EP1165223A1 - Procede pour l'enrobage de particules - Google Patents
Procede pour l'enrobage de particulesInfo
- Publication number
- EP1165223A1 EP1165223A1 EP00915229A EP00915229A EP1165223A1 EP 1165223 A1 EP1165223 A1 EP 1165223A1 EP 00915229 A EP00915229 A EP 00915229A EP 00915229 A EP00915229 A EP 00915229A EP 1165223 A1 EP1165223 A1 EP 1165223A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- particles
- precursor
- fluid
- coating material
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
-
- 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
- B22F1/17—Metallic particles coated with metal
-
- 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
-
- 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.]
-
- 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.]
- Y10T428/2991—Coated
Definitions
- the present invention relates to a method of coating particles, and the coated particles obtained.
- Particles of the “core-shell” type are of double interest. On the one hand, they allow either to increase the specific surface of a material by dispersing it in the form of nanoparticles, thus causing a significant increase in its activity, or to isolate a particle from the other particles by a protective layer and modify thus the properties of the medium.
- the coating of the particles makes it possible to make the particles compatible with the matrix. Pn can cite for example the use of nanometric magnetic particles for recording data in computer science. We can also cite the use of particles as solder binder in electronics. In the medical field, magnetic particles coated with organic substances are used. Various methods for depositing a thin layer on a substrate are known.
- Particularly effective methods use a fluid brought to a pressure and a temperature above normal conditions, and in particular a fluid placed under conditions very close to critical pressure and temperature.
- These methods consist in depositing a film on a planar substrate, generally heated, placed in a reactor, using a supercritical fluid containing a precursor of the compound constituting the film, said precursor being transformed before being deposited on it, substrate, and the solvent of the fluid being removed by reducing the pressure in the reactor.
- JF Bocquet, et al, Surface and Coatings Technology, 70 (1994) 73-78 describes a method for depositing a metal oxide film (Ti0 2 ) on a heated substrate placed in a reactor, from a supercritical solution of a Ti0 2 precursor, introduced into a pressure reactor.
- US-A-5, 789027 (1996) describes a method for depositing a material on the surface of a substrate or inside a porous solid.
- the method consists in dissolving a precursor of the material in a solvent under supercritical conditions, in bringing the substrate or the porous solid in contact with the supercritical solution, in adding a reagent which transforms the precursor by causing a deposit of the material on the surface of the substrate or in the porous solid, then to carry out an expansion to remove the solvent.
- the object of the present invention is to provide a process which makes it possible to coat, in a simple and reliable manner, porous particles or not with the aid of a precursor of the coating compound.
- the subject of the present invention is a method for depositing a film of a coating material on the surface of particles, or in the pores of porous particles, said method being characterized in that it consists in: a ) bringing into contact in a fluid containing one or more solvents, on the one hand the particles to be coated and on the other hand a complex organo-metallic precursor of the coating material, optionally associated with one or more additional complex organo-metal precursors or not, said particles being maintained in dispersion in the fluid subjected to supercritical or slightly subcritical temperature and pressure conditions; b) causing within the fluid, the transformation of the precursor of the coating material so that it is deposited on the particles; c) bringing the fluid under temperature and pressure conditions such that the fluid is in the gaseous state to remove the solvent.
- the term “particle” means any object which has an average size less than a millimeter, whatever its shape.
- the process of the present invention is particularly suitable for coating particles of very small dimensions, and in particular for nanometric particles and micrometric particles, in particular for particles having an average dimension of between 1 nm and 100 ⁇ m. It is also well suited for coating particles having a complex shape.
- the particles can be formed by a single chemical compound or by a mixture of compounds.
- the compounds can be mineral compounds, organic compounds or a mixture of organic or mineral compounds.
- the particles formed by a mixture of compounds can be substantially homogeneous particles. However, it may also be heterogeneous particles in which the compound constituting the core is different from the compound constituting the outer layer.
- the fluid containing the particles to be coated and the precursor of the coating material is placed under supercritical or slightly subcritical temperature and pressure conditions.
- supercritical conditions is meant conditions under which the temperature and the pressure are higher than the critical temperature T c and the critical pressure P c .
- slightly subcritical conditions is meant conditions of temperature T and pressure P such that all of the gases in the reaction medium are dissolved in the liquid phase.
- the supercritical or slightly subcritical conditions are defined with respect to the pressure and the temperature at the critical point P c and T c of the whole of the fluid constituting the reaction medium. They are generally in the range 0.5 ⁇ T c / T ⁇ 2, 0.5 ⁇ P c / P ⁇ 3.
- the reaction medium consists of one or more solvents and various compounds in solution or in suspension.
- the critical temperature and pressure of such a fluid are very close to those of the solvent mainly present in the fluid, and the supercritical or slightly subcritical conditions are defined with respect to the temperature and the critical pressure of said majority solvent.
- the temperature of the fluid will be between 50 ° C and 600 ° C, preferably between 100 ° C and 300 ° C, and the pressure of the fluid will be between 0.2 MPa and 60 MPa, preferably between 0.5 MPa and 30 MPa.
- the particular values are chosen as a function of the precursor of the coating material.
- the particles to be coated are kept dispersed in the reaction medium by mechanical stirring, by natural convection or by forced convection, by the action of ultrasound, by creating a magnetic field, by creating an electric field, or by combining several of these means.
- power ultrasound is preferably used, the frequency of which is from 20 kHz to 1 MHz.
- a magnetic field a continuous or alternating magnetic field having an intensity less than or equal to 2 Tesla is imposed on the reaction medium.
- the reaction medium essentially consists of one or more solvents, in which the precursor of the coating material is dissolved and the particles suspended.
- the solvent can be water or an organic solvent which is liquid under normal conditions of temperature and pressure, or a mixture of such solvents.
- the liquid solvents under normal conditions of temperature and pressure mention may be made of alkanes which have from 5 to 20 carbon atoms and which are liquid under normal conditions of temperature and pressure, more particularly n-pentane, l 'isopentane, hexane, heptane and octane; alkenes having 5 to 20 carbon atoms; alkynes having 4 to 20 carbon atoms; alcohols, more particularly methanol and ethanol; ketones, in particular acetone; ethers, esters, chlorinated hydrocarbons and liquid fluorinated hydrocarbons, solvents from petroleum fractions, such as white spirit, and their mixtures.
- gaseous solvents under normal conditions of temperature and pressure, mention may be made of carbon dioxide, ammonia, helium, nitrogen, nitrous oxide, sulfur hexafluoride, gaseous alkanes having from 1 to 5 carbon atoms (such as methane, ethane, propane, n-butane, isobutane and neopentane), the gaseous alkenes having from 2 to 4 carbon atoms (such as acetylene , propyne and butyne-1), gaseous dienes (such as propadiene), hydrocarbons fluorinated, and mixtures thereof.
- the solvent can itself in certain cases constitute a precursor of the coating material.
- the organo-metallic complex precursor of the coating material can be chosen from acetylacetonates of various metals, which make it possible to obtain deposits of different types depending on the reaction conditions.
- a metallic deposit is obtained in the strict absence of oxygen.
- an oxidant such as for example 0 2 , H 2 0 2 or N0 2
- an oxide deposit is obtained in the presence of an oxidant, such as for example 0 2 , H 2 0 2 or N0 2 .
- an oxide deposit is obtained in an ammoniacal medium.
- a nitride deposit is obtained.
- Copper acetylacetonate or copper hexafluoroacetylacetonate are advantageously used to obtain deposits of copper or copper oxide Cu 2 0.
- It may be a second compound of an organometallic complex, or a different compound which may or may not react with the organometallic complex compound.
- a second compound of an organometallic complex or a different compound which may or may not react with the organometallic complex compound.
- the process of the invention thus makes it possible to obtain particles whose core, which has a diameter between 1 nm and 1 ⁇ m and which is constituted by nickel, silica, iron oxide or an alloy SmCo 5 , coated with copper, copper oxide or copper nitride.
- the chemical transformation of the precursor (s) present in the reaction medium can be carried out either thermally or using a chemical reagent, depending on the nature and the reactivity of the precursor.
- the reaction medium contains several precursors of the coating material, the various precursors can be transformed simultaneously or successively, depending on their nature and their reactivity.
- a solvent can constitute a precursor.
- the procedure is as follows: * a fluid is prepared comprising at least one precursor of the coating material dissolved in a solvent Si;
- the fluid is subjected to supercritical or slightly subcritical temperature and pressure conditions; * said fluid is brought into contact with the particles to be coated, dispersed in a solvent S 2 , and the reaction medium is subjected to pressure and temperature conditions capable of causing the transformation of the precursor, the particles being maintained in dispersion; * the reaction medium is subjected to an expansion to remove the solvents.
- the procedure is as follows:
- a fluid is prepared comprising at least one precursor of the coating material dissolved in a solvent Si;
- the solvents Si and S 2 can be identical or different.
- a third solvent can be introduced into the fluid to improve the operating conditions, in particular to decrease the critical temperature and pressure of the fluid, to increase the solubility of the precursor (s), or to decrease the transformation temperature of the precursor (s).
- a variant of these modes of implementation consists in bringing the fluid containing the precursor into contact with the particles to be coated before putting the fluid in the supercritical or slightly subcritical conditions.
- the particles to be coated can be prepared in situ. The reaction fluid then contains one or more precursors of the particles, and one or more precursors of the coating material.
- precursors which transform under the action of heat the precursors of the particles having a transformation temperature lower than that of the precursors of the coating materials. It is also possible to use precursors which transform by chemical reaction with an additional reagent, provided that the transformation of the precursor of the particles takes place first.
- a fluid is prepared comprising at least one precursor of the particles to be coated, dissolved in a solvent S 2 ;
- the particles are formed by modification of the precursor (s), either by increasing the temperature, or by the action of an appropriate reagent and the particles formed are kept in dispersion;
- a fluid is prepared comprising at least one precursor of the coating material dissolved in a solvent Si;
- the fluid containing the particles to be coated is brought into contact with the fluid containing the precursor (s) of the coating material under supercritical or slightly subcritical temperature and pressure conditions to ensure good solubilization, then subjects the reaction medium to conditions capable of causing the transformation of the precursor of the coating material;
- the various fluids it is also possible to add to the various fluids, one or more additional solvents so as to adjust the properties of the reaction medium.
- the same solvent can be used where appropriate for the fluid containing the precursor of the particles and for the fluid containing the precursor of the coating material.
- This mode of implementation includes several variants.
- the transformation of the precursor of the particles can be carried out either by heat treatment or by adding an appropriate reagent.
- the transformation of the precursor of the coating material can be carried out either by heat treatment or by adding an appropriate reagent.
- Fluids can be placed in supercritical or slightly subcritical conditions when they contain all their constituents or when they contain some of them.
- the condition common to all the variants is that the reaction medium is in supercritical or slightly subcritical conditions at the time when the precursor of the coating material is chemically transformed.
- the method of the invention can be implemented for depositing several coating layers on particles. It suffices for this purpose to introduce into the reaction medium several precursors having a different reactivity and to impose successively on the reaction medium the appropriate conditions to cause the stepwise transformation of the precursors.
- the process of the invention can be carried out continuously or batchwise.
- Nickel balls coated with copper oxide For this example, we used: * nickel balls having an average size between 3 and 5 ⁇ m;
- the intensity was determined by comparison with the crystallographic data (in particular the values of d and the intensities relating to this parameter) listed in the JCPDS files.
- beads made of an alloy of samarium and cobalt and coated with copper oxide were prepared.
- the SmCo 5 alloy powder used was a 20 ⁇ m sieved powder.
- the coating of the SmCos particles with copper oxide was found by an electron microscopy study and by an X-ray examination.
- a layer of metallic copper was deposited on nickel beads by thermal decomposition of the copper hexafluoroacetylacetonate Cu (hfa) 2 in a supercritical mixture of C0 2 / ethanol.
- Cu (hfa) 2 was chosen as a precursor because of its good solubility in the CO 2 / ethanol mixture.
- the starting materials used were commercial products. Nickel beads with a diameter between 3 and 5 ⁇ m were used.
- an iron oxide powder was prepared by decomposition of the iron acetate Fe (ac) 2 in a supercritical fluid, in which the solvent was a CO 2 / ethanol 80/20 mixture in molar composition. .
- the iron oxide powder thus obtained was coated with copper hexafluoroacetylacetonate according to the procedure of Example 4.
Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9904175A FR2791580B1 (fr) | 1999-04-02 | 1999-04-02 | Procede pour l'enrobage de particules |
FR9904175 | 1999-04-02 | ||
PCT/FR2000/000771 WO2000059622A1 (fr) | 1999-04-02 | 2000-03-28 | Procede pour l'enrobage de particules |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1165223A1 true EP1165223A1 (fr) | 2002-01-02 |
EP1165223B1 EP1165223B1 (fr) | 2012-07-25 |
Family
ID=9543980
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP00915229A Expired - Lifetime EP1165223B1 (fr) | 1999-04-02 | 2000-03-28 | Procede pour l'enrobage de particules |
Country Status (5)
Country | Link |
---|---|
US (2) | US6592938B1 (fr) |
EP (1) | EP1165223B1 (fr) |
JP (1) | JP2002541320A (fr) |
FR (1) | FR2791580B1 (fr) |
WO (1) | WO2000059622A1 (fr) |
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ES2342747T3 (es) * | 1997-10-15 | 2010-07-13 | University Of South Florida | Recubrimiento de material en particulas asistido por un fluido supercritico. |
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1999
- 1999-04-02 FR FR9904175A patent/FR2791580B1/fr not_active Expired - Lifetime
-
2000
- 2000-03-28 US US09/937,748 patent/US6592938B1/en not_active Expired - Lifetime
- 2000-03-28 JP JP2000609177A patent/JP2002541320A/ja active Pending
- 2000-03-28 EP EP00915229A patent/EP1165223B1/fr not_active Expired - Lifetime
- 2000-03-28 WO PCT/FR2000/000771 patent/WO2000059622A1/fr active Application Filing
-
2003
- 2003-04-24 US US10/421,933 patent/US20030203207A1/en not_active Abandoned
Non-Patent Citations (1)
Title |
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See references of WO0059622A1 * |
Also Published As
Publication number | Publication date |
---|---|
EP1165223B1 (fr) | 2012-07-25 |
FR2791580A1 (fr) | 2000-10-06 |
US6592938B1 (en) | 2003-07-15 |
FR2791580B1 (fr) | 2001-05-04 |
US20030203207A1 (en) | 2003-10-30 |
JP2002541320A (ja) | 2002-12-03 |
WO2000059622A1 (fr) | 2000-10-12 |
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