EP1223229A1 - Nickel based alloy for casting single crystal components - Google Patents
Nickel based alloy for casting single crystal components Download PDFInfo
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- EP1223229A1 EP1223229A1 EP01129921A EP01129921A EP1223229A1 EP 1223229 A1 EP1223229 A1 EP 1223229A1 EP 01129921 A EP01129921 A EP 01129921A EP 01129921 A EP01129921 A EP 01129921A EP 1223229 A1 EP1223229 A1 EP 1223229A1
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- European Patent Office
- Prior art keywords
- weight
- percent
- rhenium
- tungsten
- based alloy
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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
- C22C19/057—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%
Definitions
- the invention relates to a nickel-based alloy for casting production monocrystalline solidified components, according to the preamble of claim 1.
- Alloys of this type belong to a group of so-called super alloys, which can be used under high temperatures and under high mechanical stresses are and therefore used in particular as turbine blade materials in gas turbines become.
- Second and third generation Ni-base alloys for single-crystalline components contain approximately 3% and 6% by weight of the refractory element rhenium and have better creep properties than corresponding alloys of the first generation with no Re content.
- the refractory element Re affects the properties of superalloys in different ways. Re has a large atomic radius, diffuses very slowly due to this and seeps into the matrix. In addition to the effect of solid solution hardening of the matrix, the rhenium atoms tend to form clusters that hinder dislocation movement. Tungsten contributes significantly to solidification. The W content influences the distribution of Re on the matrix and the ⁇ '-excretion phase.
- the alloying element tantalum (Ta) contributes to solid solution strengthening and improves the cyclic oxidation behavior, but is mainly used in W- and Re-containing Ni-based alloys added to the so-called solidification in the direction of solidification Counteract Freckle formation.
- Negative properties of Ta sharp increase in density; it promotes the unwanted TCP phase formation and increases the ⁇ '-solution annealing temperature.
- the increase in creep resistance is accompanied by a simultaneous increase in density up to 9 g cm -3 for certain alloys with 6% by weight of Re. With Re-free alloys, the density can be reduced to 8 g cm -3 .
- Ni-based alloys with a high specific weight are only suitable to a limited extent for use in modern, fast-rotating aircraft turbines.
- CMSX-6 Re-free, low density superalloy
- this alloy Apart from the mechanical advantage of a relatively low density of 7.98 g cm -3 , this alloy also has disadvantages, such as a small heat treatment window and a strong tendency to recrystallize.
- the object of the invention is nickel-based alloys for the cast-technical manufacture of solidified components specify that by optimizing the proportions of rhenium and tungsten particularly Favorable material and thus component properties, such as low density, high mechanical strength including low tendency to creep and high Temperature resistance.
- component properties such as low density, high mechanical strength including low tendency to creep and high Temperature resistance.
- it is easy to cast and inexpensive Required heat treatment properties of the alloy.
- the rhenium content should be at least 2.3 percent by weight.
- the weight ratio of tungsten to rhenium should be at least 1.1 and at most 1.6 his.
- the respective alloy always contains more tungsten than rhenium and this in a defined ratio range.
- This material which internally as “L judges in E k ristall 94" is designated (LEK94), thus has the following composition in percent by weight: al from 6.2 to 6.8 Co from 7.2 to 7.8 Cr from 5.8 to 6.4 Hf from 0.05 to 0.15 Mo from 1.7 to 2.3 re from 2.3 to 2.6 Ta from 2.0 to 2.6 Ti from 0.9 to 1.1 W from 3.0 to 3.7 Ni Rest that means from 66.55 to 70.85
- any impurities in the form of other elements or compounds are here not taken into account and individual numerical values, e.g. the Ni content, yet change slightly.
- the proportions of the above elements can e.g. two decimal places (hundredths of a percent) have deviations that are self-evident for the specialist and have no relevant influence on the Have material properties.
- This special material "LEK94” is a high-alloy single crystal alloy Density developed for use in high-speed turbines. For optimization the detrimental requirements of high heat resistance and low density the alloy contents of elements Re and W were varied.
- LEK94 is a Re-containing single crystal alloy of low density in the range from 8.1 to 8.3 g cm -3 and high heat resistance. This material is characterized by good castability and a significantly large heat treatment window.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Turbine Rotor Nozzle Sealing (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
Die Erfindung betrifft eine Nickel-Basislegierung für die gießtechnische Herstellung einkristallin erstarrter Bauteile, gemäß dem Oberbegriff des Patentanspruches 1.The invention relates to a nickel-based alloy for casting production monocrystalline solidified components, according to the preamble of claim 1.
Legierungen dieser Art gehören zu einer Gruppe von sogenannten Superlegierungen, die unter hohen Temperaturen und unter hohen mechanischen Spannungen einsetzbar sind und daher insbesondere als Turbinenschaufelwerkstoffe in Gasturbinen verwendet werden.Alloys of this type belong to a group of so-called super alloys, which can be used under high temperatures and under high mechanical stresses are and therefore used in particular as turbine blade materials in gas turbines become.
Die zukünftige Generation der Luftfahrttriebwerke mit hohem Nebenstromverhältnis
und schnelldrehender Niederdruckturbine verspricht signifikante Verbesserungen
hinsichtlich spezifischen Kraftstoffverbrauchs und Emissionen. Das Gewicht des
Triebwerks, seine Größe und die Unterhaltskosten fallen ebenso unter die heutigen
Werttreiber.
Triebwerke mit hohem Nebenstromverhältnis sind mit einem Untersetzungsgetriebe
ausgerüstet, das zwischen den Fan auf der einen Seite und den Niederdruckverdichter
und die Niederdruckturbine auf der anderen Seite geschaltet ist. Das Getriebe
ermöglicht den Betrieb des Fans im optimalen Bereich bei langsamen Drehzahlen
und bietet das Potenzial, den Verdichter und die Turbine bei höheren Drehzahlen und
damit höheren Druckverhältnissen zu betreiben, als dies bei konventionellen Turbinen
der Fall ist. Durch die höheren Umfangsgeschwindigkeiten steigen jedoch auch
die mechanischen Lasten der Beschaufelung und der Scheiben der Niederdruckturbine.The future generation of aviation engines with a high bypass ratio and high-speed low-pressure turbine promises significant improvements in terms of specific fuel consumption and emissions. The weight of the engine, its size and the maintenance costs also fall under today's value drivers.
Engines with a high bypass ratio are equipped with a reduction gear, which is connected between the fan on one side and the low-pressure compressor and the low-pressure turbine on the other side. The gearbox enables the fan to operate in the optimum range at slow speeds and offers the potential to operate the compressor and the turbine at higher speeds and thus higher pressure ratios than is the case with conventional turbines. However, the higher peripheral speeds also increase the mechanical loads on the blading and the discs of the low-pressure turbine.
Ni-Basislegierungen der 2. und 3. Generation für einkristalline Bauteile enthalten
etwa 3 Gew.-% bzw. 6 Gew.-% des Refraktärelementes Rhenium und besitzen bessere
Kriecheigenschaften als entsprechende Legierungen der ersten Generation ohne Re-Gehalt.
Das Refraktärelement Re wirkt sich in unterschiedlicher Weise auf die Eigenschaften
von Superlegierungen aus. Re besitzt einen großen Atomradius, diffundiert
aufgrund dessen sehr langsam und seigert in die Matrix. Zusätzlich zum Effekt der
Mischkristallhärtung der Matrix, neigen die Rhenium-Atome zur Bildung von Clustern,
die eine Versetzungsbewegung behindern.
Wolfram trägt erheblich zur Mischkristallverfestigung bei. Der W-Gehalt beeinflusst
die Verteilung des Re auf die Matrix und die γ'-Ausscheidungsphase.Second and third generation Ni-base alloys for single-crystalline components contain approximately 3% and 6% by weight of the refractory element rhenium and have better creep properties than corresponding alloys of the first generation with no Re content. The refractory element Re affects the properties of superalloys in different ways. Re has a large atomic radius, diffuses very slowly due to this and seeps into the matrix. In addition to the effect of solid solution hardening of the matrix, the rhenium atoms tend to form clusters that hinder dislocation movement.
Tungsten contributes significantly to solidification. The W content influences the distribution of Re on the matrix and the γ'-excretion phase.
Der hohe Schmelzpunkt und der geringe Diffusionskoeffizient sowohl von Re als auch von W führen zu einem Ansteigen der Solidustemperatur der Superlegierungen. Darüber hinaus wird die Morphologieänderung der Ausscheidungsphase γ' unter Last verzögert.The high melting point and low diffusion coefficient of both Re and also of W lead to an increase in the solidus temperature of the superalloys. In addition, the morphology change of the elimination phase γ 'under load delayed.
Das Legierungselement Tantal (Ta) trägt zwar zur Mischkristallverfestigung bei und verbessert das zyklische Oxidationsverhalten, wird aber in erster Linie in W- und Re-haltige Ni-Basislegierungen zugegeben, um bei gerichteter Erstarrung der sogenannten Freckle-Bildung entgegenzuwirken.The alloying element tantalum (Ta) contributes to solid solution strengthening and improves the cyclic oxidation behavior, but is mainly used in W- and Re-containing Ni-based alloys added to the so-called solidification in the direction of solidification Counteract Freckle formation.
Negative Eigenschaften von Ta: starke Erhöhung der Dichte; es fördert die unerwünschte TCP-Phasenbildung und erhöht die γ'-Lösungsglühtemperatur.Negative properties of Ta: sharp increase in density; it promotes the unwanted TCP phase formation and increases the γ'-solution annealing temperature.
Der Anstieg der Kriechfestigkeit geht einher mit einer gleichzeitigen Steigerung der Dichte bis auf 9 g cm-3 für gewisse Legierungen mit 6 Gew.-% Re. Bei Re-freien Legierungen kann die Dichte bis auf 8 g cm-3 abgesenkt werden. Ni-Basislegierungen mit einem hohen spezifischen Gewicht sind jedoch nur bedingt geeignet für den Einsatz in modernen, schnelldrehenden Flugturbinen.The increase in creep resistance is accompanied by a simultaneous increase in density up to 9 g cm -3 for certain alloys with 6% by weight of Re. With Re-free alloys, the density can be reduced to 8 g cm -3 . However, Ni-based alloys with a high specific weight are only suitable to a limited extent for use in modern, fast-rotating aircraft turbines.
Eine Re-freie Superlegierung mit niedriger Dichte ist beispielsweise aus der US-Patentschrift 4,721,540 bekannt, die Handelsbezeichnung dieses Werkstoffes ist "CMSX-6". Abgesehen von dem mechanischen Vorteil einer relativ niedrigen Dichte von 7,98 g cm-3 weist diese Legierung aber auch Nachteile auf, wie ein kleines Wärmebehandlungsfenster und starke Rekristallisationsneigung.A Re-free, low density superalloy is known, for example, from US Pat. No. 4,721,540, the trade name of this material is "CMSX-6". Apart from the mechanical advantage of a relatively low density of 7.98 g cm -3 , this alloy also has disadvantages, such as a small heat treatment window and a strong tendency to recrystallize.
Aus der internationalen Offenlegungsschrift WO 93/24683 sind einkristalline Gussteile bekannt, deren Legierung 0 bis 8 Gewichtsprozent Rhenium, 3 bis 10 Gewichtsprozent Wolfram (tungsten) sowie u.a. Magnesium oder Kalzium zur Erhöhung der Oxidationsbeständigkeit enthält. Bei einer speziellen Legierungszusammensetzung soll der Re-Anteil bei 2,8 bis 3,2 Gewichtsprozent, der W-Anteil bei 5,6 bis 6,2 Gewichtsprozent liegen. Da Rhenium und Wolfram schwere Metalle sind, ist hier mit einer relativ hohen Bauteildichte zu rechnen, insbesondere dann, wenn die oberen Grenzwerte von 8 Gewichtsprozent Rhenium und 10 Gewichtsprozent Wolfram benutzt werden. Rhenium ist außerdem ein sehr teueres Element, das sich spürbar auf den Bauteilpreis auswirkt. Die untere Grenze für Re ist hier mit 0 Gewichtsprozent angegeben. Kleine Re-Anteile reduzieren zwar Gewicht und Preis, führen aber auch zu einer deutlichen Verschlechterung wichtiger Werkstoffeigenschaften.The international published patent application WO 93/24683 describes single-crystalline ones Castings are known whose alloy is 0 to 8 percent by weight rhenium, 3 to 10 percent by weight Tungsten (tungsten) and others Magnesium or calcium to increase which contains resistance to oxidation. With a special alloy composition the proportion of Re should be 2.8 to 3.2 percent by weight, the proportion of W 5.6 to 6.2 Percent by weight. Since rhenium and tungsten are heavy metals, here is with a relatively high component density, especially if the upper ones Limit values of 8 percent by weight rhenium and 10 percent by weight tungsten are used become. Rhenium is also a very expensive item that can be felt on affects the component price. The lower limit for Re here is 0 percent by weight specified. Small re-shares reduce weight and price, but also lead to a significant deterioration in important material properties.
Angesichts dieser Nachteile besteht die Aufgabe der Erfindung darin, Nickel-Basislegierungen für die gießtechnische Herstellung einkristallin erstarrter Bauteile anzugeben, die durch Optimierung der Anteile an Rhenium und Wolfram besonders günstige Werkstoff- und somit Bauteileigenschaften ermöglichen, wie niedrige Dichte, hohe mechanische Festigkeit einschließlich geringer Kriechneigung sowie hohe Temperaturbeständigkeit. Darüber hinaus ist eine leichte Vergießbarkeit und günstige Wärmebehandlungseigenschaften der Legierung gefordert.In view of these disadvantages, the object of the invention is nickel-based alloys for the cast-technical manufacture of solidified components specify that by optimizing the proportions of rhenium and tungsten particularly Favorable material and thus component properties, such as low density, high mechanical strength including low tendency to creep and high Temperature resistance. In addition, it is easy to cast and inexpensive Required heat treatment properties of the alloy.
Diese Aufgabe wird durch die in Anspruch 1 gekennzeichneten Merkmale gelöst, in Verbindung mit den gattungsbildenden Merkmalen in dessen Oberbegriff.This object is achieved by the features characterized in claim 1, in Connection with the generic features in its generic term.
Erfindungsgemäß soll der Rheniumanteil mindestens 2,3 Gewichtsprozent betragen, das Gewichtsverhältnis Wolfram zu Rhenium soll mindestens 1,1 und höchstens 1,6 sein. Somit enthält die jeweilige Legierung stets mehr Wolfram als Rhenium und dies in einem definierten Verhältnisbereich.According to the invention, the rhenium content should be at least 2.3 percent by weight. the weight ratio of tungsten to rhenium should be at least 1.1 and at most 1.6 his. Thus, the respective alloy always contains more tungsten than rhenium and this in a defined ratio range.
Im Unteranspruch 2 wird zusätzlich eine Obergrenze für den Rheniumanteil angegeben im Hinblick auf Gewichts- und Kostenbegrenzung bei sehr guten Werkstoffeigenschaften. Der Gewichtsverhältnisbereich W zu Re aus Anspruch 1 wird beibehalten. An additional limit for the rhenium content is additionally specified in sub-claim 2 with regard to weight and cost limitation with very good material properties. The weight ratio range W to Re from claim 1 is maintained.
In Unteranspruch 3 ist eine konkrete Legierung mit allen relevanten Elementen und deren Anteilsbereichen gekennzeichnet. Das Verhältnis W zu Re ist hier in Relation zu den vorgenannten Ansprüchen 1 und 2 eingeschränkt, d.h. noch enger begrenzt.In claim 3 is a concrete alloy with all relevant elements and whose share areas are marked. The ratio W to Re is in relation here limited to the aforementioned claims 1 and 2, i.e. limited even more.
Dieser Werkstoff, der intern auch als "Leichter Einkristall 94"(LEK94) bezeichnet
wird, hat somit folgende Zusammensetzung in Gewichtsprozent:
Etwaige Verunreinigungen in Form weiterer Elemente bzw. Verbindungen sind hier nicht berücksichtigt und können einzelne Zahlenwerte, wie z.B. den Ni-Anteil, noch geringfügig verändern. Ebenso können die Anteile der obengenannten Elemente z.B. zwei Stellen hinter dem Komma (hundertstel Prozent) Abweichungen aufweisen, die für den Fachmann selbstverständlich sind und keinen relevanten Einfluss auf die Werkstoffeigenschaften haben.Any impurities in the form of other elements or compounds are here not taken into account and individual numerical values, e.g. the Ni content, yet change slightly. Likewise, the proportions of the above elements can e.g. two decimal places (hundredths of a percent) have deviations that are self-evident for the specialist and have no relevant influence on the Have material properties.
Dieser spezielle Werkstoff "LEK94" ist eine hochlegierte Einkristalllegierung geringer Dichte, die für den Einsatz in schnelldrehenden Turbinen entwickelt wurde. Zur Optimierung der detrimentalen Anforderungen Hochwarmfestigkeit und geringe Dichte wurden die Legierungsgehalte der Elemente Re und W variiert.This special material "LEK94" is a high-alloy single crystal alloy Density developed for use in high-speed turbines. For optimization the detrimental requirements of high heat resistance and low density the alloy contents of elements Re and W were varied.
Die Entwicklung des "LEK94" erfolgte mit folgenden Zielsetzungen (Ausgangspunkt
CMSX-6 gemäß US-Patent 4,721,540)
"LEK94" ist eine Re-haltige Einkristalllegierung geringer Dichte im Bereich von 8,1 bis 8,3 g cm-3 und hoher Warmfestigkeit. Gute Vergießbarkeit und ein signifikant großes Wärmebehandlungsfenster zeichnen diesen Werkstoff aus."LEK94" is a Re-containing single crystal alloy of low density in the range from 8.1 to 8.3 g cm -3 and high heat resistance. This material is characterized by good castability and a significantly large heat treatment window.
Claims (3)
einen Anteil an Rhenium (Re) von mindestens 2,3 Gewichtsprozent sowie ein Gewichtsverhältnis des Anteils an Wolfram (W) zu dem Anteil an Rhenium (Re) von mindestens 1,1 bis höchstens 1,6.Nickel-based alloy for the casting-producing monocrystalline solidified components, in particular blades for high-speed turbine stages in gas turbines, which contains the elements rhenium (Re), and tungsten (W) and other elements such as aluminum, chromium and cobalt, characterized by
a proportion of rhenium (Re) of at least 2.3 percent by weight and a weight ratio of the proportion of tungsten (W) to the proportion of rhenium (Re) of at least 1.1 to at most 1.6.
Aluminium (Al) von mindestens 6,2 bis höchstens 6,8 Gewichtsprozent; Kobalt (Co) von mindestens 7,2 bis höchstens 7,8 Gewichtsprozent; Chrom (Cr) von mindestens 5,8 bis höchstens 6,4 Gewichtsprozent; Hafnium (Hf) von mindestens 0,05 bis höchstens 0,15 Gewichtsprozent; Molybdän (Mo) von mindestens 1,7 bis höchstens 2,3 Gewichtsprozent; Tantal (Ta) von mindestens 2,0 bis höchstens 2,6 Gewichtsprozent; Titan (Ti) von mindestens 0,9 bis höchstens 1,1 Gewichtsprozent.Nickel-based alloy according to claim 2, characterized by a proportion of tungsten (W) of at least 3.0 to at most 3.7 percent by weight and the following proportions of further alloy elements in addition to nickel, rhenium and tungsten:
Aluminum (Al) from at least 6.2 to at most 6.8 percent by weight; Cobalt (Co) of at least 7.2 to at most 7.8 percent by weight; Chromium (Cr) from at least 5.8 to at most 6.4 percent by weight; Hafnium (Hf) from at least 0.05 to at most 0.15 percent by weight; Molybdenum (Mo) from at least 1.7 to at most 2.3 percent by weight; Tantalum (Ta) from at least 2.0 to at most 2.6 percent by weight; Titanium (Ti) from at least 0.9 to at most 1.1 percent by weight.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10100790 | 2001-01-10 | ||
DE10100790A DE10100790C2 (en) | 2001-01-10 | 2001-01-10 | Nickel-based alloy for the cast-technical production of solidified components |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1223229A1 true EP1223229A1 (en) | 2002-07-17 |
EP1223229B1 EP1223229B1 (en) | 2006-02-22 |
Family
ID=7670118
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP01129921A Expired - Lifetime EP1223229B1 (en) | 2001-01-10 | 2001-12-15 | Nickel based alloy for casting single crystal components |
Country Status (7)
Country | Link |
---|---|
US (2) | US6936116B2 (en) |
EP (1) | EP1223229B1 (en) |
JP (1) | JP4250363B2 (en) |
AT (1) | ATE318329T1 (en) |
CA (1) | CA2366997C (en) |
DE (2) | DE10100790C2 (en) |
ES (1) | ES2256147T3 (en) |
Families Citing this family (6)
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DE10339595A1 (en) * | 2003-08-26 | 2005-04-07 | Siemens Ag | Method for predicting and controlling the pourability of liquid steel |
US6969431B2 (en) | 2003-08-29 | 2005-11-29 | Honeywell International, Inc. | High temperature powder metallurgy superalloy with enhanced fatigue and creep resistance |
US7453071B2 (en) * | 2006-03-29 | 2008-11-18 | Asml Netherlands B.V. | Contamination barrier and lithographic apparatus comprising same |
US8696979B2 (en) | 2006-03-31 | 2014-04-15 | National Institute For Materials Science | Ni-base superalloy and method for producing the same |
US8216509B2 (en) * | 2009-02-05 | 2012-07-10 | Honeywell International Inc. | Nickel-base superalloys |
US20160214350A1 (en) | 2012-08-20 | 2016-07-28 | Pratt & Whitney Canada Corp. | Oxidation-Resistant Coated Superalloy |
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US4721540A (en) * | 1984-12-04 | 1988-01-26 | Cannon Muskegon Corporation | Low density single crystal super alloy |
WO1993024683A1 (en) * | 1992-05-28 | 1993-12-09 | United Technologies Corporation | Oxidation resistant single crystal superalloy castings |
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-
2001
- 2001-01-10 DE DE10100790A patent/DE10100790C2/en not_active Expired - Fee Related
- 2001-12-15 DE DE50108994T patent/DE50108994D1/en not_active Expired - Lifetime
- 2001-12-15 AT AT01129921T patent/ATE318329T1/en not_active IP Right Cessation
- 2001-12-15 ES ES01129921T patent/ES2256147T3/en not_active Expired - Lifetime
- 2001-12-15 EP EP01129921A patent/EP1223229B1/en not_active Expired - Lifetime
-
2002
- 2002-01-03 CA CA2366997A patent/CA2366997C/en not_active Expired - Fee Related
- 2002-01-10 JP JP2002003600A patent/JP4250363B2/en not_active Expired - Fee Related
- 2002-01-10 US US10/041,759 patent/US6936116B2/en not_active Expired - Lifetime
-
2005
- 2005-03-04 US US11/071,301 patent/US20050254991A1/en not_active Abandoned
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US4721540A (en) * | 1984-12-04 | 1988-01-26 | Cannon Muskegon Corporation | Low density single crystal super alloy |
WO1993024683A1 (en) * | 1992-05-28 | 1993-12-09 | United Technologies Corporation | Oxidation resistant single crystal superalloy castings |
Also Published As
Publication number | Publication date |
---|---|
DE10100790A1 (en) | 2002-07-18 |
EP1223229B1 (en) | 2006-02-22 |
US20020182100A1 (en) | 2002-12-05 |
US6936116B2 (en) | 2005-08-30 |
ES2256147T3 (en) | 2006-07-16 |
CA2366997A1 (en) | 2002-07-10 |
CA2366997C (en) | 2013-07-02 |
US20050254991A1 (en) | 2005-11-17 |
DE50108994D1 (en) | 2006-04-27 |
ATE318329T1 (en) | 2006-03-15 |
JP2002302724A (en) | 2002-10-18 |
DE10100790C2 (en) | 2003-07-03 |
JP4250363B2 (en) | 2009-04-08 |
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