WO2003056046A1 - Powder-metallurgical production of magnesium bodies from magnesium hydride - Google Patents

Powder-metallurgical production of magnesium bodies from magnesium hydride Download PDF

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Publication number
WO2003056046A1
WO2003056046A1 PCT/DE2002/004221 DE0204221W WO03056046A1 WO 2003056046 A1 WO2003056046 A1 WO 2003056046A1 DE 0204221 W DE0204221 W DE 0204221W WO 03056046 A1 WO03056046 A1 WO 03056046A1
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Prior art keywords
magnesium
sintering
hydride
semi
product
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PCT/DE2002/004221
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German (de)
French (fr)
Inventor
Eckard Aust
Tobias Benzler
Nico Eigen
Wolfgang Limberg
Original Assignee
Gkss-Forschungszentrum Geesthacht Gmbh
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Publication of WO2003056046A1 publication Critical patent/WO2003056046A1/en

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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
    • 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
    • B22F3/001—Starting from powder comprising reducible metal compounds
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0408—Light metal alloys
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the invention relates to a method for producing products such as components or semi-finished products from powdery materials by means of sintering processes based on magnesium or magnesium alloys.
  • Powdery materials based on magnesium have so far not been able to be processed into complex products in the form of components or into semi-finished products, since such products and / or semi-finished products have to be sintered in order to form their final shape or their preliminary final shape. Due to the extremely high reactivity of magnesium or magnesium base materials for oxygen sintering on an industrial scale is not possible. So far, magnesium base materials have been processed into semi-finished products or components or products by master forms from the liquid, plastic or pulpy (semi-solid or thixo,) state in the form of pressure, centrifugal, continuous or injection molding. The primary shaping of powder-form magnesium base materials has so far only been possible using the extrusion process.
  • the task is solved according to the invention in that the starting material is used in the form of the hydride of magnesium or magnesium alloys.
  • the advantage of the method according to the invention lies essentially in the fact that, as intended, metal powders based on magnesium materials make sintering possible and enable processing for the production of novel products, for example implants for medical technology.
  • the specific properties of magnesium or magnesium-based materials such as low weight with relatively high strength, can be brought to bear in combination with powder technology, which was previously not possible.
  • the close bond of magnesium to the hydrogen is used, i.e.
  • the method according to the invention also makes it possible for products to be produced in a quality close to the final shape of the product by press sintering and / or metal powder injection molding, it also being possible to achieve high production rates by means of the method according to the invention.
  • the hydrogen is expelled from the product and / or the semifinished product during the sintering process, so that components or semifinished products can then be sintered from powder particles.
  • the sintering process in which the hydrogen is expelled from the manufactured product and / or semi-finished product, can take place under inert gas or, in another embodiment of the method, can be carried out under vacuum, whereby the oxygen in the process step of expelling the hydrogen from the hydride of magnesium or Magnesium alloys is kept away.
  • the product and / or the semi-finished product are sintered above the dehydrogenation temperature of the hydride of magnesium or magnesium alloys.
  • Fig. 1 is a micrograph of sintered magnesium at 110 times magnification
  • Fig. 2 shows an X-ray diffractometer diagram.
  • the invention uses known techniques for the production of metal powders, the metal powder in the present case being powdered magnesium hydride or a powdered magnesium hydride mixture.
  • the term "powdery magnesium hydride” also includes powdery magnesium hydride alloys of any quantitative and qualitative composition.
  • techniques, process sequences and apparatuses and devices are used which are known in the prior art with regard to the processing and processing of metal powder and / or devices and equipment. Since that The method according to the invention makes extensive use of these known process techniques, so there is no need to go into further detail in order to understand the invention.
  • the invention uses pulverulent starting material based on pulverulent magnesium hydride which has been suitably produced beforehand. After the magnesium hydride has been shaped to produce a product into a shape which almost corresponds to the desired final shape, which also applies to the shape of a desired semi-finished product to be produced, the hydrogen is expelled from the product and / or the semi-finished product during the subsequent sintering process.
  • the hydrogen can be expelled under inert gas or in vacuo and at a temperature below the melting temperature of the respectively selected powdered magnesium or its desired alloys.
  • the product or the semifinished product is sintered. After the sintering process, either a finished product is available or a semi-finished product with the desired semi-finished product.
  • FIG. 1 shows an X-ray diffraction diagram of a sample which was produced by the method according to the invention.
  • the pronounced maxima correspond to the characteristic maxima for magnesium. This proves that the hydrogen is removed from the sample. is driven (no MgH2 phase in the sample).
  • Fig. 1 also shows that magnesium oxide is only present in traces in the sample.
  • FIG. 2 shows a section of the sample in a magnification of 110 times.
  • FIG. 2 also shows that the sintering process has taken place and that the sample has a dense structure.

Abstract

The invention relates to a method for preparing products and/or semi-finished products from pulverulent starting materials based on magnesium or magnesium alloys, by means of sintering. The starting material used is in the form of magnesium hydride or magnesium alloys.

Description

PÜLVERMETALLURGISCHE HERSTELLUNG VON MAGNESIUMKÖRPERN AUS IHREM HYDRIDP O LVERMETALLURGISCHE PRODUCING MAGNESIUM BODIES FROM YOUR HYDRIDE
Beschrei bungDescription
Die Erfindung betrifft ein Verfahren zum Herstellen von Erzeugnissen wie Bauteile oder Halbzeuge aus pulver- för igen Werkstoffen mittels Sinterverfahren auf der Basis von Magnesium oder Magnesiumlegierungen.The invention relates to a method for producing products such as components or semi-finished products from powdery materials by means of sintering processes based on magnesium or magnesium alloys.
Pulverförmige Werkstoffe auf der Basis von Magnesium lassen sich bisher weder zu komplexen Erzeugnissen in Form von Bauteilen noch zu Halbzeugen verarbeiten, da solche Erzeugnisse und/oder Halbzeuge zur Ausbildung ihrer Endform bzw. ihrer vorläufigen Endform gesintert werden müssen. Aufgrund der extrem hohen Reaktivität von Magnesium bzw. Magnesiumbasiswerkstoffen zum Sauerstoff ist eine Sinterung in großtechnischem Maßstab nicht möglich. Bisher wurden Magnesiumbasiswerkstoffe durch Urformen aus dem flüssigen, plastischen oder breiigen (semi-solid bzw. Thixo-,) Zustand in Form von Druck-, Schleuder-, Strang- oder Spritzguß zu Halbzeugen oder Bauteilen bzw. Erzeugnissen verarbeitet. Das Urformen aus pul verför igen Magnesiumbasiswerkstoffen ist bisher nur über das Strangpreßverfahren möglich.Powdery materials based on magnesium have so far not been able to be processed into complex products in the form of components or into semi-finished products, since such products and / or semi-finished products have to be sintered in order to form their final shape or their preliminary final shape. Due to the extremely high reactivity of magnesium or magnesium base materials for oxygen sintering on an industrial scale is not possible. So far, magnesium base materials have been processed into semi-finished products or components or products by master forms from the liquid, plastic or pulpy (semi-solid or thixo,) state in the form of pressure, centrifugal, continuous or injection molding. The primary shaping of powder-form magnesium base materials has so far only been possible using the extrusion process.
Es besteht das Bedürfnis, Halbzeuge und/oder komplexe Bauteile bzw. Erzeugnisse aus Magnesiumbasiswerkstoffen durch das Sintern von Magnesiumpulver herstellen zu können, da sich durch Herstellungsverfahren wie Preßsintern und Metall pul verspri tzgi eßen (MIM-Technol ogi e) , die Metallpulver als Ausgangsmaterial erfordern, neue Anwendungsgebiete für Magnesiumbasiswerkstoffe erschließen ließen, die die Eigenschaften von Magnesium bzw. Magnesiumbasiswerkstoffen voll zum Tragen kommen ließen, d.h., das sehr geringe Gewicht bei verhältnismäßig hoher Festigkeit.There is a need to be able to manufacture semi-finished products and / or complex components or products from magnesium base materials by sintering magnesium powder, since manufacturing processes such as press sintering and metal powder injection molding (MIM technology) require metal powder as the starting material , opened up new areas of application for magnesium-based materials that made the properties of magnesium or magnesium-based materials come into play, ie the very low weight and relatively high strength.
Es ist somit Aufgabe der vorliegenden Erfindung, ein Verfahren der eingangs genannten Art zu schaffen, mit dem pul verförmige Werkstoffe auf der Basis von Magnesium verwendet werden können, um endfertige Erzeugnisse bzw. Bauteile und/oder Halbzeuge herstellen zu können, wobei das Verfahren sowohl im Labormaßstab als auch in großtechnischem Maßstab durchführbar sein soll und dabei die herkömmlichen Verfahren, mit denen pul verförmige Metalle ver- und/oder bearbeitet werden können, herangezogen werden können.It is therefore an object of the present invention to provide a method of the type mentioned at the outset, with which pulverulent materials based on magnesium can be used in order to be able to produce finished products or components and / or semi-finished products Laboratory scale as well as on an industrial scale should be feasible and the conventional methods with which pulverulent metals can be processed and / or processed can be used.
Gelöst wird die Aufgabe gem. der Erfindung dadurch, daß der Ausgangsstoff in Form des Hydrids von Magnesium oder Magnesiumlegierungen verwendet wird. Der Vorteil des erfindungsgemäßen Verfahrens liegt im wesentlichen darin, daß nun, wie aufgabengemäß angestrebt, Metallpulver auf der Basis von Magnesiumwerkstoffen das Sintern möglich machen und eine Verarbeitung zur Herstellung neuartiger Produkte, bspw. Implantate für die Medizintechnik, ermöglichen. Dabei können erstmals die spezifischen Eigenschaften von Magnesium bzw. Magnesiumbasiswerkstoffen wie geringes Gewicht bei verhältnismäßig hoher Festigkeit, in Kombination mit der Pulvertechnologie zum Tragen gebracht werden, was bisher nicht möglich war. Dabei wird bei der Verwendung des Hydrids von Magnesium oder Magnesiumlegierung die enge Bindung von Magnesium an den Wasserstoff ausgenutzt, d.h. in den einzelnen Verfahrensschritten von der Bauteil- und/oder Halbzeugformgebung bis einschließlich des Sinterns wird die Verbindung des Magnesiums mit Sauerstoff verhindert, was, wenn man sich des lösungsgemäßen Verfahrens nicht bedienen würde, die Sintermöglichkeit von Magnesiumbasiswerkstoffen zu Bauteilen und/oder Halbzeugen verhindern würde.The task is solved according to the invention in that the starting material is used in the form of the hydride of magnesium or magnesium alloys. The advantage of the method according to the invention lies essentially in the fact that, as intended, metal powders based on magnesium materials make sintering possible and enable processing for the production of novel products, for example implants for medical technology. For the first time, the specific properties of magnesium or magnesium-based materials, such as low weight with relatively high strength, can be brought to bear in combination with powder technology, which was previously not possible. When using the hydride of magnesium or magnesium alloy, the close bond of magnesium to the hydrogen is used, i.e. in the individual process steps from component and / or semi-finished product formation up to and including sintering, the connection of magnesium with oxygen is prevented, which if one would not use the method according to the solution, would prevent the possibility of sintering magnesium-based materials into components and / or semi-finished products.
Das erfindungsgemäße Verfahren macht es auch möglich, daß Erzeugnisse durch Preßsintern und/oder Metallpulverspritzgießen in einer Qualität nahe der Endform des Erzeugnisses hergestellt werden können, wobei mittels des erfindungsgemäßen Verfahrens auch hohe Produktionsraten realisiert werden können.The method according to the invention also makes it possible for products to be produced in a quality close to the final shape of the product by press sintering and / or metal powder injection molding, it also being possible to achieve high production rates by means of the method according to the invention.
Gem. einer vorteilhaften Ausgestaltung des Verfahrens wird der Wasserstoff aus dem Erzeugnis und/oder dem Halbzeug während der Durchführung des Sinterns ausgetrieben, so daß dann Bauteile oder Halbzeuge aus Pulverpartikeln gesintert werden können. Der Sintervorgang, bei dem der Wasserstoff aus dem hergestellten Erzeugnis und/oder Halbzeug ausgetrieben wird, kann unter Inertgas erfolgen oder bei einer anderen Ausgestaltung des Verfahrens unter Vakuum ausgeführt werden, wodurch der Sauerstoff bei dem Verfahrensschritt des Austreibens des Wasserstoffs aus dem Hydrid von Magnesium oder Magnesiumlegierungen ferngehalten wird.According to an advantageous embodiment of the method, the hydrogen is expelled from the product and / or the semifinished product during the sintering process, so that components or semifinished products can then be sintered from powder particles. The sintering process, in which the hydrogen is expelled from the manufactured product and / or semi-finished product, can take place under inert gas or, in another embodiment of the method, can be carried out under vacuum, whereby the oxygen in the process step of expelling the hydrogen from the hydride of magnesium or Magnesium alloys is kept away.
Die Sinterung des Erzeugnisses und/oder des Halbzeuges erfolgt oberhalb der Dehydrierungstemperatur des Hydrids von Magnesium oder Magnesiumlegierungen.The product and / or the semi-finished product are sintered above the dehydrogenation temperature of the hydride of magnesium or magnesium alloys.
Die Erfindung wird nun nachfolgend unter Bezugnahme auf die beigefügten Darstellungen im einzelnen beschrieben. Diese zeigen:The invention will now be described in detail below with reference to the accompanying drawings. These show:
Fig. 1 ein Gefügebild von gesintertem Magnesium bei 110-facher Vergrößerung undFig. 1 is a micrograph of sintered magnesium at 110 times magnification and
Fig. 2 ein Röntgendi ffraktometerdi agramm.Fig. 2 shows an X-ray diffractometer diagram.
Zur Ausführung des Verfahrens gem. der Erfindung werden bekannte Techniken zur Herstellung von Metal 1 pul vern verwendet, wobei das Metallpulver im vorliegenden Falle pul verförmiges Magnesiumhydrid ist bzw. ein pulverförmi- ges Magnesiumhydridgemisch. Der Begriff "pul verförmiges Magnesiumhydrid" umfaßt auch pul verförmige Magnesiumhydridlegierungen beliebiger quantitativer und qualitativer Zusammensetzung. Auch bezüglich der Sinterung des pul verförmigen Metal 1 hydrids werden Techniken, Verfahrensabläufe und apparative Ein- bzw. Vorrichtungen verwendet, die im Stand der Technik bezüglich der Metallpul verherstel 1 ungs- und -bearbeitungsverfahren bzw. Vor- und Einrichtungen bekannt sind. Da das erfindungsgemäße Verfahren diese bekannten Verfahrenstechniken weitgehend nutzt, ist ein weiteres Eingehen darauf zum Verständnis der Erfindung nicht nötig.To carry out the procedure acc. The invention uses known techniques for the production of metal powders, the metal powder in the present case being powdered magnesium hydride or a powdered magnesium hydride mixture. The term "powdery magnesium hydride" also includes powdery magnesium hydride alloys of any quantitative and qualitative composition. Also with regard to the sintering of the powdered metal 1 hydride, techniques, process sequences and apparatuses and devices are used which are known in the prior art with regard to the processing and processing of metal powder and / or devices and equipment. Since that The method according to the invention makes extensive use of these known process techniques, so there is no need to go into further detail in order to understand the invention.
Zur Ausführung des Verfahrens gem. der Erfindung wird pul verförmiger Ausgangsstoff auf der Basis von pulver- förmigen Magnesiumhydrid verwendet, der zuvor geeignet hergestellt worden ist. Nach der Ausformung des Magnesiumhydrids zur Herstellung eines Erzeugnisses in eine solche Form, die nahezu der gewünschten Endform entspricht, was gleichermaßen auch für die Form eines herzustellenden gewünschten Halbzeuges gilt, wird der Wasserstoff aus dem Erzeugnis und/oder dem Halbzeug während des nachfolgenden Sintervorganges ausgetrieben.To carry out the procedure acc. The invention uses pulverulent starting material based on pulverulent magnesium hydride which has been suitably produced beforehand. After the magnesium hydride has been shaped to produce a product into a shape which almost corresponds to the desired final shape, which also applies to the shape of a desired semi-finished product to be produced, the hydrogen is expelled from the product and / or the semi-finished product during the subsequent sintering process.
Das Austreiben des Wasserstoffs kann unter Inertgas oder auch im Vakuum erfolgen und bei einer Temperatur unterhalb der Schmelztemperatur des jeweils gewählten pulver- förmigen Magnesiums bzw. seiner gewünschten Legierungen. Nachdem der Wasserstoff aus dem Erzeugnis bzw. dem Halbzeug ausgetrieben worden ist, wird das Erzeugnis bzw. das Halbzeug gesintert. Nach dem Sintervorgang liegt entweder ein Erzeugnis in Endform vor oder ein Halbzeug mit gewünschter Halbzeug-Endform.The hydrogen can be expelled under inert gas or in vacuo and at a temperature below the melting temperature of the respectively selected powdered magnesium or its desired alloys. After the hydrogen has been driven off from the product or the semifinished product, the product or the semifinished product is sintered. After the sintering process, either a finished product is available or a semi-finished product with the desired semi-finished product.
Diese Erzeugnisse bzw. Halbzeuge können dann mittels bekannter Be- bzw. Verarbeitungstechniken in eine Endform überführt werden.These products or semi-finished products can then be converted into a final shape using known machining or processing techniques.
Fig. 1 zeigt ein Röntgendiffrakto eterdi agramm einer Probe, die nach dem erfindungsgemäßen Verfahren hergestellt wurde. Die ausgeprägten Maxima stimmen mit den charakterischen Maxima für Magnesium überein. Damit wird nachgewiesen, daß der Wasserstoff aus der Probe ausge- trieben ist (keine MgH2-Phase in der Probe). Fig. 1 zeigt ferner, daß Magnesiumoxid nur noch in Spuren in der Probe vorhanden ist.1 shows an X-ray diffraction diagram of a sample which was produced by the method according to the invention. The pronounced maxima correspond to the characteristic maxima for magnesium. This proves that the hydrogen is removed from the sample. is driven (no MgH2 phase in the sample). Fig. 1 also shows that magnesium oxide is only present in traces in the sample.
Fig. 2 stellt einen Schliff der Probe in 110-facher Vergrößerung dar. Die Fig. 2 zeigt ferner, daß der Sinterprozeß erfolgt ist und die Probe an dichtes Gefüge aufweist. FIG. 2 shows a section of the sample in a magnification of 110 times. FIG. 2 also shows that the sintering process has taken place and that the sample has a dense structure.

Claims

Patentansprüche claims
1. Verfahren zum Herstellen von Erzeugnissen und/oder Halbzeugen aus pul erförmigen Ausgangsstoffen mittels Sintern auf der Basis von Magnesium und Magnesiumlegierungen, dadurch gekennzeichnet, daß der Ausgangsstoff in Form von Hydrid Magnesium und Magnesiumlegierungen verwendet wird.1. A method for producing products and / or semi-finished products from pul-shaped starting materials by means of sintering on the basis of magnesium and magnesium alloys, characterized in that the starting material is used in the form of hydride magnesium and magnesium alloys.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der Wasserstoff aus dem Erzeugnis und/oder dem Halbzeug während des oder nach der Durchführung des Sinterns ausgetrieben wird. 2. The method according to claim 1, characterized in that the hydrogen is expelled from the product and / or the semifinished product during or after the sintering.
3. Verfahren nach einem oder beiden der Ansprüche 1 oder 2, dadurch gekennzeichnet, daß das Sintern unter Inertgas durchgeführt wird.3. The method according to one or both of claims 1 or 2, characterized in that the sintering is carried out under inert gas.
4. Verfahren nach einem oder beiden der Ansprüche 1 oder 2, dadurch gekennzeichnet, daß das Sintern unter Vakuum ausgeführt wird.4. The method according to one or both of claims 1 or 2, characterized in that the sintering is carried out under vacuum.
5. Verfahren nach einem oder mehreren der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Sinterung des Erzeugnisses und/oder des Halbzeuges oberhalb der Dehydrierungstemperatur des Hydrids von Magnesium oder Magnesiumlegierungen erfolgt.5. The method according to one or more of claims 1 to 4, characterized in that the sintering of the product and / or the semi-finished product takes place above the dehydrogenation temperature of the hydride of magnesium or magnesium alloys.
mk/re mk / re
PCT/DE2002/004221 2001-12-27 2002-11-15 Powder-metallurgical production of magnesium bodies from magnesium hydride WO2003056046A1 (en)

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DE10163763.2 2001-12-27
DE10163763A DE10163763B4 (en) 2001-12-27 2001-12-27 Process for the manufacture of products such as components or semi-finished products from powdered materials based on magnesium or magnesium alloys

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006048076A1 (en) * 2004-11-04 2006-05-11 Gkss-Forschungszentrum Geesthacht Gmbh Method for producing metal components
DE102004053866A1 (en) * 2004-11-04 2006-05-11 Gkss-Forschungszentrum Geesthacht Gmbh Production of metal, especially magnesium (alloy), articles, by powder injection molding, by injecting mixture of metal (alloy) hydride powder and binder into mold
WO2006048075A2 (en) * 2004-11-04 2006-05-11 Gkss-Forschungszentrum Geesthacht Gmbh Method for the production of objects from a metallic composite material

Citations (4)

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Publication number Priority date Publication date Assignee Title
US2254549A (en) * 1938-11-12 1941-09-02 Small Louis Sintered metal composition
GB2019442A (en) * 1978-03-30 1979-10-31 Crucible Inc Method for producing powder metallurgy articles
US4560621A (en) * 1984-03-13 1985-12-24 The United States Of America As Represented By The United States Department Of Energy Porous metallic bodies
DE19827665A1 (en) * 1998-06-22 1999-12-23 Martin Kraemer Diamond-containing composite material used for grinding, drilling and cutting tools, wear resistant components and heat conducting elements

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2254549A (en) * 1938-11-12 1941-09-02 Small Louis Sintered metal composition
GB2019442A (en) * 1978-03-30 1979-10-31 Crucible Inc Method for producing powder metallurgy articles
US4560621A (en) * 1984-03-13 1985-12-24 The United States Of America As Represented By The United States Department Of Energy Porous metallic bodies
DE19827665A1 (en) * 1998-06-22 1999-12-23 Martin Kraemer Diamond-containing composite material used for grinding, drilling and cutting tools, wear resistant components and heat conducting elements

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006048076A1 (en) * 2004-11-04 2006-05-11 Gkss-Forschungszentrum Geesthacht Gmbh Method for producing metal components
DE102004053866A1 (en) * 2004-11-04 2006-05-11 Gkss-Forschungszentrum Geesthacht Gmbh Production of metal, especially magnesium (alloy), articles, by powder injection molding, by injecting mixture of metal (alloy) hydride powder and binder into mold
WO2006048075A2 (en) * 2004-11-04 2006-05-11 Gkss-Forschungszentrum Geesthacht Gmbh Method for the production of objects from a metallic composite material
WO2006048075A3 (en) * 2004-11-04 2006-06-08 Geesthacht Gkss Forschung Method for the production of objects from a metallic composite material

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DE10163763B4 (en) 2007-02-08

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