EP0196984B1 - Aluminium-based amorphous alloys containing nickel and silicon as the major constituents, and process for their manufacture - Google Patents

Aluminium-based amorphous alloys containing nickel and silicon as the major constituents, and process for their manufacture Download PDF

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EP0196984B1
EP0196984B1 EP86420062A EP86420062A EP0196984B1 EP 0196984 B1 EP0196984 B1 EP 0196984B1 EP 86420062 A EP86420062 A EP 86420062A EP 86420062 A EP86420062 A EP 86420062A EP 0196984 B1 EP0196984 B1 EP 0196984B1
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alloys
nickel
silicon
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Salim Dermarkar
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    • C22C45/00—Amorphous alloys
    • C22C45/08—Amorphous alloys with aluminium as the major constituent

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  • the invention relates to alloys based on AI, essentially containing Ni and / or Fe, Si as main alloying elements obtained in the essentially amorphous state, by relatively rapid solidification.
  • essentially amorphous is meant an alloy in which the crystallized volume fraction is at most equal to 25%.
  • alloys according to the invention contain (in atom%): (Ni) can be partially substituted by Fe up to 10% by V or B (up to 5 at.%) or completely by Mn (up to 22% at.%), the rest being consisting of AI and the usual processing impurities.
  • the alloys preferably contain: manganese being limited to 5 at. %.
  • alloys exhibit a set of remarkable properties in the amorphous or essentially amorphous state as well as in the microcrystallized state obtained by annealing of the amorphous or essentially amorphous state. These properties result from the introduction of a large quantity of alloying elements without rhedibitory effects of segregation or of the formation of fragile intermetallic phases of dimensions greater than 10 ⁇ m.
  • the unique combination of compositions and structures thus obtained gives these alloys high hardnesses, excellent heat stability for long-term annealing as well as special tribological properties.
  • a consolidation process consists of grinding the ribbons obtained by casting on a wheel, sieving below 100 ⁇ m, hot compression between 350 and 400 ° C and hot spinning around 400-450 ° C. It is thus possible to obtain massive products.
  • FIG. 5 shows the evolution of the Vickers microhardness under 10 g of the ribbons measured at 20 ° C. after isothermal annealing for one hour at different temperatures.
  • crystallization is accompanied by a significant increase in hardness.
  • the high levels of microhardness obtained (300 HV to 560 HV).
  • the alloy consists of micrograins of AI, of Si and of phase AI 3 Ni orthorhombic equilibrium.
  • the optical and transmission electron microscopy examinations show that after maintaining one hour at 400 ° C, the average grain size is between 0.05 ⁇ m and 0.5 ⁇ m. This very fine microcrystalline structure can only be obtained for such compositions by annealing an amorphous alloy and gives the alloy both mechanical strengths and high ductilities.
  • the essentially amorphous alloy according to the invention therefore exhibits very good friction and abrasion behavior.

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Abstract

The invention is directed to microcrystalline Al-based alloys produced by annealing an alloy formed initially in a substantially amorphous state by rapid solidification (about 104 K/sec) and having a composition consisting essentially of, in atomic %: from 5 to 30% Si from 11 to 22% Ni wherein the Ni may be partially substituted by Fe up to 10%, by V or B up to 5 atomic % each, or totally substituted by Mn up to 22 atomic %, and wherein Fe+Ni+Si</=42%. In the microcrystalline state, in the vicinity of the first crystallization peak, there is a metastable hexagonal phase whose crystalline parameters are about a=0.661 nm and c=0.378 nm.

Description

L'invention se rapporte à des alliages à base d'AI, contenant essentiellement du Ni et/ou du Fe, du Si comme éléments d'alliages principaux obtenus à l'état essentiellement amorphe, par solidification relativement rapide. Par essentiellement amorphe, on entend un alliage dans lequel la fraction volumique cristallisée est au plus égale à 25 %.The invention relates to alloys based on AI, essentially containing Ni and / or Fe, Si as main alloying elements obtained in the essentially amorphous state, by relatively rapid solidification. By essentially amorphous is meant an alloy in which the crystallized volume fraction is at most equal to 25%.

Bien que les alliages amorphes à base d'AI soient déjà connus de façon globale (voir la demande de brevet français n° 2 529 909), leur obtention pratique et industrielle se heurte à de grandes difficultés, en raison des paramètres de fabrication extrêmement étroits à respecter pour l'obtention de la structure essentiellement amorphe.Although amorphous alloys based on AI are already generally known (see French patent application No. 2 529 909), their practical and industrial production encounters great difficulties, due to the extremely narrow manufacturing parameters. to be observed for obtaining the essentially amorphous structure.

Ces paramètres sont principalement l'intervalle de température « de trempe depuis l'état liquide ainsi que la vitesse minimale de solidification.These parameters are mainly the temperature range "quenching from the liquid state as well as the minimum rate of solidification.

Le développement industriel de tels alliages est donc conditionné par la sélection d'alliages présentant un intervalle de trempe suffisamment large (environ 100°C entre la température de l'alliage liquide et le liquidus de celui-ci) et des vitesses de solidification pas trop rapides (de l'ordre de 10 4 K/sec.).The industrial development of such alloys is therefore conditioned by the selection of alloys having a sufficiently wide quenching interval (approximately 100 ° C. between the temperature of the liquid alloy and the liquidus thereof) and not too solidification rates. fast (of the order of 10 4 K / sec.).

Seul un petit nombre d'alliages selon l'invention répond à ces objectifs. Ces alliages contiennent (en atome %) :

Figure imgb0001
Figure imgb0002
Figure imgb0003
le (Ni) pouvant être partiellement substitué par le Fe jusqu'à 10 % par le V ou le B (jusqu'à 5 at. %) ou totalement par le Mn (jusqu'à 22 % at. %), le reste étant constitué d'AI et des impuretés d'élaboration habituelles.Only a small number of alloys according to the invention meets these objectives. These alloys contain (in atom%):
Figure imgb0001
Figure imgb0002
Figure imgb0003
 (Ni) can be partially substituted by Fe up to 10% by V or B (up to 5 at.%) or completely by Mn (up to 22% at.%), the rest being consisting of AI and the usual processing impurities.

Les alliages contiennent de préférence :

Figure imgb0004
Figure imgb0005
Figure imgb0006
le manganèse étant limité à 5 at. %.The alloys preferably contain:
Figure imgb0004
Figure imgb0005
Figure imgb0006
 manganese being limited to 5 at. %.

Dans ces conditions, il est possible d'obtenir des alliages industriels amorphes de façon reproductible.Under these conditions, it is possible to obtain reproducible amorphous industrial alloys.

Ces alliages présentent un ensemble de propriétés remarquables dans l'état amorphe ou essentiellement amorphe aussi bien que dans l'état microcristallisé obtenu par recuit de l'état amorphe ou essentiellement amorphe. Ces propriétés résultent de l'introduction d'une quantité importante d'éléments d'alliage sans effets rhédibitoires de ségrégation ou de formation de phases intermétalliques fragiles de dimensions supérieures à 10 µm. La combinaison unique des compositions et des structures ainsi obtenue confère à ces alliages des duretés élevées, une excellente stabilité à chaud pour des recuits de longue durée ainsi que des propriétés tribologiques particulières.These alloys exhibit a set of remarkable properties in the amorphous or essentially amorphous state as well as in the microcrystallized state obtained by annealing of the amorphous or essentially amorphous state. These properties result from the introduction of a large quantity of alloying elements without rhedibitory effects of segregation or of the formation of fragile intermetallic phases of dimensions greater than 10 μm. The unique combination of compositions and structures thus obtained gives these alloys high hardnesses, excellent heat stability for long-term annealing as well as special tribological properties.

La possibilité d'obtenir des structures essentiellement amorphes pour des vitesses de solidification de l'ordre de 104 K/sec. permet d'utiliser différents procédés d'obtention de ces alliages. C'est ainsi qu'outre les procédés de trempe rapide sur roue ou d'atomisation gazeuse on peut utiliser un dépôt plasma de poudres préalliées sur un substrat métallique (ou bon conducteur de la chaleur tel que le graphite) ou encore le nickelage superficiel chimique ou électrochimique d'un alliage d'AI contenant du Si (type AS), de préférence entre 10 et 25 % de Si, suivi d'une fusion du dépôt de nickel et d'une partie du substrat au moyen d'une source de chaleur concentrée et localisée telle que laser, torche plasma, chauffage HF, torche TIG, etc...The possibility of obtaining essentially amorphous structures for solidification rates of the order of 10 4 K / sec. allows the use of different processes for obtaining these alloys. Thus, in addition to the rapid quenching processes on wheels or gas atomization, it is possible to use a plasma deposition of pre-alloyed powders on a metal substrate (or good conductor of heat such as graphite) or even chemical surface nickel plating. or electrochemical of an AI alloy containing Si (AS type), preferably between 10 and 25% of Si, followed by a fusion of the nickel deposit and part of the substrate by means of a source of concentrated and localized heat such as laser, plasma torch, HF heating, TIG torch, etc ...

Un procédé de consolidation consiste en un broyage des rubans obtenus par coulée sur roue, en un tamisage au-dessous de 100 µm, une compression à chaud entre 350 et 400 °C et en un filage à chaud vers 400-450 °C. Il est ainsi possible d'obtenir des produits massifs.A consolidation process consists of grinding the ribbons obtained by casting on a wheel, sieving below 100 µm, hot compression between 350 and 400 ° C and hot spinning around 400-450 ° C. It is thus possible to obtain massive products.

L'invention sera mieux comprise à l'aide des exemples décrits ci-après et des figures suivantes :

  • - Les figures 1 à 3 donnent respectivement les diagrammes de diffraction aux rayons X, d'un alliage amorphe, essentiellement amorphe (environ 20 % à l'état cristallisé) et microcristallin.
  • - La figure 4 représente les limites de composition des alliages AI Ni Si, selon l'invention.
  • - La figure 5 représente l'évolution des microduretés Vickers de deux alliages initialement amorphes : Al70Ni15Si12Mn13 et Al70Ni15Si15 après des maintiens d'une heure à diverses températures.
  • - La figure 6 est un diffractogramme de l'alliage Al70Ni15Si15 déposé par plasma atmosphérique et obtenu avec la radiation Cu Ka.
  • - La figure 7 représente les pertes de poids (Δ°) observées sur un revêtement Al70Ni15Si15 comparativement à un alliage A-S17U4G, reconnu comme résistant à l'usure, en fonction du nombre de cycles (N) sur abrasimètre TABER.
The invention will be better understood using the examples described below and the following figures:
  • - Figures 1 to 3 respectively give the X-ray diffraction diagrams of an amorphous, essentially amorphous (about 20% in the crystallized state) and microcrystalline alloy.
  • - Figure 4 shows the limits of composition of AI Ni Si alloys according to the invention.
  • - Figure 5 shows the evolution of Vickers microduretures of two initially amorphous alloys: Al 70 Ni 15 Si 12 Mn 13 and Al 70 Ni 15 Si 15 after maintenance of one hour at various temperatures.
  • - Figure 6 is a diffractogram of the alloy Al 70 Ni 15 Si 15 deposited by atmospheric plasma and obtained with Cu Ka radiation.
  • - Figure 7 represents the weight losses (Δ °) observed on an Al 70 Ni 15 Si 15 coating compared to an A-S17U4G alloy, recognized as resistant to wear, as a function of the number of cycles (N) on the abrasimeter TABER.

Exemple 1Example 1

Le Tableau 1 rassemble des exemples de compositions d'alliages amorphes définies dans le cadre de la présente invention et obtenues sous forme de rubans de 20 µm d'épaisseur par trempe sur une roue de Cu, la vitesse linéaire d'éjection du ruban étant de 60 ms-1. La cristallisation de ces alliages a été étudiée par analyse enthalpique différentielle, par rayons X, par microscopie électronique en transmission et par mesures de microduretés. La température du 1er pic de cristallisation est reportée au Tableau 1 pour chaque composition. Ainsi, pour l'alliage Al70Ni15Si15 cette température est de 190 °C alors qu'elle est de 295 °C pour l'alliage Al70Ni15Si12Mn3. Pour les alliages ternaires (AI,Ni,Si), cette température augmente :

  • a) à teneur en AI constante, pour des teneurs croissantes en Ni
  • b) pour des teneurs croissantes d'éléments d'alliage (Ni + Si).
Table 1 brings together examples of amorphous alloy compositions defined in the context of the present invention and obtained in the form of ribbons of 20 μm thickness by quenching on a Cu wheel, the linear speed of ejection of the ribbon being 60 ms -1 . The crystallization of these alloys was studied by differential enthalpy analysis, by X-rays, by transmission electron microscopy and by measurements of microduretures. The temperature of the 1st crystallization peak is reported in Table 1 for each composition. Thus, for the Al 70 Ni 15 Si 15 alloy this temperature is 190 ° C whereas it is 295 ° C for the Al 70 Ni 15 Si 12 Mn 3 alloy. For ternary alloys (AI, Ni, Si), this temperature increases:
  • a) with constant AI content, for increasing Ni contents
  • b) for increasing contents of alloying elements (Ni + Si).

La figure 5 montre l'évolution de la microdureté Vickers sous 10 g des rubans mesurée à 20 °C après des recuits isothermes d'une heure à différentes températures. De façon générale, la cristallisation s'accompagne d'une importante augmentation de la dureté.. On notera les niveaux élevés de microdureté obtenus (300 HV à 560 HV). Après recuit d'une heure à 200 °C, l'alliage Al70Ni13Si17 présente une cristallisation abondante d'une nouvelle phase intermétallique métastable de structure hexagonale (a = 0,664 nm, c = 0,377 nm) avec un début de cristallisation de l'AI. Après une heure à 300 °C l'alliage est constitué de micrograins d'AI, de Si et de phase AI3Ni orthorhombique d'équilibre.FIG. 5 shows the evolution of the Vickers microhardness under 10 g of the ribbons measured at 20 ° C. after isothermal annealing for one hour at different temperatures. In general, crystallization is accompanied by a significant increase in hardness. Note the high levels of microhardness obtained (300 HV to 560 HV). After annealing for one hour at 200 ° C., the alloy Al 70 Ni 13 Si 17 exhibits abundant crystallization of a new metastable intermetallic phase of hexagonal structure (a = 0.664 nm, c = 0.377 nm) with an onset of crystallization. time limit. After one hour at 300 ° C., the alloy consists of micrograins of AI, of Si and of phase AI 3 Ni orthorhombic equilibrium.

Les examens en microscopie optique et électronique en transmission montrent qu'après maintien d'une heure à 400 °C, la taille moyenne des grains est comprise entre 0,05 µm et 0,5 µm. Cette structure microcristalline très fine ne peut être obtenue pour de telles compositions que par recuit d'un alliage amorphe et confère à l'alliage à la fois des résistances mécaniques et des ductilités élevées.The optical and transmission electron microscopy examinations show that after maintaining one hour at 400 ° C, the average grain size is between 0.05 µm and 0.5 µm. This very fine microcrystalline structure can only be obtained for such compositions by annealing an amorphous alloy and gives the alloy both mechanical strengths and high ductilities.

Le tableau Il donne les distances interéticulaires et les angles 6 de diffraction X (radiation Ka du Cu) relatifs à la phase hexagonale rencontrée après trempe vers 200 °C dans un échantillon initialement amorphe de l'alliage Al70Si15Ni15 (a = 0,6611 nm, c = 0,3780 nm).Table II gives the intereticular distances and the angles of X diffraction 6 (Ka radiation of Cu) relative to the hexagonal phase encountered after quenching around 200 ° C. in an initially amorphous sample of the alloy Al 70 Si 15 Ni 15 (a = 0.6611 nm, c = 0.3780 nm).

Exemple IlExample II

Nous avons élaboré 20 kg de rubans Al70Ni15Si15 par trempe sur roue. Ces rubans ont été finement broyés et la poudre ainsi obtenue a été comprimée à chaud. Le lopin de compression à chaud a été filé à 450 °C avec un rapport de filage de 16 : 1. La barre filée a été caractérisée par traction à 20 °C, à 350 °C, à 450 °C et à 500 °C. Tous les essais de traction à chaud ont été réalisés après maintien de 10 heures à 350 °C. Les résultats obtenus sont réunis dans le tableau III. Jusqu'à 350 °C le matériau est très fragile et l'on observe des ruptures prématurées sur des défauts structuraux. Cependant, le niveau de charge de rupture à 350 °C reste très élevé. A 450 °C et 500 °C le comportement est totalement différent avec des allongements élevés indicatifs d'un comportement très ductile.We produced 20 kg of Al 70 Ni 15 Si 15 ribbons by quenching on a wheel. These ribbons were finely ground and the powder thus obtained was hot pressed. The hot compression piece was spun at 450 ° C with a spinning ratio of 16: 1. The spun bar was characterized by traction at 20 ° C, 350 ° C, 450 ° C and 500 ° C . All of the hot tensile tests were carried out after maintaining for 10 hours at 350 ° C. The results obtained are collated in Table III. Up to 350 ° C the material is very fragile and premature ruptures on structural defects are observed. However, the level of breaking load at 350 ° C. remains very high. At 450 ° C and 500 ° C the behavior is totally different with high elongations indicative of a very ductile behavior.

Exemple IIIExample III

L'alliage Al70Ni15Si15 a été élaboré par trempe sur roue et broyé. La poudre obtenue a été projetée au moyen d'un plasma atmosphérique sur un substrat en alliage A-S5U3, ce qui conduit à une vitesse de solidification voisine de 104 K/sec. Le dépôt obtenu est à 75% amorphe d'après un étalonnage semi- quantitatif aux rayons X (voir figure 6). La microdureté du dépôt est de 500 Vickers. Le comportement de ce dépôt à l'abrasion comparativement à celle d'un alliage A-S17U4G non revêtu, connu pour sa résistance à l'abrasion, a été étudié sur abrasimètre TABER dans les conditions suivantes :

  • - meule type C5 17
  • - charge appliquée : 1 250 g.

avec mesure des pertes de poids au bout de 300, 500, 1 000, 2 000 et 4 000 cycles.The alloy Al 70 Ni 15 Si 15 was produced by quenching on a wheel and ground. The powder obtained was sprayed by means of an atmospheric plasma onto a substrate of A-S5U3 alloy, which leads to a solidification speed close to 10 4 K / sec. The deposit obtained is 75% amorphous according to a semi-quantitative X-ray calibration (see FIG. 6). The microhardness of the deposit is 500 Vickers. The behavior of this deposit to abrasion compared to that of an uncoated A-S17U4G alloy, known for its resistance to abrasion, was studied on a TABER abrasimeter under the following conditions:
  • - grinding wheel type C5 17
  • - applied load: 1,250 g.

with measurement of weight loss after 300, 500, 1000, 2000 and 4000 cycles.

Les résultats obtenus sont reportés au Tableau IV et représentés graphiquement sur la figure 7.The results obtained are reported in Table IV and represented graphically in FIG. 7.

On constate que l'alliage essentiellement amorphe selon l'invention présente donc un très bon comportement au frottement et à l'abrasion.

Figure imgb0007
Figure imgb0008
Figure imgb0009
Figure imgb0010
Figure imgb0011
 It can be seen that the essentially amorphous alloy according to the invention therefore exhibits very good friction and abrasion behavior.
Figure imgb0007
Figure imgb0008
Figure imgb0009
Figure imgb0010
Figure imgb0011

Claims (10)

1. Al-based alloys produced in an essentially amorphous state by rapid solidification (in the order of 104 K/sec) from a casting temperature range at around 100 °C above the liquidus of the alloy in question, and containing, in atomic percentages, from 5 to 30 % silicon and from 11 to 22 % nickel, with the total amount of iron, nickel and silicon not exceeding 42 %, and in which the nickel is optionnaly partially replaced by iron up to 10 %, by vanadium or boron up to 5 atomic % each or optionally totally replaced by manganese up to 22 atomic %, the balance being formed by aluminium and the usual production impurities.
2. Amorphous alloys according to Claim 1 containing 9 to 25 % of silicon and from 11 to 19 % of nickel, with the total of silicon, nickel and iron lying in the range 21 to 38 % and manganese being limited to 5 atomic %.
3. Alloys according to Claim 1 or 2 containing, in the recrystallised state, in the vicinity of the first crystallisation peak, a metastable hexagonal phase whose crystalline parameters are close to a = 0.661 nm and c = 0.378 nm.
4. Alloys according to Claim 1 or 2 having, in the annealed state, a grain size of 0.05 to 0.5 wm.
5. A process for producing an amorphous or essentially amorphous alloy according to Claim 1 or 2, comprising applying a nickel coating to an particle of AI Si, subjecting the deposit and the adjacent substrate to a local fusion operation by means of a concentrated heat source, and allowing the portion thus coated to cool naturally.
6. A process for producing an amorphous or essentially amorphous alloy according to Claim 1 or 2 comprising projecting under plasma pre-alloyed powder onto a metal substrate or other good conductor of heat.
7. A method of treating an alloy according to Claim 1 or 2 comprising crushing it to a grain size of less than 100 wm, compacting it in the hot condition at 350 to 400 °C and hot extruding it at 400 to 450 °C.
8. Use of alloys according to one of the claims 1 to 5 or obtained by the process according to the claims 5, 6 or 7 in the field of friction or abrasion resistance.
9. Use of alloys according to one of the claims 1 to 5 or obtained by the process according to claims 5, 6 or 7, as hot resisting alloys up to about 400 °C.
EP86420062A 1985-02-27 1986-02-26 Aluminium-based amorphous alloys containing nickel and silicon as the major constituents, and process for their manufacture Expired EP0196984B1 (en)

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AT86420062T ATE35155T1 (en) 1985-02-27 1986-02-26 AMORPHOUS ALUMINUM-BASED ALLOYS WITH NICKEL AND SILICON AS ADDITIONAL ELEMENTS AND PROCESS FOR THEIR PRODUCTION.

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FR8503318A FR2577941B1 (en) 1985-02-27 1985-02-27 AMORPHOUS AL-BASED ALLOYS CONTAINING ESSENTIALLY NI AND / OR FE AND SI AND PROCESS FOR OBTAINING SAME
FR8503318 1985-02-27

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US10294552B2 (en) 2016-01-27 2019-05-21 GM Global Technology Operations LLC Rapidly solidified high-temperature aluminum iron silicon alloys
US10260131B2 (en) 2016-08-09 2019-04-16 GM Global Technology Operations LLC Forming high-strength, lightweight alloys

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