EP1127948B1 - Superalliages monocristallins à base de nickel résistant à la corrosion à haute température - Google Patents

Superalliages monocristallins à base de nickel résistant à la corrosion à haute température Download PDF

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EP1127948B1
EP1127948B1 EP95116194A EP95116194A EP1127948B1 EP 1127948 B1 EP1127948 B1 EP 1127948B1 EP 95116194 A EP95116194 A EP 95116194A EP 95116194 A EP95116194 A EP 95116194A EP 1127948 B1 EP1127948 B1 EP 1127948B1
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percent
superalloy
alloy
gas turbine
nickel
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EP95116194A
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German (de)
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EP1127948A2 (fr
EP1127948A3 (fr
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Gary L. Erickson
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Cannon Muskegon Corp
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Cannon Muskegon Corp
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Priority to DE69527557T priority Critical patent/DE69527557T2/de
Priority to EP95116194A priority patent/EP1127948B1/fr
Priority to DK95116194T priority patent/DK1127948T3/da
Priority to AT95116194T priority patent/ATE221138T1/de
Priority to ES95116194T priority patent/ES2184779T3/es
Publication of EP1127948A2 publication Critical patent/EP1127948A2/fr
Publication of EP1127948A3 publication Critical patent/EP1127948A3/fr
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%

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  • This invention relates to single crystal nickel-based superalloys and, more particularly, single crystal nickel-based superalloys and articles made therefrom having increased resistance to bare hot corrosion for use in gas turbine engines.
  • U.K. Patent Application Publication No. 2153848A discloses nickel-base alloys having a composition within the range of 13-15.6% chromium, 5-15% cobalt, 2.5-5% molybdenum, 3-6% tungsten, 4-6% titanium, 2-4% aluminum, and the balance essentially nickel without intentional additions of carbon, boron or zirconium, which are fabricated into single crystals.
  • the alloys taught by this reference claim an improvement in hot corrosion resistance accompanied by an increase in creep rupture properties, the need remains in the art for single crystal superalloys for industrial gas turbine applications having a superior combination of increased hot corrosion resistance, oxidation resistance, mechanical strength, large component castability and adequate heat treatment response.
  • Single crystal articles are generally produced having the low-modulus (001) crystallographic orientation parallel to the component dendritic growth pattern or blade stacking axis.
  • Face-centered cubic (FCC) superalloy single crystals grown in the (001) direction provide extremely good thermal fatigue resistance relative to conventionally cast polycrystalline articles. Since these single crystal articles have no grain boundaries, alloy design without grain boundary strengtheners, such as carbon, boron and zirconium, is possible. As these elements are alloy melting point depressants, their essential elimination from the alloy design provides a greater potential for high temperature mechanical strength achievement since more complete gamma prime solution and microstructural homogenization can be achieved relative to directionally solidified (DS) columnar grain and conventionally cast materials, made possible by a higher incipient melting temperature.
  • DS directionally solidified
  • alloys must be designed to avoid tendency for casting defect formation such as freckles, slivers, spurious grains and recrystallization, particularly when utilized for large cast components. Additionally, the alloys must provide an adequate heat treatment "window" (numeric difference between an alloy's gamma prime solvus and incipient melting point) to allow for nearly complete gamma prime solutioning. At the same time, the alloy compositional balance should be designed to provide an adequate blend of engineering properties necessary for operation in gas turbine engines. Selected properties generally considered important by gas turbine engine designers include: elevated temperature creep-rupture strength, thermo-mechanical fatigue resistance, impact resistance, hot corrosion and oxidation resistance, plus coating performance. In particular, industrial turbine designers require unique blends of hot corrosion and oxidation resistance, plus good long-term mechanical properties.
  • the unique superalloy of the present invention provides an excellent blend of the properties necessary for use in producing single crystal articles for operation in industrial and marine gas turbine engine hot sections.
  • the base element is nickel.
  • the present invention provides a single crystal superalloy having an increased resistance to hot corrosion, an increased resistance to oxidation, and increased creep-rupture strength.
  • the article can be a component for a gas turbine engine and, more particularly, the component can be a gas turbine blade or gas turbine vane.
  • the superalloy compositions of this invention have a critically balanced alloy chemistry which results in a unique blend of desirable properties, including an increased resistance to hot corrosion, which are particularly suitable for industrial and marine gas turbine applications. These properties include: excellent bare hot corrosion resistance and creep-rupture strength; good bare oxidation resistance; good single crystal component castability, particularly for large blade and vane components; good solution heat treatment response; adequate resistance to cast component recrystallization; adequate component coatability and microstructural stability, such as long-term resistance to the formation of undesirable, brittle phases called topologically close-packed (TCP) phases.
  • TCP topologically close-packed
  • the hot corrosion resistant nickel-based superalloy of the present invention comprises the following elements in percent by weight: 14.2-15.5% Chromium; 2.0-4.0% Cobalt; 0.30-0.45% Molybdenum; 4.0-5.0% Tungsten; 4.5-5.8% Tantalum; 0.05-0.25% Niobium; 3.2-3.6% Aluminum; 4.0-4.4% Titanium; 0.01-0.06% Hafnium; 0-0.05% Carbon; 0-0.03% Boron; 0-0.03% Zirconium; 0-0.25% Rhenium; 0-0.10% Silicon; 0-0.10% Manganese; balance - Nickel + Incidental Impurities.
  • This superalloy composition also has a phasial stability number N V38 less than 2.45.
  • this invention has a critically balanced alloy chemistry which results in a unique blend of desirable properties useful for industrial and marine gas turbine engine applications. These properties include a superior blend of bare hot corrosion resistance and creep-rupture strength relative to prior art single crystal superalloys for industrial and marine gas turbine applications, bare oxidation resistance, single crystal component castability, and microstructural stability, including resistance to TCP phase formation under high stress, high temperature conditions.
  • Superalloy chromium content is a primary contributor toward attaining superalloy hot corrosion resistance.
  • the superalloys of the present invention have a relatively high chromium content since alloy hot corrosion resistance was one of the primary design criteria in the development of these alloys.
  • the chromium is 14.2-15.5% by weight.
  • the chromium content is from 14.3% to 15.0% by weight.
  • chromium provides hot corrosion resistance, it may also assist with the alloys' oxidation capability. Additionally, this superalloys' tantalum and titanium contents, as well as its Ti:Al ratio being greater than 1, are beneficial for hot corrosion resistance attainment.
  • chromium contributes to the formation of Cr and W-rich TCP phase and must be balanced accordingly in these compositions.
  • the cobalt content is 2.0-4.0% by weight. In another embodiment of the present invention, the cobalt content is from 2.5% to 3.5% by weight.
  • the chromium and cobalt levels in these superalloys assist in making the superalloy solution heat treatable, since both elements tend to decrease an alloy's gamma prime solvus.
  • Proper balancing of these elements in the present invention in tandem with those which tend to increase the alloy's incipient melting temperature, such as tungsten and tantalum result in superalloy compositions which have desirable solution heat treatment windows (numerical difference between an alloy's incipient melting point and its gamma prime solvus), thereby facilitating full gamma prime solutioning.
  • the cobalt content is also beneficial to the superalloy's solid solubility.
  • the tungsten content is 4.0-5.0% by weight and, advantageously, the amount of tungsten is from 4.2% to 4.8% by weight.
  • Tungsten is added in these compositions since it is an effective solid solution strengthener and it can contribute to strengthening the gamma prime. Additionally, tungsten is effective in raising the alloy's incipient melting temperature.
  • tantalum is a significant solid solution strengthener in these compositions, while also contributing to enhanced gamma prime particle strength and volume fraction.
  • the tantalum content is 4.5-5.8% by weight and, advantageously, the tantalum content is from 4.8% to 5.4% by weight.
  • tantalum is beneficial since it helps to provide bare hot corrosion and oxidation resistance, along with aluminide coating durability.
  • tantalum is an attractive single crystal alloy additive in these compositions since it assists in preventing "freckle" defect formation during the single crystal casting process particularly when present in greater proportion than tungsten (i.e., the Ta W ration is greater than 1).
  • tantalum is an attractive means of strength attairment in these alloys since it is believed not to directly participate in TCP phase formation.
  • the molybdenum content is 0.30-0.45% by weight.
  • molybdenum is present in an amount of from 0.35% to 0.43% by weight.
  • Molybdenum is a good solid solution strengthener, but it is not as effective as tungsten and tantalum, and it tends to be a negative factor toward hot corrosion capability.
  • the addition of molybdenum is a means of assisting control of the overall alloy density in the compositions of this invention. It is believed that the relatively low molybdenum content is unique in this class of bare hot corrosion resistant nickel-based single crystal superalloys.
  • the aluminum content is 3.2-3.6% by weight. Furthermore, the amount of aluminum present in these compositions is advantageously from 3.3% to 3.5% by weight.
  • Aluminum and titanium are the primary elements comprising the gamma prime phase, and the sum of aluminum plus titanium in the present invention is from 7.2 to 8.0 percent by weight. These elements are added in these compositions in a proportion and ratio consistent with achieving adequate alloy castability, solution heat treatability, phasial stability and the desired blend of high mechanical strength and hot corrosion resistance. Aluminum is also added to these alloys in proportions sufficient to provide oxidation resistance.
  • the titanium content is 4.0-4.4% by weight.
  • titanium is present in this composition in an amount from 4.1% to 4.3% by weight.
  • These alloys' titanium content is relatively high and, therefore, is beneficial to the alloys' hot corrosion resistance. However, it can also have a negative effect on oxidation resistance, alloy castability and alloy response to solution heat treatment. Accordingly, it is critical that the titanium content is maintained within the stated range of this composition and the proper balancing of the aforementioned elemental constituents is maintained. Furthermore, maintaining the alloys' Ti:Al ratio greater than 1 is critical in achieving the desired bare hot corrosion resistance in these compositions.
  • the niobium content is 0.05%-0.25% by weight and, advantageously, the niobium content is from 0.05% to 0.12% by weight.
  • Niobium is a gamma prime forming element and it is an effective strengthener in the nickel-based superalloys of this invention. Generally, however, niobium is a detriment to alloy oxidation and hot corrosion properties, so its addition to the compositions of this invention is minimized.
  • niobium is added to this invention's compositions for the purpose of gettering carbon, which can be chemi-sorbed into component surfaces during non-optimized vacuum solution heat treatment procedures.
  • any carbon pick-up will tend to form niobium carbide instead of titanium or tantalum carbide, thereby preserving the greatest proportion of titanium and/or tantalum for gamma prime and/or solid solution strengthening in these alloys. Furthermore, it is critical that the sum of niobium plus hafnium is from 0.06 to 0.31 percent by weight in these compositions in order to enhance the strength of these superalloys.
  • hafnium content is 0.01%-0.06% by weight and, advantageously, hafnium is present in an amount from 0.02% to 0.05% by weight.
  • Hafnium is added in a small proportion to the present compositions in order to assist with coating performance and adherence.
  • Hafnium generally partitions to the gamma prime phase.
  • the balance of this invention's superalloy compositions is comprised of nickel and small amounts of incidental impurities.
  • incidental impurities are entrained from the industrial process of production, and they should be kept to the least amount possible in the composition so that they do not affect the advantageous aspects of the superalloy.
  • these incidental impurities may include up to 0.05 percent carbon, up to 0.03 percent boron, up to 0.03 percent zirconium, up to 0.25 percent rhenium, up to 0.10 percent silicon, and up to 0.10 percent manganese. Amounts of these impurities which exceed the stated amounts could have an adverse effect upon the resulting alloy's properties.
  • N v38 is defined by the PWA N-35 method of nickel-based alloy electron vacancy TCP phase control factor calculation. This calculation is as follows:
  • the superalloys of this invention can be used to suitably make single crystal articles, such as components for industrial and marine gas turbine engines.
  • these superalloys are utilized to make a single crystal casting to be used under high stress, high temperature conditions characterized by an increased resistance to hot corrosion (sulfidation) under such conditions, particularly high temperature conditions involving corrosive atmospheres containing sulfur, sodium and vanadium contaminants, up to about 1922°F (1050°C). While these superalloys can be used for any purpose requiring high strength castings produced as a single crystal, their particular use is in the casting of single crystal blades and vanes for industrial and marine gas turbine engines.
  • the single crystal components made from this invention's compositions can be produced by any of the single crystal casting techniques known in the art.
  • single crystal directional solidification processes can be utilized, such as the seed crystal process and the choke process.
  • the single crystal castings made from the superalloys of the present invention can be aged at a temperature of from about 1800°F (982°C) to about 2125°F (1163°C) for about 1 to about 50 hours.
  • a temperature of from about 1800°F (982°C) to about 2125°F (1163°C) for about 1 to about 50 hours.
  • the optimum aging temperature and time for aging depends on the precise composition of the superalloy.
  • This invention provides superalloy compositions having a unique blend of desirable properties. These properties include: excellent bare hot corrosion resistance and creep-rupture strength; good oxidation resistance; good single crystal component castability, particularly for large blade and vane components; good solution heat treatment response; adequate resistance to cast component recrystallization; adequate component coatability and microstructural stability, such as long-term resistance to the formation of undesirable, brittle phases called topologically close-packed (TCP) phases.
  • TCP topologically close-packed
  • Test materials were prepared to investigate the compositional variations and ranges for the superalloys of the present invention.
  • One of the alloy compositions tested and reported below CMSX-11B falls outside the claimed scope of the present invention, but is included for comparative purposes to assist in the understanding of the invention.
  • Representative alloy aim chemistries of materials tested are reported in Table 1 below.
  • AIM CHEMISTRIES ELEMENT CMSX-11C CMSX-11C' CMSX-11C" CMSX-11B C Lap Lap Lap Lap Cr 14.5 14.5 14.4 12.5 Co 3.0 2.5 2.9 6.0 Mo .40 .35 .40 0.55 W 4.4 4.6 4.5 5.0 Ta 4.95 5.1 5.1 5.15 Cb (Nb) .10 .08 .10 0.20 Al 3.40 3.40 3.4 3.60 Ti 4.20 4.15 4.2 4.20 Hf .04 .03 .04 0.040 Ni BAL BAL BAL BAL N v38 2.41 2.40 2.42 2.42 NOTE: Chemistries are in wt. %.
  • Test materials defined by the CMSX®-11C aim chemistry shown in Table 1 were initially produced by mixing 15 lbs. of the heat R2D2 alloy (see Table 2 below) with 8 lbs. of virgin materials, melting and subsequently pouring the melt into a ceramic shell mold.
  • CMSX is a registered trademark of Cannon-Muskegon Corporation, assignee of the present application.
  • test specimens produced were used to develop appropriate solution heat treatment procedures, with the results reported in Table 3 below. Complete coarse ⁇ ' and eutectic ⁇ - ⁇ ' solutioning was achieved with a peak solution temperature of 2309°F (1265°C) applied. But variable levels of test specimen recrystallization, occurring during solution heat treatment, was observed. This problem was alleviated by reducing the CMSX-11C alloy peak solution temperature to 2289°F (1254°C), where full ⁇ ' solutioning still prevailed.
  • CMSX-11C' and CMSX-11C were solution treated to a peak temperature of 2289°F (1254°C) with similar results.
  • test specimens were further heat treated by aging initially at 2050°F (1121°C) to encourage a desirable ⁇ ' morphology and distribution, followed by secondary ages at 1600°F (871°C) and 1400°F (760°C), respectively (see Table 3 below).
  • HEAT TREATMENT ALLOY PEAK SOLUTION TEMP All test specimens were further heat treated by aging initially at 2050°F (1121°C) to encourage a desirable ⁇ ' morphology and distribution, followed by secondary ages at 1600°F (871°C) and 1400°F (760°C), respectively (see Table 3 below).
  • DTA Differential Thermal Analysis
  • test bars were machined and low-stress ground to ASIM standard proportional specimen dimension for subsequent stress - and creep-rupture testing at various conditions of temperature and stress, according to standard ASTM procedure. Specimens removed from solid turbine blades were prepared similarly.
  • Table 5 shows the results of stress - and creep-rupture tests undertaken with the CMSX-11C alloy specimens. The tests were performed at conditions ranging 1400-1900°F (760-1038°C).
  • test bars were exposed to 1600°F/39.2 ksi (870°C/270 MPa) condition for 200 hours. The respective bar gage sections were then reviewed and no sign of deleterious phase formation was observed.
  • Figure 1 illustrates the results of additional hot corrosion tests undertaken with CMSX-11C alloy and other alloys to 500 hours exposure in synthetic slag (GTV Type) plus .03 volume percent SO X in air.
  • the 500 hour tests were undertaken at 1382, 1562, 1652°F, (750, 850 and 900°C). The results indicate that the CMSX-11C alloy provides extremely good corrosion resistance at all three test temperatures.
  • the burner rig tests were performed at 1652°F (900°C) and 1922°F (1050°C), and the test results are reported below in Tables 9 and 10, respectively.
  • the .35 in. (9 mm) diameter x 3.9 in. (100 mm) long test pins utilized were mounted in a rotating cylindrical jig and exposed to a high speed gas stream. Other test conditions were as specified in the respective Tables.
  • CMSX-11C alloy oxidation tests were performed concurrent to the hot corrosion tests. Table 11 below reports the results of a crucible oxidation test performed at 1742°F (950°C) for 1000 hour duration within a laboratory furnace. Mean and maximum oxidation depth plus weight gain measurements recorded at 100 and 500 hour intervals are reported, as well as at test completion.
  • Burner rig oxidation testing was undertaken at 2192°F (1200°C), with the results presented in Table 12 below. Various alloys were tested within the same rotating carousel. Specimen weight loss was measured at intervals of 100, 200, 300, 400 and 500 hours. Additional test conditions are provided in the Table. 1200°C (2192°F) OXIDATION (BURNER RIG.) Weight Loss In Grams As a Function of Time ALLOY 100 200 300 400 500 Hrs.
  • the burner rig oxidation test results illustrate that the CMSX-11C material provides extremely good 2192°F (1200°C) oxidation resistance in comparison to widely used industrial turbine blade and vane materials.
  • FIG. 7 An alloy strength and 2192°F (1200°C) oxidation comparrison is illustrated in Figure 7. This Figure illustrates that the CMSX-11C alloy blended capability is superior to directional solidified alloys such as René 80 H, FSX 414, IN 939 and IN 738 LC alloys.

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  • Materials Engineering (AREA)
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Claims (14)

  1. Superalliage à base de nickel résistant à La corrosion aux hautes températures comprenant les éléments suivant en pourcentages pondéraux : Chrome 14,2-15,5 Cobalt 2,0-4,0 Molybdène 0,30-0,45 Tungstène 4,0-5,0 Tantale 4,5-5,8 Niobium 0,05-0,25 Aluminium 3,2-3,6 Titane 4,0-4,4 Hafnium 0,01-0,06 Carbone 0-0,05 Bore 0-0,03 Zirconium 0-0,03 Rhénium 0-0,25 Silicium 0-0,10 Manganèse 0-0,10 Nickel + impuretés fortuites complément
    ledit superalliage ayant un indice de stabilité des phases NV3B inférieur à 2,45.
  2. Superalliage selon la revendication 1, dans lequel le rapport Ti:Al est supérieur à 1.
  3. Superalliage selon la revendication 1, dans lequel le rapport Ta:W est supérieur à 1.
  4. Superalliage selon la revendication 1, dans lequel ledit superalliage possède une résistance accrue à la corrosion.
  5. Utilisation du superalliage à base de nickel selon la revendication 1 pour la fabrication d'articles monocristallins.
  6. Utilisation selon la revendication 5, dans laquelle l'article est un composant destiné à un moteur à turbine.
  7. Utilisation selon la revendication 6, dans laquelle le composant est une aube de turbine à gaz ou une ailette de turbine à gaz.
  8. Utilisation selon la revendication 5, dans laquelle une coulée de monocristal ayant une résistance accrue à la corrosion est fabriquée à partir d'un superalliage à base de nickel selon la revendication 1, comprenant les éléments suivants en pourcentages pondéraux : Chrome 14,2-15,0 Cobalt 2,5-3,5 Molybdène 0,35-0,43 Tungstène 4,2-4,8 Tantale 4,8-5,4 Niobium 0,05-0,12 Aluminium 3,3-3,5 Titane 4,1-4,3 Hafnium 0,02-0,05 Carbone 0-0,05 Bore 0-0,03 Zirconium 0-0,03 Rhénium 0-0,25 Silicium 0-0,10 Manganèse 0-0,10 Nickel + impuretés fortuites complément
    ledit superalliage ayant un indice de stabilité des phases NV3B inférieur à 2,45.
  9. Utilisation selon la revendication 8, dans laquelle le rapport Ti:Al et le rapport Ta:W sont tous deux supérieurs à 1.
  10. Utilisation selon la revendication 8, dans laquelle ladite coulée possède une résistance accrue à l'oxydation.
  11. Utilisation selon la revendication 8, dans laquelle ladite coulée possède une résistance accrue à la rupture en fluage.
  12. Utilisation selon la revendication 8, dans laquelle le composant est une aube de turbine à gaz ou une ailette de turbine à gaz.
  13. Utilisation selon la revendication 8, dans laquelle ladite coulée est fabriquée à partir d'un superalliage à base de nickel selon la revendication 1, comprenant les éléments suivants en pourcentages pondéraux : Chrome 14,5 Cobalt 3,0 Molybdène 0,40 Tungstène 4,4 Tantale 4,95 Niobium 0,10 Aluminium 3,40 Titane 4,2 Hafnium 0,04 Carbone 0-0,05 Bore 0-0,03 Zirconium 0-0,03 Rhénium 0-0,25 Silicium 0-0,10 Manganèse 0-0,10 Nickel + impuretés fortuites complément
  14. Utilisation selon la revendication 13, dans laquelle le composant est une aube de turbine à gaz ou une ailette de turbine à gaz.
EP95116194A 1995-10-13 1995-10-13 Superalliages monocristallins à base de nickel résistant à la corrosion à haute température Expired - Lifetime EP1127948B1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
DE69527557T DE69527557T2 (de) 1995-10-13 1995-10-13 Einkristalline Superlegierungen mit guter Korrosionsbeständigkeit bei hohen Temperaturen
EP95116194A EP1127948B1 (fr) 1995-10-13 1995-10-13 Superalliages monocristallins à base de nickel résistant à la corrosion à haute température
DK95116194T DK1127948T3 (da) 1995-10-13 1995-10-13 Højtemperaturkorrosionsresistente monokrystallinske nikkelbaserede superlegeringer
AT95116194T ATE221138T1 (de) 1995-10-13 1995-10-13 Einkristalline superlegierungen mit guter korrosionsbeständigkeit bei hohen temperaturen
ES95116194T ES2184779T3 (es) 1995-10-13 1995-10-13 Superaleaciones monocristalinas a base de niquel resistente a la corroosion a temperatura elevada.

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Application Number Priority Date Filing Date Title
EP95116194A EP1127948B1 (fr) 1995-10-13 1995-10-13 Superalliages monocristallins à base de nickel résistant à la corrosion à haute température

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EP1127948A2 EP1127948A2 (fr) 2001-08-29
EP1127948A3 EP1127948A3 (fr) 2001-09-05
EP1127948B1 true EP1127948B1 (fr) 2002-07-24

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AT (1) ATE221138T1 (fr)
DE (1) DE69527557T2 (fr)
DK (1) DK1127948T3 (fr)
ES (1) ES2184779T3 (fr)

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CN115044805B (zh) * 2022-05-30 2023-04-11 北京科技大学 一种多性能平衡的镍基单晶高温合金及制备方法

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* Cited by examiner, † Cited by third party
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GB2153848B (en) * 1984-02-10 1987-09-16 United Technologies Corp High strength hot corrosion resistant single crystals
US4677035A (en) * 1984-12-06 1987-06-30 Avco Corp. High strength nickel base single crystal alloys
EP0207874B1 (fr) * 1985-05-09 1991-12-27 United Technologies Corporation Revêtements protecteurs pour superalliages, bien adaptés aux substrats
CA1291350C (fr) * 1986-04-03 1991-10-29 United Technologies Corporation Articles monocristallins a anisotropie reduite
US5366695A (en) * 1992-06-29 1994-11-22 Cannon-Muskegon Corporation Single crystal nickel-based superalloy

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DE69527557D1 (de) 2002-08-29
DE69527557T2 (de) 2002-11-07
ATE221138T1 (de) 2002-08-15
DK1127948T3 (da) 2002-11-11
ES2184779T3 (es) 2003-04-16
EP1127948A2 (fr) 2001-08-29
EP1127948A3 (fr) 2001-09-05

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