EP1249512B1 - Cold work steel for powder metallurgical production of parts - Google Patents

Cold work steel for powder metallurgical production of parts Download PDF

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Publication number
EP1249512B1
EP1249512B1 EP02450076A EP02450076A EP1249512B1 EP 1249512 B1 EP1249512 B1 EP 1249512B1 EP 02450076 A EP02450076 A EP 02450076A EP 02450076 A EP02450076 A EP 02450076A EP 1249512 B1 EP1249512 B1 EP 1249512B1
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Prior art keywords
powder
cold work
tool
work steel
weight
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EP02450076A
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German (de)
French (fr)
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EP1249512A1 (en
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Werner Dipl.Ing Liebfart
Roland Dipl.Ing Rabitsch
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Voestalpine Boehler Edelstahl GmbH
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Boehler Edelstahl GmbH
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Priority to SI200230445T priority Critical patent/SI1249512T1/en
Priority to AT02450076T priority patent/ATE340877T1/en
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/56—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.7% by weight of carbon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/24—Ferrous alloys, e.g. steel alloys containing chromium with vanadium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/26—Ferrous alloys, e.g. steel alloys containing chromium with niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/36—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.7% by weight of carbon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/46—Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
    • 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
    • B22F2009/0896—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 particle transport, separation: process and apparatus
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2241/00—Treatments in a special environment
    • C21D2241/01—Treatments in a special environment under pressure
    • C21D2241/02—Hot isostatic pressing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D7/00—Modifying the physical properties of iron or steel by deformation
    • C21D7/13—Modifying the physical properties of iron or steel by deformation by hot working

Definitions

  • the invention relates to a cold work steel alloy for powder metallurgy production of parts, in particular tools, with high toughness and hardness and resistance to wear and fatigue.
  • Tools and tool parts are usually claimed multilayered, which requires the same property profile of the same.
  • a creation of a particularly good suitability for a type of stress of the material is, however, naturally associated with a deterioration in the resistance of the same against other loads, so that for a high quality of service of a tool often several property characteristics should be at a high level, in other words, the performance characteristics of a tool
  • High performance tool steel components consistently have a hard phase portion of carbides and a matrix phase portion receiving them, which phases, particularly with respect to their proportions in the material, depend on the chemical composition of the alloy.
  • PM Powder metallurgical
  • production of materials essentially involves gas atomization or dicing of molten steel into fine droplets solidified to metal powder at a high rate of solidification, introduction and compression of the metal powder into a capsule Capping the capsule and heating and hot isostatic pressing (HIP) the powder in the capsule to a dense homogeneous material.
  • HIP hot isostatic pressing
  • Such PM material made can be used directly, as as-HIPed, for the manufacture of parts or tools or prior to hot working, e.g. by forging and / or rolling.
  • Highly stressed tools or parts e.g. Knives, punches and dies and the like require the same load resistance to abrasive wear, high toughness and fatigue resistance of the material.
  • Fatigue resistance which is essentially a failure to crack under very high swelling or alternating mechanical stress on the material, is again promoted by high matrix hardness and low crack initiation of carbide grains and non-metallic inclusions
  • the quality of use of parts or tools represents a compromise between wear resistance, toughness and fatigue resistance of the material in the thermally tempered state.
  • experts have long tried to increase the overall steel property profile.
  • the present invention is now the goal of the requirements To increase the mechanical characteristics in the thermally tempered state, namely the bending strength, the impact bending work and the wear resistance of the tool steel material quality assured at the same time.
  • the carbides should be essentially monocarbides with regard to wear resistance, distributed homogeneously in the matrix and be present with a diameter of less than 10 ⁇ m, preferably less than 4 ⁇ m.
  • Vanadium and niobium are the strongest carbide formers and, for alloying reasons, are to be provided together in a concentration range of 7.05 to 9.0% by weight V and 0.25 to 2.45% by weight Nb.
  • VNb advantageous mixed carbides
  • a formation of monocarbides and that of advantageous (VNb) mixed carbides is achieved, on the other hand is in these content ranges, founded by V and Nb, such a carbon affinity in the material, that the other carbide-forming elements chromium, tungsten and molybdenum in the inventive Concentrations with the residual carbon are available for solid solution strengthening and increase the matrix hardness.
  • the Pulverkomierenverander shall be procedurally adjusted such that at least 60% of the powder grains have a particle size of less than 100 microns (microns) in powder metallurgy production or in powder production.
  • a high solidification rate of the melt droplets associated with small metal powder particles has been found to provide a uniform distribution of fine monocarbides and a supersaturated base in the powder grain, in terms of carbon content.
  • the carbide morphology is controlled in terms of minimum defect size and the matrix composition in the direction of maximizing the secondary hardness potential, assuming the composition of the invention of the material. In this case, the importance of because again the intended niobium concentration of the regulated grain growth due to be mentioned.
  • a high-purity alloy is atomized by means of nitrogen with a purity of at least 99.999% nitrogen and a physisorption of oxygen at the powder surface is avoided until it is enclosed in a capsule, whereby the hipped material has an oxygen content of less than 100 ppm and a content and a configuration of non-metallic inclusions corresponding to a K0 value of at most 3 according to DIN 50 602 testing.
  • Table 1 shows the chemical composition of a cold work steel alloy according to the present invention (Leg. A) and those of the comparative alloys (B to J).
  • Table 2 shows the test results for transverse rupture strength, the impact bending work and the wear resistance of the alloy A according to the invention and of the comparative alloys B to J.
  • the pre-load F r was 200 N
  • the pre-load speed was 2 mm / min
  • the test speed was 5 mm / min.
  • the investigations of the impact bending work of the respective steel alloys were carried out.
  • the device for determining the wear resistance in a schematic representation can be removed.
  • the flexural strength of the alloy A according to the invention is compared with that of the comparative alloys (B to J) (Tab. 2), shown in a bar graph in FIG. 4, the alloys E, F, H and I each have uniformly high values. wherein the alloy I has the highest bending strength.
  • the alloy I has the highest value.
  • the measurement data of the alloy A according to the invention and the alloy F have slightly lower values for this mechanical property.

Description

Die Erfindung betrifft eine Kaltarbeitsstahllegierung zur pulvermetallurgischen Herstellung von Teilen, insbesondere Werkzeuge, mit hoher Zähigkeit und Härte sowie Beständigkeit gegen Verschleiß und Materialermüdung.The invention relates to a cold work steel alloy for powder metallurgy production of parts, in particular tools, with high toughness and hardness and resistance to wear and fatigue.

Werkzeuge und Werkgzeugteile werden in der Regel vielschichtig beansprucht, was ein dergleichen Eigenschaftsprofil derselben erfordert. Eine Erstellung einer besonders guten Eignung für eine Beanspruchungsart des Werkstoffes ist jedoch naturgemäß mit einer Verschlechterung der Beständigkeit desselben gegen andere Belastungen verbunden, so daß für eine hohe Gebrauchsgüte eines Werkzeuges vielfach mehrere Eigenschaftsmerkmale auf hohem Niveau vorliegen sollten, mit anderen Worten, die Gebrauchseigenschaften eines Werkzeuges stellen einen Kompromiß hinsichtlich der jeweilig einzelnen Materialwerte dar. Aus wirtschaftlichen Gründen besteht jedoch allgemein der Wunsch, Werkzeuge oder Teile mit in der Gesamtheit verbesserten Materialeigenschaften verfügbar zu haben.Tools and tool parts are usually claimed multilayered, which requires the same property profile of the same. A creation of a particularly good suitability for a type of stress of the material is, however, naturally associated with a deterioration in the resistance of the same against other loads, so that for a high quality of service of a tool often several property characteristics should be at a high level, in other words, the performance characteristics of a tool However, for economic reasons, there is a general desire to have available tools or parts having improved overall material properties.

Hochleistungswerkzeugstahlkomponenten besitzen durchwegs einen Hartphasenanteil aus Karbiden und einen diese aufnehmenden Matrixphasenteil, welche Phasen insbesondere hinsichtlich deren Anteile im Werkstoff von der chemischen Zusammensetzung der Legierung abhängen.High performance tool steel components consistently have a hard phase portion of carbides and a matrix phase portion receiving them, which phases, particularly with respect to their proportions in the material, depend on the chemical composition of the alloy.

Bei einer konventionellen Herstellung mit einer Erstarrung der Legierung in Gießformen ist deren jeweiliger Gehalt an Kohlenstoff und karbidbildenden Elementen auf Grund der Erstarrungskinetik begrenzt, weil bei hohen Gehalten die primär aus der Schmelze ausgeschiedenen Karbide eine grobe inhomogene Materialstruktur bewirken, dadurch schlechte mechanische Eigenschaften begründen und eine Verarbeitbarkeit des Werkstoffes nachteilig beeinflussen oder letztlich ausschließen.In a conventional production with a solidification of the alloy in casting molds their respective content of carbon and carbide-forming elements is limited due to the solidification kinetics, because at high levels, the primary excreted from the melt carbides cause a coarse inhomogeneous material structure, thereby creating poor mechanical properties and a Processability of the material adversely affect or ultimately exclude.

Um einerseits die Konzentrationen der karbidbildenden Elemente und den Kohlenstoffanteil im Hinblick auf einen erhöhten Karbidanteil und somit eine verbesserte Verschleißbeständigkeit des Werkstoffes steigern zu können, andererseits jedoch eine ausreichende Verarbeitbarkeit, Homogenität und Zähigkeit der daraus gefertigten Teile oder Werkzeuge sicherzustellen, ist eine pulvermetallurgische Herstellung derselben vorzusehen.On the one hand to be able to increase the concentrations of the carbide-forming elements and the carbon content with regard to an increased carbide content and thus an improved wear resistance of the material, On the other hand, however, to ensure sufficient processability, homogeneity and toughness of the parts or tools made therefrom, a powder metallurgy production thereof is provided.

Eine pulvermetallurgische (PM) Herstellung von Werkstoffen beinhaltet im wesentlichen ein Gas- bzw. Stickstoff-Verdüsen oder Zerteilen einer Stahlschmelze in feine Tröpfchen, die mit hoher Erstarrungsgeschwindigkeit zu Metallpulver verfestigt werden, ein Einbringen und Verdichten des Metallpulvers in eine bzw. einer Kapsel, ein Verschließen der Kapsel und ein Erwärmen sowie heißisostatisches Pressen (HIP) des Pulvers in der Kapsel zu einem dichten homogenen Material. Ein derartig erstelltes PM-Material kann direkt, als as-HIPed, zur Fertigung von Teilen oder Werkzeugen eingesetzt oder vorher einer Warmumformung, z.B. durch Schmieden und/oder Walzen, unterworfen werden.Powder metallurgical (PM) production of materials essentially involves gas atomization or dicing of molten steel into fine droplets solidified to metal powder at a high rate of solidification, introduction and compression of the metal powder into a capsule Capping the capsule and heating and hot isostatic pressing (HIP) the powder in the capsule to a dense homogeneous material. Such PM material made can be used directly, as as-HIPed, for the manufacture of parts or tools or prior to hot working, e.g. by forging and / or rolling.

Hochbeanspruchte Werkzeuge oder Teile, z.B. Messer, Stanzstempel sowie Matrizen und dergleichen erfordern belastungsgemäß gleichzeitig Beständigkeit gegen abrasiven Verschleiß, hohe Zähigkeit und Ermüdungsbeständigkeit des Werkstoffes. Zur Verschleißerniedrigung ist ein hoher Anteil an harten, gegebenenfalls groben, Karbiden, vorzugsweise Monokarbide, anzustreben, wobei jedoch die Materialzähigkeit mit steigendem Karbidanteil erniedrigt wird. Die Ermüdungsbeständigkeit, das ist im wesentlichen ein Ausbleiben der Rißbildung bei sehr hoher schwellender oder wechselnder mechanischer Beanspruchung des Materials, wird wiederum durch eine hohe Matrixhärte und geringe Rißinitiation von Karbidkörnern und nichtmetallischen Einschlüssen gefördertHighly stressed tools or parts, e.g. Knives, punches and dies and the like require the same load resistance to abrasive wear, high toughness and fatigue resistance of the material. To reduce wear, a high proportion of hard, possibly coarse, carbides, preferably monocarbides, to strive for, but the material toughness is lowered with increasing carbide content. Fatigue resistance, which is essentially a failure to crack under very high swelling or alternating mechanical stress on the material, is again promoted by high matrix hardness and low crack initiation of carbide grains and non-metallic inclusions

Die Gebrauchsgüte von Teilen oder Werkzeugen stellt einen Kompromiß zwischen Verschleißbeständigkeit, Zähigkeit und Ermüdungsbeständigkeit des Werkstoffes im thermisch vergüteten Zustand dar. Im Sinne einer allgemeinen Anhebung der Qualität von Kaltarbeitsstählen wurde seit langem in der Fachwelt versucht, das Stahl- Eigenschaftsprofil insgesamt zu steigern.The quality of use of parts or tools represents a compromise between wear resistance, toughness and fatigue resistance of the material in the thermally tempered state. In order to generally raise the quality of cold work steels, experts have long tried to increase the overall steel property profile.

Die vorliegende Erfindung setzt sich nun zum Ziel, den Erfordernissen Rechnung tragend, die mechanischen Kennwerte im thermisch vergüteten Zustand und zwar die Biegebruchfestigkeit, die Schlagbiegearbeit und den Verschleißwiderstand des Werkzeugstahlwerkstoffes gütegesichert gleichzeitig zu erhöhen.The present invention is now the goal of the requirements To increase the mechanical characteristics in the thermally tempered state, namely the bending strength, the impact bending work and the wear resistance of the tool steel material quality assured at the same time.

Dieses Ziel wird erfindungsgemäß bei einem Teil oder Werkzeug mit hoher Zähigkeit und Härte sowie Beständigkeit gegen Verschleiß und Materialermüdung aus einer pulvermetallurgisch hergestellten Kaltarbeitstahllegierung enthaltend in Gew.-% Kohlenstoff (C) 2,05 bis 2,65 Silizium (Si) bis 2,0 Mangan (Mn) bis 2,0 Chrom (Cr) 6,10 bis 9,80 Wolfram (W) 0,50 bis 2,40 Molybdän (Mo) 2,15 bis 4,70 Vanadin (V) 7,05 bis 9,0 Niob (Nb) 0,25 bis 2,45 Kobalt (Co) bis 10,0 Schwefel (S) bis 0,3 Stickstoff (N) 0,04 bis 0,22 Nickel (Ni) bis 1,50 sowie herstellungsbedingte Verunreinigungen mit Eisen (Fe) als Rest, welcher Teil einen Gehalt an Sauerstoff (O) von kleiner als 100 ppm und einen Gehalt und eine Konfiguration von nichtmetallischen Einschlüssen entsprechend einem K0-Wert von höchstens 3 gemäß Prüfung nach DIN 50 602 sowie gleichmäßig verteilete Monokarbide mit einer Größe von unter 10 µm aufweist, erreicht.This object is achieved according to the invention in a part or tool with high toughness and hardness as well as resistance to wear and fatigue of a cold work steel alloy produced by powder metallurgy and containing in% by weight. Carbon (C) 2.05 to 2.65 Silicon (Si) to 2.0 Manganese (Mn) to 2.0 Chrome (Cr) 6.10 to 9.80 Tungsten (W) 0.50 to 2.40 Molybdenum (Mo) 2.15 to 4.70 Vanadin (V) 7.05 to 9.0 Niobium (Nb) 0.25 to 2.45 Cobalt (Co) to 10.0 Sulfur (S) to 0.3 Nitrogen (N) 0.04 to 0.22 Nickel (Ni) to 1.50 as well as production-related impurities with iron (Fe) as the remainder, which part has a content of oxygen (O) of less than 100 ppm and a content and a configuration of non-metallic inclusions corresponding to a K0 value of at most 3 according to DIN 50 602 as well as uniform distributed monocarbides having a size of less than 10 microns achieved.

Die erheblichen Güteverbesserungen des Werkstoffes nach der Erfindung werden synergetisch durch legierungstechnische und verfahrenstechnologische Maßnahmen im Hinblick auf die Optimierung der Gefügestruktur sowie Einzel- und Summeneigenschaften der Gefügephasen erreicht.The significant quality improvements of the material according to the invention are achieved synergistically by alloying and procedural measures with regard to the optimization of the microstructure and individual and sum properties of the structural phases.

Es wurde erkannt, daß nicht alleine die Karbidmenge sondern bei gleicher Menge die Karbidmorphologie für die Zähigkeit des Werkstoffes von Bedeutung ist, weil diese von der freien Weglänge zwischen den Karbiden in der Matrix, also der Defektgröße, abhängt. Im fertigen zum Einsatz bestimmten Werkzeug sollen die Karbide im Hinblick auf die Verschleißfestigkeit im wesentlichen Monokarbide sein, homogen in der Matrix verteilt und mit einem Durchmesser von kleiner als 10µm, vorzugsweise kleiner 4 µm, vorliegen.It was recognized that not only the amount of carbide but at the same amount, the carbide morphology for the toughness of the material of importance, because this depends on the free path between the carbides in the matrix, ie the defect size. In the finished tool intended for use, the carbides should be essentially monocarbides with regard to wear resistance, distributed homogeneously in the matrix and be present with a diameter of less than 10 μm, preferably less than 4 μm.

Vanadin und Niob sind die stärksten Karbidbildner und sind aus legierungstechnischen Gründen gemeinsam in einem Konzentrationsbereich von jeweils 7,05 bis 9,0 Gew.-% V und 0,25 bis 2,45 Gew.-% Nb vorzusehen. Dadurch wird einerseits eine Bildung von Monokarbiden und zwar von vorteilhaften (VNb)-Mischkarbiden erreicht, andererseits liegt in diesen Gehaltsbereichen, von V und Nb begründet, eine derartige Kohlenstoffaffinität im Werkstoff vor, daß die weiteren karbidbildenden Elemente Chrom, Wolfram und Molybdän in den erfindungsgemäßen Konzentrationen mit dem Restkohlenstoff zur Mischkristallverfestigung zur Verfügung stehen und die Matrixhärte erhöhen. Höhere Vanadin und/oder Niobgehalte als 9,0 bzw. 2,45 Gew.-% wirken erniedrigend auf die Matrixfestigkeit und vermindern insbesondere die Ermüdungsbeständigkeit des Materials, wohingegen geringere Gehalte als 7,05 Gew.-% V und/oder 0,25 Gew.-% Nb zur vermehrten Ausbildung von weicheren Karbidphasen wie M7C3- Karbiden führen, wodurch die Verschleißfestigkeit des Stahles erniedrigt wird.Vanadium and niobium are the strongest carbide formers and, for alloying reasons, are to be provided together in a concentration range of 7.05 to 9.0% by weight V and 0.25 to 2.45% by weight Nb. On the one hand, a formation of monocarbides and that of advantageous (VNb) mixed carbides is achieved, on the other hand is in these content ranges, founded by V and Nb, such a carbon affinity in the material, that the other carbide-forming elements chromium, tungsten and molybdenum in the inventive Concentrations with the residual carbon are available for solid solution strengthening and increase the matrix hardness. Higher vanadium and / or niobium contents than 9.0 and 2.45 wt%, respectively, have a degrading effect on matrix strength and, in particular, reduce the fatigue life of the material, whereas lower than 7.05 wt% V and / or 0.25 % By weight of Nb lead to increased formation of softer carbide phases such as M 7 C 3 carbides, which reduces the wear resistance of the steel.

Bei einem Kohlenstoffgehalt in dem engen Bereich von 2,05 bis 2,65 Gew.-% und den erfindungsgemäßen Konzentrationen der Monokarbidbildner können insbesondere durch 0,5 bis 2,4 Gew.-% Wolfram und 2,15 bis 4,70 Gew.-% Molybdän das Sekundärhärtepotential der Legierung beim thermischen Vergüten ausgeschöpft und die Anlaßbeständigkeit derselben verbessert werden. Für eine Mischkristallverfestigung ist Chrom mit Gehalten von 6,10 bis 9,80 Gew.-% vorgesehen, wobei zur Erhöhung der Sekundärhärte und der Matrixhärte des Werkzeugstahles Stickstoff mit einem Anteil von 0,04 bis 0,22 Gew.-% erfindungswesentlich ist.With a carbon content in the narrow range of 2.05 to 2.65 wt .-% and the concentrations of monocarbide according to the invention can in particular by 0.5 to 2.4 wt .-% tungsten and 2.15 to 4.70 wt. -% molybdenum exhausted the secondary hardening potential of the alloy during thermal quenching and the tempering resistance of the same can be improved. For a solid solution hardening chromium is provided with contents of 6.10 to 9.80 wt .-%, wherein to increase the secondary hardness and the matrix hardness of the tool steel nitrogen in a proportion of 0.04 to 0.22 wt .-% is essential to the invention.

Höhere, aber auch niedrigere Gehalte als die jeweils in den erfindungsgemäßen Grenzen für die Elemente Wolfram, Molybdän und Chrom angegeben sind, stören die Synergie und vermindern zumindest eine Eigenschaft des Werkzeugstahles, können also zum Teil dessen Verwendbarkeit nachteilig beeinflussen.Higher, but also lower contents than those indicated in the limits according to the invention for the elements tungsten, molybdenum and chromium, disturb the synergy and reduce at least one property of the tool steel, so can partially adversely affect its usability.

Wie eingangs erwähnt, sind für einen Erhalt hoher Gebrauchsgüte eines Teiles oder des Werkzeuges neben den legierungstechnischen Voraussetzungen auch die herstellungstechnologischen Maßnahmen wesentlich.Weil nun im Sinne hoher Materialzähigkeit eine örtliche Häufung von gegebenenfalls gröberen Karbiden, eine sogenannte Karbid- Clusterbildung, im heißisostatisch gepreßten Material einer Defektgrößenminimierung wegen zu vermeiden ist, soll bei der pulvermetallurgischen Herstellung bzw. bei der Pulvererzeugung die Pulverkomgrößenverteilung verfahrenstechnisch derart eingestellt werden, daß mindestens 60 % der Pulverkörner eine Partikelgröße von weniger als 100 Mikron (µm) aufweisen. Eine mit kleinen Metallpulverteilchen verbundene hohe Erstarrungsgeschwindigkeit der Schmelzentröpfchen bewirkt, wie gefunden wurde, eine gleichmäßige Verteilung feiner Monokarbide und eine, den Kohlenstoffgehalt betreffend, übersättigte Grundmasse im Pulverkorn.As mentioned above, in addition to the alloying technical prerequisites for obtaining high quality of service of a part or tool Wesent.Weil now in terms of high material toughness a local accumulation of possibly coarser carbides, a so-called carbide clustering in the hot isostatically pressed material Defect size minimization is to be avoided, the Pulverkomgrößenverteilung shall be procedurally adjusted such that at least 60% of the powder grains have a particle size of less than 100 microns (microns) in powder metallurgy production or in powder production. A high solidification rate of the melt droplets associated with small metal powder particles has been found to provide a uniform distribution of fine monocarbides and a supersaturated base in the powder grain, in terms of carbon content.

Während des heißisostatischen Pressens und während einer gegebenenfalls vorgesehenen Warmverformung des Preßlings verringert sich, begründet durch die Diffusion bei hoher Temperatur, der Übersättigungsgrad der Grundmasse, die feinen runden Monokarbide wachsen gewünscht bis zu einer Größe von weniger als 10 um, wobei die weiteren Legierungselemente sich gezielt weitgehend in den Mischkristall einlagern und letztlich die Matrix verfestigen. Durch diese Herstelltechnologie wird die Karbidmorphologie im Hinblick auf geringste Defektgröße und die Matrixzusammensetzung in Richtung auf eine Maximierung des Sekundärhärtepotentials unter Voraussetzung der erfindungsgemäßen Zusammensetzung des Werkstoffes gesteuert. Dabei soll der Wichtigkeit wegen nochmals die vorgesehene Niobkonzentration des geregelten Kornwachstums wegen erwähnt werden.During the hot isostatic pressing and during a possibly provided hot deformation of the compact, due to the diffusion at high temperature, the supersaturation degree of the matrix decreases, the fine round monocarbides grow to a size of less than 10 .mu.m, whereby the further alloying elements are targeted largely store in the mixed crystal and ultimately solidify the matrix. By this manufacturing technology, the carbide morphology is controlled in terms of minimum defect size and the matrix composition in the direction of maximizing the secondary hardness potential, assuming the composition of the invention of the material. In this case, the importance of because again the intended niobium concentration of the regulated grain growth due to be mentioned.

Von besonderer Bedeutung ist der oxidische Reinheitsgrad des erfindungsgemäßen Werkstoffes, weil durch nichtmetallische Einschlüsse nicht nur dessen mechanische Eigenschaften verschlechtert werden können, sondern es können auch durch diese Nichtmetalle nachteilige Ankeimungseffekte bei der Erstarrung und Wärmebehandlung des Materials entstehen. Es ist also erfindungswesentlich, daß eine hochreine Legierung mittels Stickstoffes mit einem Reinheitsgrad von mindestens 99,999% Stickstoff verdüst und eine Physisorption von Sauerstoff an der Pulverkomoberfläche bis zum Einschließen in eine Kapsel vermieden wird, wodurch der gehipte Werstoff einen Sauerstoffgehalt von kleiner 100 ppm und einen Gehalt und eine Konfiguration von nichtmetallischen Einschlüssen entsprechend einem K0-Wert von höchstens 3 gemäß Prüfung nach DIN 50 602 aufweist.Of particular importance is the oxidic purity of the material according to the invention, because not only its mechanical properties can be deteriorated by non-metallic inclusions, but it can also by these Non-metals disadvantageous germination effects occur during the solidification and heat treatment of the material. It is therefore essential to the invention that a high-purity alloy is atomized by means of nitrogen with a purity of at least 99.999% nitrogen and a physisorption of oxygen at the powder surface is avoided until it is enclosed in a capsule, whereby the hipped material has an oxygen content of less than 100 ppm and a content and a configuration of non-metallic inclusions corresponding to a K0 value of at most 3 according to DIN 50 602 testing.

Bevorzugte Ausführungsformen sind in den Unteransprüchen gekennzeichnet. Anhand von Ergebnissen aus vergleichenden Untersuchungen soll die Erfindung näher erläutert werden.
Es zeigen
Tab. 1 Die chemische Zusammensetzung der erfindungsgemäßen und Vergleichs-Stahllegierungen.
Tab.2 Meßwerte, ermittelt bei der mechanischen Prüfung der Stahllegierungen

  • Fig. 1 Meßanordnung zur Ermittlung der Biegebruchfestigkeit
  • Fig. Probenform für die Feststellung der Schlagbiegearbeit
  • Fig. 3 Vorrichtung zur Messung des Verschleißwiderstandes (schematisch)
  • Fig. 4 Gegenüberstellung der Biegebruchfestigkeit der Stahllegierungen
  • Fig. 5 Gegenüberstellung der Schlagbiegearbeit
  • Fig. 6 Gegenüberstellung des jeweiligen Verschleißwiderstandes der Stahllegierungen
Preferred embodiments are characterized in the subclaims. Based on results from comparative investigations, the invention will be explained in more detail.
Show it
Tab. 1 The chemical composition of the inventive and comparative steel alloys.
Tab.2 Measured values determined during mechanical testing of the steel alloys
  • Fig. 1 measuring arrangement for determining the bending strength
  • Fig. Sample shape for determining the impact bending work
  • 3 device for measuring the wear resistance (schematically)
  • Fig. 4 Comparison of the bending strength of the steel alloys
  • Fig. 5 Comparison of the impact bending work
  • Fig. 6 Comparison of the respective wear resistance of the steel alloys

Aus der Tabelle 1 ist die chemische Zusammensetzung einer erfindungsgemäßen Kaltarbeitsstahllegierung (Leg. A) und jene der Vergleichslegierungen (B bis J) ersichtlich.Table 1 shows the chemical composition of a cold work steel alloy according to the present invention (Leg. A) and those of the comparative alloys (B to J).

In Tabelle 2 sind die Erprobungsergebnisse für Biegebruchfestigkeit, die Schlagbiegearbeit und den Verschleißwiderstand der erfindungsgemäßen Legierung A und der Vergleichslegierungen B bis J angegeben.Table 2 shows the test results for transverse rupture strength, the impact bending work and the wear resistance of the alloy A according to the invention and of the comparative alloys B to J.

Die Biegebruchfestigkeit der Stahllegierungen wurde an auf 61 HRC vergüteten Rundproben (Rd = 5,0 mm) in einer Einrichtung gemäß Fig. 1 ermittelt. Die Vorkraft Fr betrug 200 N, die Geschwindigkeit bis zur Vorkraft war 2 mm/min und die Prüfgeschwindigkeit betrug 5 mm/min.
An Proben mit der Form gemäß Fig. 2 erfolgten die Untersuchungen der Schlagbiegearbeit der jeweiligen Stahllegierungen.The flexural strength of the steel alloys was tempered to 61 HRC Round samples (R d = 5.0 mm) determined in a device according to FIG. The pre-load F r was 200 N, the pre-load speed was 2 mm / min and the test speed was 5 mm / min.
On samples with the shape of FIG. 2, the investigations of the impact bending work of the respective steel alloys were carried out.

Aus Fig. 3 ist die Einrichtung zur Ermittlung des Verschleißwiderstandes in schematischer Darstellung entnehmbar.From Fig. 3, the device for determining the wear resistance in a schematic representation can be removed.

Wird nun die Biegebruchfestigkeit der erfindungsgemäßen Legierung A jener der Vergleichslegierungen (B bis J) (Tab. 2), in einer Balkendarstellung gezeigt in Fig. 4, gegenübergestellt, so weisen die Legierungen E, F, H und I jeweils gleichmaßen hohe Werte auf, wobei die Legierung I die höchste Biegebruchfestigkeit besitzt.If the flexural strength of the alloy A according to the invention is compared with that of the comparative alloys (B to J) (Tab. 2), shown in a bar graph in FIG. 4, the alloys E, F, H and I each have uniformly high values. wherein the alloy I has the highest bending strength.

Bei einem Vergleich der jeweiligen Schlagbiegearbeit (Fig. 5) der Kaltarbeitsstahllegierungen besitzt wiederum die Legierung I den höchsten Wert. Die Meßdaten der erfindungsgemäßen Legierung A und der Legierung F weisen geringfügig niedrigere Werte für diese mechanische Eigenschaft auf.In a comparison of the respective impact bending work (Fig. 5) of the cold work steel alloys in turn, the alloy I has the highest value. The measurement data of the alloy A according to the invention and the alloy F have slightly lower values for this mechanical property.

Die Ergebnisse der Untersuchungen des Verschleißwiderstandes der Legierungen sind in graphischer Darstellung in Fig. 6 gegenübergestellt,, wobei für die Legierung H und die erfindungsgemäße Legierung A die höchsten Werte ermittelt wurden.The results of the investigations of the wear resistance of the alloys are compared in a graph in FIG. 6, the highest values being determined for the alloy H and the alloy A according to the invention.

Aus den Ergebnissen der Untersuchungen ist entnehmbar, daß die wichtigen Eigenschaftsmerkmale, Biegebruchfestigkeit, Schlagbiegearbeit und Verschleißwiderstand einer erfindungsgemäßen Kaltarbeitsstahllegierung sich gleichermaßen auf hohem Niveau befinden und diese neue Legierung auszeichnen. Tabelle 1 Gew.-% Leg. A* Leg. B Leg. C Leg. D Leg. E Leg. F Leg. G Leg. H Leg. I Leg. J C 2,44 2,55 2,49 2,42 2,61 2,63 2,52 2,44 2,49 2,30 Si 0,98 1,05 0,95 1,12 0,97 1,13 0,87 0,94 0,63 0,32 Mn 0,52 0,53 0,49 0,55 0,66 0,71 0,55 0,50 0,32 0,31 Cr 6,22 6,93 6,12 6,27 6,08 6,21 6,28 5,66 4,19 12,31 W 1,41 0,95 2,74 1,30 1,06 1,50 2,22 0,05 3,68 0,35 Mo 3,98 3,95 3,78 4,00 3,60 3,98 5,05 1,31 3,21 1,17 V 8,12 7,85 7,92 7,88 6,77 7,83 8,20 9,84 8,72 3,94 Nb 1,19 1,15 1,12 1,86 1,45 0,61 0,9 0,01 -- ― S 0.008 0,011 0,03 0,012 0,028 0,009 0,039 0,07 0,01 0,013 N 0.095 0,08 0,064 ― ― 0,09 0,06 0,075 0,038 0,13 Co 0,4 <0.1 ― ― <0,1 0,13 0,038 -- ― 0,04 Nl 0,7 0,43 0,17 0,28 0,89 0,51 0,76 ― 0,36 -- O 0,0091 0,032 ― ― 0,041 0,068 0,044 ― 0,054 0,0098 * Leg. A = erfindungsgemäße Legierung

Figure imgb0001
It can be seen from the results of the investigations that the important property features, bending strength, impact bending work and wear resistance of a cold work steel alloy according to the invention are equally at a high level and distinguish this new alloy. <b><u> Table 1 </ u></b> Wt .-% Leg. A * Leg. B Leg. C Leg. D Leg. e Leg. F Leg. G Leg. H Leg. I Leg. J C 2.44 2.55 2.49 2.42 2.61 2.63 2.52 2.44 2.49 2.30 Si 0.98 1.05 0.95 1.12 0.97 1.13 0.87 0.94 0.63 0.32 Mn 0.52 0.53 0.49 0.55 0.66 0.71 0.55 0.50 0.32 0.31 Cr 6.22 6.93 6.12 6.27 6.08 6.21 6.28 5.66 4.19 12.31 W 1.41 0.95 2.74 1.30 1.06 1.50 2.22 0.05 3.68 0.35 Not a word 3.98 3.95 3.78 4.00 3.60 3.98 5.05 1.31 3.21 1.17 V 8.12 7.85 7.92 7.88 6.77 7.83 8.20 9.84 8.72 3.94 Nb 1.19 1.15 1.12 1.86 1.45 0.61 0.9 0.01 - - S 0008 0.011 0.03 0,012 0.028 0.009 0,039 0.07 0.01 0,013 N 0095 0.08 0.064 - - 0.09 0.06 0,075 0,038 0.13 Co 0.4 <0.1 - - <0.1 0.13 0,038 - - 0.04 nl 0.7 0.43 0.17 0.28 0.89 0.51 0.76 - 0.36 - O 0.0091 0.032 - - 0,041 0,068 0,044 - 0.054 0.0098 Leg. A = alloy according to the invention
Figure imgb0001

Claims (5)

  1. Part or tool of high tenacity and hardness as well as resistance against wear and material fatigue from a powder metallurgically produced cold work steel, which comprises in % by weight carbon (C) 2.05 up to 2.65 silicone (Si) up to 2.0 manganese (Mn) up to 2.0 chromium (Cr) 6.10 up to 9.80 tungsten (W) 0.50 up to 2.40 molybdenum (Mo) 2.15 up to 4.70 vanadium (V) 7.05 up to 9.0 niobium (Nb) 0.25 up to 2.45 cobalt (Co) up to 10.0 sulphur (S) up to 0.3 nitrogen (N) 0.04 up to 0.22 nickel (Ni) up to 1.50
    as well as impurities conditional to production, iron (Fe) being the remainder, which part comprises a content of oxygen (O) smaller than 100 ppm, and a content and a configuration of non-metallic inclusions corresponding to a K0 value of 3 in maximum according to a test in accordance with DIN 50 602, as well as evenly distributed monocarbides having a size of below 10 µm.
  2. Part or tool of a PM-cold work steel according to claim 1, which comprises one or more element(s) of the following concentration value(s) in % by weight C 2.30 up to 2.59 Si 0.80 up to 1.50 Mn 0.30 up to 1.40 Cr 6.12 up to 7.50 Ni up to 1.0 W 0.60 up to 1.45 Mo 2.40 up to 4,40 V 7.40 up to 8.70 Nb 0.50 up to 1.95 N 0.06 up to 0.22
    while the value of (Mn-S) amounts at least to 0.19.
  3. Part or tool of a PM-cold work steel according to claim 1 or 2, which comprises one or more element(s) of the following concentration value(s) in % by weight Si 0.85 up to 1.30 Mn 0.40 up to 0.80 Cr 6.15 up to 6.95 Ni up to 0.90 Mo 3.55 up to 4.40 V 7.80 up to 8.59 Nb 0.75 up to 1.45 N 0.06 up to 0.15
  4. A method for powder metallurgical production of a part or a tool from a cold work steel, which comprises in % by weight C 2.05 up to 2.65 Si up to 2.0 Mn up to 2.0 Cr 6.10 up to 9.80 W 0.50 up to 2.40 Mo 2.15 up to 4.70 V 7.05 up to 9.0 Nb 0.25 up to 2.45 Co up to 10.0 S up to 0.3 N 0.04 up to 0.22 Ni up to 1.50
    according to any of the preceding claims, wherein the liquid alloy is conditioned, and is pulverized by nitrogen of a percentage purity of 99.999% to form a metal powder having a grain size distribution of at least 60% with a particle size of equal to/smaller than 100 micron (µm), after which filling the powder into a capsule, while maintaining the nitrogen atmosphere and eliminating any physisorption of oxygen at the grain surfaces, and closing it, and the powder is processed to a perfectly dense material by a high-temperature isostatic compression procedure, optionally with subsequent hot deformation.
  5. Method according to claim 4, wherein growth of the uniformly distributed monocarbides is adjusted to a size of below 10 µm by temperature control during hot deformation.
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AR034306A1 (en) 2004-02-18
EP1249512A1 (en) 2002-10-16
TW589388B (en) 2004-06-01
CA2381508C (en) 2006-11-28
US20030068248A1 (en) 2003-04-10
BR0202148B1 (en) 2010-11-16
RU2221069C1 (en) 2004-01-10
BR0202148A (en) 2003-06-10
HK1051879A1 (en) 2003-08-22
ATA5872001A (en) 2002-09-15
CA2381508A1 (en) 2002-10-11
CN1164787C (en) 2004-09-01
KR20020080263A (en) 2002-10-23
AT410448B (en) 2003-04-25
ES2272662T3 (en) 2007-05-01
US6773482B2 (en) 2004-08-10
DE50208230D1 (en) 2006-11-09
DK1249512T3 (en) 2007-02-05
KR100476505B1 (en) 2005-03-17
CN1382825A (en) 2002-12-04

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