EP0255005B1 - Procédé et appareil pour la fabrication de matériaux métalliques par compression isostatique à chaud de poudre métallique - Google Patents

Procédé et appareil pour la fabrication de matériaux métalliques par compression isostatique à chaud de poudre métallique Download PDF

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Publication number
EP0255005B1
EP0255005B1 EP87110429A EP87110429A EP0255005B1 EP 0255005 B1 EP0255005 B1 EP 0255005B1 EP 87110429 A EP87110429 A EP 87110429A EP 87110429 A EP87110429 A EP 87110429A EP 0255005 B1 EP0255005 B1 EP 0255005B1
Authority
EP
European Patent Office
Prior art keywords
pressure
reaction gas
metal powder
gas
capsule
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.)
Expired - Lifetime
Application number
EP87110429A
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German (de)
English (en)
Other versions
EP0255005A2 (fr
EP0255005A3 (en
Inventor
Heinrich K. Prof. Dr.-Ing. Feichtinger
Markus O. Prof. Dr. Speidel
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.)
Vereinigte Schmiedewerke GmbH
Original Assignee
Vereinigte Schmiedewerke GmbH
Schmiedewerke Krupp Kloeckner GmbH
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Application filed by Vereinigte Schmiedewerke GmbH, Schmiedewerke Krupp Kloeckner GmbH filed Critical Vereinigte Schmiedewerke GmbH
Priority to AT87110429T priority Critical patent/ATE56380T1/de
Publication of EP0255005A2 publication Critical patent/EP0255005A2/fr
Publication of EP0255005A3 publication Critical patent/EP0255005A3/de
Application granted granted Critical
Publication of EP0255005B1 publication Critical patent/EP0255005B1/fr
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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
    • 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
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing

Definitions

  • the invention relates to a method for producing metallic materials by hot isostatic pressing of metal powder or metal powder mixtures, collectively referred to as "metal powder", with high, in particular over 1%, contents of gases or vapors, in particular nitrogen, which are caused by pressurizing the metal powder with pressurized metal Reaction gas can be introduced into the material at a higher temperature.
  • the invention also includes an apparatus for performing this method.
  • Nitrogen is a substitution element and can partially replace other alloying elements, for example nickel. Nitrogen is an austenite stabilizing element.
  • nitride-forming elements such as chromium, vanadium, niobium, zirconium can also lead to the elimination of nitride phases, which have a favorable effect on the mechanical properties via the mechanism of precipitation hardening .
  • this effect can also have an effect on improving the creep resistance in the higher temperature range.
  • Highly embroidered steels can be produced using a melt metallurgical process. Steels whose nitrogen content is so low that bubbles do not form during solidification can also be melted with conventional melting units, such as the electric arc furnace or the induction furnace.
  • the nitrogen is added in the form of a nitrogen-containing ferro alloy, such as ferrochrome or ferromanganese.
  • ferrochrome or ferromanganese Such special ferro alloys are, however, very expensive. Therefore, this melt-metallurgical route for the production of embroidered steels is relatively expensive.
  • this remelting process creates a primary structure which, while having the advantages inherent in the electroslag remelting process, has a particularly high quality, but nevertheless still certain It has disadvantages with regard to inhomogeneities, as is common to all melt metallurgical processes with regard to micro and macro segregation, blowholes, pores and other defects.
  • the final material properties can possibly only be achieved by a thermomechanical aftertreatment, and the final shape, for example in the case of cap rings, can only be achieved by extensive machining.
  • Materials with high nitrogen contents can also be produced by powder metallurgy, for example by hot isostatic pressing.
  • This process is described for example in "Encyclopedia of Materials Science and Engineering", vol. 3, 1986, page 2186.
  • the metal powder to be pressed is filled into a deformable capsule, the air is sucked out of the capsule, the capsule and its contents are heated to an elevated temperature, and at the same time pressure is applied to all sides via a suitable medium, in particular gas exerted on the capsule and the metal powder contained therein.
  • a suitable medium in particular gas exerted on the capsule and the metal powder contained therein.
  • the powder is compacted into a compact body, with the elevated temperature causing a sintering process with solid-state diffusion, sometimes even in the presence of a liquid phase.
  • CH-PS 486 563 describes a process for producing a heat-resistant material in which a powder mixture consisting of a component A (iron, cobalt or nickel) with a component B (nitride or nitride mixture) and a component C (reactive tionable aluminum compound) is subjected to a pressure sintering process.
  • the powder components must be in a fine and homogeneous distribution. It is preferred if the individual components are present in a grain spectrum of 1-10 11 m.
  • the resulting metal-ceramic materials are hard, strong and resistant to chemicals, thermal shock and high temperature.
  • EP-OS 165 732 describes a process for the production of bodies consolidated with titanium nitride in dispersion, in which a powder consisting essentially of a titanium-containing ferritic or austenitic steel, preferably with 20% chromium and 25% nickel, first in a hydrogen-containing one Atmosphere is pre-sintered so that a body with sufficient strength is formed, which is, however, gas-permeable for the subsequent nitriding treatment. Then the pre-sintered body is flowed through with a hydrogen-nitrogen mixture in the temperature range of 1000-1150 ° C until the desired nitride content has been reached.
  • the bodies produced in this way can then either be subjected to a subsequent compression treatment by rolling or forging, or a nitrided powder can be produced by grinding, which can be processed further using the known methods of powder metallurgy.
  • a metal powder produced by atomizing a melt is filled into a steel container and successively degassed and nitrided.
  • the powder is exposed to an unspecified nitrogen pressure at 1150 ° C for two hours.
  • the resulting nitrogen content in the powder is a function of the treatment temperature, the nitrogen pressure, the nitration time and the mass transfer coefficient.
  • Such an embroidered powder was then hot isostatically pressed at 2000 bar and 1100 ° C. for two hours.
  • US Pat. No. 4,140,527 provides for the nitrogen powder to flow through the metal powder for a longer period of time, for example by embroidering at a higher temperature, but the final nitrogen content is and is the result of a complex interplay of pressure, temperature and time therefore difficult to set precisely.
  • the nitriding of the powder is a separate process step, associated with considerable effort, the nitriding time being very long, in particular because of the low nitrogen pressure provided.
  • the maximum achievable nitrogen content in equilibrium is limited to values of only 1% at most.
  • the invention has for its object to provide a method for hot isostatic pressing of metal powders, in particular steel powders, with which workpieces with high gas contents up to over 1% can be produced in a simple manner.
  • reaction gas diffuses from the pores into the body formed by the compacting and is stored in it either in a solid solution or in the form of precipitates, in particular metal nitrides or carbonitrides.
  • the process is expediently controlled in such a way that a continuous process occurs, i.e. that the pressures and temperature are continuously increased until the maximum values are reached.
  • the process gas is a mixture of a gas which is insoluble in powder and the intended reaction gas, the volume fraction of which is selected such that it is approximately in equilibrium with the gas content of the metal phase under the conditions prevailing during the sintering phase. It can then be achieved that diffusion cannot lead to different gas concentrations in the edge region of the compact. In the absence of equilibrium, diffusion would result through the capsule, which would either lead to depletion or to an accumulation of reaction gas at least in the edge region of the compact.
  • the conditions (temperature and pressure) during hot isostatic pressing and the composition of the metal powder can be selected so that the gas introduced into the material remains in solid solution.
  • solid solution hardening in a manner known per se both the mechanical properties, such as strength and toughness, and the chemical properties, such as stress corrosion resistance, are influenced in a favorable manner.
  • the metal powder can also be alloyed with elements which form compounds (nitrides) with the reaction gas, in particular nitrogen, which are then present in the material as finely divided precipitates.
  • the reaction gas in particular nitrogen
  • the high-temperature stability of steel alloys is brought about in particular by the fine precipitation of special nitrides.
  • a mixture of argon and nitrogen is particularly suitable as the process gas.
  • the device for carrying out the claimed method is characterized by a pressure vessel with a heating element (s) and a process gas supply line and a capsule in the pressure chamber, filled with metal powder, to which a reaction gas supply line is connected.
  • a fine-grained powder which corresponds in its composition to the corrosion-resistant and non-magnetizable cap ring steel X10CrMn1818, is filled into a steel capsule suitable for the subsequent sintering process under the usual precautionary measures, such as protection against oxidation, whereby it may then be subjected to a vacuum treatment.
  • the metal powder used has an intermediate grain volume of 30% by volume, depending on its bulk density.
  • the capsule 2 filled with the powder mixture 1 is introduced into a pressure vessel 3 with a heating furnace 4 for hot isostatic pressing.
  • the capsule 2 is connected to a container (not shown) by means of a line 6 leading through the outer wall in order to set the desired nitrogen pressure (reaction gas) in the interior of the capsule.
  • the process gas originating from a further reservoir (also not shown) and necessary for the compression process can be admitted into the autoclave via a further line 5.
  • the process gas consists of argon with an admixture of 3% by volume nitrogen.
  • the gas supply to capsule 2 is interrupted and the process gas mixture, consisting of 3% by volume nitrogen and 97% by volume argon, is now increased to a final pressure of 2000 bar.
  • the temperature is increased to 1250 ° C at the same time.
  • the concentration of 3% by volume in the process gas is in equilibrium with the 3% nitrogen in the powder.
  • the capsule 2 used in the above process can already largely have the shape of a ring which is similar to the shape of the cap ring to be produced, so that a minimum of machining post-processing steps is created.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Powder Metallurgy (AREA)

Claims (6)

1. Procédé pour la fabrication de matériaux métalliques par compression isostatique à chaud de poudre métallique à teneur élevée en gaz, qui sont introduits dans la poudre métallique à une température plus élevée par percussion de la poudre métallique avec un gaz réactif sous pression, caractérisé en ce que:
a) la poudre métallique est frappée par le gaz réactif après le remplissage connu dans une capsule pendant que,
b) simultanément, un gaz de traitement agit sur la capsule depuis l'extérieur, sous pression avec apport de chaleur,
c) simultanément à l'augmentation de la pression du gaz de traitement, une augmentation de pression sensiblement égale du gaz de traitement étant réalisée,
d) la pression est augmentée jusqu'à ce qu'une quantité de gaz réactionnel suffisante pour attein- dre la teneur d'alliage souhaitée soit enfermée dans les interstices de la poudre métallique, dans les conditions de température qui y règnent, qu'ensuite,
e) l'apport de gaz réactionnel est arrêté et
f) la pression du gaz de traitement en dehors de la capsule et la température sont amenées à une hauteur nécessaire pour la compression isostatique à chaud.
2. Procédé selon la revendication, 1 caractérisé en ce que le gaz de traitement est un mélange d'un gaz non soluble dans la poudre métallique et du gaz réactionnel prévu, la proportion en volume du gaz réactionnel dans le mélange étant choisie de telle manière que, dans les conditions de pression et de température régnant pendant la phase de frittage isostatique à chaud, il soit sensiblement à égalité de poids avec la teneur en gaz.de la phase métallique.
3. Procédé selon la revendication 1 ou 2, caractérisé en ce que la poudre métallique est alliée à des éléments qui produisent avec le gaz réactif des combinaisons qui se présentant dans le matériau sous forme de précipitations finement réparties.
4. Procédé selon l'une des revendications 1 à 3 pour la fabrication de produits à partir de poudre d'acier, caractérisé en ce qu'on utilise de l'azote comme gaz réactionnel.
5. Procédé selon la revendication 2, caractérisé en ce que le gaz de traitement est un mélange d'argon et d'azote.
6. Dispositif pour la mise en oeuvre du procédé selon l'une des revendications 1 à 5, caractérisé par un récipient de pression (3) avec élément(s) chauffant(s) (4) et une conduite d'amenée de gaz de traitement (5), ainsi qu'une capsule (2) remplie de poudre métallique (1) se trouvant dans le volume de pression (7), à laquelle est raccordée une conduite d'amenée de gaz réactionnel (6).
EP87110429A 1986-07-21 1987-07-18 Procédé et appareil pour la fabrication de matériaux métalliques par compression isostatique à chaud de poudre métallique Expired - Lifetime EP0255005B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT87110429T ATE56380T1 (de) 1986-07-21 1987-07-18 Verfahren und vorrichtung zur herstellung metallischer werkstoffe durch isostatisches heisspressen von metallpulver.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19863624622 DE3624622A1 (de) 1986-07-21 1986-07-21 Verfahren und vorrichtung zur herstellung metallischer werkstoffe durch isostatisches heisspressen von metallpulver
DE3624622 1986-07-21

Publications (3)

Publication Number Publication Date
EP0255005A2 EP0255005A2 (fr) 1988-02-03
EP0255005A3 EP0255005A3 (en) 1988-11-09
EP0255005B1 true EP0255005B1 (fr) 1990-09-12

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ID=6305641

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87110429A Expired - Lifetime EP0255005B1 (fr) 1986-07-21 1987-07-18 Procédé et appareil pour la fabrication de matériaux métalliques par compression isostatique à chaud de poudre métallique

Country Status (5)

Country Link
EP (1) EP0255005B1 (fr)
AT (1) ATE56380T1 (fr)
DE (2) DE3624622A1 (fr)
ES (1) ES2018214B3 (fr)
SE (1) SE462641B (fr)

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3743261A (en) * 1971-07-21 1973-07-03 Crucible Inc Furnace and method for heating and compacting powdered metal charges
JPS52141406A (en) * 1976-05-21 1977-11-25 Kobe Steel Ltd Tool steel containing nitrogen made by powder metallurgy
DE3567227D1 (en) * 1984-06-15 1989-02-09 Atomic Energy Authority Uk Titanium nitride dispersion strengthened bodies

Also Published As

Publication number Publication date
SE8702834D0 (sv) 1987-07-10
EP0255005A2 (fr) 1988-02-03
DE3624622A1 (de) 1988-02-25
ES2018214B3 (es) 1991-04-01
SE462641B (sv) 1990-08-06
DE3764898D1 (de) 1990-10-18
DE3624622C2 (fr) 1988-06-16
EP0255005A3 (en) 1988-11-09
ATE56380T1 (de) 1990-09-15
SE8702834L (sv) 1988-01-22

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