10 nanomètres, produites selon la technique de dépôt par évaporation sous vide, de préférence par ablation laser. Selon ce procédé, on forme un revêtement partiel ou continu sur lesdites particules en les plaçant dans le flux d'ablation et en les fluidifiant ou en les agitant de manière à éviter leur agglomération au cours de l'étape de formation du revêtement. L'invention se rapporte également aux particules hôtes proprement dites sur lesquelles on a déposé le revêtement.
PCT/US1998/005431 1998-03-19 1998-03-19 Procede permettant de recouvrir des particules hotes avec un revetement de particules atomiques ou nanometriques WO1999047726A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU64727/98A AU6472798A (en) 1998-03-19 1998-03-19 Process for depositing atomic to nanometer particle coatings on host particles
PCT/US1998/005431 WO1999047726A1 (fr) 1998-03-19 1998-03-19 Procede permettant de recouvrir des particules hotes avec un revetement de particules atomiques ou nanometriques

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/US1998/005431 WO1999047726A1 (fr) 1998-03-19 1998-03-19 Procede permettant de recouvrir des particules hotes avec un revetement de particules atomiques ou nanometriques

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Publication Number Publication Date
WO1999047726A1 true WO1999047726A1 (fr) 1999-09-23

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Cited By (48)

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WO2000028969A2 (fr) * 1998-11-18 2000-05-25 University Of Florida Procedes de preparation de particules de medicament enrobees et formulations pharmaceutiques correspondantes
WO2000074657A1 (fr) * 1999-06-07 2000-12-14 Nanosphere, Inc. Procedes de revetement de particules et particules ainsi produites
FR2816756A1 (fr) * 2000-11-15 2002-05-17 Univ Paris Curie Procede d'obtention d'une composition polymere dopee par des nanoparticules pour la realisation de materiaux composites polymeres, dispositif pour sa mise en oeuvre, composition et materiaux obtenus
US6406745B1 (en) 1999-06-07 2002-06-18 Nanosphere, Inc. Methods for coating particles and particles produced thereby
US6984404B1 (en) 1998-11-18 2006-01-10 University Of Florida Research Foundation, Inc. Methods for preparing coated drug particles and pharmaceutical formulations thereof
EP1940735A1 (fr) * 2005-10-26 2008-07-09 P&I Corporation Procédé et dispositif d élaboration de poudre sur laquelle on dépose sous vide des nanoparticules de métal, d alliage, et de céramique de manière uniforme
EP1977816A2 (fr) 2003-09-26 2008-10-08 3M Innovative Properties Company Catalyseurs d'or de l'échelle nano, agents d'activation, moyen de support et méthodologies apparentées utiles pour la fabrication de systèmes catalyseurs lorsque le catalyseur est déposé sur le moyen de support par le dépôt de vapeur physique
WO2011105957A1 (fr) * 2010-02-24 2011-09-01 Plasmadvance Ab Procédé de pulvérisation cathodique sous plasma pour la production de particules
US8058202B2 (en) 2005-01-04 2011-11-15 3M Innovative Properties Company Heterogeneous, composite, carbonaceous catalyst system and methods that use catalytically active gold
US8137750B2 (en) 2006-02-15 2012-03-20 3M Innovative Properties Company Catalytically active gold supported on thermally treated nanoporous supports
US20130028781A1 (en) * 2009-12-08 2013-01-31 Zhiyue Xu Method of making a powder metal compact
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US9033055B2 (en) 2011-08-17 2015-05-19 Baker Hughes Incorporated Selectively degradable passage restriction and method
US9057242B2 (en) 2011-08-05 2015-06-16 Baker Hughes Incorporated Method of controlling corrosion rate in downhole article, and downhole article having controlled corrosion rate
US9068428B2 (en) 2012-02-13 2015-06-30 Baker Hughes Incorporated Selectively corrodible downhole article and method of use
US9080098B2 (en) 2011-04-28 2015-07-14 Baker Hughes Incorporated Functionally gradient composite article
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US9090956B2 (en) 2011-08-30 2015-07-28 Baker Hughes Incorporated Aluminum alloy powder metal compact
US9090955B2 (en) 2010-10-27 2015-07-28 Baker Hughes Incorporated Nanomatrix powder metal composite
US9101978B2 (en) 2002-12-08 2015-08-11 Baker Hughes Incorporated Nanomatrix powder metal compact
US9109269B2 (en) 2011-08-30 2015-08-18 Baker Hughes Incorporated Magnesium alloy powder metal compact
US9109429B2 (en) 2002-12-08 2015-08-18 Baker Hughes Incorporated Engineered powder compact composite material
US9127515B2 (en) 2010-10-27 2015-09-08 Baker Hughes Incorporated Nanomatrix carbon composite
US9133695B2 (en) 2011-09-03 2015-09-15 Baker Hughes Incorporated Degradable shaped charge and perforating gun system
US9139928B2 (en) 2011-06-17 2015-09-22 Baker Hughes Incorporated Corrodible downhole article and method of removing the article from downhole environment
US9187990B2 (en) 2011-09-03 2015-11-17 Baker Hughes Incorporated Method of using a degradable shaped charge and perforating gun system
US9243475B2 (en) 2009-12-08 2016-01-26 Baker Hughes Incorporated Extruded powder metal compact
US9267347B2 (en) 2009-12-08 2016-02-23 Baker Huges Incorporated Dissolvable tool
US9347119B2 (en) 2011-09-03 2016-05-24 Baker Hughes Incorporated Degradable high shock impedance material
US9605508B2 (en) 2012-05-08 2017-03-28 Baker Hughes Incorporated Disintegrable and conformable metallic seal, and method of making the same
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US9682425B2 (en) 2009-12-08 2017-06-20 Baker Hughes Incorporated Coated metallic powder and method of making the same
US9707739B2 (en) 2011-07-22 2017-07-18 Baker Hughes Incorporated Intermetallic metallic composite, method of manufacture thereof and articles comprising the same
US9816339B2 (en) 2013-09-03 2017-11-14 Baker Hughes, A Ge Company, Llc Plug reception assembly and method of reducing restriction in a borehole
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US9856547B2 (en) 2011-08-30 2018-01-02 Bakers Hughes, A Ge Company, Llc Nanostructured powder metal compact
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Cited By (74)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6984404B1 (en) 1998-11-18 2006-01-10 University Of Florida Research Foundation, Inc. Methods for preparing coated drug particles and pharmaceutical formulations thereof
WO2000028969A3 (fr) * 1998-11-18 2000-11-09 Univ Florida Procedes de preparation de particules de medicament enrobees et formulations pharmaceutiques correspondantes
CZ300323B6 (cs) * 1998-11-18 2009-04-22 University Of Florida Lék obsahující množství potažených cástic léciv, zpusob jejich prípravy a použití, léková forma a lécebná sada
WO2000028969A2 (fr) * 1998-11-18 2000-05-25 University Of Florida Procedes de preparation de particules de medicament enrobees et formulations pharmaceutiques correspondantes
US7063748B2 (en) 1999-06-07 2006-06-20 Nanotherapeutics, Inc. Methods for coating particles and particles produced thereby
US6406745B1 (en) 1999-06-07 2002-06-18 Nanosphere, Inc. Methods for coating particles and particles produced thereby
WO2000074657A1 (fr) * 1999-06-07 2000-12-14 Nanosphere, Inc. Procedes de revetement de particules et particules ainsi produites
FR2816756A1 (fr) * 2000-11-15 2002-05-17 Univ Paris Curie Procede d'obtention d'une composition polymere dopee par des nanoparticules pour la realisation de materiaux composites polymeres, dispositif pour sa mise en oeuvre, composition et materiaux obtenus
US9101978B2 (en) 2002-12-08 2015-08-11 Baker Hughes Incorporated Nanomatrix powder metal compact
US9109429B2 (en) 2002-12-08 2015-08-18 Baker Hughes Incorporated Engineered powder compact composite material
EP1977816A2 (fr) 2003-09-26 2008-10-08 3M Innovative Properties Company Catalyseurs d'or de l'échelle nano, agents d'activation, moyen de support et méthodologies apparentées utiles pour la fabrication de systèmes catalyseurs lorsque le catalyseur est déposé sur le moyen de support par le dépôt de vapeur physique
US7727931B2 (en) 2003-09-26 2010-06-01 3M Innovative Properties Company Catalysts, activating agents, support media, and related methodologies useful for making catalyst systems especially when the catalyst is deposited onto the support media using physical vapor deposition
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