EP3243587A1 - Procede et dispositif de fabrication et de codage de poudre metallique et gaz de codage pour poudre metallique - Google Patents

Procede et dispositif de fabrication et de codage de poudre metallique et gaz de codage pour poudre metallique Download PDF

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Publication number
EP3243587A1
EP3243587A1 EP16001092.2A EP16001092A EP3243587A1 EP 3243587 A1 EP3243587 A1 EP 3243587A1 EP 16001092 A EP16001092 A EP 16001092A EP 3243587 A1 EP3243587 A1 EP 3243587A1
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EP
European Patent Office
Prior art keywords
coding
gas
component
metal powder
isotopes
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.)
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Application number
EP16001092.2A
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German (de)
English (en)
Inventor
Jürgen Scholz
Ernst Miklos
Jim Fieret
Pierre Foret
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Linde GmbH
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Linde GmbH
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Publication date
Application filed by Linde GmbH filed Critical Linde GmbH
Priority to EP16001092.2A priority Critical patent/EP3243587A1/fr
Priority to US16/300,089 priority patent/US11020801B2/en
Priority to EP17723012.5A priority patent/EP3455017B1/fr
Priority to ES17723012T priority patent/ES2923772T3/es
Priority to PCT/EP2017/025124 priority patent/WO2017194206A1/fr
Publication of EP3243587A1 publication Critical patent/EP3243587A1/fr
Withdrawn legal-status Critical Current

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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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • 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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/084—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid combination of methods
    • 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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0844—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid in controlled atmosphere
    • 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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0848—Melting process before atomisation
    • 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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/088—Fluid nozzles, e.g. angle, distance
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/01—Reducing atmosphere
    • B22F2201/013—Hydrogen
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/02—Nitrogen
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/03—Oxygen
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/04—CO or CO2
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/10—Inert gases
    • B22F2201/11—Argon
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/10—Inert gases
    • B22F2201/12—Helium
    • 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
    • B22F2301/35—Iron
    • 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
    • B22F2303/00—Functional details of metal or compound in the powder or product
    • B22F2303/15—Intermetallic
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Definitions

  • the present invention relates to a method and apparatus for producing and encoding metal powders, and to a coding gas for encoding metal powders.
  • metal powders There are numerous processes for producing metal powder. These include the mechanical comminution of solid metal, the precipitation from salt solutions, the thermal decomposition of a chemical compound, the reduction of a chemical compound, usually the oxide in the solid phase, the electrolytic deposition and the atomization of liquid metal. The latter three methods are most commonly used in practice for the production of metal powders.
  • molten metal is broken up into small droplets and rapidly solidified before the molten droplets come into contact with each other or with a solid surface.
  • the principle of this process is based on the division of a thin liquid metal jet through a high velocity gas or liquid stream. Air, nitrogen and argon are the most commonly used gases, as a liquid, especially water is used.
  • melt disintegration is also increasingly used, such as e.g. Centrifugal atomization, in which molten droplets are ejected from a rotating source.
  • a melt of the metal to be atomized or of the alloy to be atomized is built up and correspondingly superheated.
  • This superheated melt usually runs through a second smaller crucible or a pouring funnel and forms there a melt jet, which falls vertically through a nozzle construction.
  • the melt jet is atomized by a gas (carrier gas) and the resulting droplets solidify in a Verdüsungshunt in the movement.
  • the metal powder is separated from the carrier gas.
  • High-purity powders made of special steel, superalloys and other high-alloy or oxidation-sensitive materials can be advantageously produced by atomizing with inert gas. This process usually yields spherical powders which are hardly suitable for conventional mechanical molding of molded parts, for isostatic pressing and powder injection molding processing.
  • the ASEA-STORA process is frequently used for atomising high-speed steel melts.
  • purified inert gas such as N 2 and Ar
  • powders can be produced with approximately 100 ppm oxygen.
  • the atomization chamber is cooled from the outside and a water-cooled bottom is used to collect the powders.
  • Plasma atomization Also used to make pure spherical titanium and titanium alloy powders is plasma atomization. An approximately 3 mm diameter wire made from the alloy to be atomized is fed to an array of three plasma torches, where it is melted and atomized in one step. The purity of the starting material, the absence of any crucible material and the melting under inert atmosphere gives a final product of the highest purity.
  • melts under vacuum which must be assigned to atomization in principle, is possible with the help of noble gases or hydrogen.
  • the gas-enriched melt under pressure is forced in a thin stream into an evacuated chamber.
  • the expansion of the dissolved gas in the melt divides them into fine droplets.
  • metal powders are subjected to an annealing treatment after production.
  • a reduction of the powders is e.g. necessary if, as a result of prolonged or unfavorable storage (increased humidity and temperature), the powder particles are oxidized more or less superficially.
  • the reduction is carried out in conventional ovens, which are also used for sintering. Most often, pure hydrogen and ammonia cracking gas are used as the reducing atmosphere.
  • Starting material or component is manufactured by the original manufacturer (Original Equipment Manufacture (OEM)) or whether a starting material or a component is a copy made by a third party, since they were distinguished by their appearance from each other.
  • OEM Olinal Equipment Manufacture
  • there may be considerable qualitative differences (strength, elasticity, hardness, porosity, ductility, etc.).
  • the method is characterized in that during the atomization of the melt and / or the Verdüsungsfluid a coding component or a coding gas is added so that the use of the coding component in the metal powder is detectable, wherein the gaseous coding component comprises one or more isotopes of at least one gas and the proportion of the at least one isotope is changed compared to the naturally occurring proportion of this isotope in the gas and / or wherein the gaseous coding component contains gaseous alloying elements
  • the coding takes place in that during the atomization the melt is subjected to a coding component.
  • this gaseous coding component is chemically active, it will react with the metal and the reaction product (e.g., an oxide, nitride, carbide) will be embedded in the metallic structure.
  • the reaction product e.g., an oxide, nitride, carbide
  • the reaction product e.g., an oxide, nitride, carbide
  • This mechanism also works with inert gases. These can remain trapped in their original state in the component.
  • the coding component can be detected in the metal powder and / or in the finished component, for example by means of chemical analysis methods or by means of a mass spectrometer. This can be done in a laboratory or with mobile devices.
  • Another advantage is that the production parameters do not have to be changed or adjusted during the production of the metal powder due to the coding. In addition, it is advantageous that the coding requires no additional production step.
  • coding information can be logged.
  • the powder-specific storage of the data in electronic form or the printing of the information on a certificate e.g. also be understood in machine-readable form.
  • Logging of coding information may include, for example, storing coding information in a database, on a chip, etc.
  • the coding information is logged and / or stored in a database, it is precisely recorded or recorded which coding component was introduced into the metal powder.
  • the coding information may thus contain information about the type and composition of the coding component.
  • Such encoding is almost forgery-proof, since a potential forger the coding information is not available and they are not visible from the outside.
  • the metal powder can be detected with respect to its coding component, for example by means of a chemical analysis method or by means of a mass spectrometer.
  • the production of metal powder is understood to mean a process such as, for example, atomization.
  • gaseous atomizing fluid air, nitrogen and argon can be provided. Above all, water can be provided as the liquid atomizing fluid.
  • the gaseous atomizing fluid may comprise an inert gas such as argon, helium, neon, krypton, xenon or radon or an active gas such as O 2 , CO 2 , H 2 , and N 2 , or mixtures thereof.
  • an inert gas such as argon, helium, neon, krypton, xenon or radon
  • an active gas such as O 2 , CO 2 , H 2 , and N 2 , or mixtures thereof.
  • a mixture of gaseous atomizing fluid and coding component is referred to below as the atomizing gas.
  • oxygen is preferably 18 carbon dioxide (C 18 O 2 ), carbon 13 carbon dioxide ( 13 CO 2 ), carbon 13 carbon monoxide ( 13 CO 2 ), deuterium (D 2 ), nitrogen 15 ( 15 N 2 ) and oxygen 18 ( 18 O 2 ) are provided.
  • the coding component thus comprises, for example, one or more isotopes of a gas, preferably of the atomizing medium, wherein the proportion of an isotope is changed relative to the natural proportion of the isotopes in the gas. That means the ratio of isotopes is changed from the naturally occurring ratio.
  • the frequency of isotopes versus naturally occurring frequencies may be about or greater than 0.5% or 1.0% or 1.5% or 2.5% or 5.0% or 10, 0% or 25% or 50.0% or 75% or 100% or 150% or 200% or 500% or 1000% is increased or decreased.
  • Nitrogen 15 and nitrogen 14 and / or carbon 12, carbon 13 and / or carbon 14 and / or also, for example, oxygen-16 and / or oxygen 18 are preferably provided as isotopes. Furthermore, argon -36, -38, -39, -40 can also be provided. Although argon is inert and does not react with the material, it is possible to provide gaseous inclusions for coding, since no 100% component density is achieved, in particular in powder bed processes.
  • the coding component may include one or more other than the naturally occurring isotopes of the process gas.
  • the coding component may include one or more other than the naturally occurring isotopes of the process gas.
  • oxygen isotopes with nitrogen isotopes or C isotopes in CO 2 can be combined with H isotopes in H 2
  • the coding component may additionally or alternatively to the isotopes also comprise gaseous alloying elements, wherein the proportion of the gaseous alloying element is preferably selected such that the gaseous alloying element only insignificantly alters the material properties of the metal powder.
  • the incorporation of the gaseous alloying elements in the metal powder is so great that the alloying elements in the metal powder and preferably even in the finished component can be detected eg by means of metallurgical and / or chemical and / or magnetic resonance analysis methods.
  • the device is characterized in that a Codéesskomponentezu slaughterstock is provided which the coded melt and / or the Verdüsungsfluid a coding component or a coding gas added such that the use of the coding component in the metal powder is detectable, wherein the gaseous coding component preferably comprises one or more isotopes of at least one gas and the proportion of at least one Isotops is changed compared to the naturally occurring proportion of this isotope in the gas and / or wherein the gaseous coding component contains gaseous alloying elements.
  • a database for storing coding information can be provided.
  • the coding component supply device may comprise a mixing chamber for admixing the coding component to the atomizing fluid, wherein from the mixing chamber at least partially a coding component or a process gas or a mixture of process gas and coding component can be supplied to the component.
  • the mixing chamber has a first inlet for supplying a process gas and a second inlet for supplying a coding component or a second inlet for supplying a process gas containing a coding component and an outlet connected to a nozzle.
  • Such an external mixing chamber is advantageous because existing systems or devices can be expanded so that a coding of a component is possible.
  • the coding component supply means may also include at least one nozzle for introducing the coding component or a gas containing the coding component into the atomizing chamber.
  • the nozzle device may also itself have two inlets, one inlet for supplying gaseous atomizing fluid and the other inlet for supplying a coding component or a gas containing a coding component (premix) from corresponding storage containers
  • the gaseous atomizing fluid is formed or assembled in such a way that it can ensure the chemically metallurgically desired properties of the metal powder and, in addition, permits unambiguous identification or coding.
  • gaseous atomizing fluids with appropriate coding component must be provided.
  • the coding component can thus also be provided as a premix from a gas storage container which contains both process gas and a corresponding proportion of the coding component. This gas storage container containing the premix then forms the coding component supply device.
  • the coding component supply device can thus be the mixing chamber, the premix storage container or the storage container containing the coding component, if appropriate with corresponding nozzles.
  • Volume flow or flow is understood to mean the values of the corresponding gas flows which are supplied by the coding component supply device to the atomizing chamber and / or the atomizing device.
  • a coding gas for encoding metal powder is provided according to the invention.
  • This comprises a Verdüsungsgas and is characterized in that the Verdüsungsgas contains a coding component, wherein the gaseous coding component comprises one or more isotopes of at least one gas and the proportion of the at least one isotope compared to the naturally occurring portion of this isotope is changed in the gas, and / or wherein the gaseous coding component contains gaseous alloying elements.
  • the coding component of the coding gas is introduced into the metal powder during manufacture or into the component by processing the metal powder and thus becomes part of the metal powder and of the component produced therefrom.
  • the atomizing gas may comprise an inert gas such as argon, helium, neon, krypton, xenon or radon and / or an active gas such as O 2 , CO 2 , H 2 , and N 2 or mixtures thereof.
  • an inert gas such as argon, helium, neon, krypton, xenon or radon and / or an active gas such as O 2 , CO 2 , H 2 , and N 2 or mixtures thereof.
  • the coding component may preferably comprise oxygen 18 carbon dioxide (C 18 O 2 ), carbon 13 carbon dioxide ( 13 CO 2 ), carbon 13 carbon monoxide ( 13 CO 2 ), deuterium (D2), nitrogen 15 ( 15 N 2 ) and oxygen 18 ( 18 O 2 ) or mixtures thereof.
  • the abundance of the isotope may be about 0.5% or 1.0% or 1.5% or 2.5% or 5.0%, or 10.0%, or around 25, as compared to the naturally occurring frequency % or 50%, or 75%, or 100%, or 150%, or 200%, or 500%, or 1000%.
  • Type of coding element Type of isotope used to enrich a base gas to provide coding Naturally occurring concentration of isotopes Possible molecules Range of isotopes dosing to a base gas Inert isotopes, to Ar 36 Ar 36 Ar: 0.337% N / A Between 1.1 times and 10 times the naturally occurring fraction of the isotope or less than 0.9 times the natural fraction Storing in 38 Ar: 0.063% Microporosities of a component 40 Ar: 99.6% He 3 Hey 3 He: 0.000137% Rest: 4 He N / A Between 1.1 times and 10 times the naturally occurring fraction of the isotope or less than 0.9 times the natural fraction H 2 H 2 H: 0.012% 2 H 2 2 H 2 : Between 1 ppm and 10 ppm 2 H 1 H: Between 1.1 times and 10 times the naturally occurring fraction of the isotope or less than 0.9 times the natural fraction N 2 H 3 : Between 1 ppm and 10 ppm 2 H 1 H: Between 1.1 times and 10 times the naturally occurring
  • the coding component may contain at least one isotope of an active gas which reacts with the material of the metal powder to be produced in such a way that it remains in the metal powder.
  • the coding component may comprise at least one inert gas isotope, the isotope being incorporated into the metal powder.
  • the coding component may contain a plurality of different isotopes (isotopes of different gases) in predetermined proportions, the different isotopes in the component forming the coding.
  • the isotopes may be isotopes of the gas forming the main component of the atomizing gas.
  • the isotopes can also be isotopes that do not occur in the process gas.
  • Nitrogen 15 N isotopes may sometimes be inert and sometimes reactive depending on the alloying element, temperature, concentration and / or reaction time.
  • Hydrogen isotopes can also be incorporated in the gaseous state in microporosities, react with atomic oxygen O 2 and dissolve or they can form metallic hydrides by adsorption on metallic surfaces and remain in the component.
  • Carbon isotopes 12 C and 13 C are provided in the form of carbon dioxide, which is then separated in the process.
  • Some isotopes of H, N, CO may be added to the process as part of a chemical compound such as e.g. B: C 18 , O 2 , 13 CO 2 , N 2 H 3 and 15 NH 3
  • the admixed isotopes can be formed from gases that are metallurgically harmless and do not affect the material properties otherwise. // Can this also be described differently? //
  • the coding component may comprise a gaseous alloying element, wherein the proportion of the gaseous alloying element is selected such that the gaseous alloying element only insignificantly alters the material properties of the component.
  • the coding gas may be provided for encoding metal powder during its production according to the method described above.
  • FIG. 1 a device according to the invention for coding metal powder by means of an apparatus 1 for producing metal powder by atomizing is described ( FIG. 1 ).
  • This device 1 comprises a melting crucible 2 for providing a molten metal.
  • the device 1 comprises a pouring funnel 3, which can be filled with melt by means of the melted crucible 2.
  • the pouring funnel 3 is provided with a ceramic coating.
  • An outlet channel 4 of the pouring funnel 3 opens into a nozzle device 4.
  • the nozzle device 4 comprises centrally a passage opening 5, through which a melt jet formed by the outlet channel 4 of the pouring funnel 3 can pass.
  • the passage opening 5 is surrounded by an annular atomizing fluid chamber 6 for receiving and distributing an atomizing fluid.
  • the atomizing fluid chamber 6 opens into an annular gap 7 which is arranged concentrically with respect to the passage opening 5.
  • the annular gap 7 forms an atomizing nozzle for producing melt droplets from the melt jet.
  • a Verdüsungsfluidzu slaughter 8 is provided, by means of which the Verdüsungsfluidhunt 6 can be acted upon by a Verdüsungsfluid.
  • the atomizing fluid supply device 8 has a Verdüsungsfluidvorrats maturityer 9 for the atomizing fluid, wherein the Verdüsungsfluidvorrats constituer 9 is connected via a line section 10 with the atomizing fluid chamber 6.
  • the coding component supply device 11 includes a coding component reservoir 12.
  • the coding component reservoir 12 is connected to the atomizing fluid chamber 6 via a pipe section 13.
  • a coding gas or a gaseous coding component is stored in the coding component reservoir 12.
  • a mixing chamber (not shown) may be provided.
  • the mixing chamber has an inlet for supplying atomizing fluid from the atomizing fluid reservoir 9 and an inlet for supplying a coding component from the coding component reservoir 12 for the coding component.
  • the atomizing fluid and the coding component or a coding gas may also be provided as a premix from a gas reservoir (not shown) containing both atomizing fluid and a corresponding amount of coding component.
  • This gas reservoir containing the premix then forms the coding component supply means and is connected directly to the atomizing fluid chamber 6 in addition to the atomizing fluid reservoir or connected to the mixing chamber.
  • Both the through-opening 5 and the atomizing nozzle 7 of the nozzle device open into an atomizing chamber 8 for atomizing the molten droplets into powder particles.
  • the controller includes a closed-loop encoding component controller that controls the addition.
  • the encoding component controller may include a P-controller, an I-controller, a D-controller, and combinations thereof, such as e.g. include a PID controller.
  • the coding component controller detects by means of a sensor an actual value of the one or more volume flows in the Verdüsungsfluidhunt and / or atomization chamber 8udn / or the mixing chamber compares this compares with a predetermined setpoint of one or more flow rates and via an actuator is then set the predetermined setpoint.
  • a melt of a metal to be atomized or an alloy to be atomized is first built up and superheated.
  • the superheated melt is introduced into the pouring funnel 3 and forms in its outlet channel 4 a melt jet, which passes vertically through the through hole 5 of the nozzle device 4.
  • This melt jet is atomized and coded via the atomizing nozzle 7 of the nozzle device 4 in the atomizing chamber 14 by means of the atomizing medium and the coding component.
  • the resulting droplets solidify in the atomization chamber 14 in motion.
  • the metal powder can be analyzed by means of a detection device, such as a mass spectrometer (gas chromatograph), and thus check the coding or the originality of the metal powder.
  • a detection device such as a mass spectrometer (gas chromatograph)
  • An analysis by means of magnetic resonance or chemical analysis methods are possible.
  • the coding component gives the metal powder a unique isotopic signature.
  • the coding information is stored in a database.
  • the coding gas comprises, for example, the atomizing medium and the coding component such that the proportion of nitrogen-15 and nitrogen-14 isotopes is changed relative to the natural proportion of nitrogen-15 and nitrogen-14 isotopes or their ratio.
  • the isotopes used may be isotopes of the atomizing fluid, i.
  • the ratio of nitrogen-15 to nitrogen-14 isotopes is changed.
  • carbon dioxide containing carbon-12, carbon-13 and carbon-14 isotopes may also be provided.
  • Inert isotopes can in principle be used independently of materials, since embedding in the microporosities is a purely mechanical process.
  • a gaseous alloying element is additionally or alternatively provided as the coding component.
  • it may be provided, for example, to use an inert gas such as argon as the process gas, which contains a small proportion of between 1 ppm and 10 000 ppm of nitrogen-15 as the coding component.
  • the metallic starting material contains titanium. Accordingly, in the production of the three-dimensional component, a small proportion of the titanium reacts with the nitrogen-15 and forms titanium nitride-15. This is indistinguishable from titanium nitride-14 in its chemical and physical properties, and therefore this can not be detected by chemical analysis methods. However, it is possible to analyze the component with a mass spectrometer. It is then found that the component has been produced under a nitrogen atmosphere with an increased proportion of nitrogen 15.

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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
EP16001092.2A 2016-05-13 2016-05-13 Procede et dispositif de fabrication et de codage de poudre metallique et gaz de codage pour poudre metallique Withdrawn EP3243587A1 (fr)

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EP16001092.2A EP3243587A1 (fr) 2016-05-13 2016-05-13 Procede et dispositif de fabrication et de codage de poudre metallique et gaz de codage pour poudre metallique
US16/300,089 US11020801B2 (en) 2016-05-13 2017-05-12 Method and device for producing and coding metal powder
EP17723012.5A EP3455017B1 (fr) 2016-05-13 2017-05-12 Procede de fabrication et de codage de poudre metallique
ES17723012T ES2923772T3 (es) 2016-05-13 2017-05-12 Procedimiento para la producción y codificación de polvo metálico
PCT/EP2017/025124 WO2017194206A1 (fr) 2016-05-13 2017-05-12 Procédé et dispositif de fabrication et de codage de poudre métallique

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FR3114526A1 (fr) * 2020-09-29 2022-04-01 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Dispositif et procédé de production de poudres métalliques

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EP4015109A1 (fr) * 2020-12-17 2022-06-22 Linde GmbH Procédé et dispositif de fabrication de poudre métallique pauvre en oxygène
CN113134617B (zh) * 2021-04-19 2023-01-17 山东理工大学 等离子球化脱氧3d打印金属粉体制备装置

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EP3455017B1 (fr) 2022-06-29
ES2923772T3 (es) 2022-09-30
EP3455017A1 (fr) 2019-03-20
US11020801B2 (en) 2021-06-01
US20190160543A1 (en) 2019-05-30

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