EP0792945A1 - Process for heat treatment of a nickel-base superalloy - Google Patents

Process for heat treatment of a nickel-base superalloy Download PDF

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Publication number
EP0792945A1
EP0792945A1 EP97400438A EP97400438A EP0792945A1 EP 0792945 A1 EP0792945 A1 EP 0792945A1 EP 97400438 A EP97400438 A EP 97400438A EP 97400438 A EP97400438 A EP 97400438A EP 0792945 A1 EP0792945 A1 EP 0792945A1
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temperature
gamma
superalloy
prime
minus
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German (de)
French (fr)
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EP0792945B1 (en
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Yves Philippe Marc Desvallees
Jean-Michel Patrick Maurice Franchet
Michel Marty
Henri Octor
Françoise Passilly
Michèle Soucail
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Office National dEtudes et de Recherches Aerospatiales ONERA
Safran Aircraft Engines SAS
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Office National dEtudes et de Recherches Aerospatiales ONERA
Societe Nationale dEtude et de Construction de Moteurs dAviation SNECMA
SNECMA SAS
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon

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  • the present invention relates to a process for the thermal treatment of a nickel-based superalloy whose chemical composition in weight percentages is in accordance with either EP-B-0 237 378 and belongs to the following field: Cr 11 to 13; Co 8 to 17; Mo 6 to 8; Nb less than or equal to 1.5; Ti 4 to 5; Al 4 to 5; Hf less than or equal to 1; C, B, Zr each less than or equal to 500 ppm; Neither complement to 100, ie at the request FR 95.09653 and belongs to the following domain: Cr 12 to 15; Co 14.5 to 15.5; Mo 2 to 4.5; W O to 4.5; Al 2.5-4; Ti 4 to 6; Hf less than or equal to 0.5; C 100 to 300 ppm; B 100 to 500 PPm; Zr 200 to 700 ppm; No complement to 100.
  • alloys are used in particular for the manufacture of highly stressed parts intended for aircraft engines, for example rotor disks.
  • parts of this type can in particular be produced using processing techniques from powders and their shaping calls for forging operations.
  • the heat treatments applied to the parts before use commonly comprise a solution and quenching treatment followed by an aging treatment.
  • the invention applies in particular in cases where a supersolvus heat treatment is carried out comprising complete dissolution of the gamma-prime precipitates at a temperature between + 5 ° C and + 25 ° C above the solvent temperature gamma-prime for a hold time of between 1 hour and 4 hours.
  • the final grain size depends on a succession of industrial stages which are: the possible pretreatment of the powders, densification by spinning, isothermal forging, the final heat treatment.
  • the metallurgical and thermomechanical parameters that can influence recrystallization are numerous and interdependent. These include: gamma-prime phase precipitation, oxycarbon distribution, strain rate, strain rate, stress, time, temperature.
  • the grain enlargement phenomenon caused by the heat treatment mentioned above can correspond to the following scheme: the gamma-prime precipitates which before the supersolvus heat treatment blocked the grain boundaries dissolve and the grain boundaries, released, migrate then are generally again anchored by very fine precipitates, oxycarbons, preferentially located at the old powder boundaries.
  • the result sought in this case is to obtain grains of uniform size, in particular of 50 ⁇ m on average, corresponding to a so-called normal grain growth.
  • an intermediate heat treatment succeeding the hot forging operation which is followed by cooling of the part and carried out at a temperature between the gamma-prime solvus temperature minus 95 ° C and the gamma-prime solvus temperature minus 30 ° C and between 1 and 24 hours.
  • results referred to and previously described are also obtained, in accordance with the invention, by carrying out at the end of the hot forging operation, that is to say from the moment when the alloy is still at the forging temperature isothermal maintenance at a temperature between the gamma-prime solvus temperature minus 95 ° C and the gamma-prime solvus temperature minus 30 ° C for a period of between 1 and 60 minutes.
  • the heat treatment can be carried out in two distinct stages.
  • the first step consisting of isothermal maintenance at a temperature between the gamma-prime solvus temperature minus 95 ° C and the gamma-prime solvus temperature minus 30 ° C is carried out at the end of the hot forging operation c '' is to say at the moment when the alloy is still at the forging temperature, for a period of between 1 and 30 minutes after which, the part is cooled.
  • the second step then consists of a heat treatment carried out at a temperature between the gamma-prime solvus temperature minus 95 ° C and the gamma-prime solvus temperature minus 30 ° C of the superalloy and for a period of between 1 and 24 hours, followed by a supersolvus heat treatment.
  • Alloy M has the following nominal chemical composition in weight percentages:
  • the gamma-prime phase solution temperature or solvent temperature of the alloy is 1195 ° C.
  • the material studied comes from powders atomized with argon and densified by spinning at 1120 ° C.
  • Four rollers A, B, C, D were forged by isothermal forging at 1120 ° C under the conditions of deformation, on the ordinate, and speed of deformation, on the abscissa, represented by the respective curves 1,2,3 and 4 of FIG. 1, thus covering domains greater than 0.1 in deformation and from 10 -4 s -1 to 8.10 -3 s -1 in deformation speed.
  • Other tests have been carried out in traction and are represented by points 5,6,7,8,9,10,11,12 and 13 in FIG. 1.
  • FIG. 2 shows a microstructure with some very large grains obtained after a standard supersolvus heat treatment carried out at 1205 ° C for 4 hours after a tensile test at 1120 ° C corresponding to a deformation rate of 7.10 -3 s -1 and a deformation of 0.62.
  • a sample is subjected to a one hour heat treatment at 1120 ° C. before applying the standard supersolvus heat treatment, as above.
  • Figure 3 shows the microstructure obtained in this case, having smaller grains and showing the appearance of colonies of small grains.
  • the microstructure obtained, represented in FIG. 4 is then homogeneous, completely devoid of very large grains and the average size of the grains is around 50 ⁇ m.
  • the heat treatment method according to the invention therefore makes it possible to obtain a state of use of the material concerned having a microstructure ensuring the compromise sought for the mechanical characteristics of use, in particular for parts intended for aeronautical use such as rotating aircraft engine parts, satisfactory creep resistance and good crack propagation resistance at high temperatures.
  • a tensile test piece just after having been deformed under critical conditions leading to the presence of very large grains on the final state namely a temperature of 1120 ° C and a deformation rate of 7.10 -3 s -1 , was maintained at 1120 ° C for 10 minutes.
  • the microstructure obtained is homogeneous and does not have very large grains, as shown in Figure 5.
  • temperature maintenance without intermediate cooling of the part, can be achieved by keeping the part in the forging tool at the forging temperature.
  • the maintenance at the end of the forging operation can be carried out in an oven, at a temperature between the gamma-prime solvus temperature minus 95 ° C. and the gamma-solvus temperature. prime minus 30 ° C.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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Abstract

A method for heat treating nickel superalloy forgings containing 11-13 wt % of Cr, 8-17 wt % of Co, 6-8 wt % of Mo, 4-5 wt % of Ti, 4-5 wt % of Al, no more than 0.5 wt % of Nb, and no more than 500 ppm of Hf, the balance to 100 wt % being Ni, is disclosed. According to the method, an intermediate heat treatment is carried out at a temperature between the gamma ' solvus minus 95 DEG C and the gamma ' solvus minus 30 DEG C, following hot forging at a temperature between the gamma ' solvus minus 95 DEG C and the gamma ' solvus minus 45 DEG C, with a strain rate of 5.10<-5>s<-1> to 2.10<-2>s<-1>, and a deformation ratio higher than 0.1, and prior to a supersolvus heat treatment at a temperature between the gamma ' solvus plus 5 DEG C and the gamma ' solvus plus 25 DEG C for 1 to 4 hours.

Description

La présente invention concerne un procédé de traitement thermique d'un superalliage à base de nickel dont la composition chimique en pourcentages pondéraux est conforme soit à EP-B-0 237 378 et appartient au domaine suivant : Cr 11 à 13; Co 8 à 17; Mo 6 à 8; Nb inférieur ou égal à 1,5; Ti 4 à 5; Al 4 à 5; Hf inférieur ou égal à 1; C,B,Zr chacun inférieur ou égal à 500ppm; Ni complément à 100, soit à la demande FR 95.09653 et appartient au domaine suivant : Cr 12 à 15 ; Co 14,5 à 15,5 ; Mo 2 à 4,5 ; W O à 4,5 ; Al 2,5 à 4 ; Ti 4 à 6 ; Hf inférieur ou égal à 0,5 ; C 100 à 300 ppm ; B 100 à 500 PPm ; Zr 200 à 700 ppm ; Ni complément à 100.The present invention relates to a process for the thermal treatment of a nickel-based superalloy whose chemical composition in weight percentages is in accordance with either EP-B-0 237 378 and belongs to the following field: Cr 11 to 13; Co 8 to 17; Mo 6 to 8; Nb less than or equal to 1.5; Ti 4 to 5; Al 4 to 5; Hf less than or equal to 1; C, B, Zr each less than or equal to 500 ppm; Neither complement to 100, ie at the request FR 95.09653 and belongs to the following domain: Cr 12 to 15; Co 14.5 to 15.5; Mo 2 to 4.5; W O to 4.5; Al 2.5-4; Ti 4 to 6; Hf less than or equal to 0.5; C 100 to 300 ppm; B 100 to 500 PPm; Zr 200 to 700 ppm; No complement to 100.

Ces alliages sont notamment utilisés pour la fabrication de pièces fortement sollicitées destinées à des moteurs d'avion, par exemple des disques de rotor. De manière connue en soi, les pièces de ce type peuvent notamment être élaborées à l'aide de techniques de mise en oeuvre à partir de poudres et leur mise en forme fait appel à des opérations de forgeage. Les traitements thermiques appliqués sur les pièces avant emploi comportent de manière courante un traitement de mise en solution et trempe suivi d'un traitement de vieillissement.These alloys are used in particular for the manufacture of highly stressed parts intended for aircraft engines, for example rotor disks. In a manner known per se, parts of this type can in particular be produced using processing techniques from powders and their shaping calls for forging operations. The heat treatments applied to the parts before use commonly comprise a solution and quenching treatment followed by an aging treatment.

L'invention s'applique en particulier dans les cas où est effectué un traitement thermique supersolvus comportant une mise en solution complète des précipités gamma-prime à une température comprise entre +5°C et +25°C au dessus de la température de solvus gamma-prime pendant une durée de maintien comprise entre 1 heure et 4 heures.The invention applies in particular in cases where a supersolvus heat treatment is carried out comprising complete dissolution of the gamma-prime precipitates at a temperature between + 5 ° C and + 25 ° C above the solvent temperature gamma-prime for a hold time of between 1 hour and 4 hours.

Ces traitements permettent en effet une optimisation de la microstructure des alliages vers des structures à gros grains dont l'influence favorable a été démontrée sur la tenue en fluage et en propagation de fissures aux hautes températures nécessitées par la recherche d'amélioration des performances des moteurs d'avions.These treatments indeed allow an optimization of the microstructure of the alloys towards coarse-grained structures whose favorable influence has been demonstrated on the creep behavior and in propagation of cracks at high temperatures. necessitated by the search for improvement in aircraft engine performance.

La taille de grain finale dépend d'une succession d'étapes industrielles que sont : le prétraitement éventuel des poudres, la densification par filage, le forgeage isotherme, le traitement thermique final. De plus, les paramètres métallurgiques et thermomécaniques pouvant influencer la recristallisation sont nombreux et interdépendants. Citons : la précipitation de phase gamma-prime, la distribution d'oxycarbures, le taux de déformation, la vitesse de déformation, la contrainte, le temps, la température.The final grain size depends on a succession of industrial stages which are: the possible pretreatment of the powders, densification by spinning, isothermal forging, the final heat treatment. In addition, the metallurgical and thermomechanical parameters that can influence recrystallization are numerous and interdependent. These include: gamma-prime phase precipitation, oxycarbon distribution, strain rate, strain rate, stress, time, temperature.

Le phénomène de grossissement du grain provoqué par le traitement thermique rappelé ci-dessus peut répondre au schéma suivant :
les précipités gamma-prime qui avant le traitement thermique supersolvus bloquaient les joints de grains se dissolvent et les joints de grains, libérés, migrent puis sont généralement de nouveau ancrés par de très fins précipités, les oxycarbures, situés préférentiellement aux anciennes limites de poudres. Le résultat recherché dans ce cas est d'obtenir des grains de taille homogène, notamment de 50µm en moyenne, correspondant à une croissance de grains dite normale.The grain enlargement phenomenon caused by the heat treatment mentioned above can correspond to the following scheme:
the gamma-prime precipitates which before the supersolvus heat treatment blocked the grain boundaries dissolve and the grain boundaries, released, migrate then are generally again anchored by very fine precipitates, oxycarbons, preferentially located at the old powder boundaries. The result sought in this case is to obtain grains of uniform size, in particular of 50 μm on average, corresponding to a so-called normal grain growth.

Toutefois, un grossissement de grain dit anormal conduisant à la croissance d'un ou de plusieurs très gros grains de plusieurs centaines de micromètres au détriment des autres a été observé sous l'influence des divers paramètres précédemment rappelés. La microstructure très hétérogène qui en résulte est préjudiciable à une bonne tenue des pièces et notamment à la tenue en fatigue. Un des buts de l'invention est d'éviter cette croissance dite anormale de grain tout en conservant les avantages liés à une microstructure d'alliage dite à gros grains.However, a so-called abnormal grain magnification leading to the growth of one or more very large grains of several hundred micrometers to the detriment of the others has been observed under the influence of the various parameters previously recalled. The very heterogeneous microstructure which results therefrom is detrimental to good performance of the parts and in particular to the fatigue behavior. One of the aims of the invention is to avoid this so-called abnormal grain growth while retaining the advantages linked to a so-called coarse-grain alloy microstructure.

Ces résultats sont obtenus, conformément à l'invention, en appliquant à des pièces forgées en un superalliage à base de nickel conforme à EP-B-0.237.378 ou à la demande FR 95.09653 suivant un cycle thermomécanique comportant au moins une opération de forgeage à chaud, effectué à une température comprise entre la température de solvus gamma-prime moins 95°C et la température de solvus gamma-prime moins 45°C, à une vitesse de déformation rationnelle comprise entre 5.10-5s-1 et 2.10-2s-1 et à un taux de déformation rationnelle supérieur à 0,1 et un traitement thermique supersolvus, effectué à une température comprise entre la température de solvus gamma-prime plus 5°C et la température de solvus gamma-prime plus 25°C et à une durée comprise entre 1 et 4 heures, un traitement thermique intermédiaire succédant à l'opération de forgeage à chaud qui est suivie d'un refroidissement de la pièce et effectué à une température comprise entre la température de solvus gamma-prime moins 95°C et la température de solvus gamma-prime moins 30°C et à une durée comprise entre 1 et 24 heures.These results are obtained, in accordance with the invention, by applying to forgings made of a nickel-based superalloy conforming to EP-B-0.237.378 or on request FR 95.09653 following a thermomechanical cycle comprising at least one hot forging operation, carried out at a temperature between the gamma-prime solvus temperature minus 95 ° C and the gamma-prime solvus temperature minus 45 ° C, at a rational deformation speed between 5.10 -5 s -1 and 2.10 -2 s -1 and at a rational deformation rate greater than 0.1 and a supersolvus heat treatment, carried out at a temperature between the gamma-prime solvent temperature plus 5 ° C and the gamma-prime solvus temperature plus 25 ° C. and for a period of between 1 and 4 hours, an intermediate heat treatment succeeding the hot forging operation which is followed by cooling of the part and carried out at a temperature between the gamma-prime solvus temperature minus 95 ° C and the gamma-prime solvus temperature minus 30 ° C and between 1 and 24 hours.

Dans certaines applications particulières, les résultats visés et précédemment décrits sont également obtenus, conformément à l'invention, en effectuant à la fin de l'opération de forgeage à chaud c'est à dire à partir de l'instant où l'alliage est encore à la température de forgeage un maintien isotherme à une température comprise entre la température de solvus gamma-prime moins 95°C et la température de solvus gamma-prime moins 30°C pour une durée comprise entre 1 et 60 minutes.In certain particular applications, the results referred to and previously described are also obtained, in accordance with the invention, by carrying out at the end of the hot forging operation, that is to say from the moment when the alloy is still at the forging temperature isothermal maintenance at a temperature between the gamma-prime solvus temperature minus 95 ° C and the gamma-prime solvus temperature minus 30 ° C for a period of between 1 and 60 minutes.

Suivant une autre variante de l'invention, le traitement thermique peut s'effectuer en deux étapes distinctes. La première étape consistant en un maintien isotherme à une température comprise entre la température de solvus gamma-prime moins 95°C et la température de solvus gamma-prime moins 30°C est effectué à la fin de l'opération de forgeage à chaud c'est à dire à l'instant où l'alliage est encore à la température de forgeage, pour une durée comprise entre 1 et 30 minutes après quoi, la pièce est refroidie. La deuxième étape consiste alors en un traitement thermique effectué à une température comprise entre la température de solvus gamma-prime moins 95°C et la température de solvus gamma-prime moins 30°C du superalliage et à une durée comprise entre 1 et 24 heures, suivi d'un traitement thermique supersolvus.According to another variant of the invention, the heat treatment can be carried out in two distinct stages. The first step consisting of isothermal maintenance at a temperature between the gamma-prime solvus temperature minus 95 ° C and the gamma-prime solvus temperature minus 30 ° C is carried out at the end of the hot forging operation c '' is to say at the moment when the alloy is still at the forging temperature, for a period of between 1 and 30 minutes after which, the part is cooled. The second step then consists of a heat treatment carried out at a temperature between the gamma-prime solvus temperature minus 95 ° C and the gamma-prime solvus temperature minus 30 ° C of the superalloy and for a period of between 1 and 24 hours, followed by a supersolvus heat treatment.

D'autres caractéristiques et avantages de l'invention seront mieux compris à la lecture de la description qui va suivre des modes de réalisation de l'invention, en référence aux dessins annexés sur lesquels :

  • la figure 1 représente les conditions d'essais de forgeage et de traction effectués sur des échantillons du matériau étudié à 1120°C, en vitesses de déformation en abscisses et en déformation en ordonnées ;
  • la figure 2 représente la reproduction d'une microphotographie d'une microstructure d'éprouvette soumise au traitement standard dans les conditions antérieures à l'invention ;
  • les figures 3 et 4 représentent, de manière analogue à la figure 2, une microstructure d'éprouvettes traitées dans les conditions de l'invention ;
  • la figure 5 représente, de manière analogue aux figures 2, 3 et 4 une microstructure d'éprouvette traitée dans les conditions d'une variante de l'invention.
Other characteristics and advantages of the invention will be better understood on reading the description which follows of embodiments of the invention, with reference to the appended drawings in which:
  • FIG. 1 represents the conditions of forging and tensile tests carried out on samples of the material studied at 1120 ° C., in deformation rates on the abscissa and in deformation on the ordinate;
  • FIG. 2 represents the reproduction of a microphotograph of a microstructure of test piece subjected to the standard treatment under the conditions prior to the invention;
  • Figures 3 and 4 show, similarly to Figure 2, a microstructure of test pieces treated under the conditions of the invention;
  • FIG. 5 represents, in a manner similar to FIGS. 2, 3 and 4, a microstructure of test piece treated under the conditions of a variant of the invention.

EXEMPLES DE REALISATIONEXAMPLES OF REALIZATION

Pour la réalisation des essais, un superalliage M à base de nickel dont la composition chimique est conforme à la définition donnée par EP-B-0.237.378 a été choisi. L'alliage M présente la composition chimique nominale suivante en pourcentages pondéraux :For carrying out the tests, a nickel-based superalloy M whose chemical composition conforms to the definition given by EP-B-0.237.378 was chosen. Alloy M has the following nominal chemical composition in weight percentages:

Co 15,7; Cr 11,5; Mo 6,5; Al 4,35; Ti 4,35; B 0,015; C 0,015; Hf 0,45; Ni complément à 100.
La température de mise en solution de la phase gamma-prime ou température de solvus de l'alliage est 1195°C.Co 15.7; Cr 11.5; MB 6.5; Al 4.35; Ti 4.35; B 0.015; C 0.015; Hf 0.45; No complement to 100.
The gamma-prime phase solution temperature or solvent temperature of the alloy is 1195 ° C.

Le matériau étudié provient de poudres atomisées à l'argon et densifiées par filage à 1120°C.
Quatre galets A, B, C, D ont été forgés par forgeage isotherme à 1120°C dans les conditions de déformation, en ordonnées, et de vitesse de déformation, en abscisses, représentées par les courbes respectives 1,2,3 et 4 de la figure 1, couvrant ainsi des domaines supérieurs à 0,1 en déformation et de 10-4s-1 à 8.10-3s-1 en vitesse de déformation. D'autres essais ont été effectués en traction et sont représentés par les points 5,6,7,8,9,10,11,12 et 13 sur la figure 1.
A la suite du traitement thermique supersolvus standard défini pour le matériau comportant soit un maintien à 1205°C pendant 4 heures, soit un maintien à 1200°C pendant 2 heures, des structures à très gros grains, de l'ordre du mm par exemple, ont été observées. Les essais ont montré l'influence de l'état d'écrouissage pour la croissance des très gros grains dans le matériau concerné. La figure 2 montre une microstructure présentant quelques très gros grains obtenue après un traitement thermique standard supersolvus effectué à 1205°C pendant 4 heures après un essai de traction à 1120°C correspondant à une vitesse de déformation de 7.10-3s-1 et une déformation de 0,62.
De manière remarquable et conforme à l'invention, un échantillon est soumis à un traitement thermique d'une heure à 1120°C avant de lui appliquer le traitement thermique standard supersolvus, comme ci-dessus. La figure 3 montre la microstructure obtenue dans ce cas, présentant des grains moins gros et montrant l'apparition de colonies de petits grains.The material studied comes from powders atomized with argon and densified by spinning at 1120 ° C.
Four rollers A, B, C, D were forged by isothermal forging at 1120 ° C under the conditions of deformation, on the ordinate, and speed of deformation, on the abscissa, represented by the respective curves 1,2,3 and 4 of FIG. 1, thus covering domains greater than 0.1 in deformation and from 10 -4 s -1 to 8.10 -3 s -1 in deformation speed. Other tests have been carried out in traction and are represented by points 5,6,7,8,9,10,11,12 and 13 in FIG. 1.
Following the standard supersolvus heat treatment defined for the material comprising either maintaining at 1205 ° C for 4 hours, or maintaining at 1200 ° C for 2 hours, structures with very large grains, of the order of mm for example , have been observed. Tests have shown the influence of the hardening state for the growth of very large grains in the material concerned. Figure 2 shows a microstructure with some very large grains obtained after a standard supersolvus heat treatment carried out at 1205 ° C for 4 hours after a tensile test at 1120 ° C corresponding to a deformation rate of 7.10 -3 s -1 and a deformation of 0.62.
Remarkably and in accordance with the invention, a sample is subjected to a one hour heat treatment at 1120 ° C. before applying the standard supersolvus heat treatment, as above. Figure 3 shows the microstructure obtained in this case, having smaller grains and showing the appearance of colonies of small grains.

Lorsque le traitement thermique intermédiaire à 1120°C est prolongé à 24 heures avant d'effectuer comme précédemment le traitement thermique standard supersolvus, la microstructure obtenue, représenté sur la figure 4 est alors homogène, totalement dépourvue de très gros grains et la taille moyenne des grains est d'environ 50µm.When the intermediate heat treatment at 1120 ° C. is extended to 24 hours before carrying out the standard supersolvus heat treatment as before, the microstructure obtained, represented in FIG. 4, is then homogeneous, completely devoid of very large grains and the average size of the grains is around 50µm.

Le procédé de traitement thermique conforme à l'invention permet par conséquent d'obtenir un état d'emploi du matériau concerné présentant une microstructure assurant le compromis recherché pour les caractéristiques mécaniques d'utilisation, notamment pour les pièces destinées à un usage aéronautique tel que des pièces tournantes de moteur d'avion, une tenue satisfaisante en fluage et une bonne tenue en propagation de fissures aux hautes températures.The heat treatment method according to the invention therefore makes it possible to obtain a state of use of the material concerned having a microstructure ensuring the compromise sought for the mechanical characteristics of use, in particular for parts intended for aeronautical use such as rotating aircraft engine parts, satisfactory creep resistance and good crack propagation resistance at high temperatures.

Suivant une variante de l'invention, au lieu d'effectuer le traitement thermique intermédiaire dans les conditions précédemment définies, dans un autre essai, une éprouvette de traction juste après avoir été déformée dans des conditions critiques conduisant à la présence de très gros grains sur l'état final, à savoir une température de 1120°C et une vitesse de déformation de 7.10-3s-1, a été maintenue à 1120°C pendant 10 minutes. Après traitement thermique standard supersolvus, la microstructure obtenue est homogène et ne présente pas de très gros grains, comme le montre la figure 5.According to a variant of the invention, instead of carrying out the intermediate heat treatment under the conditions defined above, in another test, a tensile test piece just after having been deformed under critical conditions leading to the presence of very large grains on the final state, namely a temperature of 1120 ° C and a deformation rate of 7.10 -3 s -1 , was maintained at 1120 ° C for 10 minutes. After standard supersolvus heat treatment, the microstructure obtained is homogeneous and does not have very large grains, as shown in Figure 5.

Pour des applications de forgeage de pièces, le maintien en température, sans refroidissement intermédiaire de la pièce, peut être réalisé en maintenant la pièce dans l'outillage de forgeage, à la température de forgeage. En variante et en fonction des applications particulières, le maintien à la fin de l'opération de forgeage peut être réalisé dans un four, à une température comprise entre la température de solvus gamma-prime moins 95°C et la température de solvus gamma-prime moins 30°C.For part forging applications, temperature maintenance, without intermediate cooling of the part, can be achieved by keeping the part in the forging tool at the forging temperature. As a variant and depending on the particular applications, the maintenance at the end of the forging operation can be carried out in an oven, at a temperature between the gamma-prime solvus temperature minus 95 ° C. and the gamma-solvus temperature. prime minus 30 ° C.

Claims (3)

Procédé de traitement thermique d'un superalliage à base de nickel dont la composition chimique en pourcentages pondéraux appartient aux domaines suivants : Cr 11 à 13; Co 8 à 17; Mo 6 à 8; Ti 4 à 5; Al 4 à 5, Nb inférieur ou égal à 1,5 ; Hf inférieur ou égal à 1 ; C,B,Zr chacun inférieur ou égal à 500 ppm ; Ni complément à 100, ou Cr 12 à 15 ; Co 14,5 à 15,5 ; Mo 2 à 4,5 ; W 0 à 4,5 ; Al 2,5 à 4 ; Ti 4 à 6 ; Hf inférieur ou égal à 0,5 ; C 100 à 300 ppm ; B 100 à 500 ppm ; Zr 200 à 700 ppm ; Ni complément à 100, appliqué à des pièces forgées suivant un traitement thermomécanique comportant une opération de forgeage à chaud, effectué à une température comprise entre la température de solvus gamma-prime moins 95°C du superalliage et la température de solvus gamma-prime moins 45°C du superalliage, à une vitesse de déformation rationnelle comprise entre 5.10-5 s-1 et 2.10-2 s-1 et à un taux de déformation rationnelle supérieur à 0,1 et un traitement thermique supersolvus, effectué à une température comprise entre la température de solvus gamma-prime plus 5°C du superalliage et la température de solvus gamma-prime plus 25°C du superalliage et à une durée comprise entre 1 et 4 heures caractérisé en ce qu'un traitement thermique intermédiaire, succédant à l'opération de forgeage à chaud qui est suivie d'un refroidissement de la pièce, est effectué à une température comprise entre la température de solvus gamma-prime moins 95°C et la température de solvus gamma-prime moins 30°C du superalliage et à une durée comprise entre 1 à 24 heures. Process for heat treatment of a nickel-based superalloy whose chemical composition in weight percentages belongs to the following fields: Cr 11 to 13; Co 8 to 17; Mo 6 to 8; Ti 4 to 5; Al 4 to 5, Nb less than or equal to 1.5; Hf less than or equal to 1; C, B, Zr each less than or equal to 500 ppm; No complement to 100, or Cr 12 to 15; Co 14.5 to 15.5; Mo 2 to 4.5; W 0 to 4.5; Al 2.5-4; Ti 4 to 6; Hf less than or equal to 0.5; C 100 to 300 ppm; B 100 to 500 ppm; Zr 200 to 700 ppm; No complement to 100, applied to forgings following a thermomechanical treatment comprising a hot forging operation, carried out at a temperature between the gamma-prime solvus temperature minus 95 ° C of the superalloy and the gamma-prime solvus temperature minus 45 ° C of the superalloy , at a rational strain rate between 5.10 -5 s -1 and 2.10 -2 s -1 and at a rational strain rate greater than 0.1 and a supersolvus heat treatment, carried out at a temperature between the solvent temperature gamma-prime plus 5 ° C of the superalloy and the gamma-prime solvus temperature plus 25 ° C of the superalloy and for a period of between 1 and 4 hours characterized in that an intermediate heat treatment, succeeding the forging operation hot which is followed by cooling of the part, is carried out at a temperature between the gamma-prime solvent temperature minus 95 ° C and the solvent temperature gamma-prime minus 30 ° C of the superalloy and for a period of between 1 to 24 hours. Procédé de traitement thermique d'un superalliage à base de nickel dont la composition chimique en pourcentages pondéraux appartient aux domaines suivants : Cr 11 à 13; Co 8 à 17; Mo 6 à 8; Ti 4 à 5; Al 4 à 5; Nb inférieur ou égal à 1,5; Hf inférieur ou égal à 1; C,B,Zr chacun inférieur ou égal à 500 ppm ; Ni complément à 100, ou Cr 12 à 15 ; Co 14,5 à 15,5 ; Mo 2 à 4,5 ; W O à 4,5 ; Al 2,5 à 4 ; Ti 4 à 6 ; Hf inférieur ou égal à 0,5 ; C 100 à 300 ppm ; B 100 à 500 ppm ; Zr 200 à 700 ppm ; Ni complément à 100, appliqué à des pièces forgées suivant un traitement thermomécanique comportant une opération de forgeage à chaud, effectué à une température comprise entre la température de solvus gamma-prime moins 95°C du superalliage et la température de solvus gamme-prime moins 45°C du superalliage, à une vitesse de déformation rationnelle comprise entre 5.10-5 s-1 et 2.10-2 s-1 et à un taux de déformation rationnelle supérieur à 0,1 et un traitement thermique supersolvus, effectué à une température comprise entre la température de solvus gamma-prime plus 5°C du superalliage et la température de solvus gamma-prime plus 25°C du superalliage et à une durée comprise entre 1 et 4 heures caractérisé en ce qu'un maintien isotherme à une température comprise entre la température de solvus gamma-prime moins 95°C et la température de solvus gamma-prime moins 30°C, est effectué à la fin de l'opération de forgeage à chaud c'est à dire à partir de l'instant où l'alliage est encore à la température de forgeage, pour une durée comprise entre 1 et 60 minutes. Process for heat treatment of a nickel-based superalloy whose chemical composition in weight percentages belongs to the following fields: Cr 11 to 13; Co 8 to 17; Mo 6 to 8; Ti 4 to 5; Al 4 to 5; Nb less than or equal to 1.5; Hf less than or equal to 1; C, B, Zr each less than or equal to 500 ppm; No complement to 100, or Cr 12 to 15; Co 14.5 to 15.5; Mo 2 to 4.5; WO at 4.5; Al 2.5-4; Ti 4 to 6; Hf less than or equal to 0.5; C 100 to 300 ppm; B 100 to 500 ppm; Zr 200 to 700 ppm; No complement to 100, applied to forgings following a thermomechanical treatment including a hot forging operation, carried out at a temperature between the gamma-prime solvus temperature minus 95 ° C of the superalloy and the premium-gamma solvus temperature minus 45 ° C of the superalloy , at a rational strain rate between 5.10 -5 s -1 and 2.10 -2 s -1 and at a rational strain rate greater than 0.1 and a supersolvus heat treatment, carried out at a temperature between the solvent temperature gamma-prime plus 5 ° C of the superalloy and the temperature of the gamma-prime plus 25 ° C of the superalloy and for a period of between 1 and 4 hours characterized in that an isothermal maintenance at a temperature of between the temperature of the solvus gamma-prime minus 95 ° C and the gamma-prime solvent temperature minus 30 ° C, is carried out at the end of the hot forging operation, i.e. from the moment the alloy is still at the forging temperature, for a period of between 1 and 60 minutes. Procédé de traitement thermique d'un superalliage à base de nickel dont la composition chimique en pourcentages pondéraux appartient aux domaines suivants : Cr 11 à 13; Co 8 à 17; Mo 6 à 8; Ti 4 à 5; Al 4 à 5; Nb inférieur ou égal à 1,5; Hf inférieur ou égal à 1 ; C,B,Zr chacun inférieur ou égal à 500 ppm ; Ni complément à 100, ou Cr 12 à 15 ; Co 14,5 à 15,5 ; Mo 2 à 4,5 ; W 0 à 4,5 ; Al 2,5 à 4 ; Ti 4 à 6 ; Hf inférieur ou égal à 0,5 ; C 100 à 300 ppm ; B 100 à 500 ppm ; Zr 200 à 700 ppm ; Ni complément à 100, appliqué à des pièces forgées suivant un traitement thermo-mécanique comportant une opération de forgeage à chaud, effectué à une température comprise entre la température de solvus gamma-prime moins 95°C du superalliage et la température de solvus gamma-prime moins 45°C du superalliage, à une vitesse de déformation rationnelle comprise entre 5.10-5s-1 et 2.102s-1 et à un taux de déformation rationelle supérieur à 0,1 et un traitement thermique supersolvus, effectué à une température comprise entre la température de solvus gamma-prime plus 5°C du superalliage et la température de solvus gamma-prime plus 25°C du superalliage et à une durée comprise entre 1 et 4 heures caractérisé en ce qu'un maintien isotherme à une température comprise entre la température de solvus gamma-prime moins 95°C et la température de solvus gamma-prime moins 30°C est effectué à la fin de l'opération de forgeage à chaud c'est à dire à partir de l'instant où l'alliage est encore à la température de forgeage, pour une durée comprise entre 1 et 60 minutes puis, après refroidissement de la pièce, un traitement thermique est effectué à une température comprise entre la température de solvus gamma-prime moins 95°C et la température de solvus gamma-prime moins 30°C du superalliage et à une durée comprise entre 1 et 24 heures. Process for heat treatment of a nickel-based superalloy whose chemical composition in weight percentages belongs to the following fields: Cr 11 to 13; Co 8 to 17; Mo 6 to 8; Ti 4 to 5; Al 4 to 5; Nb less than or equal to 1.5; Hf less than or equal to 1; C, B, Zr each less than or equal to 500 ppm; No complement to 100, or Cr 12 to 15; Co 14.5 to 15.5; Mo 2 to 4.5; W 0 to 4.5; Al 2.5-4; Ti 4 to 6; Hf less than or equal to 0.5; C 100 to 300 ppm; B 100 to 500 ppm; Zr 200 to 700 ppm; No complement to 100, applied to forgings following a thermo-mechanical treatment including a hot forging operation, carried out at a temperature between gamma-prime solvus temperature minus 95 ° C of the superalloy and gamma-prime solvus temperature minus 45 ° C of the superalloy, at a rational strain rate of between 5.10 -5 s -1 and 2.10 2 s -1 and at a rational deformation rate greater than 0.1 and a supersolvus heat treatment, carried out at a temperature between the gamma-prime solvus temperature plus 5 ° C of the superalloy and the gamma-prime solvus temperature plus 25 ° C of the superalloy and at a period of between 1 and 4 hours characterized in that an isothermal maintenance at a temperature between the gamma-prime solvus temperature minus 95 ° C and the gamma-prime solvus temperature minus 30 ° C is carried out at the end of the hot forging operation, that is to say from the moment when the alloy is still at the forging temperature, for a period of between 1 and 60 minutes then, after the part has cooled, a heat treatment is eff carried out at a temperature between the gamma-prime solvus temperature minus 95 ° C and the gamma-prime solvus temperature minus 30 ° C of the superalloy and at a time between 1 and 24 hours.
EP19970400438 1996-02-29 1997-02-27 Process for heat treatment of a nickel-base superalloy Expired - Lifetime EP0792945B1 (en)

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FR9602534 1996-02-29
FR9602534A FR2745588B1 (en) 1996-02-29 1996-02-29 METHOD FOR THE HEAT TREATMENT OF A NICKEL-BASED SUPERALLOY

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US10563293B2 (en) 2015-12-07 2020-02-18 Ati Properties Llc Methods for processing nickel-base alloys
CN110050080B (en) * 2017-11-17 2021-04-23 三菱动力株式会社 Ni-based wrought alloy material and turbine high-temperature component using same
RU2697674C1 (en) * 2019-05-24 2019-08-16 Общество с ограниченной ответственностью "НТЦ "Современные технологии металлургии" (ООО "НТЦ"СТМ") Heat-resistant nickel alloy
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JP3926877B2 (en) 2007-06-06
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RU2133784C1 (en) 1999-07-27
FR2745588A1 (en) 1997-09-05
EP0792945B1 (en) 1998-12-02
DE69700059D1 (en) 1999-01-14
FR2745588B1 (en) 1998-04-30
WO1997032052A1 (en) 1997-09-04

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