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WO1995005489A1 - Procede de traitement de materiaux de moulage metalliques - Google Patents

Procede de traitement de materiaux de moulage metalliques Download PDF

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Publication number
WO1995005489A1
WO1995005489A1 PCT/EP1994/002695 EP9402695W WO9505489A1 WO 1995005489 A1 WO1995005489 A1 WO 1995005489A1 EP 9402695 W EP9402695 W EP 9402695W WO 9505489 A1 WO9505489 A1 WO 9505489A1
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WO
WIPO (PCT)
Prior art keywords
melt
treated
treatment agent
indicates
grain
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.)
Ceased
Application number
PCT/EP1994/002695
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German (de)
English (en)
Inventor
Jürgen SCHÄDLICH-STUBENRAUCH
Pejo Stojanov
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Individual
Original Assignee
Individual
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to AU76531/94A priority Critical patent/AU7653194A/en
Publication of WO1995005489A1 publication Critical patent/WO1995005489A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C22C1/02—Making non-ferrous alloys by melting
    • 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
    • C22C1/026—Alloys based on aluminium
    • 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
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • C22C21/04—Modified aluminium-silicon alloys

Definitions

  • the invention relates to a process for the treatment of metallic casting materials, in particular for the grain refining of a metallic casting material such as aluminum, copper, magnesium, nickel, iron and / or alloys thereof, and / or for refining aluminum-silicon alloys in particular.
  • a metallic casting material such as aluminum, copper, magnesium, nickel, iron and / or alloys thereof, and / or for refining aluminum-silicon alloys in particular.
  • grain-refine metallic casting materials ie metals and / or metal alloys
  • the grain refinement of cast materials can in principle be achieved by two different measures, firstly by increasing the cooling rate (this is generally associated with subcooling the melt and thus increasing the number of bacteria) and secondly by introducing proprietary or Foreign germs as crystallization centers. Grain refinement by increasing the cooling rate is also referred to as homogeneous nucleation, while the introduction of (own or foreign) germs is also referred to as heterogeneous nucleation. Heterogeneous nucleation is sometimes referred to as "vaccination".
  • the refinement is used (exclusively) in the case of aluminum-silicon alloys in order to form the primary, coarse-grained silicon crystals which form to form fine-lamellar eutectic silicon.
  • these measures have an effect on improving the feed, mold filling and flow properties of the metal or metal alloy treated in this way. Furthermore, the susceptibility to hot cracks is reduced.
  • the improvement in the mechanical properties of the components and materials made from this material relates to their tensile strength, yield strength and elongation. Finally, this also results in an improvement in the surface of the manufactured components and materials, which is more uniform and smoother than without such a coating. action becomes.
  • treatment agent is also used in the following as a generic term for "grain refining agent” and "refining agent”.
  • the grain refinement or refinement of metals and / or metal alloys is carried out in such a way that the metal alloy to be treated is heated until it melts and the treatment agent is added in a solid form which is usually at room temperature.
  • the treatment agent itself consists of a carrier substance and one or more effective substances which contribute to grain refinement or refinement.
  • the carrier substance is generally the metal itself or the base metal of the metal alloy to be treated, whereas titanium, zirconium, rare earths, boron and / or carbon are used as germ-active substances, for example in aluminum and aluminum alloys. Strontium or sodium are often used for refining.
  • the grain refining agent supplied in the solid state of aggregation of the metal or metal alloy melt passes into the liquid state of aggregation except for its germ-active substances and is mixed with the metal or the metal alloy.
  • the mean diameters of these crystallites or particles are in the order of 5 ⁇ m to 200 ⁇ m.
  • Substances with a refining effect also dissolve in the aluminum alloy to be refined. During the solidification, they inhibit the growth of the primarily precipitated silicon crystals and thus have a refining effect on this brittle and sharp-edged structural phase.
  • aluminum-based master alloys with titanium, boron, carbon, zirconium and / or other rare earths are frequently used as grain refining agents.
  • these are overheated and poured into ingots, so that due to the relatively slow cooling in the ingot mold results in a coarse-grained structure, the primarily excreted, intermetallic, grain-refining phases being in needle form.
  • the nucleation phases in the master alloys for grain refinement of aluminum and aluminum alloys are Al 3 Ti and TiB 2 , which preferably occur in the structure of the master alloy at the grain boundaries or in the interdendritic spaces.
  • the alloyed and cast ingots, solidified with a coarsely crystalline structure, are then extruded or rolled in order to reduce the germ-effective Al 3 Ti particles in particular by means of forming technology.
  • This process has natural limits, so that the resulting grain sizes of the relatively hard Al 3 Ti particles are around 20 ⁇ m.
  • the formed grain fining agent is usually in wire form and is fed in this form to a metal or metal alloy melt to be refined. Even when the master alloy is poured into a continuously operating wire casting plant, relatively coarse-crystalline interdendritic phases still occur due to the solidification speed that occurs there. The same applies to the manufacture of finishing agents.
  • JP-A-62 133 037 describes a grain refining agent which is an aluminum-based master alloy.
  • the resulting crystallite sizes of the Al 3 Ti particles are given as ⁇ 10 ⁇ m and those of the TiB 2 particles as ⁇ 8 ⁇ m.
  • the cooling rate of the grain refining agent during its production is of the order of 100 K / s. Usually cooling rates of this type are achieved when pouring into metallic molds.
  • OS-DE-38 28 613 describes a method for producing one or more intermetallic compounds such as TiAl 3 , NiAl 3 and the like using a chamber, the outlet end of which is immersed in molten medium such as a molten metal and in which a plasma from the molten medium the outlet opening runs to a location above it.
  • molten medium such as a molten metal
  • a plasma from the molten medium the outlet opening runs to a location above it.
  • One or more components of the desired connection are fed to this location and converted into an overheated mist.
  • the components react with one another or with one or more components of the medium to form the desired compound.
  • a gas escapes from the chamber and improves the contact of the reaction participants, the reaction and also the transition into the medium.
  • the method according to the invention and the method mentioned here differ in that the aim of the method according to the invention is to introduce the melt treatment agent as effectively as possible into the material melt, the concentration of the melt treatment agent in the one to be treated Material melt is very low compared to the method mentioned.
  • the substances introduced by the method according to the invention should also not lead to any reinforcement.
  • the invention is based on the object of specifying a method for the fine treatment of metallic cast materials, in which the treated cast material has improved casting and / or mechanical properties and / or other improved usage properties.
  • the invention proposes a grain refining process for metals and / or metal alloys in which, according to the invention, the grain refining or refining agent is heated to a temperature before it is added to the melt of the material to be treated, which is greater than the temperature of the melt of the material to be treated.
  • the grain refining or refining agent is added to the metallic material to be treated in liquid and / or gaseous form, that is to say as a fluid.
  • the process according to the invention is to ensure that the temperature of the liquid treatment agent is higher than the temperature of the melt of the material to be treated.
  • the temperature must be so high that the high-melting phases of the liquid treatment agent are heated above their liquidus temperature.
  • the treatment agent is quenched when it is added to the melt of the casting material to be treated and cooled to the crystallization point (and preferably below) its grain-refining or refining phases.
  • the active substances can be dissolved more quickly (important in refining) and more effectively (applies in particular to large TiB2 and also AlTi3 particles).
  • the grain-refining or refining substances are preferably added directly as gas to the melt to be treated and finely distributed therein.
  • the substances having a grain-refining or refining effect are heated at least up to their evaporation point and then the substances to be treated Melt fed and finely distributed in it.
  • High-energy heating processes are suitable for heating, generating a plasma or arc.
  • Induction heaters can also be used.
  • the foregoing has a particularly advantageous effect with respect to the addition of the grain-refining substance boron. Due to the gaseous addition, boron is better distributed in the melt.
  • the gaseous addition of the melt treatment agent can be used optimally because its components are completely dissolved in the melt.
  • the temperature difference is at least 1.5 times the temperature of the melt of the material to be treated. This is expediently achieved in that the temperature of the material to be treated is close to its liquidus temperature, while the treatment agent to be added is greatly overheated.
  • the grain refining agent it is advantageously provided according to the invention to overheat the grain refining agent to 1,000 ° C. to 2,000 ° C. and the pure aluminum to be refined or the aluminum alloy to be refined, the melt temperature of which, depending on the composition of the alloy, at about 700 ° C. to 800 ° C. ° C, add overheated.
  • the grain refining agent is cooled rapidly when the grain refining agent is introduced into the metal or metal alloy melt.
  • nucleating crystal forms in the fine grain melt.
  • lite or particles whose diameter is preferably ⁇ 1 ⁇ m, most preferably ⁇ 0.5 ⁇ m and in particular less than 0.1 ⁇ m.
  • Al 3 Ti particles with an average size of ⁇ 2 ⁇ m and TiB 2 particles with an average size of 0 could , 5 ⁇ m in the solidified melt.
  • the grain density of this aluminum alloy which has been grain refined in accordance with the invention is at least 200 more than that density which, when using the same grain finisher, after the conventional addition in solid form to melt the material can be achieved.
  • the casting properties such as feeding, mold filling and fluidity are significantly improved. This is accompanied by a substantial reduction in the tendency to form hot cracks as well as an increase in tensile strength, yield strength and elongation, ie a noticeable improvement in the mechanical properties of the components made from the fine-grain aluminum alloy.
  • the number of nuclei per 1,000 cm 3 of the aluminum alloy grain-refined according to the invention is at least a factor of 100 higher than in the prior art, so that there is a saving in grain refining agent.
  • a tenth of the amount of the grain refining agent added by the process according to the invention already gives better results than with conventional addition of the grain refining agent to the material to be grain.
  • the grain refining agent is liquefied before being added to the melt of the material to be grain and is preferably heated to a temperature which is clearly above the highest liquidus temperature of the germ-active substance or substances contributing to grain refinement.
  • the melt of the material to be refined preferably has a temperature which is at or slightly above the liquidus temperature.
  • the particular advantage of the process according to the invention is that the large size of the crystallites, which represent the active substance in the melt treatment agent, no longer has any influence on the quality of the material treated, since the crystallites are completely dissolved.
  • concentrations of the active substances in the melt treatment agents for grain refinement or refinement are each increased far above the equilibrium concentration.
  • the concentration of the active substances in the melt treatment agents is limited because, at higher concentrations, phases precipitate which, on the one hand, have dimensions that are too large and, on the other hand, have undesired compositions.
  • the melt treatment agent is completely melted before it is added to the material melt to be treated, the concentration of the active substances in the melt treatment agent no longer plays a role. It is even possible to add the pure active substances to the material melt.
  • the dimensions of the active crystallites and phases of the melt treatment agent are expediently larger, in particular substantially larger than the crystallites acting for melt treatment. According to the invention, large crystallites of the treatment agent are melted completely. After The melt treatment agent used according to the invention can therefore have a very high concentration.
  • the liquid grain refining agent is preferably stirred with the melt of the material to be grain refined, which is done in particular mechanically, electromagnetically, piezoelectrically or by means of ultrasound. It is also conceivable to inject the liquid grain refining agent into the melt and mix it with the latter.
  • the grain refining agent can be liquefied by means of a plasma torch, inductively, by means of an arc or by means of ultrasound.
  • the grain refining agent and the material melt are expediently exposed to an inert atmosphere when the grain is heated and when the grain refining agent is introduced into the melt and when it is mixed with the same.
  • the grain refining agent is in the form of a rod or wire and is placed in a circuit with e.g. a high current source or a welding device and the melt is connected. Between the end of the one pole facing the melt and the surface of the melt, an arc is formed which liquefies the material of the other pole, ie the grain refining agent, when it is brought close enough to the melt. Continuous tracking of the pole with the grain lubricant means that the liquid introduction of grain lubricant into the melt is achieved in this way.
  • a further aspect of the invention described here is to be seen in the fact that the grain refining agent, regardless of its aggregate state, is supplied to the grain of the material to be grain to be melted at the time when this melt exhibits its strongest supercooling point. In any case, the grain refining agent should be added before the melting point of the melt.
  • the liquid grain refining agent is preferably added using a rotating feed pipe, in particular an impeller pipe, the lower end of which is immersed in the melt of the material to be refined.
  • impeller tubes are used for degassing material melts.
  • An inert gas is supplied to the impeller tube, which is supplied to the melt via the lower end of the impeller tube, which is designed in the manner of a pump impeller, when the impeller tube rotates.
  • the impeller tube is coaxially fed with grain refining agent in the form of a wire, which is drawn off from a feed roller and guided in the impeller tube up to the melt front.
  • An arc is formed between the melt connected as the anode and the end of the grain refining wire connected as the cathode facing the melt front, which melts the grain refining agent of the wire and allows it to drip onto the melt front.
  • Both a direct and an alternating current source can be used.
  • the liquefied grain refining agent gets into the melt and is advantageously evenly distributed therein.
  • the increased temperature in the area of the melt front increases the degassing effect, which leads to a further improvement in the material properties of the cast material in addition to the casting and mechanical improvements achievable by the liquid introduction of the grain refining agent.
  • a similar arrangement and mode of operation is also feasible for a finishing treatment of silicon-containing aluminum alloys.
  • the grain refining agent is expediently combined with the finishing agent in the form of a single wire, although the use of two or more wires or rods is also conceivable.
  • the semifinished products and products made from the grain-refined metal alloys have improved mechanical properties, in particular as far as the tensile strength, the yield strength and the elongation are concerned.
  • the feeding, mold-filling and fluidity of the liquid fine-grained aluminum alloy have made themselves noticeably noticeable.
  • fine-grained liquid aluminum alloys fill the molds much better due to their improved fluidity.
  • 1 is a micrograph of an aluminum investment casting component with conventional addition of the grain refining agent to the melt of the aluminum alloy to be grain refined
  • FIG. 2 shows a micrograph of an aluminum investment casting component when superheated grain refining agent is added in liquid form to the melt of the metal alloy to be refined
  • FIG. 3 shows a micrograph of an aluminum investment casting component when grain refining agent is added by melting the same from an electrode
  • FIG. 6 is a cross-sectional view through a melt bath with an impeller tube immersed therein to illustrate the addition of grain refining agent by melting an electrode and
  • FIG. 7 shows a temperature-time diagram for adding grain refining agent.
  • An aluminum alloy AlCu4Mg0.3 was melted in a conventional manner at 700 ° C.
  • a conventional grain refining agent alloy AlTi6 was melted separately in a separate induction crucible furnace and overheated to 1,100 ° C.
  • the overheated grain Finishing agent master alloy was poured into the aluminum alloy melt to be refined.
  • the content of titanium in the grain-fine alloy was set to 0.2% by weight.
  • the melt was then stirred, degassed and poured into a precision casting mold preheated to 300 ° C. 5 minutes after mixing at a temperature of 700 ° C. Samples of the cast were taken from cylinders with a diameter of 25 mm and examined metallographically.
  • the microstructure of the aluminum alloy which has been fine-grained in accordance with the above procedure is shown in FIG. 2.
  • a grain refining agent pre-alloy ALTi6 in the form of bars with a diameter of 10 mm was added to the above melt of the aluminum alloy AlCu4Mg0.3 and processed further under otherwise identical conditions. From the cast samples cast in the process, ground specimens were taken from cylinders with a diameter of 25 mm and examined metallographically. The associated micrograph is shown in Fig. 1. It can be clearly seen that the grain size in the grain refinement with liquid grain refinement agent is smaller and more uniform than in the conventional introduction of solid grain refinement agent into the melt to be grain refined.
  • Example 1 an aluminum alloy AlCu4Mg 0.3 was melted in an induction furnace and heated to 700 ° C. An aluminum-titanium pre-alloy AlTi6 was added to this melt, in such an amount that a titanium content of 0.2% by weight was obtained in the alloy to be refined.
  • the grain refining agent is added in such a way that the conventionally available AlTi6 grain refining agent is connected as a melting electrode with a diameter of 3 mm in a circuit which consisted of the melt to be grain refined as the first pole and a welding current source with which the melting electrode electrically connected as the second pole was bound.
  • the front end of the melting electrode which was brought up to the melt, was overheated by means of the arc which forms under an argon protective gas atmosphere and dripped into the melt.
  • the drops of superheated aluminum-titanium master alloy were stirred into the melt.
  • the melt was degassed and poured into a precision casting mold preheated to 300 ° C. at a casting temperature of 750 ° C. Cut specimens of cylinders with a diameter of 25 mm were examined metallographically. The micrograph of one of these samples is shown in Fig. 3.
  • the grain refining agent which was also an aluminum-titanium pre-alloy AlTi6, was added according to the temperature regime shown in FIG. 4.
  • the grain refining agent was heated to an overheating temperature T o of over 1,000 ° C.
  • T o overheating temperature
  • the aluminum alloy AlCu4MgO, 3 to be refined was at the lowest possible level, and only just above its liquidus temperature T L. This ensured the greatest possible quenching effect of the superheated grain refining agent.
  • the melt mixed with grain refining agent was heated to the optimum casting temperature T G and poured (time t G ).
  • the grain-fine alloy is produced as described in the previous example 3. After the grain-fine aluminum alloy has cooled and solidified, the alloy is reheated in the liquidus-solidus area between the liquidus temperature T L and the solidus temperature T s according to FIG. 5 Because of the globulitic structure of the structural bodies, it was possible to carry out a shaping in this temperature range. That with the temperature regime and the addition of grain refining agent according to FIGS. 4 and 5 grain-fine alloy material had finer globulites, which resulted in a changed rheological behavior of the alloy during processing.
  • the arrangement 10 schematically shows an arrangement 10 for introducing superheated drops of grain refining agent by means of a melting electrode.
  • the arrangement 10 has a rotating impeller tube 12 which is known per se and which is provided with a concentric drive pulley 14 which is driven by a belt drive 16.
  • the lower end of the impeller tube 12 carries the impeller wheel 18, which is designed in the manner of a pump impeller and has a plurality of passages 20 leading radially outwards. All passages 20 are connected to a central space 22 of the impeller wheel 18, which is open to the inside of the impeller tube 12.
  • the impeller wheel 18 and the lower section of the impeller tube 12 are immersed in a material melt 24, which is located in a crucible 26.
  • a stationary rotary leadthrough 28 coaxially surrounding the impeller tube 12 for supplying inert gas through radial passages 30 in the region of the rotary leadthrough 28.
  • Another rotary leadthrough is arranged centrally on the upper end 32 of the impeller tube 12 which is closed at the end.
  • This rotary leadthrough 32 serves to lead a wire electrode 36 made of grain refining agent removed from a supply roll 34.
  • the electrode 36 is guided coaxially to the impeller tube 12 and is arranged with its lower end 38 opposite the melt front 40 in the central space 22 of the impeller wheel 18.
  • the melt 24 is supplied with inert gas, which is introduced into the melt 24 via the passages 22 in the impeller wheel 18. This corresponds to the normal procedure for degassing melts with the help of impeller tube arrangements. If the melt 24 is now switched as the anode and the grain refinement electrode 36 as the cathode and both are fed by a welding current source, an arc 42 is formed between the melt front 40 and the lower end 38 of the grain refinement electrode 36, which material of the grain refinement Brings electrode 36 for melting and dripping into the melt 24 of the central space 22 of the impeller wheel 18.
  • the grain refining agent is preferably added within the period of time ⁇ t z during which the melt has a temperature which is the same or less is than the solidus temperature T s and is greater than or equal to the crystallization temperature T ⁇ .

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

Abstract

Dans ce procédé permettant d'affiner le grain de matériaux de moulage métalliques, notamment de l'aluminium, du cuivre, du nickel, du cobalt, du fer et/ou des alliages de ces matériaux ou pour affiner des alliages d'aluminium et de silicium, le matériau de moulage à traiter est chauffé jusqu'à ce qu'il soit en fusion et on ajoute au matériau en fusion l'agent de traitement correspondant après l'avoir porté au préalable à une température supérieure à la température de fusion du matériau de moulage. L'agent de traitement du matériau en fusion est alors refroidi brusquement au moment où il est introduit dans le matériau en fusion et les substances actives sont sensiblement mieux dissoutes dans le matériau à traiter. Ce procédé favorise l'affinage du grain et l'affinage du métal, de manière qu'après solidification du matériau fondu, l'agent de traitement du matériau en fusion présente une structure sensiblement plus fine que celles obtenues à l'aide de procédés utilisés jusqu'à présent.
PCT/EP1994/002695 1993-08-13 1994-08-12 Procede de traitement de materiaux de moulage metalliques Ceased WO1995005489A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU76531/94A AU7653194A (en) 1993-08-13 1994-08-12 Process for treating metallic materials for casting

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19934327228 DE4327228C1 (de) 1993-08-13 1993-08-13 Verfahren zum Kornfeinen von metallischen Gußwerkstoffen sowie Gußteil aus einem derartig gefeinten metallischen Gußwerkstoff
DEP4327228.2 1993-08-13

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WO1995005489A1 true WO1995005489A1 (fr) 1995-02-23

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DE (1) DE4327228C1 (fr)
WO (1) WO1995005489A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4080200A (en) * 1977-02-23 1978-03-21 A. Johnson & Co. Inc. Process for alloying metals
US4248630A (en) * 1979-09-07 1981-02-03 The United States Of America As Represented By The Secretary Of The Navy Method of adding alloy additions in melting aluminum base alloys for ingot casting
US4689199A (en) * 1984-09-27 1987-08-25 Aluminum Company Of America Process for adding material to molten media
US4793971A (en) * 1985-12-24 1988-12-27 Aluminum Company Of America Grain refining
WO1990000205A1 (fr) * 1988-06-30 1990-01-11 Norsk Hydro A.S Procede d'affinage du grain de metaux

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62133037A (ja) * 1985-12-04 1987-06-16 Ngk Insulators Ltd 結晶微細化用合金およびその製造法
US4873054A (en) * 1986-09-08 1989-10-10 Kb Alloys, Inc. Third element additions to aluminum-titanium master alloys

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4080200A (en) * 1977-02-23 1978-03-21 A. Johnson & Co. Inc. Process for alloying metals
US4248630A (en) * 1979-09-07 1981-02-03 The United States Of America As Represented By The Secretary Of The Navy Method of adding alloy additions in melting aluminum base alloys for ingot casting
US4689199A (en) * 1984-09-27 1987-08-25 Aluminum Company Of America Process for adding material to molten media
US4793971A (en) * 1985-12-24 1988-12-27 Aluminum Company Of America Grain refining
WO1990000205A1 (fr) * 1988-06-30 1990-01-11 Norsk Hydro A.S Procede d'affinage du grain de metaux

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DE4327228C1 (de) 1995-01-26
AU7653194A (en) 1995-03-14

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