EP0134403B1 - Fabrication par métallurgie des poudres d'un composé intermétallique lithium-aluminium et son utilisation - Google Patents

Fabrication par métallurgie des poudres d'un composé intermétallique lithium-aluminium et son utilisation Download PDF

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Publication number
EP0134403B1
EP0134403B1 EP84105154A EP84105154A EP0134403B1 EP 0134403 B1 EP0134403 B1 EP 0134403B1 EP 84105154 A EP84105154 A EP 84105154A EP 84105154 A EP84105154 A EP 84105154A EP 0134403 B1 EP0134403 B1 EP 0134403B1
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EP
European Patent Office
Prior art keywords
temperature
lithium
aluminium
process according
heating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP84105154A
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German (de)
English (en)
Other versions
EP0134403A1 (fr
Inventor
Gerhard Dr. Ibe
Josef Dipl.-Ing. Penkava
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Vereinigte Aluminium Werke AG
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Vereinigte Aluminium Werke AG
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Publication date
Application filed by Vereinigte Aluminium Werke AG filed Critical Vereinigte Aluminium Werke AG
Priority to AT84105154T priority Critical patent/ATE31429T1/de
Publication of EP0134403A1 publication Critical patent/EP0134403A1/fr
Application granted granted Critical
Publication of EP0134403B1 publication Critical patent/EP0134403B1/fr
Expired legal-status Critical Current

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    • 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
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • 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
    • C22C1/0408—Light metal alloys
    • C22C1/0416—Aluminium-based alloys

Definitions

  • the invention relates to a method for the powder metallurgical production of an alloy additive for lightweight aluminum components, consisting of lithium and aluminum with lithium contents of 44 to 55 at.% Or 17 to 25 wt.% And the corresponding aluminum content of 56 to 45 at. % or 83 to 75 wt .-%, and the use of such an alloy additive.
  • a similar process for producing an aluminum-lithium master alloy is known from US-A-4,389,240.
  • the lithium is brought into contact with aluminum powder above the melting point under protective gas and then kneaded until a homogeneous connection of the metals has been formed.
  • An embodiment shows the production of an aluminum alloy with 20 wt .-% lithium.
  • EP-A-0 045 622 it is known from EP-A-0 045 622 to produce a dispersion-strengthened aluminum alloy with 1.5 to 3.5% by weight of lithium by means of extrusion using powdered starting material, after which the mixture is mixed, degassed and weighed in under inert gas Extruded temperatures of about 350 ° C.
  • the LiAI is made from aluminum and lithium powder that is mixed in hot oil and heated to such an extent that the Li powder particles have melted into droplets, which, when the mixture is carefully agitated, temporarily meet with Al powder particles and reign to form LiAI.
  • the oil prevents unwanted or dangerous side reactions with oxygen, nitrogen, water vapor etc.
  • Another disadvantage of the process is the cumbersome separation of the reaction product LiAI from the oil, which makes industrial use more difficult.
  • the present invention was therefore based on the object of avoiding the described dangers and disadvantages of the previously known methods for producing the compound LiAI and of developing a process which enables easy, harmless production of lithium-aluminum compounds in which no melt liquid starting or intermediate products occur and the end products consist of a pure beta phase for the safe production of an Al-Li alloy with high modulus of elasticity and low density.
  • the idea of the invention is essentially based on the fact that lithium is not processed in pure form but as an intermetallic compound lithium aluminum.
  • an intermetallic phase AILi exists with about 50 at.% Lithium with a maximum area of existence of about 10 at.%.
  • This beta phase melts congruently (without decomposition) at 700 ⁇ 15 ° C, i.e. well above the aluminum melting point of 660 ° C.
  • the starting powders with grain sizes between 40 and 200 ⁇ m are mixed under normal protective measures and without noticeable heating.
  • the powder mixture is filled under argon into a heatable press mold, which is transferred without air into a press which is located in a closed vessel which can be evacuated or flushed with protective gas (argon).
  • the powder mixture is degassed at temperatures below the Li melting point in a vacuum, pre-pressed and reaction sintered with a continuously increasing temperature, it being possible to use a different pressing pressure.
  • the powder particles come into metallic contact with one another so that the formation reaction of the compound LiAI can start in the solid state.
  • the reaction partner Li and Al atoms - are supplied by diffusion from the powder particles.
  • Li grains can melt, which accelerates the reaction with the Al grains.
  • the heating rate should not exceed 50 ° C per minute so as not to overheat the molten, aggressive Li before the reaction with the AI has ended.
  • the heat of reaction of LiAI formation is noticeable (approx. 54 kJ / mol) and can e.g. B. by differential thermal analysis (DTA) can be detected (Fig. 2).
  • the heating of the sample should be interrupted for at least 15 minutes after reaching a temperature of approx. 200 ° C. This prevents the sample from overheating due to the interaction of heating and its own reaction heat (avoidance of an overheated, aggressive lithium melt which does not react in time with AI grains).
  • the compound LiAI thus produced can be used for the production of lithium-containing aluminum alloys by introducing the necessary amount of LiAI into the aluminum alloy melt which is not heated above the melting point of the LiAI compound and, because of its lower density, into the melt with a simple ceramic device immersed and moved until it has dissolved without melting. A weak purging of the melt surface with argon is sufficient as reaction protection.
  • This is built into a vacuum housing, which can be evacuated to about 10- 4 mbar by a turbomolecular pump or filled or flushed with protective gas from 0.1 to 1000 mbar.
  • the sample was first degassed without heating until the final pressure of 10- 4 mbar was reached.
  • the degassed sample is pre-pressed without heating at a pressure of 350 bar. Due to the frictional heat of the powder and the metallic contact between Al and Li that occurs, the formation reaction of the beta phase is already partially initiated, as can be seen from the warming of the sample and can be demonstrated by X-ray diffraction at the occurrence of the LiAl lines.
  • the compact is heated under argon (500 mbar) at a pressure of 200 bar at a rate of 5 ° C / min from room temperature to 500 ° C, starting at a temperature of about 290 ° C to a certain softening of the sample comes as a result of the remaining LiAI formation reaction, which reaches its maximum at about 450 ° C. (FIG. 2a).
  • the sample After reaching 500 ° C the sample is kept at temperature for at least 4 hours until the chemical homogeneity is large enough and an X-ray diffractogram shows practically only the lines of the beta phase.
  • the residual porosity achieved is between 2.5 and 6% depending on the pressure.
  • the compact was subjected to an interrupted heating according to FIG. 2b.
  • the heating was interrupted at 195 ° C and only continued after 16 minutes at a heating rate of 5 ° C per minute.
  • the further treatment was carried out analogously to the previous example, the residual porosity being between 1 and 2% depending on the pressure.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Claims (8)

1. Procédé de préparation par métallurgie des poudres d'un additif d'alliage pour éléments préfabriqués en aluminium, constitué d'un composé AILi pur en phase bêta, ayant des teneurs en lithium de 44 à 55 atomes % ou de 17 à 25 % en poids, et la teneur en aluminium correspondante de 56 à 45 atomes % ou de 83 à 75 % en poids, par les étapes suivantes:
a) Pesée et mélange d'une poudre de lithium élémentaire et d'une poudre d'aluminium élémentaire dans le rapport pondéral de 1:5 à 1:3, sous gaz protecteur (argon ou hélium);
b) introduction du mélange en poudre dans une matrice de compression chauffée et dégazage du mélange par application d'un vide à des températures inférieures au point de fusion de la poudre de lithium;
c) précompression du mélange;
d) frittage-réaction de la pièce pressée sous vide ou sous un gaz protecteur,

caractérisé par le fait que la pièce pressée, pour le filtrage-réaction, est chauffée dans la matrice de compression, sans pression, avec une vitesse de chauffage de 5 à 50°C/min., à une température dans le domaine compris entre 450°C et une température située au maximum juste au-dessous de la température péritectique de 520° C.
2. Procédé selon la revendication 1, caractérisé par le fait que la pièce pressée dans la matrice de compression est chauffée avec une pression de 50 à 500 bar et avec une vitesse de chauffage de 5 à 50°C/min. à une température dans le domaine compris entre 450°C et une température située au maximum juste au-dessous de la température péritectique de 520°C.
3. Procédé selon l'une des revendications précédentes, caractérisé par le fait que le chauffage est interrompu pendant au moins 15 min. dans le domaine de 190 à 230°C.
4. Procédé selon l'une des revendications précédentes, caractérisé par le fait que la vitesse de chauffage est proche de la limite supérieure et par le fait que la pression n'est appliquée à la pièce pressée que lorsqu'on a atteint une température supérieure à 400° C.
5. Procédé selon l'une des revendications précédentes, caractérisé par le fait que le mélange en poudre est comprimé sous vide, sans chauffage supplémentaire, avec une pression de compression comprise entre 50 et 500 bar, la pièce pressée atteignant une température comprise entre 100 et 300°C.
6. Procédé selon l'une des revendications précédentes, caractérisé par le fait que lorsque la température finale est atteinte, la pièce pressée est traitée (homogénéisée) à une température située entre 450°C et une température au maximum juste au-dessous de la température péritectique de 520°C pendant une durée d'au moins 4 heures.
7. Procédé selon l'une des revendications précédentes, caractérisé par le fait que la pièce pressée est retirée de la matrice immédiatement avant et/ou après la calcination d'homogénéisation, sous gaz protecteur, encapsulée dans un manchon d'aluminium et extrudée dans le domaine de températures de 300 à 500° C, avec un rapport de précompression compris entre 5:1 et 100:1.
8. Utilisation d'un additif d'alliage constitué d'un composé LiAI pur en phase bêta ayant une teneur en lithium de 44 à 55 atomes % ou de 17 à 25 % en poids, et la teneur en aluminium correspondante de 56 à 45 atomes % ou de 83 à 75 % en poids, préparé par un procédé selon l'une des revendications précédentes, pour la préparation d'alliages d'aluminium ayant un module d'élasticité élevé, la surface de la masse fondue étant protégée de l'oxydation par un gaz protecteur ou par une couche d'un sel fusible liquide, contenant du chlorure de lithium, et par le fait que l'additif d'alliage est introduit sous forme solide, en morceaux, dans la masse fondue d'alliage d'aluminium, caractérisée par le fait que la masse fondue présente une température inférieure à la température de fusion du composé lithium/aluminium.
EP84105154A 1983-08-25 1984-05-07 Fabrication par métallurgie des poudres d'un composé intermétallique lithium-aluminium et son utilisation Expired EP0134403B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT84105154T ATE31429T1 (de) 1983-08-25 1984-05-07 Pulvermetallurgische herstellung der intermetallischen verbindung lithium-aluminium und ihre verwendung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3330597 1983-08-25
DE3330597A DE3330597C2 (de) 1983-08-25 1983-08-25 Verfahren zur Herstellung eines Legierungszusatzes für Aluminium-Leichtbauteile und dessen Verwendung

Publications (2)

Publication Number Publication Date
EP0134403A1 EP0134403A1 (fr) 1985-03-20
EP0134403B1 true EP0134403B1 (fr) 1987-12-16

Family

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Family Applications (1)

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EP84105154A Expired EP0134403B1 (fr) 1983-08-25 1984-05-07 Fabrication par métallurgie des poudres d'un composé intermétallique lithium-aluminium et son utilisation

Country Status (3)

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EP (1) EP0134403B1 (fr)
AT (1) ATE31429T1 (fr)
DE (2) DE3330597C2 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3704767A1 (de) * 1987-02-16 1988-08-25 Leybold Ag Verfahren zum herstellen von chargiermaterial fuer schmelzmetallurgische prozesse und durch das verfahren hergestelltes chargiermaterial
DE19522988A1 (de) * 1995-06-28 1997-01-02 Sel Alcatel Ag Verfahren zur Gebühreninformation sowie Dienststeuereinrichtung, Teilnehmervermittlungsstelle, Endgerät und Kommunikationsnetz

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH358238A (fr) * 1955-10-31 1961-11-15 Foundry Services International Procédé de fabrication d'alliages ou de purification d'un métal
US3563730A (en) * 1968-11-05 1971-02-16 Lithium Corp Method of preparing alkali metal-containing alloys
US3957532A (en) * 1974-06-20 1976-05-18 The United States Of America As Represented By The United States Energy Research And Development Administration Method of preparing an electrode material of lithium-aluminum alloy
EP0045622B1 (fr) * 1980-07-31 1984-12-05 MPD Technology Corporation Alliages en aluminium durci par vieillissement
US4389240A (en) * 1982-07-09 1983-06-21 Novamet, Inc. Alloying method

Also Published As

Publication number Publication date
ATE31429T1 (de) 1988-01-15
DE3468128D1 (en) 1988-01-28
EP0134403A1 (fr) 1985-03-20
DE3330597C2 (de) 1986-07-24
DE3330597A1 (de) 1985-03-14

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