EP2274454A1 - Legierungszusammensetzung und herstellungsverfahren dafür - Google Patents

Legierungszusammensetzung und herstellungsverfahren dafür

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Publication number
EP2274454A1
EP2274454A1 EP08738391A EP08738391A EP2274454A1 EP 2274454 A1 EP2274454 A1 EP 2274454A1 EP 08738391 A EP08738391 A EP 08738391A EP 08738391 A EP08738391 A EP 08738391A EP 2274454 A1 EP2274454 A1 EP 2274454A1
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Prior art keywords
alloy
temperature
range
followed
weight
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EP08738391A
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English (en)
French (fr)
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EP2274454B1 (de
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Kumar Ashim Mukhopadhyay
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Director General Defence Research & Development Organisation
Director General Defence Res and Dev Organization Ministry of Defence Government of India
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Director General Defence Research & Development Organisation
Director General Defence Res and Dev Organization Ministry of Defence Government of India
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/10Alloys based on aluminium with zinc as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/053Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with zinc as the next major constituent

Definitions

  • This disclosure provides an Aluminum-Zinc-Magnesium-Copper-Zirconium alloy composition Al-(8- 12.5) wt% Zn-( 1.2-2.0) wt% Mg-( 1.4-2.2) wt% Cu-(0.10-0.18) wt%-Zr exhibiting significantly high strength. It also provides a process of preparing alloy semiproducts that are further processed into high strength alloy extrusions or alloy thin sheets. BACKGROUND
  • Aluminum-Zinc-Magnesium-Copper-Zirconium (Al-Zn-Mg-Cu-Zr) alloys are in great demand for various strength critical applications in areas of aerospace and defence. These alloys are commonly processed in the form of sheets, plates, extrusion, forgings, etc. for various structural applications. In aerospace applications, one of the requirements is the processing of these alloys in the form of thin sheets having thickness ⁇ 0.3 mm, wherein the thin sheets of Al alloys are used in combination with fibres (preferably glass fibres) to form fibre-metal laminated (FML) composites.
  • fibres preferably glass fibres
  • Copper-Zirconium (Al-Zn-Mg-Cu-Zr) alloys as a class of very high strength aluminium alloy that can be produced via ingot metallurgical route.
  • the increased strength properties of this category of alloys improve specific properties (in terms of strength per density and strength per Young's modulus, etc.) and, therefore, permit significant weight savings, the major emphasis in the development efforts of these alloys has been on the improvement of strength through various metallurgical processes.
  • U.S. Pat. Nos. 4,699,673; 4,988,394 and U.S. Patent application No.20060191609 disclose the methods of preparation of thin sheets of Al-Zn-Mg-Cu-Zr alloys having thickness up to 1 .2 mm. But there is no information regarding the preparation of high strength Al-Zn-Mg-Cu-Zr sheets having thickness as low as ⁇ 0.3 mm. The problem associated with the retention of high strength in such products is the onset of recrystallization resulting in cracking that becomes more pronounced as the sheets are progressively made thinner. However, due to the proprietary nature of the processing details of such thin sheets, there is no information on this topic in the literature.
  • the T77 temper possesses strength properties that correspond to the peak aged, T6 temper, but stress corrosion cracking resistance similar to the T76 temper [ALCOA publication. Light Metal Age, October, 1991 , p. 14].
  • US Patent Application 20040099352 discloses another high strength Al-Zn-Mg- Cu-Zr alloy comprising (in wt%) of 8.2-10%Zn, 1.95-2.5%Cu, 1.9-2.5%Mg, 0.05-0.25 % Zr.
  • the alloy when produced by extrusion processing and peak aged gives rise to 0.2 % P. S. of 703 MPa.
  • Another high strength, Al-Zn-Mg-Cu-Zr base alloy containing scandium, processed in the form of extrusions and heat treated to the peak aged T6 temper have the composition ofAl-8.6Zn-2.6Mg-2.4Cu-0.2 wt% Sc and an undisclosed amount of Zr [Metall. Mater. Trans. A, 3OA, 1017, 1999].
  • Cu-Zr-Sc alloy comprising (in wt%) of 8.5-1 1 %Zn, 1.8-2.4%Mg, 1.8-2.6%Cu, 0.05- 0.30%Sc and at least one element from the group Zr, V and Hf not exceeding 0.5wt%.
  • the alloy when produced by extrusion processing and peak aged gives rise to 0.2% P. S. values that range from 670 to 715 MPa.
  • US Patent Application 20050072497 discloses yet another high strength Al-Zn-Mg-Cu-Zr alloy comprising (in wt%) of 8.3-14%Zn, 0.3- 2%Cu, 0.5-4.5%Mg, 0.03-0.15%Zr and at least one element from the group Sc, Hf, La, Ce, Nd [the amount of the selected element ranging between 0.02 and 0.7wt%].
  • the alloy when produced by extrusion processing and peak aged showed 0.2%P.S. values ranging from 670 to 783 MPa.
  • Al-Zn-Mg-Cu-Zr Aluminium- Zinc-Magnesium-Copper-Zirconium
  • Al-Zn-Mg-Cu-Zr Aluminium- Zinc-Magnesium-Copper-Zirconium
  • This disclosure provides an Aluminum-Zinc-Magnesium-Copper-Zirconium alloy of composition Al-(8-12.5)wt%Zn-(1.2-2.0)wt%Mg-( 1.4-2.2)wt%Cu-(0.10-0.18)wt%Zr and method of its preparation.
  • the disclosure also provides a method for preparing alloy semi-products of this composition that can be further processed into significantly high strength alloy extrusions or alloy thin sheets.
  • One aspect of the disclosure provides an Aluminium-Zinc-Magnesium-Copper-
  • One aspect of the present disclosure provides a process for the preparation of an Al-Zn-Mg-Cu-Zr alloy using two-step homogenization process so as to cause more effective dissolution of the solidification products, thereby enabling the alloy to retain increased solute supersaturation during subsequent thermal and mechanical processing and to obtain high strength upon aging.
  • Another aspect of the present disclosure provides a process of preparation of Al- Zn-Mg-Cu-Zr alloy extrusions using optimized alloy composition and extrusion processing parameters so as to enable the alloy to obtain high strength through retaining essentially unrecrystallized grain structure and imparting solutionising effect during extrusion processing.
  • Another aspect of the present disclosure provides a process of preparation of an Al-
  • Zn-Mg-Cu-Zr alloy thin sheets using optimized alloy composition, homogenization treatment, rolling parameters and intermediate annealing treatments so as to enable the alloy to greatly minimize the extent of edge cracking and to obtain high strength through the retention of essentially unrecrystallized grain structure in most parts of the sheets.
  • Yet another aspect of the present disclosure provides a process of preparation of an Al-Zn-Mg-Cu-Zr alloy using two-step artificial aging treatment so as to enable the alloy to obtain reproducible strength properties.
  • Yet another aspect of the present disclosure provides a process for preparation of less than 0.30 mm thick Al-Zn-Mg-Cu-Zr alloy sheets having significantly high strength.
  • FIG. 1 Optical micrograph showing partially recrystallized grain structure in the peak aged alloy extrusions of present disclosure.
  • FIG. Optical micrograph showing essentially unrecrystallized grain structure in the peak aged alloy sheets of thickness 0.28 mm of present disclosure.
  • FIG. Transmission electron micrograph showing subgrain structure present in the unrecrystallized portion of the peak aged alloy extrusions of present disclosure.
  • FIG 4. Transmission electron micrograph showing a uniform and fine distribution of strengthening ⁇ ' precipitates in the peak aged alloy extrusions of present disclosure.
  • FIG 5. Transmission electron micrograph showing a uniform and fine distribution of strengthening ⁇ ' precipitates in the peak aged alloy sheets of thickness 0.28 mm of present disclosure.
  • the present disclosure provides an Aluminium-Zinc-Magnesium-Copper- Zirconium (Al-Zn-Mg-Cu-Zr) alloy of composition (in weight %): Zn 8- 12.5; Mg 1.2-2.0; Cu 1.4-2.2; and Zr 0.10-0.18.
  • the present disclosure also provides an Aluminium-Zinc-Magnesium-Copper- Zirconium (Al-Zn-Mg-Cu-Zr) alloy semi-product of composition (in weight %):
  • Al-Zn-Mg-Cu-Zr Aluminium-Zinc-Magnesium- Copper-Zirconium
  • Aluminium-Zinc-Magnesium-Copper-Zirconium (Al-Zn-Mg-Cu-Zr) alloy semi-products of composition AI-(8-12.5)wt%Zn-(1.2-2.0)wt%Mg-(1.4-2.2)wt%Cu-(0.10-0.18)wt%Zr.
  • the process comprising: a. melting a charge mixture of primary aluminium and Al-33wt%Cu master alloy; b. adding elemental pure Zn, followed by raising the temperature of the molten charge; c. adding AI-50wt%Mg master alloy and Mg-28wt%Zr master alloy to the molten charge followed by super heating; d.
  • One aspect of the present disclosure provides a process for preparing Aluminium- Zinc-Magnesium-Copper-Zirconium (Al-Zn-Mg-Cu-Zr) alloy semi-products wherein the primary aluminium has a minimum purity of 99.80 wt%.
  • Another aspect of the present disclosure provides a process for preparing Al-Zn-
  • Mg-Cu-Zr alloy semi-product wherein a charge mixture comprising of 76.38 to 84.81% by weight of primary aluminium and 4.54 to 6.97% by weight of the master alloy Al- 33wt%Cu is melted in an induction furnace by melting at a temperature in the range of 720 to 730 0 C.
  • Another aspect of the present disclosure provides a process for preparing Al-Zn-
  • Mg-Cu-Zr alloy semi-product wherein elemental pure Zn in the range of 8.15 to 12.65% by weight is added to the molten charge and the temperature of the charge is raised in the range of 735 to745°C. Subsequently, 2.04 to 3.32% by weight of AI-50wt%Mg master alloy and 0.46 to 0.68% by weight of Mg-28wt%Zr master alloy are added and the molten alloy is superheated to a temperature in the range of 755 to 765°C for 10 to 15 minutes.
  • Yet another aspect of the present disclosure provides a process for preparing Al- Zn-Mg-Cu-Zr alloy semi-product wherein the temperature of the superheated molten alloy is reduced to a temperature in the range of 735 to 74O 0 C and nucleant pellets in a quantity of 0.01 to 0.1 kg by weight are added for grain refinement.
  • the nucleant pellet used is either Di-Potassium Titanium Hexafluoride (K 2 TiF 6 ) or Potassium tetrafluoroborate (KBF 4 ).
  • Further aspect of the present disclosure provides a process for preparing Al-Zn- Mg-Cu-Zr alloy semi-product wherein dissolved gases like hydrogen are removed from the melt by degassing that is effected using degasser pellets such as Hexachloroethane (C 2 CIo) taken in a quantity of 0.01 to 0.5 kg by weight.
  • degasser pellets such as Hexachloroethane (C 2 CIo) taken in a quantity of 0.01 to 0.5 kg by weight.
  • An aspect of the present disclosure provides a process for preparing Al-Zn-Mg-Cu- Zr alloy semi-product wherein the melt, at a reduced temperature in the range of 710 to720°C, is poured under argon atmosphere into a metallic mould of suitable size preheated to a temperature in the range of 145 to 155 0 C.
  • Another aspect of the present disclosure provides a process for preparing Al-Zn-Mg-Cu- Zr alloy semi-product wherein the melt, at a reduced temperature in the range of 710 to720°C, is poured under argon atmosphere into a metallic mould of suitable size preheated to a temperature in the range of 145 to 155 0 C.
  • Another aspect of the present disclosure provides a process for preparing Al-Zn-
  • Mg-Cu-Zr alloy semi-product wherein the melt is solidified to obtain an as-cast billet or slab of alloy.
  • alloy semi-product refers to as cast billets and as-cast slabs of the alloy.
  • One aspect of the present disclosure provides a process for preparing high strength Al-Zn-Mg-Cu-Zr alloy extrusions, said process comprising of: a. homogenizing, scalping and extruding the as-cast billets of the alloy; b. solution treating, quenching; stretching the alloy extrusions to obtain 1 to
  • Another aspect of the present disclosure provides a process for preparing high strength Al-Zn-Mg-Cu-Zr alloy extrusions of composition AI-(1 1.5-12.5)wt%Zn-(l .3- 2.0)wt%Mg-( 1 .5-2.2) wt%Cu-(0.12-0.18) wt%, said process comprising of: a. melting a charge mixture of primary aluminium and AI-33wt%Cu master alloy; b. adding elemental pure Zn, followed by raising the temperature of the molten charge; c. adding AI-50wt%Mg master alloy and Mg-28wt%Zr master alloy to the molten charge followed by super heating; d.
  • Another aspect of the present disclosure provides a process for preparing high strength Al-Zn-Mg-Cu-Zr alloy extrusions wherein homogenization is carried out in two steps.
  • the first step is carried out at a temperature in the range of 440 to 450 0 C for 25 to 35 h followed by a second step homogenization at a temperature in the range of 450 to 460 0 C for 20 to 30 h followed by cooling in air.
  • the homogenization treatment eliminates dendritic segregation in the cast microstructure and causes more effective dissolution of the solidification products, thereby enabling the alloy to retain increased solute supersaturation during subsequent thermal and mechanical processing so as to obtain high strength upon aging.
  • the homogenized billets are scalped to remove the oxide layers formed on the surfaces.
  • the scalped billets are subjected to non-destructive testing to detect casting defects.
  • Further aspect of the present disclosure provides a process for preparing high strength Al-Zn-Mg-Cu-Zr alloy extrusions wherein the extrusion processing of the billets is carried out at an initial billet temperature in the range of 400 to 430 0 C; extrusion ratio in the range of 15: 1 to 25: 1 and a ram speed of 2-5 mm/s.
  • One aspect of the present disclosure provides a process for preparing high strength
  • I O Al-Zn-Mg-Cu-Zr alloy extrusions wherein solution treatment is carried out at a temperature in the range of 450 to 46O 0 C for 1 to 2 h followed by water quenching at room temperature.
  • the extrusions are subjected to stretching to obtain 1 to 1.5% permanent set for stress relieving purpose.
  • Another aspect of the present disclosure provides a process for preparing high
  • Yet another aspect of the present disclosure provides a process for preparing high 0 strength Al-Zn-Mg-Cu-Zr alloy extrusions using optimized extrusion processing parameters so as to enable the alloy to obtain high strength the alloy through retaining essentially unrecrystallized grain structure and imparting solutionising effect during extrusion processing.
  • Further aspect of the present disclosure provides a process for preparing high 5 strength Al-Zn-Mg-Cu-Zr alloy extrusions having minimum 0.2% tensile P. S. of 750 MPa.
  • An aspect of the present disclosure provides a process for preparing high strength Al-Zn-Mg-Cu-Zr alloy thin sheets, said process comprising of: a. homogenizing, scalping, hot rolling the as-cast slabs of the alloy into sheets and subsequent cold rolling of the sheets with intermediate annealing to
  • Another aspect of the present disclosure provides a process for preparing high strength Al-Zn-Mg-Cu-Zr alloy thin sheets of composition AI-(8- 10)wt%Zn-( 1.2- 2.0)wt%Mg-( 1.4-2.2) wt%Cu-(0.12-0.18)Zr, said process comprising of: a. melting a charge mixture of primary aluminium and AI-33wt%Cu master alloy; b. adding elemental pure Zn, followed by raising the temperature of the molten charge; c. adding AI-50wt%Mg master alloy and Mg-28wt%Zr master alloy to the molten charge followed by super heating; d. adding grain refining nucleant pellets at a reduced temperature; e.
  • Another aspect of the present disclosure provides a process for preparing high strength Al-Zn-Mg-Cu-Zr alloy thin sheets wherein the homogenization treatment of the as- cast slabs of the alloy is carried out at a temperature in the range of 445 to 455°C for 25 to35 h in the first step followed by a second step homogenization at a temperature in the t range of 455 to 465 0 C for 10 to 20 h followed by cooling in air.
  • the homogenization treatment eliminates dendritic segregation in the cast structure.
  • the homogenized slabs are scalped to remove the oxide layers formed on the surfaces. The scalped slabs are then subjected to the non-destructive testing to detect casting defects.
  • Yet another aspect of the present disclosure provides a process for preparing high strength Al-Zn-Mg-Cu-Zr alloy thin sheets wherein the scalped slabs (having an initial thickness of 100 mm) are subjected to hot rolling at an initial billet temperature in the range of 425 to 435°C and at a linear speed of 20 m/minute to produce plates having thickness of around 22 mm. These plates are then cross-rolled using the same initial billet temperature and rolling speed to finally produce sheets having thickness of about 5 mm.
  • hot rolling 4 to 8% reduction in the thickness of the billet in three passes followed by intermediate annealing at the temperature in the range of 415 to 435°C for 15 to 25 minutes. This cycle is continued till such time the targeted plate thickness of 22 mm and subsequently the sheet thickness of 5 mm is obtained.
  • the intermediate annealing treatment is given for stress relief purposes.
  • I O intermediate annealing treatment is given for stress relief purpose.
  • the process of cold rolling and subsequent intermediate annealing is repeated till the thickness of the sheet is reduced to 0.28 mm i.e. below 0.3 mm.
  • An aspect of the present disclosure provides a process for preparing high strength Al-Zn-Mg-Cu-Zr alloy thin sheets wherein solution treatment of rolled sheets is carried out
  • Another aspect of the present disclosure provides a process for preparing high strength Al-Zn-Mg-Cu-Zr alloy thin sheets wherein artificial aging is a two-step process carried out at a temperature in the range of 90 to 100 0 C for 6 to 8 h followed by aging at a
  • One aspect of the present disclosure is to provide a process for the preparation of high strength Al-Zn-Mg-Cu-Zr alloy in the form of sheets of thickness less than 0.3 mm having high, reproducible strength properties i.e. a minimum 0.2% tensile PS of 623 MPa
  • Example 1 Preparation of Al-11.8 wt% Zn-1.4 wt% Mg-1.8 wt% Cu-0.16 wt% Zr
  • the charge was superheated to 760 0 C and the whole material was held at this temperature for 10 minutes.
  • the temperature was then reduced to 740 0 C and 0.03 kg of nucleant pellets were added for grain refinement purpose. After 5 minutes, 0.04 kg of degasser pellets were added for degassing purpose.
  • the molten alloy, at a temperature of 720 0 C, was then poured under argon atmosphere into a preheated (to the temperature of 150 0 C) metallic mould of suitable size.
  • a cylindrical as-cast billet of 95 mm diameter and 250 mm height was obtained.
  • the billet was subjected to two-step homogenization treatment comprising of 24 h at 445°C followed by 24 h at 455°C followed by cooling in air.
  • the billet was scalped, machined to produce 74 mm diameter cylindrical billets and cut into two halves along the length. Cylindrical billets of 74 mm diameter and 125 mm height were ready for subsequent extrusion processing. Billets were extruded at an initial billet temperature of 420 0 C, extrusion ram speed of 3 mm/sec and extrusion ratio of 20: 1.
  • the charge was superheated to 760 0 C and the whole material was held at this temperature for 10 minutes.
  • the temperature was then reduced to 740 0 C and 0.03 kg of nucleant pellets were added for grain refinement purpose. After 5 minutes, 0.04 kg of degasser pellets were added for degassing purpose.
  • the molten alloy, at a temperature of 720 0 C, was then poured under argon atmosphere into a preheated (to the temperature of 150 0 C) metallic mould of suitable size.
  • a cylindrical as-cast billet of 95 mm diameter and 250 mm height was obtained.
  • the billet was subjected to two-step homogenization treatment comprising of 24 h at 445°C followed by 24 h at 455 0 C followed by cooling in air.
  • the billet was scalped, machined to produce 74 mm diameter cylindrical billets and cut into two halves along the length. Cylindrical billets of 74 mm diameter and 125 mm height were ready for subsequent extrusion processing. Billets were extruded at an initial billet temperature of 420 0 C, extrusion ram speed of 3 mm/sec and extrusion ratio of 20: 1.
  • the extrusions were solution treated at 460 0 C for 1.5 h, quenched in water at ambient temperature and peak aged using a two-step aging treatment involving 8 h at 100 0 C in the first step followed by aging at 120 0 C for 24 h in the second step. This heat treatment produced peak strength in the alloy. These peak aged extrusions were then utilized for evaluation of the tensile properties (see Table 2).
  • Example 3 Preparation of AI-8.3wt%Zn-1.9wtMg-1.7wt%Cu-0.18wt%Zr
  • a mixture of 41.154 kg of primary aluminium (purity 99.85 wt% Al and the balance being a maximum of 0.09 wt% Fe and 0.06 wt% Si impurities) and 2.72 kg of AI-33 wt% Cu master alloy was charged into the induction furnace.
  • the above charge mixture was melted at 725°C.
  • 4.225 kg of pure Zn in the ingot form was added.
  • the temperature of the molten charge was raised to 74O 0 C and 1.562 kg of AI-50 wt% Mg master alloy and 0.339 kg of Mg-28 wt% Zr master alloy were added in the above sequence.
  • the charge was superheated to 76O 0 C and the whole material was held at this temperature for 10 minutes.
  • the temperature was then reduced to 740 0 C and 0.10 kg of nucleant pellets were added for grain refinement purpose. After 5 minutes, 0.25 kg of degasser pellets were added for degassing purpose.
  • the molten alloy at the temperature of 720 0 C was then poured- under argon atmosphere into a preheated (to the temperature of 150 0 C) metallic mould of suitable size.
  • a rectangular as-cast billet of 340 mm (length) x 300 mm (width) x 100 mm (thickness) was then obtained.
  • the billet was subjected to the homogenization annealing in two steps annealing at 450 0 C for 25 h in the first step and annealing at 460 0 C for 15 h in the second step followed by cooling in air.
  • the homogenized billet was scalped in order to remove the oxidized layers on the surfaces of the billet.
  • the billet was subjected to hot rolling. Hot rolling was carried out at an initial billet temperature of 425 0 C and at a linear speed of 20 m per minute.
  • the same hot rolling cycle was continued till such time the targeted plate thickness of 22 mm was achieved and subsequent cross rolling was carried out to obtain the sheet thickness of 5 mm.
  • the hot rolled sheets were then subjected to cold rolling.
  • the sheets were subjected to the same cycle till such time the thickness of 0.28 mm i.e. the targeted thickness of below 0.30 mm was achieved.
  • the sheets were then subjected to solution treatment at 46O 0 C for 1 h followed by water quenching at room temperature.
  • a mixture of 40.536 kg of primary aluminium (purity 99.85 wt% Al and the balance being a maximum of 0.09 wt% Fe and 0.06 wt% Si impurities) and 3.03 kg of AI-33 wt% Cu master alloy was charged into the induction furnace.
  • the above charge mixture was melted at around 725°C.
  • 4.825 kg of pure Zn in the ingot form was added.
  • the temperature of the molten charge was raised to 740 0 C and 1.288 kg of AI-50 wt% Mg master alloy and 0.321 kg of Mg-28 wt% Zr master alloy were added in the above sequence.
  • the charge was superheated to 760 0 C and the whole material was held at this temperature for 10 minutes.
  • the temperature was then reduced to 740 0 C and 0.10 kg of nucleant pellets was added for grain refinement purpose. After 5 minutes, 0.25 kg of degasser pellets was added for degassing purpose.
  • the molten alloy at the temperature of 720 0 C was then poured under argon atmosphere into a preheated (to the temperature of 150 0 C) metallic mould of suitable size.
  • a rectangular as-cast billet of 340 mm (length) x 300 mm (width) * 100 mm (thickness) was then obtained.
  • the billet was subjected to the homogenization annealing in two steps annealing at 450 0 C for 25 h in the first step and annealing at 460 0 C for 15 h in the second step followed by cooling in air.
  • the homogenized billet was scalped in order to remove the oxidized layers on the surfaces of the billet.
  • the billet was subjected to hot rolling. Hot rolling was carried out at an initial billet temperature of 425°C and at a linear speed of 20 m per minute.
  • the same hot rolling cycle was continued till such time the targeted plate thickness of 22 mm was achieved and subsequent cross rolling was carried out to obtain the sheet thickness of 5 mm.
  • the hot rolled sheets were then subjected to cold rolling.
  • the sheets were subjected to the same cycle till such time the thickness of 0.28 mm i.e. the targeted thickness of below 0.30 mm was achieved.
  • the sheets were then subjected to solution treatment at 460 0 C for 1 h followed by water quenching at room temperature.
  • the tensile properties of the alloys of examples 1-4 of present disclosure were examined using tensile tests carried out at ambient temperature on tensile specimens (25 mm gauge length).
  • the alloys of example 1 and 2 were tested on round bar tensile specimens (25 mm gauge length) while alloy of example 3 and 4 were tested on flat tensile specimens.
  • Tables 1 to 4 represent the tensile test results for examples 1 to 4, respectively.
  • Figure 1 shows the partially recrystallized grain structure in the peak aged alloy extrusions of present disclosure.
  • the obtained data of 0.2% P.S. values is consistent with the retention of subgrain structure ( Figure 3) in the predominantly unrecrystallized grain structure in the peak aged alloy extrusions and essentially unrecrystallized grain structure in the peak aged sheets of thickness 0.28 mm ( Figure 2) of present disclosure. It also characterizes the presence of a uniform and fine distribution of strengthening ⁇ precipitates in the peak aged alloy extrusions ( Figure 4) and alloy thin sheets ( Figure 5).
  • the alloys of present disclosure was prepared using ⁇ 99.85 wt% purity primary Al. Therefore, it is understood that the ductility (i.e. % elongation) of the alloys when prepared using higher purity e.g. 99.9 wt% Al would be considerably higher.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Extrusion Of Metal (AREA)
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EP08738391.5A 2007-03-30 2008-03-27 Legierungszusammensetzung und herstellungsverfahren dafür Active EP2274454B1 (de)

Applications Claiming Priority (3)

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IN732DE2007 2007-03-30
IN731DE2007 2007-03-30
PCT/IN2008/000196 WO2008120237A1 (en) 2007-03-30 2008-03-27 Alloy composition and preparation thereof

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EP2274454B1 EP2274454B1 (de) 2020-11-25

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EP2644726A4 (de) * 2010-11-22 2016-06-29 Korea Automotive Tech Inst Aluminium-magnesium-legierung und herstellungsverfahren dafür
CN102703782A (zh) * 2012-04-20 2012-10-03 北京工业大学 一种超高强高淬透性Al-Zn-Mg-Cu合金
CN102935494A (zh) * 2012-11-13 2013-02-20 东北轻合金有限责任公司 一种小规格铝合金圆铸锭的制造方法
CN105200288A (zh) * 2015-11-02 2015-12-30 东北轻合金有限责任公司 一种超高强铝合金棒材及其制造方法
CN105671408A (zh) * 2016-04-20 2016-06-15 苏州市相城区明达复合材料厂 一种型材加工用高强度铝合金
CN106367644B (zh) * 2016-09-23 2018-03-13 北京工业大学 一种超高强、高硬度TiB2颗粒增强Al‑Zn‑Mg‑Cu复合材料及其制备方法
CN107119215B (zh) * 2017-06-27 2019-01-04 中南大学 一种超强铝合金及其制备方法
CN107460382B (zh) * 2017-08-18 2019-04-30 江苏大学 各向同性超强耐蚀铝合金轧制板材及制备方法
CN108707793A (zh) * 2018-06-01 2018-10-26 中国航发北京航空材料研究院 一种改善750MPa级超高强铝合金腐蚀性能的方法
CN109666827B (zh) * 2019-02-22 2021-02-12 洛阳华陵镁业有限公司 一种超强超韧7055Sc铝合金锻件
CN114277291B (zh) * 2021-12-24 2023-04-07 东北轻合金有限责任公司 一种航空航天用Al-Zn-Mg-Cu系铝合金挤压材及其制备方法
CN115612952B (zh) * 2022-11-07 2023-03-17 中国航发北京航空材料研究院 一种利用大规格铝合金铸锭生产大规格铝合金中厚宽板的方法

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4477292A (en) 1973-10-26 1984-10-16 Aluminum Company Of America Three-step aging to obtain high strength and corrosion resistance in Al-Zn-Mg-Cu alloys
US4832758A (en) 1973-10-26 1989-05-23 Aluminum Company Of America Producing combined high strength and high corrosion resistance in Al-Zn-MG-CU alloys
JPS619561A (ja) 1984-06-25 1986-01-17 Mitsubishi Alum Co Ltd 熱間成形性の優れたAl合金板の製造法
US4988394A (en) 1988-10-12 1991-01-29 Aluminum Company Of America Method of producing unrecrystallized thin gauge aluminum products by heat treating and further working
EP0368005B1 (de) * 1988-10-12 1996-09-11 Aluminum Company Of America Verfahren zur Herstellung eines nichtkristallisierten, flachgewalzten, dünnen, wärmebehandelten Produktes auf Aluminiumbasis
CA1340618C (en) * 1989-01-13 1999-06-29 James T. Staley Aluminum alloy product having improved combinations of strength, toughness and corrosion resistance
FR2838135B1 (fr) 2002-04-05 2005-01-28 Pechiney Rhenalu PRODUITS CORROYES EN ALLIAGES A1-Zn-Mg-Cu A TRES HAUTES CARACTERISTIQUES MECANIQUES, ET ELEMENTS DE STRUCTURE D'AERONEF
US20040099352A1 (en) 2002-09-21 2004-05-27 Iulian Gheorghe Aluminum-zinc-magnesium-copper alloy extrusion
US20050056353A1 (en) 2003-04-23 2005-03-17 Brooks Charles E. High strength aluminum alloys and process for making the same
DE102005045341A1 (de) * 2004-10-05 2006-07-20 Corus Aluminium Walzprodukte Gmbh Hochfestes, hochzähes Al-Zn-Legierungsprodukt und Verfahren zum Herstellen eines solches Produkts
RU2425902C2 (ru) 2005-02-10 2011-08-10 АЛКАН РОЛЛД ПРОДАКТС-РЕЙВЕНСВУД ЭлЭлСи Al-Zn-Cu-Mg СПЛАВЫ НА ОСНОВЕ АЛЮМИНИЯ И СПОСОБЫ ИХ ПОЛУЧЕНИЯ И ПРИМЕНЕНИЕ

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2008120237A1 *

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WO2008120237A1 (en) 2008-10-09
CN101835915B (zh) 2012-05-23

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