WO2019007699A1 - Procede de traitement de surface de particules d'une poudre metallique et particules de poudre metallique obtenues grace a ce procede - Google Patents

Procede de traitement de surface de particules d'une poudre metallique et particules de poudre metallique obtenues grace a ce procede Download PDF

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Publication number
WO2019007699A1
WO2019007699A1 PCT/EP2018/066615 EP2018066615W WO2019007699A1 WO 2019007699 A1 WO2019007699 A1 WO 2019007699A1 EP 2018066615 W EP2018066615 W EP 2018066615W WO 2019007699 A1 WO2019007699 A1 WO 2019007699A1
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WIPO (PCT)
Prior art keywords
particles
ions
radius
metal powder
metal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2018/066615
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English (en)
French (fr)
Inventor
Csilla Miko
Jean-Luc Bazin
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Swatch Group Research and Development SA
Original Assignee
Swatch Group Research and Development SA
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 Swatch Group Research and Development SA filed Critical Swatch Group Research and Development SA
Priority to US16/628,355 priority Critical patent/US11685989B2/en
Priority to CN201880045385.XA priority patent/CN110869527A/zh
Priority to KR1020207000178A priority patent/KR102319214B1/ko
Priority to SG11202000078PA priority patent/SG11202000078PA/en
Priority to JP2019571332A priority patent/JP6975263B2/ja
Publication of WO2019007699A1 publication Critical patent/WO2019007699A1/fr
Anticipated expiration legal-status Critical
Priority to US18/337,285 priority patent/US20230332284A1/en
Ceased legal-status Critical Current

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    • 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
    • C23C14/48—Ion implantation
    • 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
    • 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
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized 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
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
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    • 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
    • B22F1/09—Mixtures of metallic powders
    • 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
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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1103—Making porous workpieces or articles with particular physical characteristics
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0635—Carbides
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • 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
    • C23C14/221—Ion beam deposition
    • 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
    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
    • 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
    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
    • B22F2302/10—Carbide
    • 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
    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
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    • 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
    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
    • B22F2302/35—Complex boride, carbide, carbonitride, nitride, oxide or oxynitride
    • 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
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    • Y10T428/12576—Boride, carbide or nitride component
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    • Y10T428/12736—Al-base component
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    • Y10T428/2991—Coated
    • Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]

Definitions

  • the present invention relates to a surface treatment method of particles of a metal material in powder form as well as particles of metal powder obtained by the implementation of such a method.
  • the metal powder particles obtained by the process according to the invention are intended for the manufacture of solid parts by means of powder metallurgy processes such as the injection molding process, better known by its Anglo-Saxon name Metal Injection Molding or MIM, pressing or additive manufacturing such as 3D laser printing.
  • the present invention also relates to a particle of a metal powder with a ceramic surface and a metal core.
  • the ion implantation methods consist in bombarding the surface of an object to be treated, for example by means of a source of mono- or multicharged ions of the electron cyclotron resonance type. Such an installation is still known under the name Anglo-Saxon Electron Cyclotron Resonance or ECR.
  • An ECR ion source makes use of the cyclotron resonance of electrons to create a plasma.
  • a volume of low pressure gas is ionized by means of microwaves injected at a frequency corresponding to the electron cyclotron resonance defined by a magnetic field applied to a region located inside the volume of gas to be ionized.
  • Microwaves heat the free electrons present in the volume of gas to be ionized. These free electrons, under the effect of thermal agitation, will collide with atoms or gas molecules and cause their ionization.
  • the ions produced correspond to the type of gas used. This gas can be pure or compound. It can also be a vapor obtained from a solid or liquid material.
  • the ECR ion source is able to produce simply charged ions, i.e. ions with a degree of ionization equal to 1, or multicharged ions, i.e. ions whose degree of ionization is greater than 1.
  • FIG. 1 A source of multicharged ions of the ECR electron cyclotron resonance type is schematically illustrated in FIG. 1 appended to the present patent application.
  • a multicharged ion source ECR comprises an injection stage 2 into which a volume 4 of a gas to be ionized and a microwave wave 6, a magnetic confinement stage 8 is introduced. in which a plasma 10 is created, and an extraction stage 12 which makes it possible to extract and accelerate the ions of the plasma 10 by means of an anode 12a and a cathode 12b between which a high voltage is applied.
  • a multicharged ion beam 14 produced at the output of the multicharged ion source ECR 1 strikes a surface 16 of a workpiece 18 and penetrates more or less deeply into the volume of the workpiece 18.
  • of ions by bombarding the surface of an object to be treated has many effects among which the modification of the microstructure of the material in which the object to be treated is achieved, the improvement of the corrosion resistance, the improvement tribological properties and, more generally, the improvement of the mechanical properties.
  • the present invention aims to meet the need mentioned above as well as others by proposing a method of surface treatment of a metallic material for making objects whose geometric shapes are virtually free from any constraint while having modified and improved physical and chemical properties.
  • the present invention relates to a method of surface treatment of a metallic material, this method comprising the step of comprises providing a powder formed of a plurality of particles of a metallic material, and directing to a surface of these particles a monocharged or multicharged ion beam produced by a source of single-charged or multicharged ions, the particles having a generally spherical shape.
  • the source of mono- or multicharged ions is of the electron cyclotron resonance type ECR;
  • the particles of the metal powder are agitated during the entire duration of the ion implantation process
  • the particle size of the particles of the metal powder used is such that substantially 50% of all these particles have a diameter of between 1 and 2 micrometers, the diameter of the particles of the metal powder used not exceeding 50 microns;
  • the metallic material is a precious metal chosen from gold and platinum;
  • the metallic material is a non-precious metal chosen from magnesium, titanium and aluminum;
  • the material to be ionized is chosen from carbon, nitrogen, oxygen and argon;
  • the monocharged or multicharged ions are accelerated at a voltage of between 15 ⁇ 00 and 35 ⁇ 00 volts;
  • the dose of implant ions is between 1 .10 and 1 .10 ions.cm -2 ; the maximum implantation depth of the ions is 150 to
  • the present invention also relates to a particle of a metal powder with a ceramic surface and a metal core, and more particularly with a surface which corresponds to a metal carbide or nitride in which the particles of the metal powder are produced.
  • the present invention provides a method of treating a powdery metal material in which the particles forming this powder retain their original metal structure in depth, while from the surface and up to the at a certain depth, the monocharged or multicharged ions with which the metal powder particles are bombarded fill the defects of the meshes of the crystallographic structure of the metal, then combine with the atoms of the metallic material to form a ceramic, that is, that is, a material that is solid at room temperature and is neither organic nor metallic.
  • the metal powder particles after treatment by ion implantation, are ready to be used in powder metallurgy processes such as the injection molding process, pressing or else additive manufacturing such as three-dimensional laser printing. .
  • the surface of the particles of metal powder is converted into ceramic, in particular carbide and / or metal nitride constituting these particles, the mechanical and physical properties, in particular the hardness, corrosion resistance or still, the tribological properties of these metal powder particles are improved. The improvement of the mechanical and physical properties of the metal powder particles is maintained when these metal powders are used to produce massive pieces.
  • the particles forming the metal powder are agitated throughout the duration of the ion implantation treatment so that these particles are exposed to the ions of the implantation beam in a homogeneous manner over their entire substantially spherical surface.
  • a ceramic-metal type material also called a "cermet”
  • This technique poses the problem of precise control of the thickness of the metal layer and the quality of the interface between the metal layer and the ceramic core.
  • FIG. 1 is a schematic representation of a source of multicharged ions of the electron cyclotron resonance type ECR;
  • FIG. 2 is a sectional view of an Au gold particle having a radius of about 1 micrometer and which has been bombarded by means of a C + carbon ion beam;
  • FIG. 3 is a schematic representation of a source of multicharged ions of the ECR electron cyclotron resonance type used in the context of the present invention
  • FIG. 4A illustrates the implantation profile of the C + carbon ions in a Pt platinum particle whose radius is approximately 1 micrometer
  • FIG. 4B is an expanded view in the plane of a substantially spherical platinum Pt particle whose radius is approximately 1 micrometer and which shows the path of penetration of the carbon ions.
  • FIG. 5A illustrates the implantation profile of the N + nitrogen ions in a Pt platinum particle whose radius is about 1 micrometer;
  • FIG. 5B is an expanded view in the plane of a Pt platinum particle whose radius is approximately 1 micrometer and which shows the path of penetration of the N + nitrogen ions into the particle;
  • FIG. 6A illustrates the implantation profile of the C + carbon ions in a gold Au particle whose radius is about 1 micrometer;
  • FIG. 6B is an expanded view in the plane of a substantially spherical particle of Au gold whose radius is approximately 1 micrometer and which shows the path of penetration of the C + carbon ions into the particle;
  • FIG. 7A illustrates the implantation profile of the N + nitrogen ions in an Au gold particle whose radius is about 1 micrometer
  • FIG. 7B is an expanded view in the plane of an Au gold particle whose radius is approximately 1 micrometer and which shows the path of penetration of the N + nitrogen ions into the particle.
  • the present invention proceeds from the general inventive idea of subjecting particles of a metal powder to an ion implantation processing process in the surface of these particles.
  • ion implantation processing process in the surface of these particles.
  • these ions start by filling the defects of the meshes of the crystallographic structure of the metal, and then combine with the atoms of the metallic material to form a ceramic.
  • ceramic for example carbide or metal nitride in which the particles are made.
  • the mechanical and physical properties, in particular the hardness, the corrosion resistance or even the tribological properties of these metal powder particles with a ceramic surface layer are improved.
  • the improvement of the mechanical and physical properties of metal powder particles having a surface ceramic layer is retained when these metal powders are used to make solid parts by powder metallurgy techniques such as injection molding, pressing, additive manufacturing Or other.
  • additive manufacturing technique is meant a technique that consists of making a massive piece by adding material. In the case of additive manufacturing techniques, a massive piece is created by progressively providing a raw base material, whereas in conventional manufacturing techniques, starting from a raw material and the final piece sought is obtained by progressive removal of material.
  • FIG. 2 is a sectional view of an Au gold particle. Designated as a whole by the general numeral 20, this gold particle is substantially spherical in shape with a radius R of about 1 micrometer. This gold particle 20 was bombarded by means of a carbon ion beam C + denoted by the reference numeral 22.
  • the gold particle 20 has a heart or core 24 of pure gold and an outer layer or bark 26 mainly made of gold carbide.
  • this outer layer 26 is of the order of one tenth of the radius R of the gold particle 20, ie about 100 nanometers.
  • This outer layer 26 is mainly made of gold carbide which is a ceramic material. According to the invention, the concentration of ceramic material increases from the outer surface 28 of the gold particle 20 to about 5% of the radius R of this gold particle 20, that is to say about 50 nanometers, then decreasing to about one tenth of the radius R of the gold particle 20 where it is substantially zero.
  • particles for example gold or platinum, the core of which consists of the original metal, are thus obtained, while an outer layer which completely surrounds the core of these particles consists of a ceramic material, for example a carbide or a nitride, which results from the combination of the metal atoms with the ions with which the particles are bombarded.
  • a ceramic material for example a carbide or a nitride
  • a powder formed of a plurality of particles of a metal material to be treated This metallic material may be, without limitation, a precious metal chosen from gold and platinum. It may also be a non-precious metal selected from magnesium, titanium and aluminum.
  • the metal powder particles 30 are subjected to an ion implantation process by directing to an outer surface of these particles a monocharged or multicharged ion beam 14 produced by an ion source.
  • monocharged or multicharged electron cyclotron resonance type ECR see Figure 3).
  • the material to be ionized is chosen from carbon, nitrogen, oxygen and argon, and the monocharged or multicharged ions are accelerated under tensions included between 15 ⁇ 00 and 35 ⁇ 00 volts.
  • the dose of implanted ions is between 1 .10 1 5 and 1 .10 1 7 ions.cm ⁇ 2 .
  • the particles of metal powder 30 have a general spherical shape with a radius R and their particle size is such that about 50% of all these particles have a diameter of between 1 and 2 micrometers, the diameter of the particles of metal powder 30 not exceeding 50 micrometers.
  • the metal powder particles are agitated throughout the ion implantation process to ensure that these particles are exposed to the ion beam 14 uniformly over their entire outer surface.
  • FIG. 4A illustrates the implantation profile of the C + carbon ions in a Pt platinum particle whose radius is approximately 1 micrometer.
  • the x-axis extends along the radius R of the platinum particle Pt, with the origin of this axis corresponding to the outer surface of the platinum particle, and the value of 2000 Angstroms corresponding to about 20 % of the length of the radius R of the platinum particle Pt.
  • the ordinate represents the number of C + carbon ions implanted in the platinum particle Pt at a given depth. It can be seen that the number of C + carbon ions implanted in the platinum particle Pt grows very rapidly from the outer surface of the platinum particle to reach a maximum
  • FIG. 4B is an in-plane view of a substantially spherical platinum Pt particle having a radius of approximately 1 micrometer and showing the average free path of the individual carbon ions C + , C ++, etc. when they penetrate into a particle of platinum Pt. This figure 4B has been established for a density of the order of 4 -2
  • the abscissa of FIG. 4B shows the depth of the platinum particle Pt between the surface (0 Angstroms) and 2000 Angstroms.
  • On the ordinate of FIG. 4B is the diameter of the carbon ion beam C + .
  • the center of the carbon ion beam C + is at mid-height on the ordinate axis, between the values -1000 Angstroms and +1000 Angstroms. It can thus be seen in this FIG. 4B that the approximate diameter of the carbon ion beam C + is of the order of
  • FIG. 5A illustrates the implantation profile of the N + nitrogen ions in a Pt platinum particle whose radius R is approximately 1 micrometer.
  • the abscissa axis extends along the radius R of the platinum particle Pt, with the origin of this axis corresponding to the outer surface of the platinum particle Pt and the value of 2000 Angstroms corresponding to about 20 % of the length of the radius R of the platinum particle Pt.
  • the ordinate represents the number of N + nitrogen ions implanted in the platinum particle Pt at a given depth. It can be seen that the number of N + nitrogen ions implanted in the platinum particle Pt grows very rapidly from the outer surface of the platinum particle Pt to reach a maximum
  • 5B is a developed view in the plane of the platinum Pt substantially spherical particle with a radius of approximately 1 microns and showing the mean free path of the individual nitrogen ion N +, N ++ etc. when they enter a platinum particle Pt.
  • FIG. 4B shows the depth of the platinum particle Pt between the surface (0 Angstroms) and 2000 Angstroms.
  • N + the diameter of the nitrogen ion beam
  • the center of the N + ion beam is at mid-height on the y-axis, between the values -1000 Angstroms and +1000 Angstroms.
  • FIG. 5B shows that the approximate diameter of the N + ion beam is of the order of 150 nanometers and that the penetration depth of the N + ions in the platinum particle Pt is slightly less than 100 nanometers. It is therefore found that the N + ions penetrate the platinum particles less deeply than the C + ions.
  • FIG. 6A illustrates the implantation profile of the C + carbon ions in an Au gold particle whose radius R is approximately 1 micrometer.
  • the axis of The abscissa extends along a radius R of the Au gold particle, with the origin of this axis corresponding to the outer surface of the Au gold particle and the value of 2000 Angstroms corresponding to about 20 % of the radius R of the Au gold particle.
  • On the ordinate we represent the number of C + carbon ions implanted in the Au gold particle at a given depth. It can be seen that the number of C + carbon ions implanted in the gold particle Au grows very rapidly from the outer surface of the Au gold particle.
  • the number of ions decreases and tends to zero at about 1000 nm below the outer surface of the Au gold particle, about 10% of the length of the particle's radius R.
  • Fig. 6B is an expanded view in the plane of a substantially spherical Au gold particle having a radius of approximately 1 micrometer and showing the average free path of the individual carbon ions C + , C ++ etc. when they enter a gold Au particle.
  • This FIG. 6B has been established for an ion density of the order of 4 -2.
  • FIG. 6B On the abscissa of FIG. 6B is the depth of the Au gold particle between the surface (0 Angstroms) and 2000 Angstroms. On the ordinate of FIG. 6B is the diameter of the carbon ion beam C + . The center of the C + ion beam is halfway up the y-axis, between the values -1000 Angstroms and +1000 Angstroms. It can thus be seen in this FIG. 6B that the approximate diameter of the C + ion beam is of the order of 150 nanometers and that the penetration depth of the C + ions in the Au gold particle slightly exceeds 100 nanometers.
  • Figure 7A illustrates the implantation profile of N N ions in an Au gold particle with a radius of about 1 micrometer.
  • the x-axis extends along a radius R of the Au gold particle, with the origin of this axis corresponding to the outer surface of the Au gold particle and the value of 2000 Angstroms which corresponds to about 20% of the radius R of the Au gold particle.
  • the ordinate represents the number of N + nitrogen ions implanted in the Au gold particle at a given depth. It can be seen that the number of N + nitrate ions implanted in the Au gold particle grows very rapidly from the outer surface of the Au gold particle.
  • Fig. 7B is an expanded view in the plane of a substantially spherical Au gold particle having a radius of approximately 1 micrometer and showing the average free path of the individual N + , N ++ , and other nitrogen ions. when they enter a gold Au particle.
  • the powder obtained by the ion implantation process according to the invention is not really a composite material. Indeed, in the sense that is usually understood, a composite material results from the combination of two different materials, namely a matrix and a reinforcement.
  • the ECR ion source is able to produce ions monocharged, that is to say ions whose degree of ionization is equal to 1, or multicharged ions, that is to say ions whose degree of ionization is greater than 1.
  • the ion beam may comprise ions all having the same degree of ionization, or may result from a mixture of ions with different degrees of ionization.
  • Multi-charged ion beam 16.

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