EP0273838A2 - Process to increase the recrystillization temperature of aluminium and its alloys - Google Patents

Process to increase the recrystillization temperature of aluminium and its alloys Download PDF

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Publication number
EP0273838A2
EP0273838A2 EP87420324A EP87420324A EP0273838A2 EP 0273838 A2 EP0273838 A2 EP 0273838A2 EP 87420324 A EP87420324 A EP 87420324A EP 87420324 A EP87420324 A EP 87420324A EP 0273838 A2 EP0273838 A2 EP 0273838A2
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Prior art keywords
uranium
ppm
alloys
temperature
metal
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German (de)
French (fr)
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EP0273838A3 (en
EP0273838B1 (en
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François-Régis Boutin
Guy-Michel Raynaud
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Constellium Issoire SAS
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Cegedur Societe de Transformation de lAluminium Pechiney SA
Pechiney Rhenalu SAS
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Priority to AT87420324T priority Critical patent/ATE62714T1/en
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium

Definitions

  • the invention relates to a method for increasing the recrystallization temperature of aluminum and its alloys and minimizing the size of the grains.
  • this metal is annealed, it evolves towards a more stable equilibrium state which is a function of the temperature and the duration of the annealing.
  • the retarding effect increases as the uranium concentration increases, but reaches a maximum around 200 ppm.
  • the optimum concentration is around 50 ppm in the first case and around 150 ppm in the second case.
  • FIGS. 1 to 21 represent photos of granular structures of several aluminum alloys having been doped with different quantities of uranium and subjected to specific annealing conditions.
  • the addition of uranium at contents between 50 and 200 ppm has a retarding effect in an alloy of the type 1085 and therefore increases the recrystallization temperature.
  • the optimum concentration depends on the transformation range of the metal: - around 50 ppm if the metal is homogenized - approximately 150 ppm if it is reheated.
  • uranium greatly reduces the magnification of the grain, especially in the case of alloys homogenized at high temperature.
  • This invention is applied in particular to obtaining aluminum-based sheets intended to be subjected to heating at a relatively high temperature, such as, for example, that which accompanies enamelling or brazing operations, without this treatment could alter the mechanical properties of said sheets.

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  • Manufacture And Refinement Of Metals (AREA)
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  • Waste-Gas Treatment And Other Accessory Devices For Furnaces (AREA)
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Abstract

L'invention est relative à un procédé permettant d'augmenter la température de recristallisation de l'aluminium et de ses alliages, et de minimiser la taille des grains. Elle consiste à ajouter 5 à 1000 ppm d'uranium au moment de l'élaboration du métal. Ce procédé est appliqué notamment à l'obtention de tôles à base d'aluminium destinées à être soumises à un chauffage à température relativement élevée, comme par exemple, celui qui accompagne les opérations d'émaillage ou de brasage et ce, sans que ce traitement puisse altérer les propriétés mécaniques desdites tôles.The invention relates to a method for increasing the recrystallization temperature of aluminum and its alloys, and minimizing the size of the grains. It consists of adding 5 to 1000 ppm of uranium at the time of metal production. This process is applied in particular to obtaining aluminum-based sheets intended to be subjected to heating at a relatively high temperature, such as, for example, that which accompanies enameling or brazing operations, without this treatment. could alter the mechanical properties of said sheets.

Description

L'invention est relative à un procédé permettant d'augmenter la température de recristallisation de l'aluminium et de ses alliages et de minimiser la taille des grains.The invention relates to a method for increasing the recrystallization temperature of aluminum and its alloys and minimizing the size of the grains.

Il est connu que lors des transformations dimensionnelles d'un métal à l'état solide telles que le laminage par exemple, il se produit un phénomène dit d'écrouissage, c'est-à-dire que la structure cristalline du métal se modifie : il apparaît des défauts, des dislocations et des cellules d'écrouissage.It is known that during dimensional transformations of a metal in the solid state such as rolling for example, there is a phenomenon known as hardening, that is to say that the crystal structure of the metal changes: defects, dislocations and work hardening cells appear.

Si ce métal est recuit, il évolue vers un état d'équilibre plus stable qui est fonction de la température et de la durée du recuit.If this metal is annealed, it evolves towards a more stable equilibrium state which is a function of the temperature and the duration of the annealing.

Ainsi, dans un premier stade dit de restauration, une restructuration du métal se produit tendant à organiser les défauts linéaires en paroi polygonisée. Puis, dans un stade dit de recristallisation primaire, des grains presque parfaits apparaissent en certaines régions et se développent jusqu'à arriver au contact les uns des autres. Enfin, le nombre de grains diminue pour aboutir à la structure recristallisée la plus stable qui correspond à une surface minimale de joints de grains.Thus, in a first stage known as restoration, a restructuring of the metal occurs tending to organize the linear defects in polygonized wall. Then, in a so-called primary recrystallization stage, almost perfect grains appear in certain regions and develop until they come into contact with each other. Finally, the number of grains decreases to result in the most stable recrystallized structure which corresponds to a minimum surface of grain boundaries.

Il est également connu que l'ajout de certains éléments aux alliages lors de leur élaboration ou même la présence de certaines impuretés peuvent avoir un effet ralentisseur sur cette évolution, c'est-à-dire que la température à laquelle débute la recristallisation primaire est alors plus élevée et qu'à une température donnée la taille des grains formés est plus petite. C'est ainsi, par exemple, que de nombreux auteurs ont signalé l'effet ralentisseur du zirconium pour des concentrations de l'ordre de 2000 ppm, lorsqu'il est précipité finement dans les sousjoints au moment du recuit.It is also known that the addition of certain elements to the alloys during their preparation or even the presence of certain impurities can have a retarding effect on this development, that is to say that the temperature at which the primary recrystallization begins is then higher and at a given temperature the size of the grains formed is smaller. Thus, for example, many authors have reported the retarding effect of zirconium for concentrations of the order of 2000 ppm, when it is finely precipitated in the subjoints at the time of annealing.

Il en est de même pour le fer mais, à des concentrations moins grandes et de l'ordre de quelques centaines de ppm.The same is true for iron, but at lower concentrations of the order of a few hundred ppm.

La demanderesse a trouvé que cet effet ralentissuer pouvait également être obtenu par ajout d'uranium mais, en mettant en oeuvre des quantités de cet élément beaucoup plus petites que le zirconium et le fer puisque cet effet apparaît pour des concentrations aussi petites que 5 ppm. D'où le procédé, objet de l'invention, permettant d'augmenter la température de recristallisation de l'aluminium et de ses alliages et de minimiser la taille des grains et caractérisé en ce que l'on ajoute entre 5 et 1000 ppm d'uranium au moment de son élaboration.The Applicant has found that this slowing down effect could also be obtained by adding uranium, but by using quantities of this element much smaller than zirconium and iron since this effect appears for concentrations as small as 5 ppm. Hence the process, object of the invention, making it possible to increase the recrystallization temperature of aluminum and its alloys and to minimize the grain size and characterized in that between 5 and 1000 ppm d are added. 'uranium at the time of its development.

L'effet ralentisseur s'accroît à mesure que la concentration en uranium augmente mais, atteint un maximum aux environs de 200 ppm.The retarding effect increases as the uranium concentration increases, but reaches a maximum around 200 ppm.

L'existence d'une limitation de l'efficacité de l'effet retardateur pour les fortes concentrations en uranium semble due au fait que seul l'uranium qui se trouve en solution solide avant le recuit a une action.The existence of a limitation of the effectiveness of the retarding effect for high concentrations of uranium seems to be due to the fact that only the uranium which is in solid solution before annealing has an action.

Ceci est confirmé par des expériences qui ont montré que pour obtenir un effet similaire, il fallait moins d'uranium lorsque le métal est soumis après coulée à une opération d'homogénéisation à température élevée au lieu d'un simple réchauffage à température plus basse. Pratiquement, l'optimum de concentration se situe vers 50 ppm dans le premier cas et vers 150 ppm dans le second cas.This is confirmed by experiments which have shown that to obtain a similar effect, less uranium is required when the metal is subjected after casting to a homogenization operation at high temperature instead of a simple reheating at lower temperature. In practice, the optimum concentration is around 50 ppm in the first case and around 150 ppm in the second case.

La demanderesse a constaté également que dans le cas d'un simple réchauffage, on obtenait un effet similaire en diminuant d'autant plus la quantité d'uranium que le métal contenait de fer.The Applicant has also found that in the case of simple reheating, a similar effect is obtained by decreasing the amount of uranium the more the metal contains iron.

On a donc un effet combiné de ces deux éléments qui permet suivant la pureté en fer plus ou moins grande du métal mis en oeuvre de compléter l'effet de cet élément par une quantité réduite d'uranium.There is therefore a combined effect of these two elements which makes it possible, depending on the greater or lesser iron purity of the metal used, to complete the effect of this element with a reduced amount of uranium.

A cet effet retardateur de l'uranium s'ajoute également l'autre effet qui est, dans le cas où on dépasse néanmoins la température de recristallisation d'obtenir une minimisation de la taille des grains.To this retarding effect of uranium is also added the other effect which is, in the event that the recrystallization temperature is nevertheless exceeded, to obtain a minimization of the grain size.

L'invention peut être illustrée à l'aide des figures 1 à 21 qui représentent des photos de structures granulaires de plusieurs alliages d'aluminium ayant été dopés avec différentes quantités d'uranium et soumis à des conditions particulières de recuit.The invention can be illustrated with the aid of FIGS. 1 to 21 which represent photos of granular structures of several aluminum alloys having been doped with different quantities of uranium and subjected to specific annealing conditions.

En l'occurrence, il s'agit de 3 alliages d'aluminium du type 1085 suivant les normes de l'Aluminium Association ayant la composition suivante:

Figure imgb0001
In this case, it is 3 aluminum alloys of type 1085 according to the standards of the Aluminum Association having the following composition:
Figure imgb0001

A partir de chacun d'eux, on a élaboré une série de 7 lingotins référencés de 1 à 7 pour l'alliage A, de 8 à 14 pour l'alliage B et de 14 à 21 pour l'alliage C et tels que dans chaque série les teneurs en uranium soit respectivement 0,20, 50, 100, 200, 500 et 1000 ppm.
Ces lingotins ont ensuite subi les transformations suivantes :
- les lingotins 1 à 7 ont été homogénéisés pendant 60 heures à 620° C, puis trempés à l'eau, laminés à froid jusqu'à l'épaisseur de 0,45 mm et la tôle obtenue a été recuite pendant 1 heur à 350° C.
- les lingotins 8 à 21 ont été réchauffés à 465° C et maintenus à cette température pendant 5 heures, puis refroidis naturellement, laminés à froid jusqu'à l'épaisseur de 0,45 mm et la tôle obtenue a été recuite pendant 30 minutes à 310° C.From each of them, we developed a series of 7 ingots referenced from 1 to 7 for alloy A, from 8 to 14 for alloy B and from 14 to 21 for alloy C and such as in each series the uranium contents is respectively 0.20, 50, 100, 200, 500 and 1000 ppm.
These ingots then underwent the following transformations:
- ingots 1 to 7 were homogenized for 60 hours at 620 ° C, then quenched with water, cold rolled to the thickness of 0.45 mm and the sheet obtained was annealed for 1 hour at 350 ° C.
- ingots 8 to 21 were reheated to 465 ° C and maintained at this temperature for 5 hours, then cooled naturally, cold rolled to the thickness of 0.45 mm and the sheet obtained was annealed for 30 minutes at 310 ° C.

Les structures granulaires observées sur les tôles recuites obtenues à partir des 21 lingotins sont représentées sur les figures 1 à 21, correspondant aux références de lingotins.The granular structures observed on the annealed sheets obtained from the 21 ingots are shown in Figures 1 to 21, corresponding to the references of ingots.

Elles permettent de montrer que l'on obtient les résultats de cristallisation suivants :

Figure imgb0002
They show that the following crystallization results are obtained:
Figure imgb0002

De ce tableau, on déduit que :
- l'effet de l'uranium sur la vitesse de recristallisation est très sensible à partir de 50 ppm,
- l'effet est très important dans le cas de l'homogénéisation. Lorsque le métal est seulement réchauffé, il faut plus d'uranium pour obtenir un effet similaire,
- dans le cas du métal réchauffé, l'effet de l'uranium est d'autant plus prononcé que la teneur en fer du métal est élevée (comparaison teneur ref. C < teneur réf. B),
- l'effet de l'uranium ne s'accroît plus au-delà de 200 ppm.From this table, we deduce that:
- the effect of uranium on the recrystallization rate is very noticeable from 50 ppm,
- the effect is very significant in the case of homogenization. When the metal is only heated, more uranium is needed to achieve a similar effect,
- in the case of heated metal, the effect of uranium is all the more more pronounced than the iron content of the metal is high (comparison content ref. C <content ref. B),
- the effect of uranium no longer increases beyond 200 ppm.

En conséquence, l'ajout d'uranium a des teneurs comprises entre 50 et 200 ppm a un effet ralentisseur dans un alliage du type 1085 et augmente donc la température de recristallisation.
L'optimum de concentration dépend de la gamme de transformation du métal:
- 50 ppm environ si le métal est homogénéisé
- 150 ppm environ s'il est réchauffé.Consequently, the addition of uranium at contents between 50 and 200 ppm has a retarding effect in an alloy of the type 1085 and therefore increases the recrystallization temperature.
The optimum concentration depends on the transformation range of the metal:
- around 50 ppm if the metal is homogenized
- approximately 150 ppm if it is reheated.

De plus, dès 200 ppm, l'uranium diminue fortement le grossissement du grain notamment dans le cas d'alliages homogénéisés à haute température.In addition, from 200 ppm, uranium greatly reduces the magnification of the grain, especially in the case of alloys homogenized at high temperature.

Cette invention est appliquée notamment à l'obtention de tôles à base d'aluminium destinées à être soumises à un chauffage à température relativement élevée, comme, par exemple, celui qui accompagne les opérations d'émaillage ou de brasage, et ce, sans que ce traitement puisse altérer les propriétés mécaniques desdites tôles.This invention is applied in particular to obtaining aluminum-based sheets intended to be subjected to heating at a relatively high temperature, such as, for example, that which accompanies enamelling or brazing operations, without this treatment could alter the mechanical properties of said sheets.

Claims (4)

1. Procédé permettant d'augmenter la température de recristallisation de l'aluminium et de ses alliages et de minimiser la taille des grains caractérisé en ce que l'on ajoute entre 5 et 1000 ppm d'uranium au moment de son élaboration.1. Method for increasing the recrystallization temperature of aluminum and its alloys and minimizing the size of the grains, characterized in that between 5 and 1000 ppm of uranium are added at the time of its preparation. 2. Procédé selon la revendication 1 caractérisé en ce que l'on ajoute entre 50 et 150 ppm d'uranium.2. Method according to claim 1 characterized in that between 50 and 150 ppm of uranium is added. 3. Procédé selon la revendication 1, caractérisé en ce que l'on ajoute une quantité d'uranium plus petite dans le cas où le métal subit une opération d'homogénéisation après coulée au lieu d'un réchauffage.3. Method according to claim 1, characterized in that a smaller quantity of uranium is added in the case where the metal undergoes a homogenization operation after casting instead of reheating. 4. Procédé selon la revendication 1, caractérise en ce que lorsque le métal subit une opération de réchauffage après coulée, on ajoute une quantité d'uranium d'autant plus petite que la teneur en fer du métal est grande.4. Method according to claim 1, characterized in that when the metal undergoes a reheating operation after casting, an amount of uranium is added the smaller the higher the iron content of the metal.
EP87420324A 1986-12-02 1987-12-01 Process to increase the recrystillization temperature of aluminium and its alloys Expired - Lifetime EP0273838B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT87420324T ATE62714T1 (en) 1986-12-02 1987-12-01 METHOD OF INCREASING THE RECRYSTALLIZATION TEMPERATURE OF ALUMINUM AND ALUMINUM ALLOYS.

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FR8617015A FR2607522B1 (en) 1986-12-02 1986-12-02 PROCESS FOR INCREASING THE TEMPERATURE OF RECRYSTALLIZATION OF ALUMINUM AND ITS ALLOYS
FR8617015 1986-12-02

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EP0273838A2 true EP0273838A2 (en) 1988-07-06
EP0273838A3 EP0273838A3 (en) 1988-07-20
EP0273838B1 EP0273838B1 (en) 1991-04-17

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EP (1) EP0273838B1 (en)
JP (1) JPS63143244A (en)
AT (1) ATE62714T1 (en)
CA (1) CA1311631C (en)
DE (1) DE3769454D1 (en)
DK (1) DK631187A (en)
ES (1) ES2021745B3 (en)
FI (1) FI88311C (en)
FR (1) FR2607522B1 (en)
GR (1) GR3001797T3 (en)
IE (1) IE60679B1 (en)
IS (1) IS1402B6 (en)
NO (1) NO168186C (en)
PT (1) PT86268B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2637914A1 (en) * 1988-10-17 1990-04-20 Pechiney Rhenalu Process making it possible to lower the degree of recrystallisation of aluminium and of its alloys

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB870261A (en) * 1956-11-23 1961-06-14 Pechiney Prod Chimiques Sa Improvements in or relating to aluminium lithium alloys
US3147111A (en) * 1961-11-27 1964-09-01 Dow Chemical Co Article of aluminum-base alloy
GB1292508A (en) * 1969-10-24 1972-10-11 Sumitomo Electric Industries Improved heat resistant alloys for electrical conductors
DE3406406A1 (en) * 1983-02-22 1984-10-04 Fuji Photo Film Co., Ltd., Minami-Ashigara, Kanagawa SUPPORT FOR FLAT PRINTING FORMS

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1415733A (en) * 1920-02-02 1922-05-09 Light Metals Company Process of making and using metal scavenging alloy
NL246223A (en) * 1958-12-29

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB870261A (en) * 1956-11-23 1961-06-14 Pechiney Prod Chimiques Sa Improvements in or relating to aluminium lithium alloys
US3147111A (en) * 1961-11-27 1964-09-01 Dow Chemical Co Article of aluminum-base alloy
GB1292508A (en) * 1969-10-24 1972-10-11 Sumitomo Electric Industries Improved heat resistant alloys for electrical conductors
DE3406406A1 (en) * 1983-02-22 1984-10-04 Fuji Photo Film Co., Ltd., Minami-Ashigara, Kanagawa SUPPORT FOR FLAT PRINTING FORMS

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Aluminium Alloys : Structure and Properties; L.F. Mondolfo, P. 389-391, Butterworths; London 1976 *
METALLURGICAL TRANSACTIONS A, vol. 13A, mars 1982, pages 401-410, American Society for Metals and the Metallurgical Society of Aime, New York, US; F.S. LIN et al.: "Microstructure-property relationships of two A1-3Li-2Cu-0.2Zr-XCd alloys" *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2637914A1 (en) * 1988-10-17 1990-04-20 Pechiney Rhenalu Process making it possible to lower the degree of recrystallisation of aluminium and of its alloys

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NO168186C (en) 1992-01-22
FI875303A0 (en) 1987-12-01
CA1311631C (en) 1992-12-22
NO875004L (en) 1988-06-03
EP0273838A3 (en) 1988-07-20
DK631187D0 (en) 1987-12-01
FR2607522A1 (en) 1988-06-03
FR2607522B1 (en) 1992-04-30
ATE62714T1 (en) 1991-05-15
JPS63143244A (en) 1988-06-15
IS1402B6 (en) 1989-12-15
NO875004D0 (en) 1987-12-01
JPH0261532B2 (en) 1990-12-20
PT86268B (en) 1990-11-07
FI88311C (en) 1993-04-26
GR3001797T3 (en) 1992-11-23
EP0273838B1 (en) 1991-04-17
IS3291A7 (en) 1988-06-03
IE873260L (en) 1988-06-02
NO168186B (en) 1991-10-14
US4816088A (en) 1989-03-28
FI875303A (en) 1988-06-03
DK631187A (en) 1988-06-03
IE60679B1 (en) 1994-08-10
DE3769454D1 (en) 1991-05-23
ES2021745B3 (en) 1991-11-16
FI88311B (en) 1993-01-15
PT86268A (en) 1988-01-01

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