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EP3320287B1 - Method for heat treating a preform made of titanium alloy powder - Google Patents

Method for heat treating a preform made of titanium alloy powder Download PDF

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Publication number
EP3320287B1
EP3320287B1 EP16750926.4A EP16750926A EP3320287B1 EP 3320287 B1 EP3320287 B1 EP 3320287B1 EP 16750926 A EP16750926 A EP 16750926A EP 3320287 B1 EP3320287 B1 EP 3320287B1
Authority
EP
European Patent Office
Prior art keywords
preform
titanium
holder
based alloy
sintering
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.)
Active
Application number
EP16750926.4A
Other languages
German (de)
French (fr)
Other versions
EP3320287A1 (en
Inventor
Guillaume Fribourg
Jean-Claude Bihr
Clément GILLOT
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.)
Safran Aircraft Engines SAS
Alliance Systems Inc
Original Assignee
Safran Aircraft Engines SAS
Alliance Systems Inc
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Publication date
Application filed by Safran Aircraft Engines SAS, Alliance Systems Inc filed Critical Safran Aircraft Engines SAS
Publication of EP3320287A1 publication Critical patent/EP3320287A1/en
Application granted granted Critical
Publication of EP3320287B1 publication Critical patent/EP3320287B1/en
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • 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
    • B22F3/003—Apparatus, e.g. furnaces
    • 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
    • B22F3/10—Sintering only
    • 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
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C16/00—Alloys based on zirconium
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D3/00—Charging; Discharging; Manipulation of charge
    • F27D3/12—Travelling or movable supports or containers for the charge
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D5/00—Supports, screens, or the like for the charge within the furnace
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D5/00—Supports, screens, or the like for the charge within the furnace
    • F27D5/0006—Composite supporting structures
    • F27D5/0018—Separating elements
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D5/00—Supports, screens, or the like for the charge within the furnace
    • F27D5/0062—Shields for the charge
    • 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
    • B22F3/10—Sintering only
    • B22F2003/1042—Sintering only with support for articles to be sintered
    • B22F2003/1046—Sintering only with support for articles to be sintered with separating means for articles to be sintered
    • 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
    • B22F2203/00—Controlling
    • B22F2203/11—Controlling temperature, temperature profile
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/20—Refractory metals
    • B22F2301/205—Titanium, zirconium or hafnium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • 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
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/04—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of turbine blades
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium

Definitions

  • the present invention relates to the general field of heat treatments of powder preforms.
  • the invention applies more particularly, but not exclusively, to the sintering of preforms of three-dimensional parts obtained by shaping a titanium-based alloy powder.
  • the sintering of the preform consists of a heat treatment at high temperature (typically the sintering temperature is between 70% and 99% of the melting temperature of the material forming the powder of the preform, or even greater than this melting temperature in the case of a liquid phase sintering), intended to densify the powder in order to obtain a consolidated monobloc part.
  • JP-A 2006 104,559 discloses a method of heat treating a titanium-based alloy powder preform in a protective atmosphere in a chamber furnace, the preform being supported by a graphite plate having a Y 2 O diffusion-resistant layer 3 or ZrO 2 .
  • titanium-based alloys eg TiAl6V4, TiAl-48-2-2 type alloys, etc.
  • TiAl6V4, TiAl-48-2-2 type alloys, etc. which are particularly sensitive to oxidation
  • the sintering conditions must be carefully controlled to minimize contamination of the finished part in oxygen. Indeed, the presence of oxygen in the finished part significantly deteriorates its properties and mechanical strength.
  • the main purpose of the present invention is therefore to overcome such drawbacks by proposing a method of heat treatment of a powder piece preform comprising a titanium-based alloy, the process comprising the heat treatment of the preform in an oven at a temperature of predefined temperature, the preform being on a support during the heat treatment.
  • the method is characterized in that the support comprises a titanium-based alloy whose titanium mass content is greater than or equal to 45%, or a zirconium-based alloy whose zirconium content by mass is greater than or equal to 95% the support material having a melting temperature above the predefined temperature of the heat treatment, and in that an anti-diffusion barrier is disposed between the preform and the support to prevent the preform from being welded to the support .
  • the process according to the invention is notably remarkable in that the support on which the preform is placed makes it possible to reduce the oxygen contamination of the final part following the heat treatment (this heat treatment can be sintering).
  • the support comprises a high titanium mass content alloy (typically more than 45%) or a high zirconium mass content alloy (typically more than 95%), it can absorb traces of oxygen in the atmosphere present in the furnace enclosure. Indeed, titanium or zirconium can easily absorb the surrounding oxygen by oxidizing.
  • the support makes it possible to absorb the oxygen that may have already contaminated the preform.
  • titanium and zirconium are more reductive than the titanium oxide (TiO 2 ) formed during the oxidation of titanium present in the preform.
  • the support acts as an oxygen trap for the oxygen present in the preform.
  • the preform is typically disposed on a ceramic tray (for example, zirconia, alumina or yttrine). It has been observed that the ceramic tray is progressively degraded after several sintering cycles. An oxidation-reduction reaction occurs between the ceramic tray and the workpiece, resulting in the reduction of the ceramic of the tray, and the enrichment of the oxygen part.
  • a ceramic tray for example, zirconia, alumina or yttrine
  • the preform is disposed on the support it is not in contact with other tools present in the oven (such as a sole, or a ceramic tray such as those presented above), which advantageously prevents these tools from contaminating the preform.
  • the support acts as a barrier or buffer for oxygen between these tools and the preform.
  • the support consists of a material having a melting point higher than the predetermined temperature of the heat treatment (for example the temperature of a sintering stage)
  • the plate is plastically deformable, that is to say that it undergoes in particular no irreversible modifications of its structure when it is brought to this temperature. Thus, it can be reused for several heat treatment cycles without deforming.
  • the support comprises a titanium-based alloy whose titanium mass content is greater than or equal to 90%, more preferably greater than or equal to 99%.
  • the support may comprise a titanium-based alloy selected from the following: T40, T60, TiAl6V4, TiAl-48-2-2.
  • the support may comprise a zirconium-based alloy selected from Zircaloy-2, Zircaloy-4.
  • the support has a thickness of between 0.1 mm and 20 mm.
  • the anti-diffusion barrier comprises alumina or yttrium oxide (Yttrine).
  • the plate is etched.
  • stripped is meant any treatment intended to erode the upper surface of the support intended to support the preform, such as for example: by polishing, by milling, by sandblasting ... This treatment makes it possible to eliminate the oxide layer which can form on the support when it is in the presence of oxygen (the oxygen of the air for example), but also to increase the reactive surface to capture the oxygen during the heat treatment.
  • the heat treatment of the preform may be a sintering of the preform, the preset temperature of the heat treatment being the temperature of a sintering stage.
  • the invention will now be described in its application to sintering a titanium-based alloy powder part preform for the purpose of reducing oxygen contamination of the sintered workpiece.
  • the invention is not limited only to the sintering of powder preforms, but can also be implemented in any type of heat treatment requiring protection against oxidation, for example debinding a blank of powder mixed with a binder.
  • the figure 1 illustrates very schematically the chamber 2 of a furnace 1, used to carry out the high temperature sintering of a preform 3.
  • the preform 3 is made by shaping a powder of a titanium-based alloy.
  • a titanium-based alloy for example, it is possible to use alloys based on titanium such as: TiAl6V4, Ti-17, Ti-6242, Ti-5553, TiAl-48-2-2, TNMB1, etc.
  • the shaping of the powder to make the preform 3 can be done using a method of the type MIM ("Metal Injection Molding"), HIP ("Hot Isostatic Pressing"), by casting powder, by film casting (“Tape Casting”), extrusion, etc.
  • MIM Metal Injection Molding
  • HIP Hot Isostatic Pressing
  • a sole 4 disposed in the enclosure, which can also be integrated in the oven.
  • This sole 4 may consist of a molybdenum alloy plate (for example of the TZM type) or graphite. Note that in practice several soles 4 may be present in the sintering chamber. For reasons of simplification, only one sole 4 has been shown.
  • a tray 5 of ceramic material may possibly overcome the hearth 4 of the oven.
  • This ceramic tray 5 can for example comprise zirconia (ZrO 2 ), alumina (Al 2 O 3 ) or Yttrine (Y 2 O 3 ).
  • a support 6 is arranged on the ceramic plate 5.
  • This support 6, here taking the form of a support plate 6, consists of a metal or a metal alloy which has reducing properties with respect to titanium dioxide (TiO 2 ) in particular.
  • TiO 2 titanium dioxide
  • the support plate 6 then acts as an oxygen trap, not only for the oxygen present in the atmosphere of the chamber 2, but also for the oxygen present in the preform 3 which will be positioned on the support plate 6 and the tools present in the oven.
  • this support plate 6 also acts as a barrier for the oxygen present in the ceramic tray 5 and the sole 4, which can no longer reach the preform 3 during sintering.
  • the support plate 6 covers as much as possible the ceramic tray 5 or the hearth 4, in order to limit the contamination of oxygen coming from these tools.
  • the support plate 6 covers the base of the chamber 2 of the oven 1.
  • the thickness e of the support plate 6 may for example be between 0.1 mm and 20 mm.
  • Materials which have the required reducing properties may be chosen for example from titanium-based alloys or zirconium-based alloys which have mass contents in these sufficiently high elements.
  • a titanium-based alloy for the support plate 6 according to the invention preferably has a titanium mass content greater than or equal to 45%, more preferably a titanium content by mass greater than or equal to 90%, or even more preferably a content of mass of titanium greater than or equal to 99%.
  • such an alloy may be selected from the following known alloys: T40, T60, TiAl6V4, TiAl-48-2-2.
  • a zirconium-based alloy for the support plate 6 according to the invention preferably has a zirconium content greater than or equal to 95%.
  • such an alloy may be selected from the following known alloys: Zircaloy-2, Zircaloy-4.
  • the support plate 6 is preferably virtually plastically deformable at the heat treatment temperatures envisaged, which means that its mechanical properties and its shape are not affected by the temperatures to which it will be subjected. In other words, the support plate 6 must be dimensionally stable, it may however undergo slight deformations due to the mass of the part that it supports.
  • the melting temperature of the material constituting the support plate 6 is greater than the highest temperature at which it will be subjected during the heat treatment.
  • the sintering temperature is generally greater than 1100 ° C.
  • the melting temperature of the material constituting the support plate 6 is at least greater than 1100 ° C.
  • the support plate 6 it is advantageous to strip the support plate 6 before positioning it in the oven 1. To do this, it can be polished, milled or sanded. This pickling treatment makes it possible to remove any oxide layer that may have formed on the support plate 6 in the open air. In addition, the etching also makes it possible to increase the reactive surface of the support plate 6 to improve the oxygen scavenging.
  • the support plate 6 is covered at least in part with an anti-diffusion barrier 7 (for example based on alumina or yttrine), so that to prevent the preform 3 which is then positioned on the support plate 6 does not adhere with it because of the diffusion of the metal elements (by a welding-diffusion phenomenon).
  • the anti-diffusion barrier is thus disposed between the support plate 6 and the preform 3.
  • the deposition of the anti-diffusion barrier 7 can be done directly by applying a layer of powder by brush or spray from a solution.
  • an anti-diffusion barrier similar to that described above may be arranged between the ceramic plate 5 and the support plate 6 (or between the sole plate 4 and the support plate 6, if appropriate) in order to avoid that they adhere to each other.
  • sintering of the preform 3 can be carried out.
  • the operating conditions for sintering a titanium-based alloy powder preform are known to those skilled in the art. art and will not be described in more detail here.
  • the sintering of an aeronautical turbine engine turbine blade preform is carried out, shaped by a metal injection molding (MIM) process.
  • the powder used comprises a titanium-based alloy of TiAl-48-2-2 type.
  • the support plate 6 used in this example comprises a titanium-based alloy of the TiAl6V4 type, and was covered with an anti-diffusion yttrium (Yttrine) diffusion barrier by spray from a solution.
  • Yttrine anti-diffusion yttrium
  • the sintering of the preform is carried out at a temperature of between 1380 ° C. and 1445 ° C. for a period of between 2 hours and 10 hours under a neutral atmosphere of argon.
  • the oxygen content in the final piece after sintering (measured according to EN10276) is in the order of 1300 ppm.
  • the oxygen content in the part reaches 4500 ppm.
  • the use of a plate according to the invention allows to divide the oxygen contamination in the final piece by a factor of 3.5.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Powder Metallurgy (AREA)
  • Furnace Charging Or Discharging (AREA)

Description

Arrière-plan de l'inventionBackground of the invention

La présente invention se rapporte au domaine général des traitements thermiques de préformes en poudre. L'invention s'applique plus particulièrement, mais non exclusivement, au frittage de préformes de pièces tridimensionnelles obtenues par mise en forme d'une poudre d'alliage à base de titane.The present invention relates to the general field of heat treatments of powder preforms. The invention applies more particularly, but not exclusively, to the sintering of preforms of three-dimensional parts obtained by shaping a titanium-based alloy powder.

Il est aujourd'hui courant d'avoir recours à des procédés de fabrication de pièces tridimensionnelles en métal (ou alliage métallique) ou en céramique mettant en oeuvre une étape de mise en forme d'une poudre afin d'obtenir une préforme (par exemple en utilisant une technique de moulage par injection de poudre (PIM ou MIM) à l'aide d'un liant, par compression isostatique à chaud, ou encore par « tape casting »), suivie d'une étape de frittage de la préforme.It is nowadays common to use processes for manufacturing three-dimensional parts made of metal (or metal alloy) or ceramic implementing a step of forming a powder in order to obtain a preform (for example using a powder injection molding technique (PIM or MIM) using a binder, hot isostatic pressing, or "tape casting"), followed by a step of sintering the preform.

Le frittage de la préforme consiste en un traitement thermique à haute température (typiquement la température de frittage est comprise entre 70% et 99% de la température de fusion du matériau formant la poudre de la préforme, voire supérieure à cette température de fusion dans le cas d'un frittage en phase liquide), destiné à densifier la poudre afin d'obtenir une pièce monobloc consolidée. JP-A 2006 104 559 divulgue un procédé de traitement thermique d'une préforme en poudre d'alliage à base de titane dans une atmosphère protectrice dans un four à chambre, la préforme entant supportée par une plaque à graphité ayant une couche anti-diffusion à base de Y2O3 ou ZrO2.The sintering of the preform consists of a heat treatment at high temperature (typically the sintering temperature is between 70% and 99% of the melting temperature of the material forming the powder of the preform, or even greater than this melting temperature in the case of a liquid phase sintering), intended to densify the powder in order to obtain a consolidated monobloc part. JP-A 2006 104,559 discloses a method of heat treating a titanium-based alloy powder preform in a protective atmosphere in a chamber furnace, the preform being supported by a graphite plate having a Y 2 O diffusion-resistant layer 3 or ZrO 2 .

Pour les alliages à base de titane (par exemple les alliages du type TiAl6V4, TiAI-48-2-2, etc.), qui sont particulièrement sensibles à l'oxydation, les conditions de frittage doivent être soigneusement contrôlées pour minimiser la contamination de la pièce finie en oxygène. En effet, la présence d'oxygène dans la pièce finie détériore significativement ses propriétés et sa tenue mécaniques.For titanium-based alloys (eg TiAl6V4, TiAl-48-2-2 type alloys, etc.), which are particularly sensitive to oxidation, the sintering conditions must be carefully controlled to minimize contamination of the finished part in oxygen. Indeed, the presence of oxygen in the finished part significantly deteriorates its properties and mechanical strength.

Dans les conditions de frittage généralement utilisées pour ces alliages à base de titane, notamment une température de frittage supérieure à 1100°C, la contamination des pièces finies est relativement importante à la suite du frittage. Des sources d'oxygène pouvant potentiellement contaminer la pièce au cours du frittage ont été identifiées parmi les suivantes :

  • les traces de dioxygène contenues dans l'atmosphère de l'enceinte du four,
  • l'humidité du four, et
  • l'oxygène présent dans les outillages de frittage (tel que le plateau supportant le préforme ou le four lui-même).
In the sintering conditions generally used for these titanium-based alloys, especially a sintering temperature greater than 1100 ° C., the contamination of the finished parts is relatively significant following the sintering. Oxygen sources potentially contaminating the part during sintering have been identified among the following:
  • traces of oxygen contained in the atmosphere of the furnace enclosure,
  • the humidity of the oven, and
  • the oxygen present in the sintering tools (such as the tray supporting the preform or the oven itself).

Il est connu d'utiliser des « getters » d'oxygène ou pièges à oxygène, par exemple sous la forme de copeaux métalliques disposés autour de la préforme, qui absorbent l'oxygène en s'oxydant.It is known to use "getters" of oxygen or oxygen traps, for example in the form of metal chips arranged around the preform, which absorb oxygen by oxidizing.

Cependant, ces pièges à oxygène ne permettent pas d'obtenir un niveau de contamination en oxygène satisfaisant sur les alliages précités, ce qui entraîne une tenue mécanique insuffisante de la pièce finale.However, these oxygen traps do not provide a satisfactory level of oxygen contamination on the aforementioned alloys, resulting in insufficient mechanical strength of the final part.

Objet et résumé de l'inventionObject and summary of the invention

La présente invention a donc pour but principal de pallier de tels inconvénients en proposant un procédé de traitement thermique d'une préforme de pièce en poudre comprenant un alliage à base de titane, le procédé comprenant le traitement thermique de la préforme dans un four à une température prédéfinie, la préforme étant sur un support pendant le traitement thermique. Le procédé est caractérisé en ce que le support comprend un alliage à base de titane dont la teneur massique en titane est supérieure ou égale à 45%, ou un alliage à base de zirconium dont la teneur massique en zirconium est supérieure ou égale à 95%, le matériau formant le support ayant une température de fusion supérieure à la température prédéfinie du traitement thermique, et en ce qu'une barrière anti-diffusion est disposée entre la préforme et le support afin d'empêcher la soudure de la préforme sur le support.The main purpose of the present invention is therefore to overcome such drawbacks by proposing a method of heat treatment of a powder piece preform comprising a titanium-based alloy, the process comprising the heat treatment of the preform in an oven at a temperature of predefined temperature, the preform being on a support during the heat treatment. The method is characterized in that the support comprises a titanium-based alloy whose titanium mass content is greater than or equal to 45%, or a zirconium-based alloy whose zirconium content by mass is greater than or equal to 95% the support material having a melting temperature above the predefined temperature of the heat treatment, and in that an anti-diffusion barrier is disposed between the preform and the support to prevent the preform from being welded to the support .

Le procédé selon l'invention est notamment remarquable en ce que le support sur lequel est placée la préforme permet de réduire la contamination en oxygène de la pièce finale suite au traitement thermique (ce traitement thermique pouvant être un frittage).The process according to the invention is notably remarkable in that the support on which the preform is placed makes it possible to reduce the oxygen contamination of the final part following the heat treatment (this heat treatment can be sintering).

Tout d'abord, comme le support comprend un alliage à haute teneur massique en titane (typiquement plus de 45%) ou un alliage à haute teneur massique en zirconium (typiquement plus de 95%), il peut absorber les traces d'oxygène dans l'atmosphère présente dans l'enceinte du four. En effet, le titane ou le zirconium peuvent absorber facilement l'oxygène environnant en s'oxydant.First of all, since the support comprises a high titanium mass content alloy (typically more than 45%) or a high zirconium mass content alloy (typically more than 95%), it can absorb traces of oxygen in the atmosphere present in the furnace enclosure. Indeed, titanium or zirconium can easily absorb the surrounding oxygen by oxidizing.

En outre, le support permet d'absorber l'oxygène qui a pu déjà contaminer la préforme. En effet, le titane et le zirconium sont plus réducteur que l'oxyde de titane (TiO2) formé lors de l'oxydation du titane présent dans la préforme. Ainsi, le support joue le rôle d'un piège à oxygène pour l'oxygène présent dans la préforme.In addition, the support makes it possible to absorb the oxygen that may have already contaminated the preform. Indeed, titanium and zirconium are more reductive than the titanium oxide (TiO 2 ) formed during the oxidation of titanium present in the preform. Thus, the support acts as an oxygen trap for the oxygen present in the preform.

Dans l'art antérieur, lors du frittage de préformes en poudre d'alliage à base de titane, on dispose typiquement la préforme sur un plateau en céramique (par exemple en zircone, en alumine ou en Yttrine). Il a été observé que le plateau en céramique se dégrade progressivement après plusieurs cycles de frittage. Une réaction d'oxydo-réduction se produit entre le plateau céramique et la pièce, entraînant la réduction de la céramique du plateau, et l'enrichissement de la pièce en oxygène.In the prior art, during the sintering of titanium-based alloy powder preforms, the preform is typically disposed on a ceramic tray (for example, zirconia, alumina or yttrine). It has been observed that the ceramic tray is progressively degraded after several sintering cycles. An oxidation-reduction reaction occurs between the ceramic tray and the workpiece, resulting in the reduction of the ceramic of the tray, and the enrichment of the oxygen part.

Avec le procédé selon l'invention, comme la préforme est disposée sur le support elle n'est pas au contact d'autres outillages présents dans le four (comme une sole, ou un plateau en céramique tel que ceux présentés ci-dessus), ce qui évite avantageusement que ces outillages ne contaminent la préforme. En d'autres termes, le support joue un rôle de barrière ou de tampon pour l'oxygène entre ces outillages et la préforme.With the method according to the invention, as the preform is disposed on the support it is not in contact with other tools present in the oven (such as a sole, or a ceramic tray such as those presented above), which advantageously prevents these tools from contaminating the preform. In other words, the support acts as a barrier or buffer for oxygen between these tools and the preform.

Enfin, comme le support est constitué d'un matériau ayant une température de fusion supérieure à la température prédéfinie du traitement thermique (par exemple la température d'un palier de frittage), le plateau est indéformable plastiquement, c'est-à-dire qu'il ne subit notamment pas de modifications irréversibles de sa structure lorsqu'il est porté à cette température. Ainsi, il peut être réutilisé pour plusieurs cycles de traitement thermique sans se déformer.Finally, since the support consists of a material having a melting point higher than the predetermined temperature of the heat treatment (for example the temperature of a sintering stage), the plate is plastically deformable, that is to say that it undergoes in particular no irreversible modifications of its structure when it is brought to this temperature. Thus, it can be reused for several heat treatment cycles without deforming.

Dans certains modes de réalisation, le support comprend un alliage à base de titane dont la teneur massique en titane est supérieure ou égale à 90%, plus préférentiellement supérieure ou égale à 99%. Par exemple, le support peut comprendre un alliage à base de titane choisi parmi les suivants : T40, T60, TiAl6V4, TiAl-48-2-2.In some embodiments, the support comprises a titanium-based alloy whose titanium mass content is greater than or equal to 90%, more preferably greater than or equal to 99%. For example, the support may comprise a titanium-based alloy selected from the following: T40, T60, TiAl6V4, TiAl-48-2-2.

En variante, le support peut comprendre un alliage à base de zirconium choisi parmi les suivants : Zircaloy-2, Zircaloy-4.Alternatively, the support may comprise a zirconium-based alloy selected from Zircaloy-2, Zircaloy-4.

De préférence, le support présente une épaisseur comprise entre 0,1 mm et 20 mm.Preferably, the support has a thickness of between 0.1 mm and 20 mm.

De préférence également, la barrière anti-diffusion comprend de l'alumine ou de l'oxyde d'yttrium (Yttrine).Also preferably, the anti-diffusion barrier comprises alumina or yttrium oxide (Yttrine).

De préférence encore, la plaque est décapée. Par « décapée » on entend tout traitement visant à éroder la surface supérieure du support destinée à supporter la préforme, comme par exemple : par polissage, par fraisage, par sablage... Ce traitement permet d'éliminer la couche d'oxyde qui peut se former sur le support lorsqu'il est en présence d'oxygène (le dioxygène de l'air par exemple), mais aussi d'augmenter la surface réactive pour capter l'oxygène au cours du traitement thermique.More preferably, the plate is etched. By "stripped" is meant any treatment intended to erode the upper surface of the support intended to support the preform, such as for example: by polishing, by milling, by sandblasting ... This treatment makes it possible to eliminate the oxide layer which can form on the support when it is in the presence of oxygen (the oxygen of the air for example), but also to increase the reactive surface to capture the oxygen during the heat treatment.

Le traitement thermique de la préforme peut être un frittage de la préforme, la température prédéfinie du traitement thermique étant la température d'un palier de frittage.The heat treatment of the preform may be a sintering of the preform, the preset temperature of the heat treatment being the temperature of a sintering stage.

Brève description des dessinsBrief description of the drawings

D'autres caractéristiques et avantages de la présente invention ressortiront de la description faite ci-dessous, en référence aux dessins annexés qui en illustrent un exemple de réalisation dépourvu de tout caractère limitatif. Sur la figure :

  • la figure 1 est une vue schématique en coupe d'un support selon l'invention positionné dans l'enceinte d'un four et surmonté par une préforme destinée à être traitée thermiquement.
Other features and advantages of the present invention will emerge from the description given below, with reference to the accompanying drawings which illustrate an embodiment having no limiting character. On the face :
  • the figure 1 is a schematic sectional view of a support according to the invention positioned in the enclosure of an oven and surmounted by a preform intended to be heat treated.

Description détaillée de l'inventionDetailed description of the invention

L'invention va maintenant être décrite dans son application au frittage d'une préforme de pièce en poudre en alliage à base de titane dans le but de réduire la contamination en oxygène de la pièce frittée.The invention will now be described in its application to sintering a titanium-based alloy powder part preform for the purpose of reducing oxygen contamination of the sintered workpiece.

Il est à noter que l'invention ne se limite pas seulement au frittage de préformes en poudre, mais peut aussi être mise en oeuvre dans tout type de traitement thermique nécessitant une protection contre l'oxydation, par exemple le déliantage d'une ébauche de poudre mélangée à un liant.It should be noted that the invention is not limited only to the sintering of powder preforms, but can also be implemented in any type of heat treatment requiring protection against oxidation, for example debinding a blank of powder mixed with a binder.

La figure 1 illustre de façon très schématique l'enceinte 2 d'un four 1, utilisé pour réaliser le frittage à haute température d'une préforme 3.The figure 1 illustrates very schematically the chamber 2 of a furnace 1, used to carry out the high temperature sintering of a preform 3.

La préforme 3 est réalisée par mise en forme d'une poudre d'un alliage à base de titane. Par exemple, on peut utiliser des alliages à base de titane tels que : TiAl6V4, Ti-17, Ti-6242, Ti-5553, TiAl-48-2-2, TNMB1, etc.The preform 3 is made by shaping a powder of a titanium-based alloy. For example, it is possible to use alloys based on titanium such as: TiAl6V4, Ti-17, Ti-6242, Ti-5553, TiAl-48-2-2, TNMB1, etc.

De façon connue en soi, la mise en forme de la poudre pour réaliser la préforme 3 peut se faire en utilisant un procédé du type MIM (« Metal Injection Molding »), HIP (« Hot Isostatic Pressing »), par coulée de poudre, par coulée de film (« Tape Casting »), extrusion, etc.In a manner known per se, the shaping of the powder to make the preform 3 can be done using a method of the type MIM ("Metal Injection Molding"), HIP ("Hot Isostatic Pressing"), by casting powder, by film casting ("Tape Casting"), extrusion, etc.

Dans l'enceinte 2 se trouve une sole 4 disposée dans l'enceinte, qui peut aussi être intégrée au four. Cette sole 4 peut consister en une plaque en alliage de molybdène (par exemple du type TZM) ou en graphite. On notera qu'en pratique plusieurs soles 4 peuvent être présentes dans l'enceinte de frittage. Pour des raisons de simplification, une seule sole 4 a été représentée.In the chamber 2 is a sole 4 disposed in the enclosure, which can also be integrated in the oven. This sole 4 may consist of a molybdenum alloy plate (for example of the TZM type) or graphite. Note that in practice several soles 4 may be present in the sintering chamber. For reasons of simplification, only one sole 4 has been shown.

Un plateau 5 en matériau céramique peut éventuellement surmonter la sole 4 du four. Ce plateau céramique 5 peut par exemple comprendre de la zircone (ZrO2), de l'alumine (Al2O3) ou encore de l'Yttrine (Y2O3).A tray 5 of ceramic material may possibly overcome the hearth 4 of the oven. This ceramic tray 5 can for example comprise zirconia (ZrO 2 ), alumina (Al 2 O 3 ) or Yttrine (Y 2 O 3 ).

Conformément à l'invention, un support 6 est disposé sur le plateau céramique 5. Ce support 6, prenant ici la forme d'une plaque support 6, est constitué d'un métal ou d'un alliage métallique qui présente des propriétés réductrices vis-à-vis du dioxyde de titane (TiO2) notamment. La plaque support 6 joue alors le rôle de piège à oxygène, non seulement pour l'oxygène présent dans l'atmosphère de l'enceinte 2, mais aussi pour l'oxygène présent dans la préforme 3 qui sera positionnée sur la plaque support 6 et les outillages présents dans le four. En outre, cette plaque support 6 fait également office de barrière pour l'oxygène présent dans le plateau céramique 5 et la sole 4, qui ne peut plus atteindre la préforme 3 pendant le frittage.According to the invention, a support 6 is arranged on the ceramic plate 5. This support 6, here taking the form of a support plate 6, consists of a metal or a metal alloy which has reducing properties with respect to titanium dioxide (TiO 2 ) in particular. The support plate 6 then acts as an oxygen trap, not only for the oxygen present in the atmosphere of the chamber 2, but also for the oxygen present in the preform 3 which will be positioned on the support plate 6 and the tools present in the oven. In addition, this support plate 6 also acts as a barrier for the oxygen present in the ceramic tray 5 and the sole 4, which can no longer reach the preform 3 during sintering.

Il est préférable que la plaque support 6 recouvre le plus possible le plateau céramique 5 ou la sole 4, afin de limiter la contamination en oxygène provenant de ces outillages. Avantageusement, la plaque support 6 recouvre la base de l'enceinte 2 du four 1.It is preferable that the support plate 6 covers as much as possible the ceramic tray 5 or the hearth 4, in order to limit the contamination of oxygen coming from these tools. Advantageously, the support plate 6 covers the base of the chamber 2 of the oven 1.

L'épaisseur e de la plaque support 6 peut par exemple être comprise entre 0,1 mm et 20 mm.The thickness e of the support plate 6 may for example be between 0.1 mm and 20 mm.

Des matériaux qui présentent les propriétés réductrices requises peuvent être choisis par exemple parmi les alliages à base de titane ou les alliages à base de zirconium qui présentent des teneurs massique en ces éléments suffisamment élevées.Materials which have the required reducing properties may be chosen for example from titanium-based alloys or zirconium-based alloys which have mass contents in these sufficiently high elements.

Un alliage à base de titane pour la plaque support 6 conforme à l'invention présente préférentiellement une teneur massique en titane supérieure ou égale à 45%, plus préférentiellement une teneur massique en titane supérieure ou égale à 90%, ou encore plus préférentiellement une teneur massique en titane supérieure ou égale à 99%. Par exemple, un tel alliage peut être choisi parmi les alliages connus suivants : T40, T60, TiAl6V4, TiAl-48-2-2.A titanium-based alloy for the support plate 6 according to the invention preferably has a titanium mass content greater than or equal to 45%, more preferably a titanium content by mass greater than or equal to 90%, or even more preferably a content of mass of titanium greater than or equal to 99%. For example, such an alloy may be selected from the following known alloys: T40, T60, TiAl6V4, TiAl-48-2-2.

En variante, un alliage à base de zirconium pour la plaque support 6 conforme à l'invention présente préférentiellement une teneur massique en zirconium supérieure ou égale à 95%. Par exemple, un tel alliage peut être choisi parmi les alliages connus suivants : Zircaloy-2, Zircaloy-4.As a variant, a zirconium-based alloy for the support plate 6 according to the invention preferably has a zirconium content greater than or equal to 95%. For example, such an alloy may be selected from the following known alloys: Zircaloy-2, Zircaloy-4.

En outre, la plaque support 6 est de préférence quasiment indéformable plastiquement aux températures de traitement thermique envisagées, ce qui signifie que ses propriétés mécaniques et sa forme ne sont pas altérées par les températures auxquelles elle sera soumise. En d'autres termes, la plaque support 6 doit être dimensionnellement stable, elle peut subir toutefois de légères déformations dues à la masse de la pièce qu'elle supporte.In addition, the support plate 6 is preferably virtually plastically deformable at the heat treatment temperatures envisaged, which means that its mechanical properties and its shape are not affected by the temperatures to which it will be subjected. In other words, the support plate 6 must be dimensionally stable, it may however undergo slight deformations due to the mass of the part that it supports.

En pratique, la température de fusion du matériau constituant la plaque support 6 est supérieure à la température la plus élevée à laquelle elle sera soumise lors du traitement thermique. Dans le cas du frittage d'une préforme en poudre d'alliage à base de titane, la température de frittage est généralement supérieure à 1100°C. Ainsi, il faudra par exemple que la température de fusion du matériau constituant la plaque support 6 soit au moins supérieure à 1100°C.In practice, the melting temperature of the material constituting the support plate 6 is greater than the highest temperature at which it will be subjected during the heat treatment. In the case of sintering a titanium-based alloy powder preform, the sintering temperature is generally greater than 1100 ° C. Thus, it will be necessary for example that the melting temperature of the material constituting the support plate 6 is at least greater than 1100 ° C.

Il est avantageux de décaper la plaque support 6 avant de la positionner dans le four 1. Pour ce faire, on peut la polir, la fraiser ou la sabler. Ce traitement de décapage permet d'enlever l'éventuelle couche d'oxyde qui a pu se former sur la plaque support 6 à l'air libre. En outre, le décapage permet également d'augmenter la surface réactive de la plaque support 6 pour améliorer le piégeage de l'oxygène.It is advantageous to strip the support plate 6 before positioning it in the oven 1. To do this, it can be polished, milled or sanded. This pickling treatment makes it possible to remove any oxide layer that may have formed on the support plate 6 in the open air. In addition, the etching also makes it possible to increase the reactive surface of the support plate 6 to improve the oxygen scavenging.

La plaque support 6 est recouverte au moins en partie d'une barrière anti-diffusion 7 (par exemple à base d'alumine ou d'Yttrine), afin d'éviter que la préforme 3 qui est ensuite positionnée sur la plaque support 6 n'adhère avec celle-ci à cause de la diffusion des éléments métalliques (par un phénomène de soudure-diffusion). La barrière anti-diffusion est donc disposée entre la plaque support 6 et la préforme 3. Le dépôt de la barrière anti-diffusion 7 peut se faire directement en appliquant une couche de poudre par pinceau, ou par spray à partir d'une solution.The support plate 6 is covered at least in part with an anti-diffusion barrier 7 (for example based on alumina or yttrine), so that to prevent the preform 3 which is then positioned on the support plate 6 does not adhere with it because of the diffusion of the metal elements (by a welding-diffusion phenomenon). The anti-diffusion barrier is thus disposed between the support plate 6 and the preform 3. The deposition of the anti-diffusion barrier 7 can be done directly by applying a layer of powder by brush or spray from a solution.

Il est à noter également qu'une barrière anti-diffusion similaire à celle décrite ci-dessus peut être disposée entre le plateau céramique 5 et la plaque support 6 (ou entre la sole 4 et la plaque support 6, le cas échéant) afin d'éviter qu'elles n'adhèrent l'une avec l'autre.It should also be noted that an anti-diffusion barrier similar to that described above may be arranged between the ceramic plate 5 and the support plate 6 (or between the sole plate 4 and the support plate 6, if appropriate) in order to avoid that they adhere to each other.

Une fois tous les outillages et la préforme positionnés dans le four, on peut procéder au frittage de la préforme 3. Les conditions opératoires pour réaliser le frittage d'une préforme en poudre d'alliage à base de titane sont connues de l'homme de l'art et ne seront pas décrites plus en détail ici.Once all the tools and the preform are positioned in the furnace, sintering of the preform 3 can be carried out. The operating conditions for sintering a titanium-based alloy powder preform are known to those skilled in the art. art and will not be described in more detail here.

ExempleExample

On réalise le frittage d'une préforme d'aube de turbine de turbomachine aéronautique en poudre, mise en forme par un procédé de moulage par injection de métal (MIM ou « Metal Injection Molding »). La poudre utilisée comprend un alliage à base de titane du type TiAl-48-2-2.The sintering of an aeronautical turbine engine turbine blade preform is carried out, shaped by a metal injection molding (MIM) process. The powder used comprises a titanium-based alloy of TiAl-48-2-2 type.

La plaque support 6 utilisée dans cet exemple comprend un alliage à base de titane du type TiAl6V4, et a été recouverte d'une barrière anti-diffusion à base d'oxyde d'yttrium (Yttrine) par spray à partir d'une solution.The support plate 6 used in this example comprises a titanium-based alloy of the TiAl6V4 type, and was covered with an anti-diffusion yttrium (Yttrine) diffusion barrier by spray from a solution.

Le frittage de la préforme est réalisé à une température comprise entre 1380°C et 1445°C pendant une durée comprise entre 2 heures et 10 heures, sous atmosphère neutre d'argon.The sintering of the preform is carried out at a temperature of between 1380 ° C. and 1445 ° C. for a period of between 2 hours and 10 hours under a neutral atmosphere of argon.

La teneur en oxygène dans la pièce finale après le frittage (mesurée conformément à la norme EN10276) est de l'ordre de 1300 ppm. A titre de comparaison, lorsque l'on fritte la préforme dans les mêmes conditions sans utiliser une plaque selon l'invention, la teneur en oxygène dans la pièce atteint 4500 ppm. Ainsi, dans cet exemple, l'utilisation d'une plaque selon l'invention permet diviser par un facteur 3,5 la contamination en oxygène dans la pièce finale.The oxygen content in the final piece after sintering (measured according to EN10276) is in the order of 1300 ppm. By way of comparison, when the preform is sintered under the same conditions without using a plate according to the invention, the oxygen content in the part reaches 4500 ppm. Thus, in this example, the use of a plate according to the invention allows to divide the oxygen contamination in the final piece by a factor of 3.5.

Claims (9)

  1. Method for heat treating a powder part preform (3) comprising a titanium-based alloy, wherein the method comprises the heat treatment of the preform in a furnace (1) at a predetermined temperature, wherein the preform is on a holder (6) during the heat treatment,
    characterized in that the holder (6) comprises a titanium-based alloy having a titanium content greater than or equal to 45% by weight, or a zirconium-based alloy having a zirconium content greater than or equal to 95% by weight, wherein the holder material has a melting temperature higher than the predefined temperature of the heat treatment, and wherein an anti-diffusion barrier (7) is arranged between the preform (3) and the holder (6) in order to prevent welding of the preform to the holder.
  2. Method according to claim 1, characterized in that the holder (6) comprises a titanium-based alloy having a titanium content that is greater than or equal to 90% by weight.
  3. Method according to any one of the claims 1 and 2, characterized in that the holder (6) comprises a titanium-based alloy having a titanium content that is greater than or equal to 99% by weight.
  4. Method according to any one of the claims 1 to 3, characterized in that the holder (6) comprises a titanium-based alloy selected from among the following: T40, T60, TiAl6V4, TiAl-48-2-2.
  5. Method according to claim 1, characterized in that the holder (6) comprises a zirconium alloy selected from among the following: Zircaloy-2, Zircaloy-4.
  6. Method according to any one of the claims 1 to 5, characterized in that the holder has a thickness (e) of between 0.1 mm and 20 mm.
  7. Method according to any one of the claims 1 to 6, characterized in that the anti-diffusion barrier (7) comprises alumina or yttrium oxide.
  8. Method according to any one of the claims 1 to 7, characterized in that the holder (6) is stripped.
  9. Method according to any one of the claims 1 to 8, characterized in that the heat treatment of the preform (3) is sintering of the preform, wherein the predefined temperature of the heat treatment is the temperature of a sintering step.
EP16750926.4A 2015-07-06 2016-07-06 Method for heat treating a preform made of titanium alloy powder Active EP3320287B1 (en)

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FR1556375A FR3038622B1 (en) 2015-07-06 2015-07-06 METHOD FOR THERMALLY PROCESSING TITANIUM ALLOY POWDER PREFORM
PCT/FR2016/051710 WO2017006053A1 (en) 2015-07-06 2016-07-06 Method for heat treating a preform made of titanium alloy powder

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EP3320287A1 (en) 2018-05-16
US20180193915A1 (en) 2018-07-12
CN108291776A (en) 2018-07-17
US20210187609A1 (en) 2021-06-24
JP7119183B2 (en) 2022-08-16
CA2991283C (en) 2023-04-04
RU2711395C2 (en) 2020-01-17
RU2018104320A (en) 2019-08-06
US10967430B2 (en) 2021-04-06
JP6987751B2 (en) 2022-01-05
US11440095B2 (en) 2022-09-13
JP2021179011A (en) 2021-11-18
BR112018000280B1 (en) 2022-03-03
CA2991283A1 (en) 2017-01-12
FR3038622B1 (en) 2017-08-04
JP2018529027A (en) 2018-10-04
FR3038622A1 (en) 2017-01-13
BR112018000280A2 (en) 2018-09-04
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RU2018104320A3 (en) 2019-11-18
CN108291776B (en) 2020-11-17

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