US20170009322A1 - Method for the manufacturing of products with anodized high gloss surfaces from extruded profiles of al-mg-si or al-mg-si cu extrusion alloys - Google Patents

Method for the manufacturing of products with anodized high gloss surfaces from extruded profiles of al-mg-si or al-mg-si cu extrusion alloys Download PDF

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US20170009322A1
US20170009322A1 US15/124,726 US201515124726A US2017009322A1 US 20170009322 A1 US20170009322 A1 US 20170009322A1 US 201515124726 A US201515124726 A US 201515124726A US 2017009322 A1 US2017009322 A1 US 2017009322A1
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profile
temperature
billet
extruded
cold
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Ulf Tundal
Oddvin Reiso
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Norsk Hydro ASA
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/043—Changing 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 silicon as the next major constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
    • B22D21/002—Castings of light metals
    • B22D21/007—Castings of light metals with low melting point, e.g. Al 659 degrees C, Mg 650 degrees C
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/20—Measures not previously mentioned for influencing the grain structure or texture; Selection of compositions therefor
    • 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
    • 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
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C22C21/08—Alloys based on aluminium with magnesium as the next major constituent with silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/05—Changing 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 of the Al-Si-Mg type, i.e. containing silicon and magnesium in approximately equal proportions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
    • B21B2003/001—Aluminium or its alloys

Definitions

  • the present invention relates to a method for the manufacturing of products with anodized high gloss surfaces from extruded profiles of Al—Mg—Si or Al—Mg—Si—Cu alloys.
  • the oxide layer (Al 2 O 3 ) formed during anodizing is build up by dissolving the outer layer of the aluminium. For each 3 ⁇ m of oxide layer formed 2 ⁇ m of the aluminium is dissolved. Since the oxide layer is bulkier than the aluminium the total thickness will then increase by 1 ⁇ m.
  • it is important to keep the amount of constituent particles with a diameter larger than approximately 0.3 ⁇ m S. Wernick, R. Pinner and P. G. Sheasby, The Surface Treatment and Finishing of Aluminium and its Alleys , ASM INTERNATIONAL, FINISHING PUBLICATIONS LTD, fifth Edition Vol 1, 1987, p.
  • Hardening precipitates are formed during the artificial ageing process (e.g. ( ⁇ ′′-MgSi) from the addition of Mg and Si. If Cu is added in sufficient amount other phases than ⁇ ′′ may form (e.g. Q′ and L) (Calin D. Marioara, et. al., Improving Thermal Stability in Cu - Containing Al—Mg—Si Alloys by Precipitate Optimization, METALLURGICAL AND MATERIALS TRANSACTIONS A, March 2014). These hardening precipitates are much smaller than 0.3 ⁇ m and are therefore net reducing the gloss in the same way as the primary AlFeSi particles. The strength requirement for the alloy determines the necessary amount of Mg, Si and Cu in the alloy.
  • Alloying elements such as Mn, Cr, Zr or Sc can be added to form dispersold particles during homogenisation. Frequently, these elements are added in high amounts in order to prevent recrystallization in the extruded profile. However, it can be beneficial to add these elements in smaller amounts to only have some dispersold particles in the alloy in order to avoid grain growth during homogenisation and after the recrystallization process occurring in the extrusion process or in a separate recrystallization and solutionising process for the cold deformed material.
  • the size of these particles is typically between 0.01-0.2 ⁇ m. Thus, such particles can be added, at least in a relative low number, without significantly affecting the gloss.
  • the number of dispersoid particles should not be so high that the exposed areas of the profile surface get a mixture of a non-recrystallized and a recrystallized structure or a fully recrystallized structure with a large and uneven grain size. Addition of elements that form dispersold particles can also give an unwanted colour of the anodising layer, or they can give an unwanted surface appearance due to a strong texture of the recrystallized grains.
  • an anodized surface contains large grains the individual grains can be detected by the naked eye. This surface defect is frequently called mottling. The best surface appearance is obtained when the average grain size Is smaller than approximately 70 ⁇ m and the grains mainly are randomly orientated.
  • the method according to the invention is characterized by the features as defined in the accompanying independent claim 1 .
  • FIG. 1 is a photo of a quarter of a macro etched billet slice ( ⁇ 228 mm in diameter) with abnormal grains.
  • FIG. 2 is a light optical micrograph showing a typical grain structure through the thickness of a thick solid shape extruded profile which is anodised and viewed in polarised light
  • FIG. 3 is a principal sketch of an industrial processing line for performing the cold rolling and the annealing process described in the present invention.
  • FIG. 4 shows light optical micrographs of samples from example 1 showing the grain structure in the middle of the cross section for the as extruded profile and for the samples that were cold rolled to give 10, 20, 40 and 60% reduction in the thickness prior to annealing. All samples are anodised and viewed in polarized light.
  • FIG. 5 shows grain structure in an as cast billet ( ⁇ 95 mm diameter) without grain refiner, which was used in example 2 of the present application. Picture of a macro etched billet slice to the left and anodised sample viewed in polarized light in a light optical microscope to the right.
  • FIG. 6 are light optical micrographs showing the AlFeSi particles in a homogenised billet cast without grain refiner (upper picture) and in a homogenised billet cast with grain refiner (lower picture). The position of the samples in the billet is approximately half radius.
  • FIG. 7 is alight optical micrograph of an as extruded sample in example 2 of the application, showing the grain structure close to the surface. Anodised and viewed in polarized light.
  • FIG. 8 shows light optical micrographs of samples from example 2, showing the gram structure in the middle of the cross section for the as extruded profile and the samples that were cold rolled to give 20, 30, 40 and 50% reduction in the thickness poor to annealing. All samples are anodised and viewed in polarized light.
  • FIG. 9 shows further light optical micrographs of samples from example 2 of the present application, showing the grain structure in the middle of the cross section for samples that were cold rolled to 40% reduction in the thickness prior to annealing in air (upper) and in a salt bath (lower). Both samples are anodised and viewed in polarized light.
  • the billet grain size will probably not affect the grain size in the extruded profile much if the extent of deformation is high, for example when extruding thin walled hollow profiles. For solid shapes, and especially for thick walled profiles, the billet grain size will most likely affect the grain size in the extruded profile.
  • An additional challenge is that the billet temperature needs to be rather high in order to dissolve the Mg 2 Si particles, and a high billet temperature makes it more difficult to obtain a small gram size after extrusion.
  • an extruded profile In an extruded profile one usually sees a surface layer of mainly randomly oriented grains and typically one or a few grains in thickness. Underneath this layer one typically finds a region of larger grains. The thickness of this layer varies, and is usually thicker for a thick walled solid shape profile and thicker towards the back end of the extruded length.
  • An example of a typical grain structure in a cross section of a thick walled industrially extruded profile can be seen in FIG. 2 .
  • Below the layer of larger grains the grain structure is typically more homogeneous. The grains in the homogeneous center region of the cross section are predominantly aligned in one direction, with a strong cube texture. This is often seen in s micrograph of the grain structure in the cross section by small differences in the colour of the grains.
  • More and more consumer electronics like mobile phones, tablets and lap tops are made of aluminium from extruded profiles. If the profile surface could have been used without any machining the grain structure in the anodised surface would probably be okay in most cases. However, very often them is a need to machine the extruded profile to make the shape and the dimensional tolerances of the final product. In that case the exposed surface can consist of grains from the coarse grain layer beneath the surface layer of the extruded profile. Due to this the entire coarse grain layer has to be removed before starting to machine the shape of the final product. The thickness of the layer that has to be removed due to coarse grains will very with the size of the profile and the extrusion conditions and is typicality in the range of 0.2 to 1 mm.
  • the present invention deals with the task to get a homogeneous grain structure with an average grain size below approximately 70 ⁇ m irrespective of the Fe content, the grain size in the billet prior to extrusion and the extrusion conditions.
  • Solid shape profiles which are blanks for consumer electronics will be more or less flat, but could possibly have some features in the cross section in order to save material and machining Such profiles are therefore very well suited for cold rolling after extrusion.
  • cold rolling a profile by a minimum of 10% followed by flash annealing a new recrystallization process will take place.
  • the resulting grain structure will be homogeneous over the cross section with a much more random orientation of the grains than in the as extruded profile.
  • the grain size will in addition to the alley content, depend on the degree of cold deformation, the annealing temperature, the heat up conditions and the time at the annealing temperature.
  • the annealing temperature should preferably be above the solvus temperature for Mg 2 Si particles in order to avoid particles that can reduce the strength and the gloss of the anodised material.
  • the time at this annealing temperature should be as short as possible in order to avoid grain growth. Therefore, the material should be processed through extrusion in a way that Mg 2 Si particles are avoided. This means sufficiently high billet temperature in combination with a high enough exit temperature from extrusion and fast cooling of the profile after extrusion. With no particles in the material prior to cold rolling and annealing there is no need for a holding time for the material at the annealing temperature.
  • Mg—Si containing precipitates larger than approximately 0.3 ⁇ m may form. These particles will contribute to a reduction in the gloss and in the strength of the material. The amount of this reduction will depend on the actual time-temperature history during the flash annealing and cooling operation and the composition of the alloy.
  • An industrial process to perform the cold rolling and the annealing process could be done as shown schematically in FIG. 3 .
  • the cold rolling station should be followed by a station for performing fast hasting to the annealing temperature.
  • Using induction heating is probably the best way to do this.
  • the profile In order to avoid precipitation of Mg—Si containing particles larger than approximately 0.3 ⁇ m the profile needs to be cooled rather rapidly down to room temperature. The reason for this is described in a previous section.
  • the profile is flash annealed wild a heating time of maximum two minutes to a temperature of between 450-530° C. for not more than 5 minutes and subsequently quenched.
  • one option could be a second cold rolling operation to remove residual stresses from the quenching operation.
  • An alternative to cold rolling to remove residual stresses would be to stretch the material in way similar to what is done after extrusion, or performing a cold forging operation en blanks from the flash annealed and cooled material.
  • the profile could optionally be subjected to ageing after extrusion and prior to cold deforming.
  • the profile could be overaged to a T7 condition, for example at 200-230° C. for 1-5 hours.
  • the final ageing of the material can for example be done with the patented dual rate ageing cycle (U Tundal and O. Reiso, EP 1 155 161 B1) to get maximum strength with minimum amount of alloying elements.
  • Billets with diameter 95 mm were cast in a lab casting facility using the Hycast hot-top gas-slip technology (as described in EP 0 778 097 B1) and a TiB 2 based grain refiner.
  • the composition of the alloy is shown in Table 1.
  • the billets were homogenised at 575° C. for 2 hours and 13 minutes followed by cooling at a rata of approximately 400° C. per hour.
  • Extrusion of the billets was performed at an 8 MN laboratory extrusion press with a 100 mm diameter container to a profile with 5 ⁇ 40 mm 2 cross section.
  • the billet preheating temperature was approximately 500° C. and the extrusion speed 20 m/min. After extrusion the profile was quenched in water.
  • a 50 cm long piece from the front part of the extruded profile was cold rolled to give 10, 20, 40 and 60% reduction in the thickness.
  • the samples that were cold rolled to different thicknesses were then annealed in a salt bath which had been preheated to 500° C.
  • a hole was drilled into each of the samples to fit a thermocouple.
  • the heating time to temperature was in the range 5-10 seconds, depending on the thickness of the sample.
  • a holding time of 10 seconds started when the temperature reached 490° C. After annealing the samples were quenched in water.
  • the billets Prior to extrusion the billets had an even and small grain size.
  • the as extruded sample in FIG. 4 shows a homogeneous grain size throughout the cross section. In this case there is no coarse grain layer below the surface. This is maybe because the sample is smaller then the sample shown in FIG. 2 and maybe also because it is taken from the front part of the extruded length. It is evident that the grains under the randomly oriented layer of grains in the profile surface area are predominantly aligned in one direction since the colour contrast between the grains is low.
  • the cold rolled and annealed samples show a much more random orientation of the grains than the as extruded sample. This confirms that these samples are fully recrystallized after annealing.
  • the samples that were cold rolled to 10 and 20% reduction in thicknesses clearly have an uneven grain structure with the largest grains in the middle of the cross section.
  • the samples that were cold rolled to 40 and 60% reduction m thicknesses hove an even grain structure throughout the cross section.
  • the grain sizes of the samples shown in FIG. 4 (measured 250 ⁇ m below the surface of the cross sections) are shown in Table 2.
  • Billets with diameter 95 mm were cast in a lad casting facility using the Hycast hot-top gas-slip technology without using a grain refiner.
  • the composition of the alloy is shown in Table 3.
  • the cast billets were homogenised at 575° C. for 2 hours and 15 minutes followed by cooling at a rate of approximately 400° C. per hour.
  • Micrographs of the particle structure in the billets from the two different alloys in examples 1 and 2 are shown in FIG. 6 .
  • the material cast without grain refiner shows Fe containing particles (mainly ⁇ -AlFeSi) that are smaller and mush more evenly distributed than the Fe containing particles (mainly ⁇ -AlFeSi) in material cast with grain refine (lower picture).
  • the AlFeSi particles mainly are located at the grain boundaries.
  • the Fe/Si ratio is very low, which makes ⁇ -AlFeSi particles very stable in the homogenising process.
  • a particle structure as shown in the material cast without a grain refiner would be beneficial in avoiding alignment of particles and possible visible dark lines in the extruded and anodized high gloss surface.
  • the billets where extruded at an 8 MN laboratory extrusion press with a 100 mm diameter container to a profile with a cross section of 5 ⁇ 40 mm 2 .
  • the billet preheating temperature was approximately 500° C. and the extrusion speed 20 m/min. After extrusion the profile was quenched in water.
  • a 100 cm long piece from the back pad of the extruded profile was cold rolled to give 20, 30, 40 and 50% reduction in the thickness.
  • the samples that were cold rolled to different thicknesses were then annealed in a salt bath which had been preheated to 500° C.
  • a hole was drilled Into each of the samples to fit a thermocouple.
  • the holding time of 10 seconds started when the temperature reached 490° C.
  • one sample of the material cold roiled to 40% reduction in thickness was held 5 minutes at 500° C.
  • Yet another sample of the material cold rolled to 40% reduction in thickness was heated in an air circulating oven at a considerably lower heating rate to the annealing temperature than that obtained in a salt bath.
  • FIG. 7 A micrograph of the as extruded sample is shown in FIG. 7 . It seems like some of the grains below the surface are considerably larger than 100 ⁇ m, which could give some unwanted effects in the surface appearance. Inside the surface region the grains are strongly aligned in one direction, which gives very little contrast between each individual grain in the micrograph.
  • FIG. 8 shows micrographs of the grain structure in the as extruded sample as well as samples that have been cold roiled 20, 30, 40 and 50% and thereafter annealed.
  • the samples that were cold rolled to 20% reduction in thickness clearly have an uneven grain structure with the largest grains in the middle of the cross section.
  • the sample cold rolled to 30% reduction in thickness has smaller grains and a more even grain structure, but the grains in the middle still are somewhat larger than those towards the surfaces.
  • the samples that were cold rolled to 40 and 50% reduction in thicknesses have a smaller grain size and an even grain structure throughout the cross section. As also shown in Table 4 the grain size seems to be similar for the samples cold rolled to 40 and 50% reduction in thicknesses.
  • FIG. 9 shows that the sample heated in an air-circulating furnace (6-7 minutes heating time) has a more uneven grain structure and a slightly larger grain size than the sample that was rapidly heated (5-10 seconds) in a salt bath up to the solutionising temperature.
  • the reason for this is probably linked to precipitation of Mg—Si particles at the grain boundaries, which are pinning the nuclei for new grams during the heat up process.
  • Mg—Si particles In a sample which is slowly heated in air there is enough time for precipitation of Mg—Si particles to prevent the nuclei tor new grains from growing until the particles start to dissolve again, i.e., when the sample is approaching the solves temperature of the alloy. In this process some grains will probably start to grew earlier than others and therefore get larger, resulting in an uneven grain structure when the recrystallization process is complete.
  • Example 2 shows that it is beneficial to heat the cold rolled sample fast to the solutionising temperature to obtain en even grain size and that a holding time of only 10 seconds is sufficient to obtain a fully recrystallized grain structure.
  • Example 2 also shows that the final grain structure in the blanks could be perfect for providing attractive high gloss anodized surfaces even though the billet grain structure is regarded as being far from optimum when it is cast without grain refiner.
  • the main benefit of the present invention is a grain structure with an even grain size end a dose to random texture throughout the cross section o the profile irrespective of the grain size prior to cold rolling (and thus also of the grain structure of the billet).
  • An extruded thick welled flat profile will in most cases have a coarse grain layer that has to be removed in order to obtain a smooth anodized surface with a minimum of defects in the final product.
  • the amount of material that would have to be removed in the as extruded cross section is typically in the range 7-15%.
  • the cold rolling will ensure a very accurate thickness and flatness of the profile, and for that reason considerably reduce the need for machining.
  • An extruded profile will have much more variation in the thickness, typically ⁇ 0.1 mm.
  • the grain size in the billet end is of little importance for the resulting grain size in the cold rolled and annealed blanks there is a possibility of casting the billets with a minimum or even completely without the use of a grain refiner.
  • a grain refiner In order to avoid centre cracks in the billets in the startup of the cast it could be beneficial to add some grain refiner in the first metal in cast.
  • the grain refiner itself could be a source for inclusions that can cause failures in the anodized surface.
  • the possibility of reducing the Fe content and still obtain an adequate grain structure will significantly improve with the use of the present invention.
  • the lower Fe content can either be used to improve the gloss, or to keep the current gloss but add a thicker and more wear resistant oxide layer to the anodized product. The latter will make the product more durable.

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  • Mechanical Engineering (AREA)
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US15/124,726 2014-03-27 2015-03-24 Method for the manufacturing of products with anodized high gloss surfaces from extruded profiles of al-mg-si or al-mg-si cu extrusion alloys Abandoned US20170009322A1 (en)

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NO20140383 2014-03-27
NO20140383 2014-03-27
PCT/NO2015/000005 WO2015147648A1 (fr) 2014-03-27 2015-03-24 Procédé de fabrication de produits ayant des surfaces anodisées extrêmement brillantes à partir de profilés extrudés constitués d'alliages d'extrusion d'al-mg-si ou d'al-mg-si-cu

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US20180291482A1 (en) * 2017-04-05 2018-10-11 Novelis Inc. Anodized quality 5xxx aluminum alloys with high strength and high formability and methods of making the same
CN110669964A (zh) * 2019-10-31 2020-01-10 辽宁忠旺集团有限公司 一种高性能稀土Al-Mg-Si铝合金挤压材料及其制备方法
CN111549260A (zh) * 2019-02-08 2020-08-18 通用汽车环球科技运作有限责任公司 高强度延性铝合金挤压件

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CN106086553B (zh) * 2016-08-12 2018-01-23 浙江博奥铝业有限公司 一种用于穿条式隔热型材的铝合金型材及其制造方法
CN107541622B (zh) * 2017-08-10 2019-01-08 广东兴发铝业有限公司 一种交通运输工具用铝合金型材及其挤压方法
CN111304563B (zh) * 2020-03-26 2021-08-13 苏州铭德铝业有限公司 一种铝合金型材的加工方法及由其制备的铝合金型材
CN111945087B (zh) * 2020-09-02 2022-04-19 盐城工业职业技术学院 一种铝合金挤压型材的加工热处理工艺

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CN103409671B (zh) * 2013-07-26 2016-01-06 广东伟业铝厂集团有限公司 一种建筑模板用铝合金型材及其制备方法

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US20180291482A1 (en) * 2017-04-05 2018-10-11 Novelis Inc. Anodized quality 5xxx aluminum alloys with high strength and high formability and methods of making the same
US11821061B2 (en) * 2017-04-05 2023-11-21 Novelis Inc. Anodized quality 5XXX aluminum alloys with high strength and high formability and methods of making the same
CN111549260A (zh) * 2019-02-08 2020-08-18 通用汽车环球科技运作有限责任公司 高强度延性铝合金挤压件
US11359269B2 (en) 2019-02-08 2022-06-14 GM Global Technology Operations LLC High strength ductile 6000 series aluminum alloy extrusions
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CN110669964A (zh) * 2019-10-31 2020-01-10 辽宁忠旺集团有限公司 一种高性能稀土Al-Mg-Si铝合金挤压材料及其制备方法

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