Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
  • B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
  • B29C64/10—Processes of additive manufacturing
  • B29C64/141—Processes of additive manufacturing using only solid materials
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
  • B01J13/02—Making microcapsules or microballoons
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
  • B01J13/02—Making microcapsules or microballoons
  • B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
  • B01J13/043—Drying and spraying
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
  • B01J2/003—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic followed by coating of the granules
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
  • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
  • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
• • 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
  • B22F1/05—Metallic powder characterised by the size or surface area of the particles
  • B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
• • 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
  • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
  • B22F1/102—Metallic powder coated with organic material
• • 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
  • B22F1/16—Metallic particles coated with a non-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
  • B22F1/17—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
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B33—ADDITIVE MANUFACTURING TECHNOLOGY
  • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
  • B33Y70/00—Materials specially adapted for additive manufacturing
  • B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D11/00—Inks
  • C09D11/02—Printing inks
  • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
  • C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D11/00—Inks
  • C09D11/02—Printing inks
  • C09D11/10—Printing inks based on artificial resins
  • C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
• • 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
  • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
  • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
  • C23C4/06—Metallic material
• • 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
  • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
  • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
  • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
  • B01J2219/0894—Processes carried out in the presence of a plasma
• • 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
  • B22F2301/00—Metallic composition of the powder or its coating
  • B22F2301/05—Light metals
  • B22F2301/052—Aluminium
• • 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
  • B22F2301/00—Metallic composition of the powder or its coating
  • B22F2301/10—Copper
• • 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
  • B22F2301/00—Metallic composition of the powder or its coating
  • B22F2301/15—Nickel or cobalt
• • 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
  • B22F2304/00—Physical aspects of the powder
  • B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
• • 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
  • B22F9/00—Making metallic powder or suspensions thereof
  • B22F9/02—Making metallic powder or suspensions thereof using physical processes
  • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
• • 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
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
  • Y02P10/00—Technologies related to metal processing
  • Y02P10/25—Process efficiency

Definitions

• the present invention relates to the manufacture of multimaterial powders used in various fields (metallurgy, plastics, etc.) for applications in the techniques of additive synthesis and projection surface treatment.
• additive synthesis techniques is intended to mean any technique which makes it possible to obtain three-dimensional objects by consolidation of powders.
• Nonlimiting examples include: 3D printing techniques (SLM, SLS %), injection techniques (PIM, MIM), powder projection techniques (cold spray, D-gun %) and conventional compaction / sintering techniques.
• the atomization technique of a molten metal makes it possible in particular to obtain dense powders of spherical morphology.
• the materials obtained by this technique are either pure elements or single-phase alloys miscible elements such as, for example, some steels, alloys of nickel, aluminum or titanium. These powders constitute today the essential of the offer for the applications in additive manufacturing.
• the technique by co-grinding makes it possible to produce multimaterial powders by intimately mixing under high energy, assisted by grinding balls, powders of different natures, as described in US Patents 3,816,080, US 3,591,362 and US 4,706,894.
• this method it is possible to obtain composite grains with a great latitude of composition.
• the morphology and / or particle size of the powders obtained by this embodiment are not favorable for their applications in additive manufacturing.
• the grains obtained by this technique consist of a more or less homogeneous dispersion of the various constituents and do not have the structure of a functionalized core surface.
• the spray-drying technique also makes it possible to produce multi-material powders by atomizing and drying a suspension composed of powders, a solvent and an organic binder. as described in US Pat. Nos. 5,122,182, 3,617,358 and 4,915,733. Composite grains resulting from agglomeration are thus obtained, by the organic binder which acts as glue, elementary powders present in the suspension.
• the grains obtained by this embodiment have a spherical morphology. However, their intragranular porosity and the presence of organic binders make them unfit for use in additive manufacturing.
• it is possible to add a debinding and densification step of the particles by means of various techniques based on a rise in temperature of the particles following the drying atomization operation.
• the grains thus obtained are agglomerates consisting of a non-homogeneous dispersion of the various constituents and do not have the structure of a functionalized core on the surface.
• dry deposition technologies such as chemical vapor deposition (commonly referred to as CVD) or physical vapor deposition (commonly referred to as PVD) can also be used on granular substrates. to synthesize multi-material powders.
• PVD technology is very limited in that it does not allow to be able to perform the treatment of fine particles (whose diameter is less than 100 pm). It is also very limited in terms of functionalization rates for reasonable processing times. CVD technology is in most cases neither technically nor economically favorable considering the toxicity and cost of the precursors used.
• the Applicant has developed a method for obtaining composite grains obtained by functionalizing the surface of grains or support particles by addition elements in granular form to obtain a microstructure strata.
• the subject of the present invention is therefore a multimaterial powder comprising support particles with a median particle size d50 of between 1 ⁇ and 100 ⁇ and functionalization particles having a median particle size d50 of a factor of 10 to 1000 compared with to the support particles,
• a core constituted by a support particle, and o an envelope, which covers between 10 and 100% of the surface of said support particle and which is formed by at least one surface layer of said functionalization particles.
• the ranges of particle size claimed correspond to a given range d10-d90, assuming that the multimaterial powder according to the invention has a number distribution.
• median particle size d50 (or median diameter d50) is meant, in the sense of the present invention, the dimension below which are 50% of the particles.
• the functionalization particles have a median particle size d50 equal to or greater than 100 nm, which has the consequence that the envelope has a thickness greater than or equal to 100 nm. This size of functionalization particles makes it possible in particular to limit the health and safety problems related to the toxicity of the nanoparticles during their handling.
• the proportion of support particles coated by the functionalization layer may be between 0.8 and 1, and preferably between 0.9 and 1.
• proportion of coated support particles is meant in the sense of the present invention, the ratio between the number of functionalized particles and the number of total particles for a multimaterial powder sample. This proportion is determined by microscopic image analyzes of a population of multi-material grains.
• the total roughness Rt of the surface of the functionalization layer at the grain scale may be less than ⁇ , and preferably between 0.1 and 5 ⁇ .
• a rough surface typically has asperities called “peaks” and cavities called “hollow”.
• total roughness Rt is meant, in the sense of the present invention, the greatest difference in level between the highest peak of a peak and the lowest bottom of a hollow.
• the total roughness of the particle-scale functionalization layer is determined by cross-sectional grained image analyzes taken under the microscope.
• the advantage offered by a total roughness of the functionalization layer at the grain scale of less than 10 ⁇ is related to the flow characteristics of the support particle which could be deteriorated following the functionalization treatment. Indeed, a too large total roughness on the scale of the particle causes a decrease in the flowability of the powder and makes its use difficult in additive manufacturing technologies and thermal projections where the flow characteristics of the powders are parameters essential. On the other hand, a total roughness close to zero is undesirable if one considers the decrease in the specific surface area associated with it, for a grain size and a morphology of given grain media.
• the median particle size d50 of said support particles may be between 1 and 45 ⁇ , these values possibly corresponding respectively to a preferred dimension d10 of 1 ⁇ and a d90 dimension of 45 ⁇ .
• the median particle size d50 of said carrier particles may be between 10 and 45 ⁇ , which corresponds to a particle size distribution particularly well suited for additive manufacturing processes.
• the composite grains may have an irregular morphology, with a form factor greater than 1 or a substantially spherical morphology, with a form factor close to 1.
• the term "form factor” means the ratio between the size of the axis of greater dimension, called the main axis, and the size of the axis of smaller dimension, called the secondary axis, of the particle.
• the grains Composites according to the invention may preferably have a substantially spherical morphology.
• carrier particles that may be used in the context of the present invention, mention may in particular be made of metal, ceramic or organic particles.
• functionalization particles that may be used in the context of the present invention, mention may in particular be made of ceramic and / or metallic and / or organic particles and / or particles comprising at least one element chosen from the group consisting of boron. carbon, oxygen and / or nitrogen.
• Ceramic grains functionalized with a metal for the production of cermets for example: WC / Co, WC / Cu, WC / NiCr, TiC / Ni, B4C / A1, Fe x N y / Ni, Fe (N) / Ni ...;
• CMC metal matrix composites
• metal-functionalized metal grains for the production of alloys, intermetallics and pseudoalloys, for example: W / Cu, W / Ni, Ti / Al, Ti / Al / C, Al / Cu, Al / Zn, Cu / Ni, Ti / AgCu, Ti / Mo, Mg / TiNi, Al / TiNi, Al6061 / TiNi / SiC ...;
• Ceramic grains functionalized with a ceramic such as, for example: ZrB 2 / SiC, Al 2 O 3 / SiO 2, Si 3 N 4 / SiC 2; metal functionalized organic grains for the production of functional composites, for example: PA / Ag, PEKK / Ag, PTFE / Ag, PE / Ni, etc .; and
• the metallic or ceramic grains functionalized with an organic material for example Fe 3 O 4 / PA, C / PEKK or Cu / PE.
• the subject of the present invention is also the use of the multimaterial powder according to the invention as a material that can be used for sintering techniques such as additive synthesis and / or for surface treatments by projection, such as projection at the flame, HVOF, plasma projection or cold spraying ("cold spray" in English).
• the subject of the present invention is also a process for producing a powder according to the invention (first embodiment) comprising:
• the support particles and functionalization particles, used in the process according to the invention to obtain composite grains forming the powder according to the invention, are as defined above.
• Recirculating fluidized bed means, in the sense of the present invention, a fluidized bed reactor equipped with a system for one hand to trap the particles in its upper part and another to reintroduce in its lower part.
• a reactor can operate in two-phase mode (solid / gas) or three-phase (solid / gas / liquid). It can also be advantageously assisted by cold plasma torches at atmospheric pressure, for example, to facilitate diffusion treatments of heteroatoms such as nitrogen, carbon, boron and oxygen.
• the subject of the present invention is also a process for producing a powder according to the invention (second embodiment) in which a high-energy mechanical reactor specifically designed to implant functionalization particles on the surface is used as reactor. of support grains.
• the method is as follows:
• the support particles and functionalization particles, used in this process according to the invention to obtain composite grains forming the powder according to the invention, are also as defined above.
• the method according to the invention may further comprise, after the grafting step, a step of heat treatment and / or surface of the composite grains, using a recirculating fluidized bed as defined above. .
• the method according to the invention may furthermore comprise, in the case where the composite grains do not have a spherical morphology, a step of spheroidizing said grains by hot plasma in a fluidized bed.
• FIG. 1 shows a block diagram of the device used for carrying out the method according to the invention according to the first embodiment (fluidized bed reactor);
• FIG. 2 represents a schematic diagram of the device in section used for the implementation of the method according to the invention according to the first embodiment (grinding device));
• FIGS. 3A to 6B are photographs taken by scanning electron microscope (SEM) of composite grains according to the invention.
• FIGS. 7A and 7B are photographs taken under an optical microscope showing the sectional micrograph of an iron-copper composite material prepared by compacting / sintering, starting from a conventional mixture of iron and copper (FIG. 7A) and from an iron powder functionalized with copper (Figure 7B).
• FIGS. 1 and 2 are identical elements shown in FIGS. 1 and 2 are identified by identical reference numerals.
• FIG. 1 represents a schematic diagram of the device used for the implementation of the method according to the invention according to the first embodiment (recirculating fluid bed reactor). It consists of the following elements:
• reaction chamber 3 cylindrical
• FIG. 2 represents a schematic diagram of the device in section used for the implementation of the method according to the invention according to the second embodiment (mechanical device). It consists of the following elements:
• EXAMPLE 1 A tungsten carbide powder with a particle size d50 of ⁇ is functionalized using a cobalt powder with a particle size d50 of 0.9 m.
• the operation is conducted according to the second embodiment.
• the powders are introduced into the high-energy mechanical device in a weight ratio of 80% C and 20% Co.
• a water recirculating cooling system keeps the reaction chamber at 20 ° C.
• the chamber is purged with argon to perform the operation in an inert atmosphere.
• the end of the compression piece is adjusted to a distance of between 1 and 3 mm from the wall of the enclosure. This is rotated at a speed between 4000 and 6000 rev / min, for a reaction time between 30 min and 60 min.
• the temperatures measured inside the enclosure are between 50 and 80 ° C.
• the composite powder thus obtained, shown in FIG. 3A is composed of tungsten carbide grains functionalised on the surface by cobalt grains covering more than 90% of the surface of the support particles.
• Example 2 The same tungsten carbide powder as in Example 1 is functionalized using a copper powder having a particle size d50 of 0.9 ⁇ m, according to the same operating parameters as in example 1.
• the composite powder thus obtained, illustrated in FIG. 4A, is formed of tungsten carbide grains functionalised on the surface by copper grains covering more than 60% of the surface of the support particles.
• An aluminum powder having a particle size d50 of 40 ⁇ is functionalized with a silicon carbide powder having a particle size d50 of 3.5 ⁇ .
• Example 1 The operation is conducted according to the same operating parameters as in Example 1.
• the powders are introduced into the high-energy mechanical device in a mass ratio of 85% Al and 15% SiC.
• the composite powder thus obtained shown in FIG. 3B (sectional view), is composed of aluminum grains functionalized on the surface by grains of silicon carbide forming a layer greater than ⁇ .
• a cobalt alloy powder (stellite) with a particle size centered on 50 ⁇ is introduced into a recirculating fluidized bed, according to the first embodiment of the method according to the invention.
• the powder is fluidized with nitrogen at a gas flow rate of between 1000 and 1500 l / h.
• the powder is heated to a temperature between 150 and 200 ° C.
• An aqueous suspension of a nickel powder, of a particle size centered on 2 ⁇ , to which polyvinyl alcohol is added as organic binder, is introduced into the chamber of the fluidized bed by spraying with a atomizing nozzle.
• Nitrogen is used as atomizing gas, at a pressure of between 3 and 8 bar, and for a flow rate of 300 and 700 l / h.
• the suspension is pumped at flow rates of between 0.8 and 1.2 l / h.
• the powder is heated to a temperature of between 250 ° C. and 350 ° C., corresponding to a first debinding step. This is then subjected to diffusion heat treatment at a temperature between 500 ° C and 700 ° C.
• the powder is finally cooled and packaged.
• EXAMPLE 5 According to the same embodiment as in Example 4 (according to the first embodiment of the process according to the invention), the same cobalt alloy powder is functionalized with copper using a copper powder. a particle size centered on 5 ⁇ .
• the suspension of the copper powder is carried out in an organic solvent using polyvinyl acetate as organic binder.
• the cobalt alloy powder is maintained in fluidization at a temperature of between 80 and 150 ° C.
• the functionalized powder then undergoes the same cycles of heat treatments as before.
• a copper spherical powder with a particle size centered on 40 ⁇ (d50) is functionalized by nickel covering more than 95% of the surface of the support particles, as illustrated in Figure 4b.
• a 60 m diameter polyamide (PA) powder is functionalized with a silver powder with a d50 particle size of 2 ⁇ .
• the operation is conducted according to the second embodiment of the method according to the invention.
• the powders are introduced into the high energy mechanical device in a weight ratio of 93% PA and 7% silver.
• a water recirculating cooling system allows cooling of the reaction chamber.
• the end of the compression piece is adjusted to a distance of between 1 and 3mm from the wall of the enclosure. This is rotated at a speed of between 3000 and 5000 rpm, for a grinding time of between 10 minutes and 30 minutes.
• the temperatures measured inside the chamber are between 20 and 50 ° C.
• the composite powder thus obtained is composed of polyamide grains functionalized on the surface by silver grains covering more than 10% of the surface of the support particles.
• FIGS. 7a and 7b are photographs taken under an optical microscope showing the sectional micrograph of a Fer-Copper composite material produced by compacting / sintering, on the one hand from a conventional mixture of iron and copper (as illustrated in FIG. 7a) and on the other hand from an iron powder functionalized with copper (as illustrated in FIG. 7a).
• the powders are previously compressed into a uniaxial press matrix at 700 MPa, and the resulting tablets are sintered under a controlled atmosphere at 1120 ° C.
• FIG. 7A shows the microstructure of the material obtained from a conventional mixture of iron powders (d50 of 50 ⁇ ) and copper (d50 of 5 ⁇ ).
• FIG. 7B shows the microstructure of the same material obtained from a copper functionalized iron powder according to the same embodiment of the process according to the invention as in Example 5.
• microstructure obtained from the functionalized powder illustrated in Figure 7b
• a particular microstructure consisting of a copper matrix interconnected with a homogeneous dispersion of iron grains.

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• 2016
  • 2016-09-09 FR FR1658443A patent/FR3055813B1/fr active Active
• 2017
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