EP1188845A1 - Nickel based alloy for high temperature technology - Google Patents
Nickel based alloy for high temperature technology Download PDFInfo
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- EP1188845A1 EP1188845A1 EP01890180A EP01890180A EP1188845A1 EP 1188845 A1 EP1188845 A1 EP 1188845A1 EP 01890180 A EP01890180 A EP 01890180A EP 01890180 A EP01890180 A EP 01890180A EP 1188845 A1 EP1188845 A1 EP 1188845A1
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- nickel
- based alloy
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 36
- 239000000956 alloy Substances 0.000 title claims abstract description 36
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 25
- 238000005516 engineering process Methods 0.000 title claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052768 actinide Inorganic materials 0.000 claims abstract description 4
- 150000001255 actinides Chemical class 0.000 claims abstract description 4
- 229910052796 boron Inorganic materials 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 3
- 239000011574 phosphorus Substances 0.000 claims abstract description 3
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 3
- 239000011593 sulfur Substances 0.000 claims abstract description 3
- 230000007797 corrosion Effects 0.000 claims description 10
- 238000005260 corrosion Methods 0.000 claims description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- 239000011733 molybdenum Substances 0.000 claims description 6
- 230000000737 periodic effect Effects 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 239000011572 manganese Substances 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 238000011109 contamination Methods 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 239000011651 chromium Substances 0.000 abstract description 22
- 229910052804 chromium Inorganic materials 0.000 abstract description 12
- 239000012535 impurity Substances 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 abstract 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 abstract 1
- 239000000463 material Substances 0.000 description 14
- 239000013078 crystal Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 238000005728 strengthening Methods 0.000 description 5
- 150000004767 nitrides Chemical class 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000010955 niobium Substances 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- 229910019590 Cr-N Inorganic materials 0.000 description 2
- 229910019588 Cr—N Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052735 hafnium Inorganic materials 0.000 description 2
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000029142 excretion Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910001120 nichrome Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- -1 nitrogen form chromium nitrides Chemical class 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical group [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052566 spinel group Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
-
- 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
- C22C19/053—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 30% but less than 40%
Definitions
- the invention relates to a creep-resistant, corrosion-resistant nickel-based alloy for Applications in high temperature technology.
- a nickel-based alloy with the short name NiCr 7030 accordingly DIN material number 2.4658 is considered heat-resistant and is used for heating conductors, Furnace components and the like used. Although such a material depends on Silicon and aluminum content has good oxidation resistance, this shows however low strength and low creep properties as well as high Creep values at operating temperatures around 1000 ° C.
- DE-C-4411228 discloses a high-temperature nickel base alloy become.
- This highly heat-resistant, oxidation-resistant, massively embroidered, warm and cold-formable nickel-based alloy essentially consists of (in Mass%) 0.001 to 0.15 carbon, 0.10 to 3.0 nitrogen, 25.0 to 30.0 chromium, more than 0.3 to 1.2 nitrogen, 0.001 to 0.01 boron, 0.01 to 0.5 yttrium, cerium, Lanthanum, hafnium and tantalum, individually or in combination, the rest nickel with one Proportion of at least 64.0%. Due to the carbon content one can Mixed crystal strengthening can be achieved, the main effective elements However, the above alloy in terms of high temperature properties Chromium and nitrogen. Chromium and nitrogen form chromium nitrides, which are the Improve creep rupture strength, with nitrogen additionally Solid crystal strengthening provides. With the alloy according to DE-C-4411228 significantly improved creep rupture strength and heat resistance values appear reachable.
- the object of the present invention is to overcome this defect eliminate and an improved nickel base alloy for To create high temperature applications.
- the elements of groups 4, 5 and 6 are in the essential titanium (Ti), zirconium (Zr), hafnium (Hf), vanadium (V), niobium (Nb), tantalum (Ta), molybdenum (Mo) and tungsten (W) have a solid solution strengthening and have different activities related to non-metallic elements Carbon and nitrogen.
- Ti titanium
- Zr zirconium
- hafnium Hf
- V vanadium
- Nb tantalum
- Mo molybdenum
- W tungsten
- Ta and Nb form thermally highly stable Nitrides, on the other hand, is the nitrogen affinity of the strong carbide formers Mo and W low.
- a degree of solidification can be determined by the carbon content and the content of strong carbide formers can be adjusted. For example, if Low carbon content of the alloy, the strong carbide-forming elements increasingly installed in the crystal lattice of the mixed crystals and brace it.
- Another decisive advantage of the alloy according to the invention is that the elements mentioned above, in particular the elements Mo and W, shift the peritectic conversion of the II phase to higher temperatures by substitution of Cr atoms and thereby stabilize the II precipitates under conditions of use is effected.
- the addition of Mo does not result in volume changes even at high operating temperatures, which improves the high-temperature corrosion resistance because there is no initiation to flake off parts of the chrome spinel surface layer.
- Carbon with a content of more than 0.0015 wt .-% promotes the nitride and Carbonitride formation, but withdraws at a content of greater than 0.6 wt .-% Alloy too large amounts of carbide-forming elements, which one Counteracts matrix consolidation. Carbon contents of 0.16 are preferred up to 0.5% by weight.
- the ratio value nitrogen - to carbon content in the Alloy in the range of 0.5 to 5.5, preferably 1.0 to 4.0, optionally 1.0 up to 3.0, are particularly effective and stable Carbonitride precipitates formed and an efficient solid solution strengthening reached.
- Chromium contents in% by weight of 25 to 30 are preferred High temperature corrosion, it is important that the material at least 0.03 wt .-% Al and contains at least 0.4 wt .-% Si. Levels higher than 3.0% by weight of Al lead to disadvantageous excretion behavior, stress cracks and one Coarse grain formation and contents higher than 3.0% Si deteriorate the Hot formability of the alloy.
- the corrosion resistance at high temperatures can be increased if the material with elements of group 3 of the periodic table, that is Scandium (Sc), yttrium (Y) lanthanum (La) and lantanide up to a concentration of 0.15% by weight is alloyed.
- the contents are between 0.01 and 0.12% by weight. prefers.
- Nickel-based alloys with a composition according to the invention can with the help of pressure metallurgy, in which the liquid melt to solidification it is kept under high pressure (e.g. DESU process) or be produced by powder metallurgy.
- pressure metallurgy in which the liquid melt to solidification it is kept under high pressure (e.g. DESU process) or be produced by powder metallurgy.
- PM technology first a metal powder with the desired content of metallic elements prepared, then this powder via the gas phase at elevated temperature embroidered on and hot isostatically pressed.
- the cast or sintered block is usually deformed after one Homogenization of the material at 1250 ° C with forming at 1200 ° C. Grain sizes from 35 to 80 ⁇ m and nitride precipitates with a Diameters of 1 to 5 ⁇ m created in the material.
- the transition temperature of the II phase is determined by a Presence of elements of groups 4,5 and 6 (except Cr) increased.
- Tab. 1 are the determined dissolution and formation temperatures, the composition of the II phase and that of the - mixed crystal for a Mo-free Ni-Cr-N alloy and for those with a Mo content of 4 and 8% by weight and one with 4% by weight W specified.
- concentrations of 8% by weight Mo and 0.7% by weight N are for example, both temperature values for a ⁇ ⁇ ⁇ conversion above 1300 ° C.
- the II phase has a reduced chromium content of 45% by weight with a molybdenum concentration of 11% by weight. With a reduced nickel concentration, the ⁇ mixed crystal has increased chromium values of 29% by weight and a molybdenum content of 6.5% by weight. Influence of the molybdenum and tungsten content on the interval of the ⁇ + Cr 2 N transition temperature ⁇ T (dilatometer - examinations) Chemical composition [wt.
- Table 2 shows the chemical composition of the invention Alloys (alloys 1 to 5) and comparative alloys (alloys 6 to 9).
- Table 3 shows the mechanical properties of the alloys at 800 ° C. at 1000 ° C and at 1100 ° C.
- the resistance to high temperature corrosion was improved in the alloys according to the invention by approximately 16% (alloy 3 by more than 22%) compared to those in the prior art.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Turbine Rotor Nozzle Sealing (AREA)
- Soft Magnetic Materials (AREA)
- Chemically Coating (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
- Heat Treatment Of Steel (AREA)
- Contacts (AREA)
Abstract
Description
Die Erfindung betrifft eine kriechfeste korrosionsbeständige Nickelbasislegierung für Anwendungen in der Hochtemperaturtechnik.The invention relates to a creep-resistant, corrosion-resistant nickel-based alloy for Applications in high temperature technology.
An metallische Werkstoffe, insbesondere für Warmarbeitswerkzeuge, für Komponenten von Gasturbinen und Motoren, für Elemente im Ofenbau sowie in der chemischen Industrie, werden in zunehmendem Maße erhöhte mechanische und korrosionschemische Anforderungen bei Einsatztemperaturen von über 900°C gestellt. Der Korrosionsbeanspruchungen wegen, aber auch im Hinblick auf die Festigkeit und die Zeitstandseigenschaften des Werkstoffes eignen sich chromhältige Nickelbasislegierungen gut für einen Einsatz bei höchsten Temperaturen.On metallic materials, especially for hot work tools, for Components of gas turbines and engines, for elements in furnace construction and in the chemical industry, are increasing mechanical and increasing Corrosion-chemical requirements at operating temperatures of over 900 ° C posed. Because of the corrosion stresses, but also with regard to the Strength and the creep properties of the material are suitable Chromium-containing nickel-based alloys are good for use at the highest Temperatures.
Eine Nickelbasislegierung mit der Kurzbezeichnung NiCr 7030 entsprechend DIN-Werkstoffnummer 2.4658 gilt als hitzebeständig und wird für Heizleiter, Ofenbauteile und dergleichen eingesetzt. Obwohl ein derartiger Werkstoff je nach Silizium- und Aluminiumgehalt gute Oxidationsbeständigkeit besitzt, weist dieser jedoch geringe Festigkeit und niedrige Dauerstandseigenschaften sowie hohe Kriechwerte bei Einsatztemperaturen um 1000°C auf.A nickel-based alloy with the short name NiCr 7030 accordingly DIN material number 2.4658 is considered heat-resistant and is used for heating conductors, Furnace components and the like used. Although such a material depends on Silicon and aluminum content has good oxidation resistance, this shows however low strength and low creep properties as well as high Creep values at operating temperatures around 1000 ° C.
Aus der DE-C- 4411228 ist eine hochwarmfeste Nickelbasislegierung bekannt geworden. Diese hochwarmfeste, oxidationsbeständige, massiv aufgestickte, warm- und kaltverformbare Nickelbasislegierung besteht im wesentlichen aus ( in Masse-%) 0,001 bis 0,15 Kohlenstoff, 0,10 bis 3,0 Stickstoff, 25,0 bis 30,0 Chrom, mehr als 0,3 bis 1,2 Stickstoff, 0,001 bis 0,01 Bor, 0,01 bis 0,5 Yttrium, Cer, Lanthan, Hafnium und Tantal, einzeln oder in Kombination, Rest Nickel mit einem Anteil von mindestens 64,0 %. Durch den Kohlenstoffgehalt kann zwar eine Mischkristallverfestigung erreicht werden, die hauptsächlich wirksamen Elemente obiger Legierung im Hinblick auf die Hochtemperatureigenschaften sind jedoch Chrom und Stickstoff. Chrom und Stickstoff bilden Chromnitride, welche die Zeitstandsfestigkeit verbessern, wobei Stickstoff zusätzlich eine Mischkristallverfestigung erbringt. Mit der Legierung gemäß DE-C-4411228 erscheinen deutlich verbesserte Zeitstandsfestigkeits- und Warmfestigkeitswerte erreichbar.DE-C-4411228 discloses a high-temperature nickel base alloy become. This highly heat-resistant, oxidation-resistant, massively embroidered, warm and cold-formable nickel-based alloy essentially consists of (in Mass%) 0.001 to 0.15 carbon, 0.10 to 3.0 nitrogen, 25.0 to 30.0 chromium, more than 0.3 to 1.2 nitrogen, 0.001 to 0.01 boron, 0.01 to 0.5 yttrium, cerium, Lanthanum, hafnium and tantalum, individually or in combination, the rest nickel with one Proportion of at least 64.0%. Due to the carbon content one can Mixed crystal strengthening can be achieved, the main effective elements However, the above alloy in terms of high temperature properties Chromium and nitrogen. Chromium and nitrogen form chromium nitrides, which are the Improve creep rupture strength, with nitrogen additionally Solid crystal strengthening provides. With the alloy according to DE-C-4411228 significantly improved creep rupture strength and heat resistance values appear reachable.
Bei den bekannten Nickelbasiswerkstoffen, die in zunehmendem Maße höheren Beanspruchungen ausgesetzt werden, treten im Temperaturbereich zwischen 900°C und 1200°C ein sogenanntes Kriechen des Werkstoffes unter Belastung und eine Verschlechterung der Korrosionsbeständigkeit, insbesondere bei zyklischer Beanspruchung auf. Aufgabe der vorliegenden Erfindung ist es, diesen Mangel zu beseitigen und eine verbesserte Nickelbasislegierung für Hochtemperaturanwendungen zu schaffen.In the known nickel-based materials, the increasingly higher Exposed to stress occur in the temperature range between 900 ° C and 1200 ° C a so-called creep of the material under load and a Deterioration of corrosion resistance, especially with cyclical Stress on. The object of the present invention is to overcome this defect eliminate and an improved nickel base alloy for To create high temperature applications.
Diese Aufgabe löst eine kriechfeste korrosionsbeständige Nickelbasislegierung bestehend aus in Gew.-%
- 0,0015
- bis 0,60 Kohlenstoff (C)
- 0,20
- bis 0,90 Stickstoff (N)
- 22,0
- bis 32,0 Chrom (Cr)
- 5,0
- bis 20,0 Elemente der Gruppe 4,5 und 6 des Periodensystems ausgenommen Cr
- 0,03
- bis 3,0 Aluminium (Al)
- 0,4
- bis 3,0 Silizium (Si)
bis 0,15 Elemente der Gruppe 3 des Periodensystems ausgenommen Actinoide
bis 0,60 Mangan (Mn)
bis 14,8 Eisen (Fe)
bis 0,01 Bor (B)
max 0,014 Phosphor (P)
max 0,004 Schwefel (S)
min 51 Nickel (Ni) und/oder Cobalt (Co)
Die mit der Erfindung erreichten Vorteile sind im wesentlichen darin begründet, daß im Werkstoff bei Temperaturen bis 1200°C ein Korngrenzengleiten durch stabile Ausscheidungen in den Korngrenzenbereichen weitgehend verhindert und eine gesteigerte Mischkristallverfestigung erreicht werden. Weiters ist die Haftfestigkeit der Chrom-Spinelle oder dergleichen Schichten an der Oberfläche erhöht, wodurch eine verbesserte Hochtemperaturkorrosionsbeständigkeit der Teile gegeben ist.This problem is solved by a creep-resistant, corrosion-resistant nickel-based alloy consisting of
- 0.0015
- up to 0.60 carbon (C)
- 0.20
- up to 0.90 nitrogen (N)
- 22.0
- up to 32.0 chrome (Cr)
- 5.0
- up to 20.0 elements of groups 4.5 and 6 of the periodic table except Cr
- 0.03
- up to 3.0 aluminum (Al)
- 0.4
- up to 3.0 silicon (Si)
up to 0.15 elements of group 3 of the periodic table except actinoids
up to 0.60 manganese (Mn)
up to 14.8 iron (Fe)
up to 0.01 boron (B)
max 0.014 phosphorus (P)
max 0.004 sulfur (S)
min 51 nickel (Ni) and / or cobalt (Co)
The advantages achieved with the invention are essentially due to the fact that grain boundary sliding in the material at temperatures up to 1200 ° C. is largely prevented by stable precipitations in the grain boundary regions and an increased solid solution strengthening is achieved. Furthermore, the adhesive strength of the chromium spinels or similar layers on the surface is increased, which results in improved high-temperature corrosion resistance of the parts.
Nachfolgend sollen die Wirkung und Wechselwirkung der Elemente der erfindungsgemäßen Nickelbasislegierung näherbeschrieben werden.The effect and interaction of the elements of the nickel-based alloy according to the invention are described in more detail.
Die Elemente der Gruppe 4,5 und 6 ( ausgenommen Chrom), das sind im wesentlichen Titan (Ti), Zirkonium (Zr), Hafnium (Hf), Vanadin (V), Niob (Nb), Tantal (Ta), Molybdän (Mo) und Wolfram (W) wirken mischkristallverfestigend und besitzen unterschiedliche Aktivitäten bezüglich der nichtmetallischen Elemente Kohlenstoff und Stickstoff. Ta und Nb bilden beispielsweise thermisch hochstabile Nitride, hingegen ist die Stickstoffaffinität der starken Karbidbildner Mo und W gering. Es hat sich gezeigt, daß die Elemente der Gruppe 4,5 und 6 ( ausgenommen Cr) mit einer Konzentration im Werkstoff von mindestens 5, höchstens jedoch 20 Gew.-% teilweise festigkeitssteigernd im Atomgitter der Matrix eingelagert sind und teilweise Nitrid- und/oder Karbonitridausscheidungen bilden, welche die Korngrenzenfestigkeit erhöhen und somit eine Korngrenzengleiten bei Temperaturen über 1000°C erschweren. Weiters verhindern die Ausscheidungen ein Kornwachstum bei diesen Bedingungen wirkungsvoll.The elements of groups 4, 5 and 6 (except chrome) are in the essential titanium (Ti), zirconium (Zr), hafnium (Hf), vanadium (V), niobium (Nb), tantalum (Ta), molybdenum (Mo) and tungsten (W) have a solid solution strengthening and have different activities related to non-metallic elements Carbon and nitrogen. For example, Ta and Nb form thermally highly stable Nitrides, on the other hand, is the nitrogen affinity of the strong carbide formers Mo and W low. It has been shown that the elements of groups 4, 5 and 6 (except Cr) with a concentration in the material of at least 5, but not more than 20 % By weight are embedded in the atomic lattice of the matrix, increasing strength and partially form nitride and / or carbonitride precipitates which Grain boundary strength increase and thus a grain boundary sliding Temperatures above 1000 ° C make it difficult. Eliminations also prevent grain growth is effective in these conditions.
Ein Ausmaß der Mischkristallverfestigung kann dabei durch den Kohlenstoffgehalt und den Gehalt an starken Karbidbildnern eingestellt werden. Ist beispielsweise der Kohlenstoffanteil der Legierung gering, werden die stark karbidbildenden Elemente verstärkt im Kristallgitter der Mischkristalle eingebaut und verspannen dieses.A degree of solidification can be determined by the carbon content and the content of strong carbide formers can be adjusted. For example, if Low carbon content of the alloy, the strong carbide-forming elements increasingly installed in the crystal lattice of the mixed crystals and brace it.
Ein weiterer entscheidender Vorteil der erfindungsgemäßen Legierung besteht darin,
daß die oben angeführten Elemente, insbesondere die Elemente Mo und W, die
peritektische Umwandlung der II-Phase durch Substitution von Cr-Atomen zu
höheren Temperaturen verschieben und dadurch eine Stabilisierung der
II-Ausscheidungen unter Anwendungsbedingungen bewirkt wird. Eine mit steigender
Temperatur bei etwa 1000°C stattfindende Umwandlung
γ + π → γ + ε entsprechend γ + Cr13Ni7N4 → γ + Cr2N
in Ni-Cr-N- Legierungen,welche mit einer Volumsänderung von etwa 1 x 10-3 %
verbunden ist, wird beispielsweise, wie aus Tabelle 1 ersehen werden kann, durch
eine Mo-Konzentration von 4 Gew.-% auf eine Temperatur von über 1210°C
angehoben. Bei zyklischer Temperaturbeaufschlagung und Materialbeanspruchung
sind durch den Zusatz von zum Beispiel Mo Volumsänderungen auch bei hohen
Einsatztemperaturen nicht gegeben, was eine Verbesserung der
Hochtemperaturkorrosions- Beständigkeit bewirkt, weil keine Initiation zum
Abplatzen von Teilen der Chrom-Spinell-Oberflächenschicht vorliegt.Another decisive advantage of the alloy according to the invention is that the elements mentioned above, in particular the elements Mo and W, shift the peritectic conversion of the II phase to higher temperatures by substitution of Cr atoms and thereby stabilize the II precipitates under conditions of use is effected. A transformation taking place with increasing temperature at about 1000 ° C
γ + π → γ + ε corresponding to γ + Cr 13 Ni 7 N 4 → γ + Cr 2 N
in Ni-Cr-N alloys, which is associated with a change in volume of approximately 1 × 10 -3 %, for example, as can be seen from Table 1, by a Mo concentration of 4% by weight to a temperature of raised above 1210 ° C. With cyclic temperature exposure and material stress, the addition of Mo, for example, does not result in volume changes even at high operating temperatures, which improves the high-temperature corrosion resistance because there is no initiation to flake off parts of the chrome spinel surface layer.
Kohlenstoff mit einem Gehalt von größer als 0,0015 Gew.-% fördert die Nitrid- und Karbonitridbildung, entzieht jedoch bei einem Gehalt von größer als 0,6 Gew.-% der Legierung zu große Mengen an karbidbildenden Elementen, was einer Matrixverfestigung entgegenwirkt. Bevorzugt werden Kohlenstoffgehalte von 0,16 bis 0,5 Gew.-%.Carbon with a content of more than 0.0015 wt .-% promotes the nitride and Carbonitride formation, but withdraws at a content of greater than 0.6 wt .-% Alloy too large amounts of carbide-forming elements, which one Counteracts matrix consolidation. Carbon contents of 0.16 are preferred up to 0.5% by weight.
Wenn in günstiger Weise der Verhältniswert Stickstoff - zu Kohlenstoffgehalt in der Legierung im Bereich von 0,5 bis 5,5, vorzugsweise 1,0 bis 4,0, gegebenenfalls 1,0 bis 3,0, liegt, werden besonders wirkungsvolle und stabile Karbonitridausscheidungen gebildet und eine effiziente Mischkristallverfestigung erreicht.If the ratio value nitrogen - to carbon content in the Alloy in the range of 0.5 to 5.5, preferably 1.0 to 4.0, optionally 1.0 up to 3.0, are particularly effective and stable Carbonitride precipitates formed and an efficient solid solution strengthening reached.
Um eine möglichst stabile π- Phase bei hohen Verwendungstemperaturen des
Werkstoffes , aber auch gleichzeitig eine wirksame Mischkristallhärtung zu
erreichen, ist es von Vorteil, wenn die Nickelbasislegierung eine
Summenkonzentration von Molybdän und Wolfram in Gew.-% gemäß dem
Zusammenhang
Mo + W / 2 = 3,0 bis 10, vorzugsweise 4,0 bis 8,0 aufweist.In order to achieve the most stable π phase possible at high use temperatures of the material, but also to achieve effective mixed crystal hardening, it is advantageous if the nickel-based alloy has a total concentration of molybdenum and tungsten in% by weight according to the relationship
Mo + W / 2 = 3.0 to 10, preferably 4.0 to 8.0.
Bevorzugt werden Chromgehalte in Gew.-% von 25 bis 30. Zur Minimierung der Hochtemperaturkorrosion ist es wichtig, daß der Werkstoff mindestens 0,03 Gew.-% Al und mindestens 0,4 Gew.-% Si enthält. Höhere Gehalte als 3,0 Gew.-% Al führen zu einem nachteiligen Ausscheidungsverhalten, zu Spannungsrissen und zu einer Grobkornbildung und höhere Gehalte als 3,0 % Si verschlechtern die Warmverformbarkeit der Legierung.Chromium contents in% by weight of 25 to 30 are preferred High temperature corrosion, it is important that the material at least 0.03 wt .-% Al and contains at least 0.4 wt .-% Si. Levels higher than 3.0% by weight of Al lead to disadvantageous excretion behavior, stress cracks and one Coarse grain formation and contents higher than 3.0% Si deteriorate the Hot formability of the alloy.
Die Korrosionsbeständigkeit bei hohen Temperaturen kann gesteigert werden, wenn der Werkstoff mit Elementen der Gruppe 3 des Periodensystems, das sind Scandium (Sc), Yttrium ( Y) Lanthan ( La) und Lantanide bis zu einer Konzentration von 0,15 Gew.-% legiert ist. Dabei sind Gehalte zwischen 0,01 und 0,12 Gew.-% bevorzugt.The corrosion resistance at high temperatures can be increased if the material with elements of group 3 of the periodic table, that is Scandium (Sc), yttrium (Y) lanthanum (La) and lantanide up to a concentration of 0.15% by weight is alloyed. The contents are between 0.01 and 0.12% by weight. prefers.
Im folgenden soll die Erfindung weiter erläutert werden:The invention is to be explained further below:
Nickelbasislegierungen mit einer erfindungsgemäßen Zusammensetzung können mit Hilfe der Druckmetallurgie, bei welcher die flüssige Schmelze bis zur Erstarrung derselben unter hohem Druck gehalten wird, (z. B. DESU- Verfahren) oder pulvermetallurgisch hergestellt werden. Bei Anwendung einer PM- Technologie wird erst ein Metallpulver mit den gewünschten Gehalten an metallischen Elementen hergestellt, anschließend dieses Pulver über die Gasphase bei erhöhter Temperatur aufgestickt und heißisostatisch gepreßt.Nickel-based alloys with a composition according to the invention can with the help of pressure metallurgy, in which the liquid melt to solidification it is kept under high pressure (e.g. DESU process) or be produced by powder metallurgy. When using a PM technology first a metal powder with the desired content of metallic elements prepared, then this powder via the gas phase at elevated temperature embroidered on and hot isostatically pressed.
Eine Verformung des Guß- oder Sinterblockes erfolgt meist nach einer Homogenisierung des Materials bei 1250 °C bei einem Umformen bei 1200°C. Dabei werden Korngrößen von 35 bis 80µm und Nitridausscheidungen mit einem Durchmesser von 1 bis 5 µm im Werkstoff erstellt.The cast or sintered block is usually deformed after one Homogenization of the material at 1250 ° C with forming at 1200 ° C. Grain sizes from 35 to 80µm and nitride precipitates with a Diameters of 1 to 5 µm created in the material.
Wie früher erwähnt, wird die Umwandlungstemperatur der II-Phase durch eine Anwesenheit von Elementen der Gruppe 4,5 und 6 ( außer Cr) erhöht. In Tab. 1 sind die ermittelten Auflösungs- und Bildungstemperaturen, die Zusammensetzung der II-Phase und jene des - Mischkristalles für eine Mo-freie Ni-Cr-N- Legierung und für solche mit einem Mo- Gehalt von 4 und 8 Gew,-% sowie eine mit 4 Gew.-% W angegeben. Bei Konzentrationen von 8 Gew.-% Mo und 0,7 Gew.-% N liegen beispielsweise beide Temperaturwerte für eine π ↔ ε - Umwandlung über 1300°C.As mentioned earlier, the transition temperature of the II phase is determined by a Presence of elements of groups 4,5 and 6 (except Cr) increased. In Tab. 1 are the determined dissolution and formation temperatures, the composition of the II phase and that of the - mixed crystal for a Mo-free Ni-Cr-N alloy and for those with a Mo content of 4 and 8% by weight and one with 4% by weight W specified. At concentrations of 8% by weight Mo and 0.7% by weight N are for example, both temperature values for a π ↔ ε conversion above 1300 ° C.
Die II- Phase weist dabei einen erniedrigten Chromgehalt von 45 Gew.-% bei einer
Molybdänkonzentration von 11 Gew.-% auf. Der γ- Mischkristall besitzt bei einer
verminderten Nickelkonzentration erhöhte Chromwerte von 29 Gew.-% und einen
Molybdängehalt von 6,5 Gew.-% .
4W 0,7N
4Mo 0,7N
8Mo 0,7N
4W 0.7N
4Mo 0.7N
8Mo 0.7N
Die Tabelle 2 zeigt die chemische Zusammensetzung von erfindungsgemäßen Legierungen ( Leg. 1 bis 5) und Vergleichslegierungen ( Leg. 6 bis 9).Table 2 shows the chemical composition of the invention Alloys (alloys 1 to 5) and comparative alloys (alloys 6 to 9).
In Tabelle 3 sind die mechanischen Eigenschaften der Legierungen bei 800°C. bei 1000° C und bei 1100°C angeführt.Table 3 shows the mechanical properties of the alloys at 800 ° C. at 1000 ° C and at 1100 ° C.
Im Vergleich ist festzustellen, daß durch die erfindungsgemäßen legierungstechnischen Maßnahmen die 0,2% Dehngrenzen ( Rp0,2) des Werkstoffes wesentlich erhöht sind und die Bruchdehnung (A) jeweils geringere Werte aufweist. Gegenüber dem Stand der Technik ist insbesondere die Kriechfestigkeit bei 1% Dehnung der Nickelbasislegierungen nach der Erfindung wesentlich verbessert.In comparison it should be noted that the inventive alloying measures the 0.2% proof stress (Rp0.2) of Material are significantly increased and the elongation at break (A) lower Has values. Compared to the prior art, in particular Creep resistance at 1% elongation of the nickel-based alloys according to the invention significantly improved.
Die Beständigkeit gegen Hochtemperaturkorrosion war bei den erfindungsgemäßen Legierungen um etwa 16% (Legierung 3 um mehr als 22%) gegenüber jenen des Standes der Technik verbessert. The resistance to high temperature corrosion was improved in the alloys according to the invention by approximately 16% (alloy 3 by more than 22%) compared to those in the prior art.
Claims (7)
- 0,0015
- bis 0,60 Kohlenstoff (C)
- 0,20
- bis 0,90 Stickstoff (N)
- 22,0
- bis 32,0 Chrom (Cr)
- 5,0
- bis 20,0 Elemente der Gruppe 4,5 und 6 des Periodensystems, ausgenommen Cr
- 0,03
- bis 3,0 Aluminium (Al)
- 0,4
- bis 3,0 Silizium (Si)
bis 0,15 Elemente der Gruppe 3 des Periodensystems, ausgenommen Actinoide
bis 0,60 Mangan (Mn)
bis 14,8 Eisen (Fe)
bis 0,01 Bor (B)
max 0,014 Phosphor (P)
max 0,004 Schwefel (S)
min 51 Nickel (Ni) und/oder Cobalt (Co)
- 0.0015
- up to 0.60 carbon (C)
- 0.20
- up to 0.90 nitrogen (N)
- 22.0
- up to 32.0 chrome (Cr)
- 5.0
- up to 20.0 elements of groups 4.5 and 6 of the periodic table, except Cr
- 0.03
- up to 3.0 aluminum (Al)
- 0.4
- up to 3.0 silicon (Si)
up to 0.15 elements of group 3 of the periodic table, excluding actinoids
up to 0.60 manganese (Mn)
up to 14.8 iron (Fe)
up to 0.01 boron (B)
max 0.014 phosphorus (P)
max 0.004 sulfur (S)
min 51 nickel (Ni) and / or cobalt (Co)
N / C = 0,5 bis 5,5, vorzugsweise 1,0 bis 4,0, gegebenenfalls 1 bis 3Nickel-based alloy according to claim 1 or 2 with the proviso that the ratio of nitrogen to carbon is 0.5 to 5.5, preferably 1 to 4, optionally 1 to 3
N / C = 0.5 to 5.5, preferably 1.0 to 4.0, optionally 1 to 3
Mo + W / 2 = 3,0 bis 10,0, vorzugsweise 4,0 bis 8,0Nickel-based alloy according to one of claims 1 to 3, containing a total concentration of molybdenum and tungsten in wt .-% according to the relationship:
Mo + W / 2 = 3.0 to 10.0, preferably 4.0 to 8.0
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT01890180T ATE301730T1 (en) | 2000-09-14 | 2001-06-08 | NICKEL-BASED ALLOY FOR HIGH TEMPERATURE TECHNOLOGY |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT0156200A AT408665B (en) | 2000-09-14 | 2000-09-14 | NICKEL BASE ALLOY FOR HIGH TEMPERATURE TECHNOLOGY |
AT15622000 | 2000-09-14 |
Publications (2)
Publication Number | Publication Date |
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EP1188845A1 true EP1188845A1 (en) | 2002-03-20 |
EP1188845B1 EP1188845B1 (en) | 2005-08-10 |
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EP01890180A Expired - Lifetime EP1188845B1 (en) | 2000-09-14 | 2001-06-08 | Nickel based alloy for high temperature technology |
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US (1) | US6797232B2 (en) |
EP (1) | EP1188845B1 (en) |
AT (2) | AT408665B (en) |
CA (1) | CA2355446C (en) |
DE (1) | DE50107021D1 (en) |
Cited By (3)
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WO2019020145A1 (en) * | 2017-07-28 | 2019-01-31 | Vdm Metals International Gmbh | High-temperature nickel-base alloy |
CN113555068A (en) * | 2021-07-13 | 2021-10-26 | 北京航空航天大学 | Method for calculating concentration of alloying elements in near layer of nickel-based single crystal superalloy double-phase interface |
DE102022211589A1 (en) | 2022-11-02 | 2024-05-02 | Siemens Energy Global GmbH & Co. KG | Cobalt-based alloy, powder, processes and components |
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US7211346B2 (en) * | 2002-04-03 | 2007-05-01 | Ut-Battelle, Llc | Corrosion resistant metallic bipolar plate |
US7829194B2 (en) * | 2003-03-31 | 2010-11-09 | Ut-Battelle, Llc | Iron-based alloy and nitridation treatment for PEM fuel cell bipolar plates |
US20060110626A1 (en) * | 2004-11-24 | 2006-05-25 | Heraeus, Inc. | Carbon containing sputter target alloy compositions |
EP1777312B1 (en) * | 2005-10-24 | 2008-09-10 | Siemens Aktiengesellschaft | Welding material, use of the welding material and process of welding |
ES2403027T3 (en) * | 2006-08-08 | 2013-05-13 | Huntington Alloys Corporation | Welding alloy and articles for use in welding, welded assemblies and procedure for producing welded assemblies |
US8858874B2 (en) * | 2007-11-23 | 2014-10-14 | Rolls-Royce Plc | Ternary nickel eutectic alloy |
JP2013181190A (en) * | 2012-02-29 | 2013-09-12 | Seiko Instruments Inc | Co-BASED ALLOY FOR LIVING BODY AND STENT |
US9540714B2 (en) | 2013-03-15 | 2017-01-10 | Ut-Battelle, Llc | High strength alloys for high temperature service in liquid-salt cooled energy systems |
US9377245B2 (en) | 2013-03-15 | 2016-06-28 | Ut-Battelle, Llc | Heat exchanger life extension via in-situ reconditioning |
US10017842B2 (en) | 2013-08-05 | 2018-07-10 | Ut-Battelle, Llc | Creep-resistant, cobalt-containing alloys for high temperature, liquid-salt heat exchanger systems |
US9435011B2 (en) | 2013-08-08 | 2016-09-06 | Ut-Battelle, Llc | Creep-resistant, cobalt-free alloys for high temperature, liquid-salt heat exchanger systems |
US9683280B2 (en) | 2014-01-10 | 2017-06-20 | Ut-Battelle, Llc | Intermediate strength alloys for high temperature service in liquid-salt cooled energy systems |
US9683279B2 (en) | 2014-05-15 | 2017-06-20 | Ut-Battelle, Llc | Intermediate strength alloys for high temperature service in liquid-salt cooled energy systems |
US9605565B2 (en) | 2014-06-18 | 2017-03-28 | Ut-Battelle, Llc | Low-cost Fe—Ni—Cr alloys for high temperature valve applications |
CN105238958A (en) * | 2015-10-28 | 2016-01-13 | 无棣向上机械设计服务有限公司 | Nickel-base superalloy |
EP3269472B1 (en) * | 2016-07-13 | 2022-09-07 | Ansaldo Energia IP UK Limited | Method for manufacturing mechanical components |
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-
2001
- 2001-06-08 EP EP01890180A patent/EP1188845B1/en not_active Expired - Lifetime
- 2001-06-08 AT AT01890180T patent/ATE301730T1/en active
- 2001-06-08 DE DE50107021T patent/DE50107021D1/en not_active Expired - Lifetime
- 2001-06-14 US US09/880,068 patent/US6797232B2/en not_active Expired - Fee Related
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Cited By (4)
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WO2019020145A1 (en) * | 2017-07-28 | 2019-01-31 | Vdm Metals International Gmbh | High-temperature nickel-base alloy |
US11193186B2 (en) | 2017-07-28 | 2021-12-07 | Vdm Metals International Gmbh | High-temperature nickel-base alloy |
CN113555068A (en) * | 2021-07-13 | 2021-10-26 | 北京航空航天大学 | Method for calculating concentration of alloying elements in near layer of nickel-based single crystal superalloy double-phase interface |
DE102022211589A1 (en) | 2022-11-02 | 2024-05-02 | Siemens Energy Global GmbH & Co. KG | Cobalt-based alloy, powder, processes and components |
Also Published As
Publication number | Publication date |
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US20020057984A1 (en) | 2002-05-16 |
ATA15622000A (en) | 2001-06-15 |
AT408665B (en) | 2002-02-25 |
CA2355446C (en) | 2011-11-22 |
EP1188845B1 (en) | 2005-08-10 |
DE50107021D1 (en) | 2005-09-15 |
US6797232B2 (en) | 2004-09-28 |
ATE301730T1 (en) | 2005-08-15 |
CA2355446A1 (en) | 2002-03-14 |
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