EP1346075B1 - Aushärtbare aluminium-legierungen - Google Patents

Aushärtbare aluminium-legierungen Download PDF

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Publication number
EP1346075B1
EP1346075B1 EP01271462A EP01271462A EP1346075B1 EP 1346075 B1 EP1346075 B1 EP 1346075B1 EP 01271462 A EP01271462 A EP 01271462A EP 01271462 A EP01271462 A EP 01271462A EP 1346075 B1 EP1346075 B1 EP 1346075B1
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Prior art keywords
alloy
casting
temperature
hot
hot working
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Expired - Lifetime
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EP01271462A
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English (en)
French (fr)
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EP1346075A1 (de
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Gary John Mahon
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Rio Tinto Alcan International Ltd
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Alcan International Ltd Canada
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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
    • C22F1/047—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 magnesium 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

Definitions

  • This invention concerns AA5000 series alloys with the addition of Cu that can be retained in a solution treated condition after hot working, for example by hot rolling on a hot mill or by hot extruding.
  • the novel feature of this invention is the discovery that for certain Cu - containing AA5000 series alloys sufficient solution treatment occurs during hot working, for example hot rolling, to render the alloys age hardenable without a further expensive solution treating step. This gives a very significant economic advantage especially for commodity products such as can end stock, automotive sheet products, or extruded products such as structural sections.
  • EP-A-0605947 describes manufacturing can body sheet using two sequences of continuous operations. The described additional steps of uncoiling the hot coiled sheet, quenching the sheet without intermediate cooling, cold rolling and re-coiling the sheet are required, but these additional steps are not needed in the method of the present invention.
  • WO-A-99/39019 describes a method for making can end and tab stock but annealing of the sheet is required as a separate operation after hot rolling which is not needed in the method of the present invention.
  • WO-A-98/01593 describes a process for producing aluminium alloy can body stock but again a separate annealing step is required.
  • JP-A-100121179 describes aluminium alloy sheet for carbonated beverage can lids but a formal solution heat treatment is required, which is not needed in the method of the present invention.
  • US-A-5655593 describes aluminium alloy sheet manufacture in which the hot strip is cooled rapidly to minimise the precipitation of the alloying elements. This teaching of rapid cooling is contrary to that of the present invention.
  • US-A-3464866 describes a process for obtaining aluminium alloy conductors but again teaches rapid cooling.
  • the intermediate product is generally maintained at a temperature below the solvus temperature of the alloy, provided that if the intermediate product is heated above the alloy's solvus temperature then cooling thereof is effected at a rate less than 2°C/sec.
  • the solvus temperature of the alloy is meant the temperature below which under equilibrium conditions the copper begins to be removed from solid solution to form a precipitate. However, as to the rate of copper removed that will depend on the kinetics of the reaction.
  • the precipitation phase if formed is believed to be S phase (an AlCuMg phase) or its metastable precursors.
  • the alloy may be cast by DC casting to form an ingot or by continuous casting, for example in a belt caster or a twin roll casting machine, to form a sheet.
  • the cast and preferably homogenised alloy can be extruded but for the production of can end stock it is generally hot rolled. After casting the preferred steps are:
  • the metal temperature generally rises to about 100-200°C as it is passed through the mill.
  • the metal is coiled and being so massive the coiled metal takes a long time to cool down to room temperature. Phase precipitation and hardening can occur during this cooling down period without the need forcibly to cool the coil. Additional cooling can, however, be used if required.
  • re-heating can be effected if desired, for example to control the amount of cold work in the alloy. If this re-heating takes the alloy above its solvus temperature then cooling is preferably effected at a rate less than 2°C/sec to avoid distortion or to avoid the need for a separate quench stage.
  • the alloy could be cast continuously by for example belt casting or twin roll casting. These techniques allow thin strip to be produced of a thickness of generally as low as 5mm, and sometimes as low as 2mm. Such thin cast strip may or may not require homogenisation before hot rolling since it tends to cool so quickly that the Cu and Mg present are likely to remain in solid solution.
  • the casting could be extruded using direct or indirect extrusion.
  • the casting is homogenised as described above and then cooled to room temperature before being re-heated to 400 to 500°C for extrusion.
  • the casting can be cooled directly from its homogenisation temperature to the desired extrusion temperature.
  • the extrudate is cooled preferably with still air or with forced air. If desired, the extrudate can be re-heated to above the solvus temperature of the alloy and then cooled at a rate of less than 2°C/sec. This re-heating treatment may be needed for texture and/or grain size control. After extrusion the extrudate is generally stretched by about 1 ⁇ 2 to 2% and then aged.
  • the present invention has particular applicability for the production of can stock, especially can end stock (CES) which possesses a combination of high strength and formability.
  • CES can end stock
  • the combination of composition and process of the present invention overcomes many of the manufacturing difficulties of the conventional AA5182 sheet currently in use and is capable of producing CES at lower cost. It also improves the subsequent performance of the can end, most notably its scoreline corrosion resistance.
  • the invention is particularly suitable for downgauging to produce lighter weight can ends, i.e. gauges down to say 0.150mm.
  • the preferred method is to cast an ingot, homogenise it, and hot roll to, say, 2mm to form strip.
  • a key aspect of the invention is that the strip does not need an additional solution heat treatment step.
  • the material does not need to be rapidly cooled, e.g. does not need to be quenched into water; the cooling is generally air cooled (possible forced air).
  • the coil is then cold rolled to final gauge and lacquered.
  • the range (in weight percent) for the principal elements over which this invention is operable is:
  • the hot rolling conditions are selected to ensure that the hot rolled sheet recrystallises on or before coiling or very shortly thereafter.
  • the sheet is fully recrystallised resulting in a low dislocation density. Recrystallisation is encouraged by arranging for the minimum temperature of the sheet as it exits from the rolling mill to be 250°C, preferably 270°C and more preferably 300°C and/or arranging for the cooling rate of the sheet to be sufficiently slow to allow time for the sheet to recrystallise when in its coiled form or during coiling.
  • the coiling temperature is approximately the same as the exit rolling mill temperature.
  • additional cooling means are provided after the mill the minimum coiling temperature should be in the range of minimum mill exit temperatures mentioned above. In practice acceptable cooling rates are found to be of the order of 0.1 and preferably 0.2 to 5°C/minute over the temperature range of 400-200°C. There is no need to uncoil the sheet during cooling in order, for example, to quench it.
  • a high rolling mill exit temperature encourages precipitation of S phase or its precursors while the strip or coil is cooling. Cooling more quickly can counter this and prevent precipitation but if the exit temperature becomes too high, the cooling rate required is too fast to be practically useful.
  • the upper limit to the mill exit temperature especially for the alloys richer in Cu and Mg, should preferably be lower than the solvus temperature of the alloy.
  • Figure 1 gives an indication of the solvus temperature as a function of the Mg and Cu contents.
  • the maximum exit temperature should be between 340°C and 360°, although up to 380°C is possible for some alloys.
  • the location of the nose of the c-curve for these alloys when recrystallised varies with the composition of the alloy.
  • the nose of the curve is located at a time of around 100 to 1000 seconds.
  • the nose is moved to longer times whilst for more concentrated alloys the nose is moved to shorter times.
  • the time indicated in Figure 2 compares with times of between 1 and 100 seconds for conventional age hardening systems such as AA7075, AA2017, AA6061 and AA6063.
  • this provides longer times at temperatures below the solvus temperature in which to cool the strip and still maintain the Cu (and Mg) in solid solution.
  • a cooling rate of 5°C/min is sufficient substantially to miss the nose of the c-curve and provide a substantial age hardening response during subsequent processing.
  • This cooling rate can be achieved by, for example, forced air cooling of a coil.
  • Previous art regarding solution heat treatment of these Al-Mg-Cu alloys teaches that, not only is a separate solution heat treatment stage required, but that the strip must be quenched with a cooling rate of 2°C/second or faster. For the present invention it has been found that neither of these steps need to be used, thereby providing a lower cost manufacturing route for these alloys. Likewise no separate annealing step is needed after the hot working step and before the cooling step.
  • This solute is then used to give a significant precipitation hardening effect during subsequent thermomechanical processing.
  • an increased dislocation density is introduced giving enhanced nucleation sites for the strengthening phase.
  • This deformation may not be needed for all applications of this invention, since for these compositions it is known that the precipitation can also occur in the absence of dislocations, albeit at slower rates.
  • the precipitating phase is believed to be S-phase which can form as needles or rods on the dislocation structure. In the case of CES this precipitation could occur during a separate ageing step or during the thermal history which the material would experience during deformation in, for example, strip rolling.
  • Mn can be added as a strengthening element and to control grain size and is therefore desirably kept as high as possible.
  • Mn inhibits recrystallisation after hot rolling or during annealing, and so a maximum Mn content of 0.4% may have to be set in order to achieve full recrystallisation for some alloys under certain conditions.
  • it may be desirable to have a minimum of at least 0.05%Mn and preferably at least 0.1%Mn present in the alloy.
  • Recrystallisation may also be important for crystallographic texture control in CES, but this may not be necessary if the can end tooling is modified to take significantly higher levels of earing into account. Crystallographic texture control can also be important for automotive sheet formability; another potential application of this invention.
  • composition used in the present invention is the importance of having low Fe and Si in the alloy, since this will prevent the presence of excessive numbers of coarse constituent particles in the sheet. These form during solidification and cannot be fully dissolved during homogenisation of the ingot. Although they break up during rolling, their presence is sufficient adversely to affect formability. Since this invention has been found to produce improved formability over existing AA5182 CES, the strip may be able to tolerate higher levels of these elements, thus reducing cost. Tolerance of higher levels of Si and Fe may allow greater use of recycled aluminium scrap and this is another important aspect of this invention. Up to 0.5%Fe may be tolerated in the alloy and preferably up to 0.3%Fe. The minimum amount of Fe present will be dictated by cost and there is unlikely to be less than 0.1Fe. Silicon up to 0.3% may be present, preferably up to 0.2%.
  • Another advantage over conventional AA5182 CES is that the lower Mg content will also make the can end less susceptible to stress corrosion cracking (SCC), which can lead to catastrophic failure of the end under the stressed conditions which are encountered in the pressurised can.
  • SCC stress corrosion cracking
  • the invention described here will make the end less sensitive to these conditions, since the lower Mg content reduces beta-phase precipitation, which has been linked to SCC. Avoidance of SCC is also important in many other applications including car body sheet.
  • CES is currently made from AA5182 and gets its strength predominantly from a combination of solute hardening and strain hardening. This makes it difficult to roll and gives a relatively high manufacturing cost.
  • the alloy used in the present invention has lower strength during the rolling operations, but develops its strength during subsequent thermal exposure during fabrication. Thus there is the benefit of rolling a lower strength sheet, but still enabling the desired sheet properties to be obtained ultimately. It is also possible to produce a higher strength sheet suitable for downgauging without a reduction in rollability (higher rolling loads, more difficulties in performing the rolling operation) encountered in higher Mg containing alloys such as AA5182 and AA5019A.
  • the present invention is also applicable to production of low cost automotive sheet where the material could be used in the hot rolled condition (Direct Hot Roll to Gauge), thereby potentially avoiding the need to solution heat treat the sheet.
  • the sheet could be cold rolled to gauge, as for CES, with a final continuous anneal to impart the formability required for this application and to take the solute into solution. Cooling after annealing should be sufficiently rapid to retain substantially all of the solute in solution. Ageing could be carried out in a separate operation before or after forming, for example during the paint bake stoving of the automotive part.
  • An alloy of the following composition was cast as a 225mm x 75mm cross section DC ingot; Magnesium 3.0 wt.% Copper 0.4 wt.% Manganese 0.25 wt.% Iron 0.20 wt.% Silicon 0.12 wt.% Balance aluminium with incidental impurities.
  • the ingot was not grained refined during casting and as a consequence the Ti level was 0.0018% and B was less than 0.0001%.
  • the strip was either solution heat treated (SHT) (5 minutes at 550°C) and cold water quenched (CWQ) or it was solution heat treated and then air cooled to temperatures in the range 300 to 340°C and then cooled at 1°C/min. Conductivity was measured at this stage to determine how much solute remained in solid solution. These conditions were selected to simulate the conditions which might be expected to exist during commercial use of this invention. Until the strip temperature drops below the solvus temperature for the alloy the S phase therein cannot precipitate and therefore the Cu (and Mg) would be substantially in solid solution. The strip could then be quenched at the end of hot rolling or, preferably, cooled after coiling.
  • SHT solution heat treated
  • CWQ cold water quenched
  • the starting temperature could be in the range 300 to 340°C and a typical initial cooling rate would be 1°C/min.
  • the temperature range between the solvus temperature (about 390°C for the alloy) and the coiling temperature is passed through very quickly since this is when the strip might typically be in the hot tandem mill and, hence, there is lubricant applied to the strip which acts as a coolant.
  • This phase was simulated using the air cool from the solution heat treatment temperature.
  • the strip was then cold rolled to 0.24mm and given a simulation of a coil cool down to ambient temperature from 150°C at 0.4°C/min. It was then given a simulation of a lacquer curing cycle for 3 minutes at 205°C. Tensile testing was performed at each stage of the treatment and the results compared with results on conventional AA5182 CES materials processed in the laboratory.
  • the levels of cold reduction needed to generate the desired strength level are lower and thus the weakest direction is likely to be this longitudinal value.
  • the combination of the composition and processing route of the present invention is capable of producing a strength level approximately 45 MPa stronger than existing AA5182.
  • Comparison of properties with conventional CES Condition 5182 CES This alloy As-rolled at final gauge 430 MPa 399 MPa As-rolled and coil annealed 358 MPa 386 MPa As-lacquered 345 MPa 370 MPa
  • An alloy of the following composition was DC cast for processing within an industrial plant: Magnesium 2.9 wt.% Copper 0.4 wt.% Manganese 0.1 wt.% Iron 0.20 wt.% Silicon 0.08 wt.% Balance aluminium with incidental impurities. The ingots were cast with additional grain refiner.
  • the ingot were homogenised at 540°C and hot rolled on a single stand reversing mill to a thickness of 38mm at which point the temperature was around 480°C.
  • the strip was then hot rolled through a 3-stand hot tandem mill to a gauge of 2.5mm.
  • the conditions were adjusted to give two different coiling temperatures in order to show the effects at opposite extremes of this invention. In both cases the coils were forced-air cooled, giving a cooling rate measured on the outer laps of the coil of around 0.7°C/min.
  • the cooler coil was processed to give a sidewall temperature of 280-290°C.
  • the microstructure of the strip was largely unrecrystallised.
  • the solute was easily removed from solid solution on the pre-existing dislocation structure from the hot deformation.
  • the conductivity of this strip is shown in Table 4, showing that the %IACS value is similar to that in which all of the precipitation has been allowed to occur.
  • Table 4 is presented the conductivity obtained by using a still-air cool on strips of the 2.5mm thick metal at the end of the hot rolling (approximately 60°C per minute), showing that at these cooling rates a significant amount of the solute can be kept in solid solution.
  • the hotter coil was processed to give a coil sidewall temperature of 330-340°C.
  • Table 4 shows that in this case the forced air cooling leaves more solute in solid solution as a consequence of the fully recrystallised grain structure achieved with the higher coiling temperature.
  • the amount of solute in solid solution with the faster cool is even higher and approaches that of the conventional solution heat treated (SHT) and cold water quenched (CWQ) material.
  • SHT solution heat treated
  • CWQ cold water quenched

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Claims (13)

  1. Verfahren zur Herstellung von aushärtenden Aluminiumlegierungen, das die folgenden Schritte umfasst:
    a) Gießen einer Legierung, die das Folgende in Gewichtsprozent ausgedrückt enthält: Magnesium 1,0 bis 4,0 Kupfer 0,1 bis 0,6 Mangan bis zu 0,8 Eisen bis zu 0,5 Silizium bis zu 0,3 Chrom bis zu 0,15 Titan bis zu 0,15 Rest Aluminium mit allfälligen Verunreinigungen
    b) wahlweise Homogenisieren der gegossenen Legierung
    c) Warmumformen des Gussstücks bei einer anfänglichen Temperatur von mindestens 400 °C , um ein Zwischenprodukt zu erhalten, wobei mindestens ein Teil der Warmumformung durchgeführt wird, während das Gussstück eine Temperatur oberhalb der Lösungstemperatur der Legierung hat,
    d) Kühlen des Zwischenprodukts entweder während dem Warmumformen oder in einem darauffolgenden Schritt mit einer Geschwindigkeit von weniger als 5 °C/min , so dass mindestens eine teilweise erholte oder rekristallisierte Struktur gebildet wird, und dass in der festen Lösung in der Legierung genügend Kupfer verbleibt, um einen Aushärtungseffekt bei der Legierung hervorzurufen, wenn während der weiteren thermischen Geschichte der Legierung Phasenauskristallisierung eintritt, und
    e) wahlweise Zulassen oder Herbeiführen des Eintretens von Phasenauskristallisierung in der Legierung.
  2. Verfahren nach Anspruch 1, wobei die Legierung die folgende Zusammensetzung, in Gewichtsprozent ausgedrückt hat: Magnesium 1,0 bis 4,0 Kupfer 0,2 bis 0,5 Mangan bis zu 0,6, vorzugsweise bis zu 0,5 Eisen 0,1 bis 0,3 Silizium bis zu 0,2 Chrom bis zu 0,15 Titan bis zu 0,15 Bor oder Kohlenstoff bis zu 0,01 Rest Aluminium mit allfälligen Verunreinigungen
  3. Verfahren nach Anspruch 2, wobei der Magnesiumgehalt 2,5 bis 4 % ist.
  4. Verfahren nach einem der Ansprüche 1 bis 3, wobei das Zwischenprodukt eine praktisch vollständig erholte oder rekristallisierte Struktur hat.
  5. Verfahren nach einem der vorhergehenden Ansprüche, wobei das Gussstück vor der Warmumformung bei einer Temperatur von mindestens 480 °C, vorzugsweise 500 bis 600 °C homogenisiert wird, so dass praktisch alles Kupfer und Magnesium in dem Gussstück in fester Lösung sind.
  6. Verfahren nach einem der vorhergehenden Ansprüche, wobei das Gusstück warmumgeformt wird, wahlweise mit Wiedererhitzen des Gussstückes über die Lösungstemperatur der Legierung, und vorzugsweise auf mindestens 450 °C, um praktisch alles vorhandene Magnesium und Kupfer in die feste Lösung zu nehmen.
  7. Verfahren nach einem der vorhergehenden Ansprüche, wobei der Warmumformungsschritt durchgeführt wird, wenn das Gussstück eine anfängliche Temperatur von 450 °C bis 580 °C hat.
  8. Verfahren nach einem der vorhergehenden Ansprüche, wobei die Legierung stranggegossen wird.
  9. Verfahren nach einem der vorhergehenden Ansprüche, das den Schritt des Kaltwalzens des warmumgeformten Gussstücks, wahlweise mit Aufwickeln, umfasst.
  10. Verfahren nach einem der Ansprüche 1 bis 9, wobei die Warmumformung durch Strangpressen durchgeführt wird.
  11. Verfahren nach einem der Ansprüche 1 bis 9, wobei die Warmumformung durch Warmwalzen durchgeführt wird.
  12. Verfahren nach einem der vorhergehenden Ansprüche, wobei das warmumgeformte Gussstück mit einer Geschwindigkeit von weniger als 1 °C/min abgekühlt wird.
  13. Verfahren nach einem der vorhergehenden Ansprüche, wobei, wenn nach dem Warmumformungsschritt die Temperatur des Zwischenproduktes die Lösungstemperatur der Legierung überschreitet, das Kühlen des Zwischenprodukts unter die Lösungstemperatur mit einer Geschwindigkeit von weniger als 2 °C/sec durchgeführt wird.
EP01271462A 2000-12-20 2001-12-20 Aushärtbare aluminium-legierungen Expired - Lifetime EP1346075B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GB0031104 2000-12-20
GBGB0031104.3A GB0031104D0 (en) 2000-12-20 2000-12-20 Age hardened aluminium alloys
PCT/GB2001/005686 WO2002050329A1 (en) 2000-12-20 2001-12-20 Age-hardenable aluminium alloys

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EP1346075A1 EP1346075A1 (de) 2003-09-24
EP1346075B1 true EP1346075B1 (de) 2004-10-13

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US (1) US20040089379A1 (de)
EP (1) EP1346075B1 (de)
JP (1) JP2004522854A (de)
AT (1) ATE279546T1 (de)
AU (1) AU2002216221A1 (de)
CA (1) CA2431029A1 (de)
DE (1) DE60106488T2 (de)
GB (1) GB0031104D0 (de)
WO (1) WO2002050329A1 (de)

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CN101440448B (zh) * 2008-10-23 2010-06-16 无锡麟龙铝业有限公司 一种能在±125℃下使用的铸铝合金及其制造方法
RU2468113C1 (ru) * 2011-11-09 2012-11-27 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Российский государственный профессионально-педагогический университет" (РГППУ) Способ обработки изделий из алюминиевых сплавов (варианты)
CN105896118A (zh) * 2016-04-15 2016-08-24 河北欣意电缆有限公司 Al-Fe-B-RE铝合金电缆铜铝过渡端子及其制备方法
CN105896119A (zh) * 2016-04-15 2016-08-24 河北欣意电缆有限公司 Al-Fe-Be-RE铝合金电缆铜铝过渡端子及其制备方法

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US9217622B2 (en) * 2009-07-24 2015-12-22 Alcoa Inc. 5XXX aluminum alloys and wrought aluminum alloy products made therefrom
KR101191772B1 (ko) 2010-01-08 2012-10-16 (주)일우정밀 자동차 핸들용 알루미늄 합금 조성물의 제조방법
US9587298B2 (en) * 2013-02-19 2017-03-07 Arconic Inc. Heat treatable aluminum alloys having magnesium and zinc and methods for producing the same
CN104451285A (zh) * 2014-11-28 2015-03-25 苏州有色金属研究院有限公司 车身用Al-Mg合金板材及其制造方法
JP6208389B1 (ja) 2016-07-14 2017-10-04 株式会社Uacj 曲げ加工性及び耐リジング性に優れたアルミニウム合金からなる成形加工用アルミニウム合金圧延材の製造方法
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CN113646116A (zh) * 2019-02-07 2021-11-12 埃奎斯费雷斯公司 用于包括再熔工艺的应用的具有低沉淀物密度的合金及其制备方法
CN109772893B (zh) * 2019-02-18 2020-02-14 重庆大学 最大化轧辊利用的多热轧单元批量计划优化方法及控制系统
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US20230016262A1 (en) * 2019-12-16 2023-01-19 Rio Tinto Alcan International Limited High Strength Aluminum Alloys
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CN101440448B (zh) * 2008-10-23 2010-06-16 无锡麟龙铝业有限公司 一种能在±125℃下使用的铸铝合金及其制造方法
RU2468113C1 (ru) * 2011-11-09 2012-11-27 Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Российский государственный профессионально-педагогический университет" (РГППУ) Способ обработки изделий из алюминиевых сплавов (варианты)
CN105896118A (zh) * 2016-04-15 2016-08-24 河北欣意电缆有限公司 Al-Fe-B-RE铝合金电缆铜铝过渡端子及其制备方法
CN105896119A (zh) * 2016-04-15 2016-08-24 河北欣意电缆有限公司 Al-Fe-Be-RE铝合金电缆铜铝过渡端子及其制备方法

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CA2431029A1 (en) 2002-06-27
US20040089379A1 (en) 2004-05-13
DE60106488T2 (de) 2005-12-01
JP2004522854A (ja) 2004-07-29
WO2002050329A1 (en) 2002-06-27
EP1346075A1 (de) 2003-09-24
DE60106488D1 (de) 2004-11-18
ATE279546T1 (de) 2004-10-15
GB0031104D0 (en) 2001-01-31

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