EP0289432A1 - Process for forming at the surface of an aluminium alloy a zone rich in aluminium of at least one of the elements nickel, iron, cobalt - Google Patents

Process for forming at the surface of an aluminium alloy a zone rich in aluminium of at least one of the elements nickel, iron, cobalt Download PDF

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Publication number
EP0289432A1
EP0289432A1 EP88420105A EP88420105A EP0289432A1 EP 0289432 A1 EP0289432 A1 EP 0289432A1 EP 88420105 A EP88420105 A EP 88420105A EP 88420105 A EP88420105 A EP 88420105A EP 0289432 A1 EP0289432 A1 EP 0289432A1
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EP
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Prior art keywords
substrate
nickel
rich
treatment
al3ni
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EP88420105A
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German (de)
French (fr)
Inventor
Michel Badia
Clément Laviron
Guy-Michel Raynaud
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Pechiney Recherche GIE
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Cegedur Societe de Transformation de lAluminium Pechiney SA
Pechiney Recherche GIE
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C26/00Coating not provided for in groups C23C2/00 - C23C24/00
    • C23C26/02Coating not provided for in groups C23C2/00 - C23C24/00 applying molten material to the substrate
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34Pretreatment of metallic surfaces to be electroplated
    • C25D5/42Pretreatment of metallic surfaces to be electroplated of light metals
    • C25D5/44Aluminium
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48After-treatment of electroplated surfaces
    • C25D5/50After-treatment of electroplated surfaces by heat-treatment

Definitions

  • the invention relates to a process for forming on the surface of an aluminum alloy substrate a zone rich in aluminide of at least one of the elements nickel, iron, cobalt.
  • These coatings are generally formed of several layers formed from the inside towards the outside of the part, by NiAl aluminide, Ni2Al3 aluminide and an alloy of aluminum and mischemetal.
  • Said layers are obtained either by immersing the part in a bath of heated metallic powder or in molten metal, or by spraying on the surface of the part metallic compounds capable, by a suitable heat treatment, of developing the desired compounds.
  • coated parts generally find their application in the aeronautical industry, in particular for the manufacture of reactor turbine components.
  • aluminides are used mainly as an intermediate layer ensuring the attachment of other materials.
  • aluminide itself as the ultimate coating.
  • these aluminides are endowed with remarkable properties such as high hardness, remarkable resistance to wear, to oxidation and to corrosion.
  • their elastic limit can be greatly improved by the addition of certain elements such as for example hafnium, molybdenum, zirconium. It therefore seems interesting to be able to develop these properties.
  • the Applicant proposes in the present invention a means making it possible to overcome these obstacles and, therefore, to go beyond the current methods of external supply of aluminides by developing the in situ formation of these compounds from simple elements aluminum, nickel, iron, cobalt.
  • This means is a process for forming on the surface of an aluminum alloy substrate a zone rich in aluminide of at least one of the elements nickel, iron, cobalt, characterized in that: - depositing at least one of said elements on the substrate without an intermediate sub-layer - The assembly is subjected to a diffusion heat treatment at a temperature above the starting melting temperature of at least one of the intermetallic compounds present in the substrate.
  • the process consists, not in depositing an aluminide on the substrate and then hanging it on said substrate but, in depositing a metallic element such as nickel, iron, cobalt and then transform it in situ into an aluminide using the aluminum from the substrate.
  • the deposition must be carried out directly on the substrate and not by means of sub-bonding layer which would prevent the formation of the aluminide.
  • the implementation of the method according to the invention therefore requires the use of a direct deposition method which nevertheless leads to suitable attachment which allows during the heat treatment to ensure the diffusion essential for the formation of the aluminide. .
  • the deposit is chosen at a thickness of less than 800 ⁇ m.
  • the second phase of the process according to the invention consists in subjecting the coated substrate to a heat treatment at a temperature which, for practical reasons of duration and of metal quality, does not exceed more than a few degrees the starting melting point of at least one of the intermetallic compounds present in the substrate.
  • the difference between the two temperatures is between 5 and 25 ° C because below 5 ° C there is no adhesion between the aluminide layers and the substrate and above 25 ° C, there is too much deformation of the substrate.
  • This treatment can be carried out in a conventional heat treatment oven where the coated substrate is kept for a variable period depending on the type of aluminide that one wants to form and consequently the properties that one wants to develop.
  • this duration is between 1 and 150 hours, range outside which either the thickness of the zone rich in aluminide is insignificant or changes too slowly.
  • the thickness and the composition of the aluminides formed are varied.
  • a zone rich in Al3Ni is overcome as a function of the duration of holding, first in contact with the substrate, surmounted by a zone rich in Al3Ni2 and an external zone rich in nickel. If the temperature maintenance is continued, the nickel-rich zone gradually disappears while the thicknesses of Al3Ni and Al3Ni2 vary in favor of Al3Ni. After a certain time, only the Al3Ni phase remains with a final thickness five times greater than the thickness of the initial nickel deposit.
  • the first, in contact with the aluminum substrate, consists of Al3Ni and has a thickness of 40 ⁇ m and a hardness of 700 Hv.
  • the second is above and made of Al3Ni2 with a thickness of 30 ⁇ m and a hardness of 1000 Hv.
  • Figure 1 attached shows at 200 magnification in section a micrographic view of the coating obtained at 530 ° C.
  • Example 2 The same sample was used as in Example 1 and after degreasing and depositing the same thickness of nickel, it was placed in an enclosure at 530 ° C for 15 hours.
  • the sample can be subjected to rapid cooling by water quenching without noticing any decohesion of the layer and then to an annealing heat treatment for 24 hours at 120 ° C. so as to restore the mechanical characteristics of the AA.7075 alloy in the T6 state while maintaining the intrinsic properties of the layer.
  • Figure 2 attached shows at 200 magnification in section a micrographic view of the coating obtained.
  • Example 2 The same sample was used as in Example 1, on which 100 ⁇ m of nickel was deposited.
  • a sample of AA.5086 alloy was used on which 20 ⁇ m of nickel was deposited according to the same method.
  • Example 4 The same results were obtained as in Example 4 with an AA.6061 alloy treated for 15 hours at 610 ° C, ie 15 ° C above the starting melting temperature.
  • Such coatings make it possible to improve the hardness, the resistance to wear, to oxidation and to corrosion of aluminum alloy substrates. This also makes it possible to obtain aluminum alloy parts having, with the proposed coating, an improved elastic modulus.

Abstract

The invention relates to a process for forming at the surface of an aluminium alloy substrate a region rich in aluminide of at least one of the elements nickel, iron, cobalt. The process consists in performing an electrochemical deposition of at least one of the elements on the substrate without using an intermediate coat and then subjecting the whole to a diffusion heat treatment at a temperature above the initial melting temperature of at least one of the intermetallic compounds present in the substrate. It makes it possible to improve the hardness and the resistance to wear, to oxidation and to corrosion, as well as the elasticity modulus of aluminium alloy substrates. <IMAGE>

Description

L'invention est relative à un procédé pour former à la surface d'un substrat en alliage d'aluminium une zone riche en aluminiure d'au moins un des éléments nickel, fer, cobalt.The invention relates to a process for forming on the surface of an aluminum alloy substrate a zone rich in aluminide of at least one of the elements nickel, iron, cobalt.

Il est connu de revêtir la surface de pièces en superalliages à base de nickel ou de cobalt d'aluminiure de nickel ou de cobalt afin d'améliorer leur tenue à la fatigue thermique et aux milieux sulfurés.It is known to coat the surface of parts made of nickel or cobalt-based superalloys of nickel or cobalt aluminide in order to improve their resistance to thermal fatigue and to sulfurized media.

Ces revêtements sont généralement formés de plusieurs couches constituées de l'intérieur vers l'extérieur de la pièce, par de l'aluminiure NiAl, de l'aluminiure Ni₂Al₃ et un alliage d'aluminium et de mischemetal.These coatings are generally formed of several layers formed from the inside towards the outside of the part, by NiAl aluminide, Ni₂Al₃ aluminide and an alloy of aluminum and mischemetal.

Lesdites couches sont obtenues soit en plongeant la pièce dans un bain de poudre métallique chauffée ou dans du métal fondu, soit en pulvérisant à la surface de la pièce des composés métalliques susceptibles par un traitement thermique convenable de développer les composés souhaités.Said layers are obtained either by immersing the part in a bath of heated metallic powder or in molten metal, or by spraying on the surface of the part metallic compounds capable, by a suitable heat treatment, of developing the desired compounds.

Ces pièces revêtues trouvent généralement leur application dans l'industrie aéronautique notamment pour la fabrication de composants de turbines de réacteur.These coated parts generally find their application in the aeronautical industry, in particular for the manufacture of reactor turbine components.

Dans le domaine des alliages d'aluminium, il est connu par le brevet US N° 3 888 746 de projeter de l'aluminiure de nickel NiAl ou Ni₃Al à la surface du trochoïde d'un moteur rotatif en alliage d'aluminium comme sous couche à un revêtement ultérieur d'acier puis de chrome. Cette couche d'aluminiure augmente la force de liaison entre l'aluminium et les couches extérieures.
Il est également connu, par la demande de brevet allemand DE 2 545 242 dans lequel on protège les pistons ou les chemises en alliages d'aluminium contre le grippage en déposant un film de molybdène, d'améliorer l'adhérence de ce film par l'interposition d'une sous couche d'aluminiure de nickel déposée au moyen d'un chalumeau.
In the field of aluminum alloys, it is known from US Pat. No. 3,888,746 to project nickel aluminide NiAl or Ni₃Al onto the surface of the trochoid of a rotary aluminum alloy motor as an undercoat. to a subsequent coating of steel and then of chromium. This layer of aluminide increases the bonding strength between the aluminum and the outer layers.
It is also known, from German patent application DE 2,545,242 in which pistons or liners made of aluminum alloys are protected against seizure by depositing a film of molybdenum, to improve the adhesion of this film by l interposition of a nickel aluminide sublayer deposited by means of a blowtorch.

Bien que cela ne soit pas précisé, il s'agit vraisemblablement d'aluminiure de formule chimique Ni₃Al ou NiAl, les seuls actuellement disponibles dans le commerce.Although this is not specified, it is probably an aluminide with the chemical formula Ni₃Al or NiAl, the only ones currently available commercially.

Les documents cités montrent donc, qu'en ce qui concerne l'aluminium, les aluminiures sont utilisés principalement comme couche intermédiaire assurant l'accrochage d'autres matériaux. Mais, en aucun cas, il n'est question d'utiliser l'aluminiure lui-même comme revêtement ultime. Or, ces aluminiures sont doués de propriétés remarquables telles qu'une forte dureté, une résistance remarquable à l'usure, à l'oxydation et à la corrosion. De plus, leur limite élastique peut être fortement améliorée par l'addition de certains éléments tels que par exemple le hafnium, le molybdène, le zirconium. Il paraît donc intéressant de pourvoir mettre ces propriétés en valeur.The documents cited therefore show that, as regards aluminum, aluminides are used mainly as an intermediate layer ensuring the attachment of other materials. However, there is no question of using the aluminide itself as the ultimate coating. However, these aluminides are endowed with remarkable properties such as high hardness, remarkable resistance to wear, to oxidation and to corrosion. In addition, their elastic limit can be greatly improved by the addition of certain elements such as for example hafnium, molybdenum, zirconium. It therefore seems interesting to be able to develop these properties.

Ces documents montrent également que sur les alliages d'aluminium le revêtement est obtenu à partir d'un aluminiure ayant été fabriqué antérieurement au dépôt alors que sur les superalliages on peut, en raison de leur température de fusion élévée, développer des aluminiures in situ. D'où une possibilité d'application limitée aux aluminiures commercialisés et parmi lesquels l'Al₃Ni par exemple ne figure pas.
En outre, le procédé de projection à chaud d'un aluminiure a pour inconvénients par rapport au procédé de formation in situ de conduire à une liaison moins bonne du revêtement avec le substrat, de créer des porosités induites et de former des couches épaisses par rapport à la granulométrie de la poudre projetée.
These documents also show that on aluminum alloys the coating is obtained from an aluminide having been manufactured prior to deposition whereas on superalloys it is possible, because of their high melting temperature, to develop aluminides in situ. Hence a possibility of application limited to aluminides sold and among which Al₃Ni for example is not included.
In addition, the process of hot spraying of an aluminide has the disadvantages compared to the process of in situ formation of leading to a poorer bond of the coating with the substrate, of creating induced porosities and of forming thick layers with respect to the particle size of the sprayed powder.

La demanderesse propose dans la présente invention un moyen permettant de s'affranchir de ces obstacles et, de ce fait, d'aller au-delà des méthodes actuelles d'apport extérieur d'aluminiures en développant la formation in situ de ces composés à partir des éléments simples aluminium, nickel, fer, cobalt.The Applicant proposes in the present invention a means making it possible to overcome these obstacles and, therefore, to go beyond the current methods of external supply of aluminides by developing the in situ formation of these compounds from simple elements aluminum, nickel, iron, cobalt.

Ce moyen est un procédé pour former à la surface d'un substrat en alliage d'aluminium une zone riche en aluminiure d'au moins un des éléments nickel, fer, cobalt caractérisé en ce que :
- on effectue un dépôt d'au moins un desdits éléments sur le substrat sans sous couche intermédiaire
- on soumet l'ensemble à un traitement thermique de diffusion à une température supérieure à la température de fusion commençante d'au moins un des composés intermétalliques présents dans le substrat.
This means is a process for forming on the surface of an aluminum alloy substrate a zone rich in aluminide of at least one of the elements nickel, iron, cobalt, characterized in that:
- depositing at least one of said elements on the substrate without an intermediate sub-layer
- The assembly is subjected to a diffusion heat treatment at a temperature above the starting melting temperature of at least one of the intermetallic compounds present in the substrate.

Ainsi, à la différence des procédés de l'air antérieur, le procédé consiste, non pas à déposer un aluminiure sur le substrat puis à l'accrocher sur ledit substrat mais, à déposer un élément métallique tel que le nickel, le fer, le cobalt puis à le transformer in situ en aluminiure en utilisant l'aluminium du substrat.Thus, unlike prior air processes, the process consists, not in depositing an aluminide on the substrate and then hanging it on said substrate but, in depositing a metallic element such as nickel, iron, cobalt and then transform it in situ into an aluminide using the aluminum from the substrate.

Il est à noter que lors de la première phase du procédé, le dépôt doit être effectué directement sur le substrat et non par l'intermédiaire de sous couche d'accrochage qui empêcherait la formation de l'aluminiure.It should be noted that during the first phase of the process, the deposition must be carried out directly on the substrate and not by means of sub-bonding layer which would prevent the formation of the aluminide.

Dans le cas de dépôts électrolytiques, il est connu que la plupart des procédés de dépôt sur un substrat aluminium d'un métal comme le nickel par exemple nécessitent, pour obtenir un bon accrochage, le passage par des sous couches telles que par exemple de bronze et/ou de cuivre obtenues en bain cyanure.In the case of electrolytic deposits, it is known that most of the methods of depositing on a aluminum substrate a metal such as nickel for example require, in order to obtain good adhesion, the passage by under layers such as for example bronze and / or copper obtained in a cyanide bath.

Ces procédés ne sont pas recommandés et on utilisera de préférence le procédé de dépôt électronchimique revendiqué dans l'US 4 492 615 et qui consiste à décaper le substrat en le soumettant à une tension positive dans une solution de chlorure de nickel, d'acide borique et d'acide fluorhydrique avant d'effectuer le dépôt.These methods are not recommended and the electrochemical deposition method claimed in US 4,492,615 will preferably be used and which consists in pickling the substrate by subjecting it to a positive voltage in a solution of nickel chloride, boric acid. and hydrofluoric acid before depositing.

Dans tous les cas, la mise en oeuvre du procédé selon l'invention oblige donc à recourir à une méthode de dépôt direct conduisant néanmoins à un accrochage convenable qui permette lors du traitement thermique d'assurer la diffusion indispensable à la formation de l'aluminiure.In all cases, the implementation of the method according to the invention therefore requires the use of a direct deposition method which nevertheless leads to suitable attachment which allows during the heat treatment to ensure the diffusion essential for the formation of the aluminide. .

Pour assurer une diffusion régulière et les améliorations souhaitées, le dépôt est choisi à une épaisseur inférieure à 800 µm.To ensure regular diffusion and the desired improvements, the deposit is chosen at a thickness of less than 800 µm.

En ce qui concerne la deuxième phase du procédé selon l'invention, elle consiste à soumettre le substrat revêtu à un traitement thermique à une température qui, pour des raisons pratiques de durée et de qualité métal, n'excède pas de plus de quelques degrés la température de fusion commençante d'au moins un des composés intermétalliques présents dans le substrat. De préférence, l'écart entre les deux températures est compris entre 5 et 25°C car en-dessous de 5°C il n'y a pas d'adhérence entre les couches d'aluminiure et le substrat et au-dessus de 25°C, il y a déformation trop importante du substrat.As regards the second phase of the process according to the invention, it consists in subjecting the coated substrate to a heat treatment at a temperature which, for practical reasons of duration and of metal quality, does not exceed more than a few degrees the starting melting point of at least one of the intermetallic compounds present in the substrate. Preferably, the difference between the two temperatures is between 5 and 25 ° C because below 5 ° C there is no adhesion between the aluminide layers and the substrate and above 25 ° C, there is too much deformation of the substrate.

Ce traitement peut être effectué dans un four conventionnel de traitement thermique où on maintient le substrat revêtu pendant une durée variable suivant le type d'aluminiure qu'on veut former et par suite les propriétés qu'on veut développer. De manière préférentielle, cette durée est comprise entre 1 et 150 heures, fourchette en dehors de laquelle soit l'épaisseur de la zone riche en aluminiure est insignifiante ou évolue trop lentement. Suivant la durée du maintien en température, on fait varier à la fois l'épaisseur et la composition des aluminiures formés.This treatment can be carried out in a conventional heat treatment oven where the coated substrate is kept for a variable period depending on the type of aluminide that one wants to form and consequently the properties that one wants to develop. Preferably, this duration is between 1 and 150 hours, range outside which either the thickness of the zone rich in aluminide is insignificant or changes too slowly. Depending on the duration of the temperature maintenance, the thickness and the composition of the aluminides formed are varied.

Ainsi, dans le cas particulier des aluminiures de nickel, on obtient en fonction de la durée de maintien d'abord au contact du substrat une zone riche en Al₃Ni surmontée d'une zone riche en Al₃Ni₂ et d'une zone externe riche en nickel.
Si on continue le maintien en température, la zone riche en nickel disparaît progressivement tandis que les épaisseurs d'Al₃Ni et d'Al₃Ni₂ varient au profit de Al₃Ni.
Au bout d'un certain temps, seule la phase Al₃Ni subsiste avec une épaisseur finale cinq fois plus importante que l'épaisseur du dépôt initial de nickel.
Thus, in the particular case of nickel aluminides, a zone rich in Al₃Ni is overcome as a function of the duration of holding, first in contact with the substrate, surmounted by a zone rich in Al₃Ni₂ and an external zone rich in nickel.
If the temperature maintenance is continued, the nickel-rich zone gradually disappears while the thicknesses of Al₃Ni and Al₃Ni₂ vary in favor of Al₃Ni.
After a certain time, only the Al₃Ni phase remains with a final thickness five times greater than the thickness of the initial nickel deposit.

On conçoit l'intérêt de ce procédé dans lequel, par un simple chauffage, dans des conditions telles qu'elles ne modifient pas la forme du substrat, on peut faire évoluer les propriétés du revêtement dans un domaine très étendu.We can understand the advantage of this process in which, by simple heating, under conditions such that they do not modify the shape of the substrate, the properties of the coating can be changed in a very wide range.

L'invention peut être illustrée à l'aide de cinq exemples d'applications suivants:The invention can be illustrated by means of five examples of following applications:

EXEMPLE 1EXAMPLE 1

Après dégraissage selon les méthodes conventionnelles, un échantillon en alliage AA.7075 suivant les normes d'Aluminium Association, sous forme de tôle laminée (état T6) a été revêtu d'un dépôt de nickel d'une épaisseur de 20 µm selon la méthode décrite dans l'US 4 492 615.
Cet échantillon revêtu a ensuite été placé dans une enceinte à 530°C pendant 5 heures de manière à dépasser sa température de fusion commençante qui est voisine de 520°C à l'état homogénéisé.
After degreasing according to conventional methods, a sample of AA.7075 alloy according to the standards of Aluminum Association, in the form of laminated sheet (state T6) was coated with a nickel deposit with a thickness of 20 μm according to the method described in US 4,492,615.
This coated sample was then placed in an enclosure at 530 ° C for 5 hours so as to exceed its starting melting temperature which is close to 520 ° C in the homogenized state.

On a observé la formation de deux couches superposées homogènes et adhérentes:
- la première, en contact avec le substrat d'aluminium, est constituée d'Al₃Ni et présente une épaisseur de 40 µm et une dureté de 700 Hv.
- la deuxième est au-dessus et constituée d'Al₃Ni₂ avec une épaisseur de 30 µm et une dureté de 1000 Hv.
We observed the formation of two superimposed homogeneous and adherent layers:
- The first, in contact with the aluminum substrate, consists of Al₃Ni and has a thickness of 40 µm and a hardness of 700 Hv.
- the second is above and made of Al₃Ni₂ with a thickness of 30 µm and a hardness of 1000 Hv.

Un échantillon revêtu, identique au précédent, placé dans une enceinte à 510°C pendant 5 heures à conduit à la formation de couches non adhérentes.A coated sample, identical to the previous one, placed in an enclosure at 510 ° C for 5 hours resulted in the formation of non-adherent layers.

La figure 1 ci-jointe montre au grossissement 200 en coupe une vue micrographique du revêtement obtenu à 530°C.Figure 1 attached shows at 200 magnification in section a micrographic view of the coating obtained at 530 ° C.

EXEMPLE 2EXAMPLE 2

On a utilisé le même échantillon que dans l'exemple 1 et après dégraissage et dépôt de la même épaisseur de nickel, on l'a placé dans une enceinte à 530°C pendant 15 heures.The same sample was used as in Example 1 and after degreasing and depositing the same thickness of nickel, it was placed in an enclosure at 530 ° C for 15 hours.

Au cours de ce traitement thermique, on a observé une diffusion conduisant à une couche homogène et adhérente d'Al₃Ni faisant 100 µm d'épaisseur et présentant une dureté de 700 Hv.During this heat treatment, a diffusion was observed leading to a homogeneous and adherent layer of Al₃Ni making 100 μm thick and having a hardness of 700 Hv.

A la sortie de l'enceinte, on peut soumettre l'échantillon à un refroi­dissement rapide par trempe à l'eau sans constater de décohésion de la couche puis à un traitement thermique de revenu durant 24 heures à 120°C de manière à restaurer les caractéristiques mécaniques de l'alliage AA.7075 à l'état T6 tout en maintenant les propriétés intrinsèques de la couche.At the exit of the enclosure, the sample can be subjected to rapid cooling by water quenching without noticing any decohesion of the layer and then to an annealing heat treatment for 24 hours at 120 ° C. so as to restore the mechanical characteristics of the AA.7075 alloy in the T6 state while maintaining the intrinsic properties of the layer.

La figure 2 ci-jointe montre au grossissement 200 en coupe une vue micrographique du revêtement obtenu.Figure 2 attached shows at 200 magnification in section a micrographic view of the coating obtained.

EXEMPLE 3EXAMPLE 3

On a utilisé le même échantillon que dans l'exemple 1 sur lequel on a déposé 100 µm de nickel.The same sample was used as in Example 1, on which 100 μm of nickel was deposited.

Après un traitement thermique de 120 heures à 530°C, on a obtenu une couche homogène d'Al₃Ni de 500 µm d'épaisseur.After a heat treatment of 120 hours at 530 ° C, a homogeneous layer of Al₃Ni 500 μm thick was obtained.

EXEMPLE 4EXAMPLE 4

On a utilisé un échantillon en alliage AA.5086 sur lequel on a déposé 20 µm de nickel selon la même méthode.A sample of AA.5086 alloy was used on which 20 μm of nickel was deposited according to the same method.

On l'a ensuite placé pendant une durée de 5 heures dans une enceinte à 600°C soit 15°C de plus que la température de fusion commençante.It was then placed for a period of 5 hours in an enclosure at 600 ° C, 15 ° C above the starting melting temperature.

On a obtenu une couche d'Al₃Ni de 100 µm.A 100 µm layer of Al₃Ni was obtained.

EXEMPLE 5EXAMPLE 5

On a obtenu les mêmes résultats que dans l'exemple 4 avec un alliage AA.6061 traité pendant 15 heures à 610°C soit 15°C de plus que la température de fusion commençante.The same results were obtained as in Example 4 with an AA.6061 alloy treated for 15 hours at 610 ° C, ie 15 ° C above the starting melting temperature.

De tels revêtements permettent d'améliorer la dureté, la résistance à l'usure, à l'oxydation et à la corrosion de substrats en alliage d'aluminium. Cela permet aussi d'obtenir des pièces en alliage d'aluminium présentant, avec le revêtement proposé, un module d'élasticité amélioré.Such coatings make it possible to improve the hardness, the resistance to wear, to oxidation and to corrosion of aluminum alloy substrates. This also makes it possible to obtain aluminum alloy parts having, with the proposed coating, an improved elastic modulus.

Claims (10)

1 - Procédé pour former à la surface d'un substrat en alliage d'aluminium une zone riche en aluminiure d'au moins un des éléments nickel, fer, cobalt caractérisé en ce que l'
- on effectue du dépôt d'au moins un desdits éléments sur le substrat sans sous couche intermédiaire,
- on soumet l'ensemble à un traitement thermique de diffusion pendant une durée comprise entre 1 et 150 heures à une température supérieure à la température de fusion commençante d'au moins un des composés intermétalliques présents dans le substrat.
1 - Process for forming on the surface of an aluminum alloy substrate a zone rich in aluminide of at least one of the elements nickel, iron, cobalt characterized in that the
- at least one of said elements is deposited on the substrate without an intermediate sub-layer,
- The assembly is subjected to a heat diffusion treatment for a period of between 1 and 150 hours at a temperature above the starting melting temperature of at least one of the intermetallic compounds present in the substrate.
2 - Procédé selon la revendication 1 caractérisé en ce que le dépôt est effectué par voie électrochimique.2 - Method according to claim 1 characterized in that the deposition is carried out electrochemically. 3 - Procédé selon la revendication 2 caractérisé en ce que le substrat est décapé par voie électrolytique avant dépôt.3 - Method according to claim 2 characterized in that the substrate is pickled electrolytically before deposition. 4 - Procédé selon la revendication 3 caractérisé en ce que dans le cas où l'élément déposé est le nickel, le substrat est décapé en le soumettant à une tension positive dans une solution de chlorure de nickel, d'acide borique et d'acide fluorhydrique.4 - Method according to claim 3 characterized in that in the case where the deposited element is nickel, the substrate is pickled by subjecting it to a positive voltage in a solution of nickel chloride, boric acid and acid hydrofluoric. 5 - Procédé selon la revendication 1 caractérisé en ce que le dépôt à une épaisseur inférieure à 800 µm.5 - Process according to claim 1 characterized in that the deposit at a thickness less than 800 µm. 6 - Procédé selon la revendication 1 caractérisé en ce que lors du traitement thermique, l'écart entre la température de traitement et la température de fusion commençante est compris entre 5 et 25°C.6 - Process according to claim 1 characterized in that during the heat treatment, the difference between the treatment temperature and the starting melting temperature is between 5 and 25 ° C. 7 - Procédé selon la revendication 1 caractérisé en ce que le traitement thermique s'effectue par chauffage dans un four conventionnel.7 - Method according to claim 1 characterized in that the heat treatment is carried out by heating in a conventional oven. 8 - Procédé selon la revendication 1 caractérisé en ce que dans le cas où l'élément déposé est le nickel, la durée de traitement est réglée de manière à développer la formation au contact du substrat d'une zone riche en Al₃Ni, recouverte d'une zone riche en Al₃Ni₂ et d'une zone riche en nickel.8 - Method according to claim 1 characterized in that in the case where the deposited element is nickel, the treatment time is adjusted so as to develop the formation in contact with the substrate of a zone rich in Al₃Ni, covered with a zone rich in Al₃Ni₂ and a zone rich in nickel. 9 - Procédé selon la revendication 8 caractérisé en ce que la durée du traitement est prolongée, de manière à obtenir uniquement une zone riche en Al₃Ni recouverte d'une zone riche en Al₃Ni₂.9 - Method according to claim 8 characterized in that the duration of the treatment is extended, so as to obtain only an area rich in Al₃Ni covered with an area rich in Al₃Ni₂. 10 - Procédé selon la revendication 9 caractérisé en ce que la durée de traitement est prolongée de manière à obtenir exclusivement une zone riche en Al₃Ni.10 - Process according to claim 9 characterized in that the duration of treatment is extended so as to obtain exclusively an area rich in Al₃Ni.
EP88420105A 1987-03-30 1988-03-29 Process for forming at the surface of an aluminium alloy a zone rich in aluminium of at least one of the elements nickel, iron, cobalt Withdrawn EP0289432A1 (en)

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FR8704589 1987-03-30
FR8704589 1987-03-30

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0892088A2 (en) * 1997-07-04 1999-01-20 Nippon Platec Kabushiki Kaisha Method of making iron electroplated aluminium materials
WO2005045102A2 (en) * 2003-11-07 2005-05-19 Aluminal Oberflächentechnik Gmbh & Co. Kg Coating of substrates
EP1533401A1 (en) * 2003-11-14 2005-05-25 Aluminal Oberflächtentechnik GmbH & Co. KG Electroplating of substrates followed by a diffusion step
DE19962641B4 (en) * 1999-12-23 2012-04-19 Erlus Aktiengesellschaft Method for producing a microstructure on a metallic surface and microstructured metallic surface

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2362026A1 (en) * 1973-12-13 1975-06-26 Aluminium Werke Ag Surface hardening of aluminium (alloys) - by applying a metal coating followed by a fusion treatment
EP0093681A1 (en) * 1982-04-29 1983-11-09 Aluminium Pechiney Process and apparatus for plating great lengths of metallic strip material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2362026A1 (en) * 1973-12-13 1975-06-26 Aluminium Werke Ag Surface hardening of aluminium (alloys) - by applying a metal coating followed by a fusion treatment
EP0093681A1 (en) * 1982-04-29 1983-11-09 Aluminium Pechiney Process and apparatus for plating great lengths of metallic strip material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
S. WERNICK et al.: "The suface treatment and finishing of aluminium and its alloys", vol. 2, 4ième édition, 1972, pages 874,875, Robert Draper Ltd, Teddington, GB, 1972 *
S. WERNICK et al.: "The suface treatment and finishing of aluminium and its alloys", vol. 2, édition 4ième, pages 874,875, Robert Draper Ltd, Teddington, GB, 1972 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0892088A2 (en) * 1997-07-04 1999-01-20 Nippon Platec Kabushiki Kaisha Method of making iron electroplated aluminium materials
EP0892088A3 (en) * 1997-07-04 1999-02-03 Nippon Platec Kabushiki Kaisha Method of making iron electroplated aluminium materials
DE19962641B4 (en) * 1999-12-23 2012-04-19 Erlus Aktiengesellschaft Method for producing a microstructure on a metallic surface and microstructured metallic surface
WO2005045102A2 (en) * 2003-11-07 2005-05-19 Aluminal Oberflächentechnik Gmbh & Co. Kg Coating of substrates
WO2005045102A3 (en) * 2003-11-07 2006-02-16 Aluminal Oberflaechentechnik Coating of substrates
EP1533401A1 (en) * 2003-11-14 2005-05-25 Aluminal Oberflächtentechnik GmbH & Co. KG Electroplating of substrates followed by a diffusion step

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