EP3455017A1 - Procédé et dispositif de fabrication et de codage de poudre métallique - Google Patents

Procédé et dispositif de fabrication et de codage de poudre métallique

Info

Publication number
EP3455017A1
EP3455017A1 EP17723012.5A EP17723012A EP3455017A1 EP 3455017 A1 EP3455017 A1 EP 3455017A1 EP 17723012 A EP17723012 A EP 17723012A EP 3455017 A1 EP3455017 A1 EP 3455017A1
Authority
EP
European Patent Office
Prior art keywords
coding
gas
coding component
isotopes
gaseous
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP17723012.5A
Other languages
German (de)
English (en)
Other versions
EP3455017B1 (fr
Inventor
Jürgen Scholz
Ernst Miklos
Jim Fieret
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.)
Linde GmbH
Original Assignee
Linde GmbH
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 Linde GmbH filed Critical Linde GmbH
Publication of EP3455017A1 publication Critical patent/EP3455017A1/fr
Application granted granted Critical
Publication of EP3455017B1 publication Critical patent/EP3455017B1/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • 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 an apparatus for producing and encoding metal powder.
  • melt disintegration is also increasingly used, such as e.g. Centrifugal atomization, in which melt droplets 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-alloyed or
  • oxidation-sensitive materials can be advantageously produced by atomization 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 atomization chamber is cooled from the outside and used for collecting the powder, a water-cooled soil.
  • Another method involves atomization with gases in a Laval nozzle
  • Induction coil supplied and melted here superficially.
  • the rod undergoes a rotary movement during the process.
  • the melt thus produced finally drips in free fall through an annular nozzle, is atomized and solidified here. Then the powder is in a
  • Atomizing container deposited Atomizing container deposited.
  • plasma atomization is used for the production of pure spherical titanium and titanium alloy powder.
  • 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.
  • An overarching problem in the production of starting materials is that it is currently not possible to distinguish the starting materials, such as metal powder, and thus also components made from them easily and safely from counterfeit or cheap copies. It is usually difficult to determine if one 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. However, there may be considerable qualitative differences (strength, elasticity, hardness, porosity, ductility, etc.).
  • a method for coding metal powder is provided. This includes the following steps:
  • Forming metal powder particles from the melt jet Forming metal powder particles from the melt jet.
  • 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 such 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 compared to the naturally occurring proportion of this isotope in the gas is changed 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 be in theirs
  • 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.
  • Logging 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.
  • the logging of coding information can, for example, the storage of
  • 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.
  • atomization 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 method is based on the division of a thin, liquid metal beam through a high velocity incident current
  • Atomizing fluids e.g. a gas or liquid stream.
  • gaseous atomizing fluid air, nitrogen and argon can be provided. Above all, water can be provided as the liquid atomizing fluid. Preferably, a gaseous atomizing fluid is used.
  • Atomization with gas, water or centrifugal force referred.
  • 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.
  • Verdüsungsgas A mixture of gaseous atomizing fluid and coding component is referred to below as Verdüsungsgas.
  • 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.
  • two or more different isotopes may also be included in the coding component. Accordingly, the
  • Encoding component include one or more other than the naturally occurring isotopes of the process gas. For example. can oxygen isotopes with nitrogen isotopes or C isotopes in the CO2 with H isotopes in H 2 be combined
  • the coding component may additionally or alternatively to the isotopes include gaseous alloying elements, wherein the proportion of the gaseous alloying element is preferably selected such that the gaseous alloying element the
  • Provided metal powder This includes:
  • a nozzle device for atomizing the melt by means of an atomizing fluid; an atomization chamber for forming metal powder particles from the atomized melt by means of an atomizing fluid.
  • Codiansskomponentenzu classroom pain 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 fed 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 gas containing a coding component (premix) from respective storage containers.
  • the gaseous atomizing fluid is configured such that it can ensure the chemically metallurgically desired properties of the metal powder and also allows a clear identification or coding. Thus, 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 containing both process gas and a
  • 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.
  • the addition of the coding component can be controlled by a control device.
  • This controller may include a closed-loop encoding component controller that controls the addition.
  • Codiansskomponteeregler raised detected by means of a sensor an actual value of one or more volume flows in the atomization chamber and / or a Verdüsungsdüse and / or the Verdüsungshunt and / or the mixing chamber and / or a
  • Verdüsungsfluidtting this compares with a predetermined setpoint of one or more flow rates and an actuator is then set the default value.
  • 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 atomizing gas contains a coding component, wherein the gaseous
  • Coding component comprises one or more isotopes of at least one gas and the proportion of at least one isotope compared to the naturally occurring proportion 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 0 2 , C0 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 0 2 , C0 2 , H 2 , and N 2 or mixtures thereof.
  • the coding component may preferably be oxygen 18 carbon dioxide (C 18 O 2 ), carbon 13 carbon dioxide ( 13 C0 2 ), carbon 13 carbon monoxide ( 13 C0 2 ), deuterium (D2), nitrogen 15 ( 15 N 2 ) and oxygen 18 ( 18 0 2 ) or mixtures thereof.
  • the abundance of the isotope may be about 0.5% or about 1.0% or about 1.5% or about 2.5% or about 5.0% or about 10.0% or about 25% over the naturally occurring frequency % or 50%, or 75%, or 100%, or 150%, or 200%, or 500%, or 1000%.
  • 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
  • the isotopes may be isotopes of the gas that is the main component of the 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 microporosities in the gaseous state, 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 , 0 2 , 13 C0 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.
  • 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.
  • the coded metal powder is then used, for example, in the additive production of components (also referred to as “additive manufacturing” or “3-D printing”).
  • Figure 1 is a schematic, side-sectional view of a
  • FIG. 2 shows a schematic, laterally sectioned illustration of a nozzle device of the device from FIG. 1.
  • FIG. 1 a device according to the invention for coding metal powder by means of a device 1 for producing metal powder by atomizing is described (FIG. 1).
  • This device 1 comprises a melting crucible 2 for providing a
  • the device 1 comprises a pouring funnel 3, which by means of
  • Melted crucible 2 can be filled with melt.
  • 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.
  • 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 atomising 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 feeding device 1 1 comprises a
  • the Coding Component reservoir 12 is connected to the atomizing fluid chamber 6 via a conduit 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.
  • Mixing chamber has an inlet for supplying atomizing fluid from the
  • Coding component from the coding component storage container 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 proportion
  • Encoding component contains. This containing the premix gas storage tank then forms the Kod istskomponentezulite nails and is with the
  • Atomizing fluid chamber 6 directly, in addition to the reservoir for the Verdüsungsfluid connected or connected to the mixing chamber. Both the passage opening 5 and the atomizing nozzle 7 of
  • Nozzle device open into a Verdüsungshunt 8 for atomizing the
  • control device for controlling the addition of the coding component.
  • the control device comprises a
  • 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 control device detects an actual value of the one or more volume flows in the atomizing fluid chamber and / or atomization chamber and / or the mixing chamber, compares this with a predetermined desired value of one or more volume flows, and then sets the predetermined desired value via an actuator.
  • 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 via the atomizing nozzle 7 of the nozzle device 4 in the atomization chamber 14 by means of the atomizing medium and the
  • Coding component atomized and coded.
  • the resulting droplets solidify in the atomization chamber 14 in motion. Furthermore, it can be provided to separate the metal powder from the atomizing fluid either in the atomization chamber 14 and / or in downstream gas purification systems (cyclones, filters). In a next step, the metal powder can be with the help of a
  • Detection device such as a mass spectrometer
  • the coding component gives the metal powder a unique isotopic signature.
  • the coding information is stored in a database.
  • the coding gas includes, for example, the atomizing medium and the
  • Coding component such that the proportion of nitrogen-15 and nitrogen-14
  • Isotopes compared to the natural proportion of nitrogen-15 and nitrogen-14 isotopes or their ratio is changed.
  • 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. However, it is also possible to add to the atomizing fluid as the coding component other isotopes of another gas together with a portion of this other gas. According to a further embodiment of the method according to the invention is additionally or alternatively a gaseous as coding component
  • an inert gas such as argon as a process gas containing a minor proportion of between 1 ppm and "l O.OOOppm nitrogen-1 5 as an encoding component.
  • titanium is included. Accordingly, reacts in the preparation of This is not distinguishable in its chemical and physical properties from titanium nitride-14 and therefore can not be detected by means of chemical analysis methods, however, it is possible to detect the Analyze the component with a mass spectrometer to determine 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)

Abstract

L'invention concerne un procédé de codage de poudre métallique. Ce procédé comprend les étapes consistant à : prendre une matière en fusion, former un jet de matière en fusion, atomiser le jet de matière en fusion au moyen d'un fluide d'atomisation, former des particules de poudre métallique à partir du jet de matière en fusion. Le procédé est caractérisé en ce que, à au moins un intervalle de temps prédéfini pendant le chauffage, un constituant de codage ou un gaz de codage contenant le constituant de codage est ajouté de manière à permettre la détection de l'utilisation des constituants de codage dans la poudre métallique, les constituants de codage gazeux contenant au moins un isotope d'au moins un gaz, et la fraction dudit au moins un isotope pouvant être modifiée par rapport à la fraction d'occurrence naturelle de cet isotope dans le gaz et/ou les constituants de codage gazeux contenant des éléments d'alliage gazeux.
EP17723012.5A 2016-05-13 2017-05-12 Procede de fabrication et de codage de poudre metallique Active EP3455017B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
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
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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EP3455017A1 true EP3455017A1 (fr) 2019-03-20
EP3455017B1 EP3455017B1 (fr) 2022-06-29

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EP16001092.2A Withdrawn 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
EP17723012.5A Active EP3455017B1 (fr) 2016-05-13 2017-05-12 Procede de fabrication et de codage de poudre metallique

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EP16001092.2A Withdrawn 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

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US (1) US11020801B2 (fr)
EP (2) EP3243587A1 (fr)
ES (1) ES2923772T3 (fr)
WO (1) WO2017194206A1 (fr)

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KR102192388B1 (ko) * 2018-09-21 2020-12-17 이윤경 인위적 핵산서열이 탑재된 미술품의 제작과 거래를 위한 시스템 및 방법
CN111230131B (zh) * 2020-03-18 2023-07-21 宁波江丰电子材料股份有限公司 一种钛粉的制备方法及由其制备的钛粉和用途
FR3114526B1 (fr) * 2020-09-29 2023-04-21 Air Liquide Dispositif et procédé de production de poudres métalliques
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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Publication number Publication date
WO2017194206A1 (fr) 2017-11-16
US20190160543A1 (en) 2019-05-30
ES2923772T3 (es) 2022-09-30
US11020801B2 (en) 2021-06-01
EP3243587A1 (fr) 2017-11-15
EP3455017B1 (fr) 2022-06-29

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