WO2013034851A1 - Method for preparing test parts for the mechanical characterisation of a titanium alloy - Google Patents

Method for preparing test parts for the mechanical characterisation of a titanium alloy Download PDF

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Publication number
WO2013034851A1
WO2013034851A1 PCT/FR2012/051987 FR2012051987W WO2013034851A1 WO 2013034851 A1 WO2013034851 A1 WO 2013034851A1 FR 2012051987 W FR2012051987 W FR 2012051987W WO 2013034851 A1 WO2013034851 A1 WO 2013034851A1
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WIPO (PCT)
Prior art keywords
temperature
billet
microstructure
forging
titanium alloy
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PCT/FR2012/051987
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French (fr)
Inventor
Adeline BENETEAU
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Snecma
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Publication date
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Publication of WO2013034851A1 publication Critical patent/WO2013034851A1/en

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/183High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/026Specifications of the specimen
    • G01N2203/0298Manufacturing or preparing specimens

Definitions

  • the present invention relates to the field of the forging of titanium alloy parts, the titanium alloy having a ⁇ -domain at a temperature higher than the ⁇ -transus temperature, and aims at a method of producing by forging a roll of alloy of titanium having, at least in part, a "skin forge" type microstructure comprising alpha needles, thick, numerous and fragmented, so as to allow the extraction of mechanical characterization specimens of the material thus produced.
  • Titanium alloys because of their high strength / mass ratios are used in the aeronautical field, in particular for making turbomachine parts, subjected to high stresses and high temperatures of up to 600 ° C.
  • Pure titanium exists in two crystallographic forms: The phase a compact hexagonal structure is stable at room temperature, and the ⁇ phase of cubic structure centered is stable above the temperature called ⁇ -transus or transus ⁇ , which is equal to 883 ° C for pure titanium.
  • ⁇ -transus temperature On the phase diagrams of titanium alloys combined with other elements, we find the ⁇ phase above the ⁇ -transus temperature, and below this temperature a balance between the ⁇ phase and the ⁇ phase whose proportions depend on the alloying elements.
  • the ⁇ - ⁇ microstructure consists of a mixture of phase a and phase ⁇ .
  • the alloy elements have the effect in particular of varying the ⁇ -transus temperature around 883 ° C.
  • the development of a titanium alloy having the desired properties includes selecting alloying elements, and choosing the thermomechanical treatment undergone by the alloy.
  • the present applicant has developed processes for forging titanium alloy mechanical parts, for example the processes described in patent applications WO2010031982, WO2010031985, FR2952559 and FR2899241.
  • a process for manufacturing alloy compressor disks Til7, whose formula is ⁇ -5 ⁇ 1-2Sn-2Zr-4Mo-4Cr, comprises several forging steps, one of which is carried out in the ⁇ -domain, ie ie, whose stamping operation is performed at a temperature above the ⁇ -transus temperature.
  • a means for characterizing a metallic material consists of extracting specimens of this material and subjecting them to mechanical tests to determine their mechanical characteristics at ambient temperature and at the temperatures of use: Young's modulus, elongation at break, resistance tensile strength, elastic limit, oligocyclic or vibratory fatigue, more particularly fatigue failure limit, etc.
  • the Applicant has set itself the objective of reproducing the desired microstructure in sufficient quantity to allow the machining of at least one specimen with which it will be possible to carry out mechanical characterization, fatigue or other tests.
  • the method according to the invention for manufacturing one or more test specimens for the mechanical characterization of a titanium alloy with a ⁇ -transus temperature, ⁇ , having a microstructure of forge skin type with thick and fragmented needles, includes the following steps:
  • the method of the invention has the advantage of providing, by simple forging operations, any desired quantity of material for the analysis of the mechanical properties.
  • the parameters being perfectly defined, the method makes it possible to extract the specimens reproducibly on a large number of rollers.
  • the method is directed in particular to the Til7 alloy because of the application thereof to the manufacture of parts such as DAM type compressor discs, which is the acronym for monobloc blisk, where the blades form a single blade. block with the disc being obtained by machining a forged disc blank.
  • the present process is applicable to other equivalent titanium alloys such as the ⁇ 6242 alloy or any other titanium alloy used to obtain a final beta-shaped workpiece.
  • the heating temperature T2 in the second oven is between 750 ° C and 850 ° C; it is chosen according to the family of microstructure that one wishes to obtain.
  • the heating time is preferably 2 hours longer.
  • the forging dies are heated and are preferably maintained at a temperature between T2 minus 50 ° C (T2-50 ° C) and T2.
  • the overall deformation rate ⁇ is less than 2, preferably between 1 and 1.5.
  • the overall deformation rate ⁇ is defined as the logarithm of the ratio of the height or thickness of the billet before deformation and its thickness after deformation: If the part is not deformed, the deformation ratio is equal to 0. It has been found that that the deformation of the slug should be sufficient, therefore> 0.5, to obtain the formation of a microstructure of "forge skin" type.
  • the present invention also relates to a method for controlling a beta-forged titanium alloy having a forge-skin type microstructure with thick and fragmented needles comprising the manufacture of a test piece according to the above method and then the submission. from the test piece to mechanical characterization tests.
  • FIG. 1 shows schematically the various steps of preparation of a roller having the desired microstructure
  • FIG. 2 is a photograph of a section of a roller obtained by the method illustrated in Figure 1;
  • FIGS. 3 and 4 are optical micrographs of the two distinct zones of the section of the roller of FIG. 2
  • the method comprises a step of producing a billet of titanium alloy such as Ti 17 in which cylindrical slugs L are taken.
  • the slugs have a height of 160 mm for a diameter of 80 mm. They are then enamelled; enamel having a lubricating function.
  • a billet L is placed in a furnace 1.
  • the slug is maintained at this temperature for 2h30, long enough for the temperature of the slug to be substantially homogeneous and equal to T1.
  • step B The billet is taken out of the oven 1 and then transferred to a second furnace 2 in which, step B, it is maintained at a temperature T2, lower than the ⁇ -transus temperature. As for the previous heating, the billet is maintained at this temperature T2 sufficiently long, about 2 hours to 2:30, so that its temperature is homogenized. During this step B, thick needles are formed in the ⁇ matrix.
  • step C the billet is transferred rapidly, in less than 30s, to a press 3, for example a 1000 ton Cosmo press where it undergoes the forging operation, stage D, and is shaped into matrices which are heated to a temperature between T2-50 ° C and T2, here the matrices are flat.
  • the forging is done at this temperature.
  • the displacement of the upper slider supporting the upper die is determined by the desired strain rate ⁇ for the slug. Rates ⁇ of between 1 and 1.5 are suitable for obtaining the desired structure.
  • the slug took the form of a pebble which after cooling with air is heat-treated T3, R2, step E.
  • the treatment T3 comprises heating at 800 ° C for 4 h followed by quenching with water and the Treatment R2 comprises heating at 625 ° C for 8 h followed by quenching in air.
  • the rolls thus obtained are ready for one or more cylindrical cylindrical test pieces to be taken there to undergo the mechanical characterization tests.
  • the roller is shown in axial section in FIG. 2.
  • the first zone I has a microstructure, called a forge-skin type, which is characterized by the presence of ⁇ , or short-needle, apertures at the grain boundaries or generalized, formed during forging, by fragmentation of the thick needles appeared in the furnace T2. It was noted that different families of microstructures were obtained depending on the forging temperature between 750 ° C and 850 ° C.
  • the second zone II is a dead zone in which the rate of local deformation is zero or very low.

Abstract

The invention relates to a method for manufacturing one or more test parts for the mechanical characterisation of a forged titanium alloy β, having a forge-skin microstructure with thick, fragmented needles, said method including the following steps: a) manufacturing a billet using said alloy, and sampling a cylindrical slug in the billet; b) heating the slug in a kiln (1) at a dissolution temperature T1, which is higher than the temperature Τβ, for a period of time t1 for rendering the temperature uniform; c) transferring the slug into a kiln (2) at a temperature T2, which is lower than Τβ, for a period of time t2 for rendering the temperature uniform; d) forging a roller by means of the hot axial die-forging of the slug, the deformation rate ε being higher than 0.5 (ε>0.5), so as to obtain said microstructure, followed by cooling to ambient temperature; and e) heat-treating the resulting roller, and machining of test parts for mechanical characterisation in the portion of the roller having said microstructure.

Description

Procédé de préparation d'éprouvettes de caractérisation mécanique  Process for the preparation of mechanical characterization specimens
d'un alliage de titane  of a titanium alloy
La présente invention concerne le domaine du forgeage de pièces en alliage de titane, l'alliage de titane ayant un domaine β à une température supérieure à la température β-transus, et vise un procédé de réalisation par forgeage d'un galet en alliage de titane présentant, au moins en partie, une microstructure de type « peau de forge » comprenant des aiguilles alpha, épaisses, nombreuses et fragmentées, de manière à en permettre l'extraction d'éprouvettes de caractérisation mécanique du matériau ainsi réalisé. The present invention relates to the field of the forging of titanium alloy parts, the titanium alloy having a β-domain at a temperature higher than the β-transus temperature, and aims at a method of producing by forging a roll of alloy of titanium having, at least in part, a "skin forge" type microstructure comprising alpha needles, thick, numerous and fragmented, so as to allow the extraction of mechanical characterization specimens of the material thus produced.
Art antérieur Prior art
Les alliages de titane en raison de leurs rapports résistance/masse élevés sont utilisés dans le domaine aéronautique, en particulier pour fabriquer des pièces de turbomachine, soumises à des contraintes importantes et à des températures élevées pouvant aller jusqu'à 600°C. Le titane pur existe sous deux formes cristallographiques : La phase a de structure hexagonale compacte est stable à température ambiante, et la phase β de structure cubique centrée est stable au dessus de la température appelée β-transus ou transus β, qui est égale à 883°C pour le titane pur. Sur les diagrammes de phase d'alliages de titane alliés à d'autres éléments, on retrouve la phase β au dessus de la température β-transus, et en dessous de cette température un équilibre entre la phase β et la phase a dont les proportions dépendent des éléments d'alliage. La microstructure α-β est constituée d'un mélange de phase a et de phase β. Les éléments alliés ont notamment pour effet de faire varier la température β-transus autour de 883°C. La mise au point d'un alliage de titane possédant les propriétés voulues consiste notamment à sélectionner des éléments d'alliage, et à choisir le traitement thermomécanique subi par l'alliage. Le présent demandeur a développé des procédés de forgeage de pièces mécaniques en alliage de titane dont par exemple les procédés décrits dans les demandes de brevet WO2010031982, WO2010031985, FR2952559 et FR2899241. Un procédé de fabrication de disques de compresseur en alliage Til7, dont la formule est ΤΊ-5Α1- 2Sn-2Zr-4Mo-4Cr, comprend plusieurs étapes de forgeage dont l'une est effectuée dans le domaine β, c'est-à-dire dont l'opération de matriçage est effectuée à une température supérieure à la température β-transus. Il se forme en surface de ces pièces des zones dont les propriétés mécaniques sont moindres et dont la microstructure présente des aiguilles ou navettes de phase alpha, relativement épaisses. Ces zones constituent ce que l'on désigne par l'expression de « peau de forge ». L'épaisseur de cette dernière varie selon la forme de la pièce forgée et aussi selon les paramètres du procédé de forgeage dans le domaine β de celle-ci. Elle peut aller, pour un disque de compresseur, de 0 à 10 mm. Cette microstructure apparaît si le procédé utilisé est un forgeage à l'air libre en matrices chaudes. Plus la température des matrices se rapproche de la température de la pièce à forger (forgeage quasi-isotherme), plus l'épaisseur de la microstructure de type « peau de forge » diminue. Titanium alloys because of their high strength / mass ratios are used in the aeronautical field, in particular for making turbomachine parts, subjected to high stresses and high temperatures of up to 600 ° C. Pure titanium exists in two crystallographic forms: The phase a compact hexagonal structure is stable at room temperature, and the β phase of cubic structure centered is stable above the temperature called β-transus or transus β, which is equal to 883 ° C for pure titanium. On the phase diagrams of titanium alloys combined with other elements, we find the β phase above the β-transus temperature, and below this temperature a balance between the β phase and the α phase whose proportions depend on the alloying elements. The α-β microstructure consists of a mixture of phase a and phase β. The alloy elements have the effect in particular of varying the β-transus temperature around 883 ° C. The development of a titanium alloy having the desired properties includes selecting alloying elements, and choosing the thermomechanical treatment undergone by the alloy. The present applicant has developed processes for forging titanium alloy mechanical parts, for example the processes described in patent applications WO2010031982, WO2010031985, FR2952559 and FR2899241. A process for manufacturing alloy compressor disks Til7, whose formula is ΤΊ-5Α1-2Sn-2Zr-4Mo-4Cr, comprises several forging steps, one of which is carried out in the β-domain, ie ie, whose stamping operation is performed at a temperature above the β-transus temperature. On the surface of these parts, areas are formed whose mechanical properties are lower and the microstructure of which has relatively thick needles or alpha phase shuttles. These areas constitute what is known as the expression of "Blacksmith skin" The thickness of the latter varies according to the shape of the forging and also according to the parameters of the forging process in the β domain thereof. It can go, for a compressor disk, from 0 to 10 mm. This microstructure appears if the process used is forging in the open air in hot matrices. The more the temperature of the dies approaches the temperature of the part to be forged (quasi-isothermal forging), the more the thickness of the microstructure of the "forge skin" type decreases.
Il serait souhaitable de pouvoir caractériser le matériau dans cette zone, c'est-à-dire d'en analyser les propriétés mécaniques, dans le but d'en évaluer son acceptabilité sur pièces. En effet dans la mesure où sur les pièces telles que les disques en alliage de titane forgés dans le domaine β, des structures de type peau de forge sont formées et si ces structures s'étendent jusque dans la pièce pré-usinée, elles entraînent une mise sous dérogation et des contrôles supplémentaires pour décider si la pièce doit être rebutée ou non. It would be desirable to be able to characterize the material in this zone, that is to say to analyze the mechanical properties, in order to evaluate its acceptability on parts. Indeed, on the parts such as titanium alloy discs forged in the β domain, forge skin type structures are formed and if these structures extend into the pre-machined part, they cause a override and additional controls to decide whether the part should be discarded or not.
Un moyen pour caractériser un matériau métallique consiste à extraire des éprouvettes de ce matériau et à les soumettre à des tests mécaniques pour en déterminer des caractéristiques mécaniques à température ambiante et aux températures d'utilisation : module d'Young, allongement à la rupture, résistance à la traction, limite élastique, fatigue oligocyclique ou vibratoire, plus particulièrement limite de rupture en fatigue, etc. Pour que la partie utile de l'éprouvette mécanique contienne un volume de matière représentatif, il est préférable d'utiliser des éprouvettes à fût cylindrique plutôt que des éprouvettes plates. A means for characterizing a metallic material consists of extracting specimens of this material and subjecting them to mechanical tests to determine their mechanical characteristics at ambient temperature and at the temperatures of use: Young's modulus, elongation at break, resistance tensile strength, elastic limit, oligocyclic or vibratory fatigue, more particularly fatigue failure limit, etc. In order for the useful part of the mechanical test piece to contain a representative volume of material, it is preferable to use cylindrical test pieces rather than flat test pieces.
Cependant dans les conditions usuelles de forgeage, l'épaisseur obtenue est trop faible pour que l'on puisse en extraire des éprouvettes de caractérisation mécanique à fût cylindrique. Une solution serait de dégrader volontairement les conditions de forgeage d'une pièce sacrifiée, un disque de compresseur en ΤΊ17, pour obtenir une microstructure de type peau de forge en forte épaisseur. Mais une telle méthode serait coûteuse à mettre en œuvre à la fois en temps et en pièces sacrifiées car elle demanderait, pour chaque condition testée, à réitérer les essais avec modification des paramètres de forgeage jusqu'à obtenir l'épaisseur recherchée. Exposé de l'invention However, under the usual forging conditions, the thickness obtained is too small to extract cylindrical barrel mechanical characterization specimens. One solution would be to voluntarily degrade the forging conditions of a sacrificed part, a compressor disc in ΤΊ17, to obtain a microstructure of forge skin type in thick. But such a method would be expensive to implement both time and sacrificed parts because it would require, for each condition tested, to repeat the tests with modification of the forging parameters to obtain the desired thickness. Presentation of the invention
C'est ainsi que la demanderesse s'est fixé comme objectif de reproduire la microstructure recherchée en quantité suffisante pour permettre l'usinage d'au moins une éprouvette avec laquelle on pourra réaliser des essais de caractérisation mécanique, de fatigue ou autre. Thus, the Applicant has set itself the objective of reproducing the desired microstructure in sufficient quantity to allow the machining of at least one specimen with which it will be possible to carry out mechanical characterization, fatigue or other tests.
Le procédé conforme à l'invention, de fabrication d'une ou plusieurs éprouvettes de caractérisation mécanique d'un alliage de titane avec une température β-transus, Τβ, présentant une microstructure de type peau de forge avec des aiguilles a épaisses et fragmentées, comprend les étapes suivantes: The method according to the invention, for manufacturing one or more test specimens for the mechanical characterization of a titanium alloy with a β-transus temperature, Τβ, having a microstructure of forge skin type with thick and fragmented needles, includes the following steps:
Réalisation d'une billette en ledit alliage,  Producing a billet of said alloy,
Prélèvement d'un lopin de forme cylindrique dans la billette,  Sampling of a cylindrical slug in the billet,
Chauffage du lopin dans un four à une température Tl de mise en solution, supérieure à la température Τβ, pendant une durée tl d'homogénéisation de la température. Transfert du lopin dans un four à une température T2 inférieure à Heating the slug in an oven at a solution temperature Tl, higher than the temperature Τβ, for a time tl homogenization of the temperature. Transfer of the slug in an oven to a temperature T2 lower than
Τβ, pendant une durée t2 d'homogénéisation de la température. Forgeage d'un galet par matriçage axial à chaud du lopin, le taux de déformation ε étant supérieur à 0,5, ε>0,5, de manière à obtenir ladite microstructure, puis refroidissement à la température ambiante ; Ββ during a time t2 for homogenizing the temperature. Forging a roller by axial die stamping of the billet, the deformation rate ε being greater than 0.5, ε> 0.5, so as to obtain said microstructure, then cooling to room temperature;
- Traitement thermique du galet obtenu ;  - Heat treatment of the wheel obtained;
Extraction d' éprouvettes de caractérisation mécanique dans la partie du galet présentant ladite microstructure.  Extraction of mechanical characterization specimens in the part of the roller having said microstructure.
Le procédé de l'invention présente l'avantage de mettre à disposition, par des opérations de forge simples, toute quantité souhaitée de matériau pour l'analyse des propriétés mécaniques. En outre, les paramètres étant parfaitement définis, la méthode permet d'extraire les éprouvettes de manière reproductible sur un grand nombre de galets. The method of the invention has the advantage of providing, by simple forging operations, any desired quantity of material for the analysis of the mechanical properties. In addition, the parameters being perfectly defined, the method makes it possible to extract the specimens reproducibly on a large number of rollers.
La méthode vise en particulier l'alliage Til7 en raison de l'application de celui-ci à la fabrication de pièces telles que les disques de compresseur de type DAM, qui est l'acronyme de disque aubagé monobloc, où les aubes forment un seul bloc avec le disque en étant obtenus par usinage d'une ébauche de disque forgée. Le présent procédé s'applique à d'autres alliages de titane équivalents tels que l'alliage ΤΊ6242 ou tout autre alliage de titane utilisé pour obtenir une pièce à mise en forme finale dans le domaine bêta. The method is directed in particular to the Til7 alloy because of the application thereof to the manufacture of parts such as DAM type compressor discs, which is the acronym for monobloc blisk, where the blades form a single blade. block with the disc being obtained by machining a forged disc blank. The present process is applicable to other equivalent titanium alloys such as the ΤΊ6242 alloy or any other titanium alloy used to obtain a final beta-shaped workpiece.
De préférence, la température de chauffage d'homogénéisation est Tl = Τβ + 25°C soit environ 915°C pour le Til7 pendant une durée de 2 heures, Τβ se situant entre 880°C et 900°C. Preferably, the homogenization heating temperature is Tl = Τβ + 25 ° C, ie about 915 ° C for the Til7 for a period of 2 hours, Τβ being between 880 ° C and 900 ° C.
De préférence encore, la température T2 de chauffage dans le second four est comprise entre 750°C et 850°C ; elle est choisie en fonction de la famille de microstructure que l'on souhaite obtenir. La durée de chauffage est de préférence encore de 2 heures. More preferably, the heating temperature T2 in the second oven is between 750 ° C and 850 ° C; it is chosen according to the family of microstructure that one wishes to obtain. The heating time is preferably 2 hours longer.
Conformément à une autre caractéristique, les matrices de forgeage sont chauffées et sont de préférence maintenues à une température comprise entre T2 moins 50°C (T2-50°C) et T2. According to another characteristic, the forging dies are heated and are preferably maintained at a temperature between T2 minus 50 ° C (T2-50 ° C) and T2.
Conformément à une autre caractéristique, le taux de déformation global ε est inférieur à 2, de préférence entre 1 et 1,5. Le taux de déformation global ε est défini comme le logarithme du rapport de la hauteur ou épaisseur du lopin avant déformation et de son épaisseur après déformation : Si la pièce n'est pas déformée, le taux de déformation est égal à 0. On a constaté que la déformation du lopin devait être suffisante, donc >0,5, pour obtenir la formation d'une microstructure de type « peau de forge ». According to another characteristic, the overall deformation rate ε is less than 2, preferably between 1 and 1.5. The overall deformation rate ε is defined as the logarithm of the ratio of the height or thickness of the billet before deformation and its thickness after deformation: If the part is not deformed, the deformation ratio is equal to 0. It has been found that that the deformation of the slug should be sufficient, therefore> 0.5, to obtain the formation of a microstructure of "forge skin" type.
La présente invention porte également sur un procédé de contrôle d'un alliage de titane forgé béta, présentant une microstructure de type peau de forge avec des aiguilles a épaisses et fragmentées comprenant la fabrication d'une éprouvette selon le procédé ci-dessus puis la soumission de l'éprouvette à des essais de caractérisation mécanique. The present invention also relates to a method for controlling a beta-forged titanium alloy having a forge-skin type microstructure with thick and fragmented needles comprising the manufacture of a test piece according to the above method and then the submission. from the test piece to mechanical characterization tests.
Présentation des figures Presentation of figures
L'invention sera mieux comprise, et d'autres buts, détails, caractéristiques et avantages de celle- ci apparaîtront plus clairement au cours de la description explicative détaillée qui va suivre, mode de réalisation de l'invention donné à titre d'exemple purement illustratif et non limitatif, en référence aux dessins annexés. The invention will be better understood, and other objects, details, features and advantages thereof will become more apparent in the following detailed explanatory description, embodiment of the invention given by way of example purely illustrative and not limiting, with reference to the accompanying drawings.
Sur ces dessins : - La figure 1 représente de façon schématique les différentes étapes de préparation d'un galet présentant la microstructure souhaitée ; On these drawings: - Figure 1 shows schematically the various steps of preparation of a roller having the desired microstructure;
- La figure 2 est une photographie d'une coupe d'un galet obtenu par le procédé illustré par la figure 1 ;  - Figure 2 is a photograph of a section of a roller obtained by the method illustrated in Figure 1;
- les figures 3 et 4 sont des micrographies optiques des deux zones distinctes de la coupe du galet de la figure 2  FIGS. 3 and 4 are optical micrographs of the two distinct zones of the section of the roller of FIG. 2
Description détaillée d'un mode de réalisation de l'invention Detailed description of an embodiment of the invention
Le procédé comprend une étape de réalisation d'une billette d'alliage de titane tel que Ti 17 dans laquelle on prélève des lopins cylindriques L. Dans l'exemple considéré les lopins ont une hauteur de 160 mm pour un diamètre de 80 mm. Ils sont ensuite émaillés ; l'émail ayant une fonction de lubrification. Comme on le voit sur la figure 1, on dispose un lopin L dans un four 1. Etape A, le lopin est chauffé à une température Tl supérieure à la température β-transus pour cet alliage soit Tp+25°C = 915°C environ pour l'alliage ΤΊ17. Le lopin est maintenu à cette température pendant 2h30, suffisamment longtemps pour que la température du lopin soit sensiblement homogène et égale à Tl. Le lopin est sorti du four 1 puis est transféré dans un second four 2 dans lequel, étape B, il est maintenu à une température T2, inférieure à la température β-transus. Comme pour le chauffage précédent, le lopin est maintenu à cette température T2 suffisamment longtemps, environ 2h à 2h30, pour que sa température soit homogénéisée. Au cours de cette étape B, des aiguilles a épaisses se forment dans la matrice β. The method comprises a step of producing a billet of titanium alloy such as Ti 17 in which cylindrical slugs L are taken. In the example in question, the slugs have a height of 160 mm for a diameter of 80 mm. They are then enamelled; enamel having a lubricating function. As can be seen in FIG. 1, a billet L is placed in a furnace 1. Stage A, the slug is heated to a temperature T1 higher than the β-transus temperature for this alloy, ie Tp + 25 ° C. = 915 ° C. about for the alloy ΤΊ17. The slug is maintained at this temperature for 2h30, long enough for the temperature of the slug to be substantially homogeneous and equal to T1. The billet is taken out of the oven 1 and then transferred to a second furnace 2 in which, step B, it is maintained at a temperature T2, lower than the β-transus temperature. As for the previous heating, the billet is maintained at this temperature T2 sufficiently long, about 2 hours to 2:30, so that its temperature is homogenized. During this step B, thick needles are formed in the β matrix.
Dans l'étape C suivante le lopin est transféré rapidement, en moins de 30s, dans une presse 3, par exemple une presse Cosmo 1000 tonnes où il subit l'opération de forgeage, étape D, et est mis en forme dans des matrices qui sont chauffées à une température comprise entre T2-50°C et T2, ici les matrices sont planes. Le forgeage est donc effectué à cette température. Le déplacement du coulisseau supérieur supportant la matrice supérieure est déterminé par le taux de déformation ε voulu pour le lopin. Des taux ε compris entre 1 et 1,5 conviennent pour obtenir la structure souhaitée. Le lopin a pris la forme d'un galet qui après refroidissement à l'air est traité thermiquement T3, R2, étape E. Le traitement T3 comprend un chauffage à 800°C pendant 4h suivi d'une trempe à l'eau et le traitement R2 comprend un chauffage à 625°C pendant 8h suivi d'une trempe à l'air. Les galets ainsi obtenus sont prêts pour qu'y soit prélevées une ou plusieurs éprouvettes mécaniques à fût cylindrique pour subir les essais mécaniques de caractérisation.. In the following step C the billet is transferred rapidly, in less than 30s, to a press 3, for example a 1000 ton Cosmo press where it undergoes the forging operation, stage D, and is shaped into matrices which are heated to a temperature between T2-50 ° C and T2, here the matrices are flat. The forging is done at this temperature. The displacement of the upper slider supporting the upper die is determined by the desired strain rate ε for the slug. Rates ε of between 1 and 1.5 are suitable for obtaining the desired structure. The slug took the form of a pebble which after cooling with air is heat-treated T3, R2, step E. The treatment T3 comprises heating at 800 ° C for 4 h followed by quenching with water and the Treatment R2 comprises heating at 625 ° C for 8 h followed by quenching in air. The rolls thus obtained are ready for one or more cylindrical cylindrical test pieces to be taken there to undergo the mechanical characterization tests.
On a représenté le galet vu en coupe axiale sur la figure 2. On distingue une première zone I en forme de sablier couché et deux zones II l'une supérieure, l'autre inférieure, de part et d'autre de la partie centrale du sablier. The roller is shown in axial section in FIG. 2. There is a first zone I in the shape of a coated hourglass and two zones II, one upper and the other lower, on either side of the central portion of the hourglass.
Comme on le voit sur les figures 3 et 4, la première zone I présente une microstructure, dite de type peau de forge, qui se caractérise par la présence de navettes a, ou aiguilles a courtes, aux joints de grains ou bien généralisées, formées, lors du forgeage, par fragmentation des aiguilles a épaisses apparues dans le four T2. On a noté que l'on obtenait différentes familles de microstructure selon la température de forgeage entre 750°C et 850°C. La seconde zone II est une zone morte dans laquelle le taux de déformation local est nul ou très faible. As can be seen in FIGS. 3 and 4, the first zone I has a microstructure, called a forge-skin type, which is characterized by the presence of α, or short-needle, apertures at the grain boundaries or generalized, formed during forging, by fragmentation of the thick needles appeared in the furnace T2. It was noted that different families of microstructures were obtained depending on the forging temperature between 750 ° C and 850 ° C. The second zone II is a dead zone in which the rate of local deformation is zero or very low.

Claims

Revendications claims
1. Procédé de fabrication d'au moins une éprouvette de caractérisation mécanique d'un alliage de titane forgé β, présentant une microstructure de type peau de forge avec des aiguilles a épaisses et fragmentées, comprenant les étapes suivantes: A method of manufacturing at least one specimen for the mechanical characterization of a forged β titanium alloy, having a forge-skin type microstructure with thick and fragmented needles, comprising the following steps:
a. Réalisation d'une billette en ledit alliage,- Prélèvement d'un lopin de forme cylindrique dans la billette,  at. Production of a billet made of said alloy, - sampling of a billet of cylindrical shape in the billet,
b. Chauffage du lopin dans un four (1) à une température Tl de mise en solution, supérieure à la température Τβ, pendant une durée tl d'homogénéisation de la température, ,  b. Heating the slug in an oven (1) at a solution temperature Tl, higher than the temperature Τβ, during a time tl homogenization of the temperature,,
c. Transfert du lopin dans un four (2) à une température T2 inférieure à Τβ, pendant une durée t2 d'homogénéisation de la température,  vs. Transfer of the billet in an oven (2) to a temperature T2 less than Τβ, during a period t2 of homogenizing the temperature,
d. Forgeage d'un galet par matriçage axial à chaud du lopin, le taux de déformation ε étant supérieur à 0,5, ε>0,5, de manière à obtenir ladite microstructure, puis refroidissement à la température ambiante.  d. Forging a roller by axial die stamping of the billet, the deformation rate ε being greater than 0.5, ε> 0.5, so as to obtain said microstructure, then cooling to room temperature.
e. Traitement thermique du galet obtenu,- usinage d'éprouvettes de caractérisation mécanique dans la partie du galet présentant ladite microstructure,  e. Heat treatment of the obtained roller, - machining of mechanical characterization specimens in the part of the roller having said microstructure,
2. Procédé selon la revendication 1, l'alliage de titane étant l'alliage Til7. 2. Method according to claim 1, the titanium alloy being the Til7 alloy.
3. Procédé selon l'une des revendications précédentes, avec Tl= Tp+25°C. 3. Method according to one of the preceding claims, with Tl = Tp + 25 ° C.
4. Procédé selon la revendication 2, T2 étant compris entre 750 et 850°C. 4. Method according to claim 2, T2 being between 750 and 850 ° C.
5. Procédé selon l'une des revendications précédentes, les matrices de forgeage étant à une température comprise entre T2-50°C et T2. 5. Method according to one of the preceding claims, the forging dies being at a temperature between T2-50 ° C and T2.
6. Procédé selon l'une des revendications précédentes, le taux de déformation global ε étant inférieur à 2, de préférence entre 1 et 1,5. 6. Method according to one of the preceding claims, the overall deformation rate ε being less than 2, preferably between 1 and 1.5.
7. Procédé selon la revendication 2 dont le traitement thermique comprend une étape de chauffage à 800°C pendant 4 heures puis un refroidissement et une étape de chauffage à 625°C pendant 8 heures suivi d'un refroidissement à l'air. 7. The method of claim 2, the heat treatment comprises a heating step at 800 ° C for 4 hours and cooling and a heating step at 625 ° C for 8 hours followed by cooling in air.
8. Procédé de contrôle d'un alliage de titane forgé béta, présentant une microstructure de type peau de forge avec des aiguilles a épaisses et fragmentées comprenant la fabrication d'une éprouvette selon le procédé de l'une des revendications précédentes puis la soumission de Γ éprouvette à des essais de caractérisation mécanique. 8. A method for controlling a beta-forged titanium alloy, having a forging-skin type microstructure with thick and fragmented needles, comprising the manufacture of a test piece according to the method of one of the preceding claims and then the submission of Γ test specimen with mechanical characterization tests.
PCT/FR2012/051987 2011-09-05 2012-09-05 Method for preparing test parts for the mechanical characterisation of a titanium alloy WO2013034851A1 (en)

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