EP1211336B1 - Superlegierung auf Nickelbasis für Einkristallturbinenschaufeln von industriellen Turbinen mit hoher Beständigkeit gegen Heisskorrosion - Google Patents

Superlegierung auf Nickelbasis für Einkristallturbinenschaufeln von industriellen Turbinen mit hoher Beständigkeit gegen Heisskorrosion Download PDF

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Publication number
EP1211336B1
EP1211336B1 EP00403362A EP00403362A EP1211336B1 EP 1211336 B1 EP1211336 B1 EP 1211336B1 EP 00403362 A EP00403362 A EP 00403362A EP 00403362 A EP00403362 A EP 00403362A EP 1211336 B1 EP1211336 B1 EP 1211336B1
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European Patent Office
Prior art keywords
alloy
resistance
phase
hot corrosion
corrosion
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EP00403362A
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English (en)
French (fr)
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EP1211336A1 (de
Inventor
Pierre Caron
Michael Blackler
Gordon Malcolm Mccolvin
Rajeshwar Prasad Wahi
André Marcel Escale
Laurent Lelait
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hahn Meitner Institut Berlin GmbH
Electricite de France SA
Office National dEtudes et de Recherches Aerospatiales ONERA
Safran Helicopter Engines SAS
Howmet Ltd
Alstom NV
Original Assignee
Hahn Meitner Institut Berlin GmbH
Electricite de France SA
Office National dEtudes et de Recherches Aerospatiales ONERA
Turbomeca SA
Howmet Ltd
Alstom Power NV
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Application filed by Hahn Meitner Institut Berlin GmbH, Electricite de France SA, Office National dEtudes et de Recherches Aerospatiales ONERA, Turbomeca SA, Howmet Ltd, Alstom Power NV filed Critical Hahn Meitner Institut Berlin GmbH
Priority to EP00403362A priority Critical patent/EP1211336B1/de
Priority to DE60035052T priority patent/DE60035052T2/de
Priority to US10/008,745 priority patent/US20030047252A1/en
Priority to JP2001365810A priority patent/JP2002194467A/ja
Publication of EP1211336A1 publication Critical patent/EP1211336A1/de
Priority to US10/636,024 priority patent/US20040069380A1/en
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Publication of EP1211336B1 publication Critical patent/EP1211336B1/de
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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%

Definitions

  • the invention relates to a nickel-based superalloy suitable for the controlled solidification production of stationary and mobile monocrystalline blades of industrial gas turbines.
  • Nickel-based superalloys are the most efficient materials used today for the manufacture of stationary and mobile blades for industrial gas turbines. The two main features required so far for these alloys for these specific applications are good creep resistance at temperatures up to 850 ° C and very good resistance to hot corrosion. Reference alloys commonly used in this field are those known as IN738, IN939 and IN792.
  • the blades made with these reference alloys are prepared by conventional lost-wax casting and have a polycrystalline structure, that is to say that they consist of the juxtaposition of randomly oriented crystals with respect to one another. and called grains. These grains are themselves constituted by a nickel-based austenitic gamma ( ⁇ ) matrix in which gamma prime ( ⁇ ') phase hardening particles whose base is the Ni 3 Al intermetallic compound are dispersed. These grains give these alloys high creep resistance up to temperatures close to 850 ° C., which guarantees the longevity of the blades for which life times of between 50 000 and 100 000 hours are generally sought.
  • the chemical composition of the IN939, IN738 and IN792 alloys has been defined in order to give them an excellent resistance to the environment of the combustion gases, in particular with respect to hot corrosion, a particularly aggressive phenomenon in the case of gas turbines industrial.
  • Important additions of chromium, typically between 12 and 22% by weight, are thus necessary to give these alloys the hot corrosion resistance required for the applications concerned.
  • the classification of these alloys is: IN939 ⁇ IN738 ⁇ IN792. From the point of view of resistance to hot corrosion, the classification is reversed, ie: IN792 ⁇ IN738 ⁇ IN939.
  • These monocrystalline blades are manufactured by solidification directed in lost-wax foundry.
  • the elimination of grain boundaries, which are preferred locations for creep deformation at high temperatures, has dramatically increased the performance of nickel-based superalloys.
  • the monocrystalline solidification process makes it possible to select the preferential orientation of growth of the monocrystalline part and thus to choose the ⁇ 001> orientation which is optimal from the point of view of resistance to creep and to thermal fatigue, these two mechanical stressing modes being the most harmful for turbine blades.
  • the superalloy chemical compositions developed for monocrystalline turbine blades for aeronautical applications are not suitable for blades for terrestrial or marine applications, so-called industrial applications. These alloys are indeed defined so as to favor their mechanical strength up to temperatures above 1100 ° C, and this to the detriment of their resistance to hot corrosion.
  • the chromium concentration of the superalloys for single-crystal blades of aeronautical turbines is generally less than 8% by weight, which makes it possible to reach ⁇ 'phase volume fractions of the order of 70%, favorable to resistance to high creep. temperature.
  • a chromium-rich nickel-based superalloy capable of monocrystalline solidification of industrial gas turbine parts is known under the name SC16 and described in FR 2 643 085 A. Its chromium concentration is equal to 16% by weight.
  • the creep resistance characteristics of the SC16 alloy are such that this alloy provides, relative to the reference polycrystalline alloy IN738, an operating temperature gain of approximately 30 ° C. (830 ° C. instead of 800 ° C.). at about 50 ° C (950 ° C instead of 900 ° C). Comparative tests for cyclic corrosion at 850 ° C in air at atmospheric pressure with Na 2 SO 4 contamination showed that the hot-corrosion resistance of the SC16 alloy was at least equivalent to that of the alloy polycrystalline reference IN738.
  • the object of the invention is to provide a nickel-based superalloy having a resistance to hot corrosion, in the aggressive environment of the combustion gases of industrial gas turbines, at least equivalent to that of the reference polycristalline superalloy IN792 , with a creep resistance greater than or equal to that of the IN792 reference alloy in a temperature range of up to 1000 ° C.
  • This superalloy must in particular be suitable for the production by directed solidification of fixed and mobile monocrystalline blades of large dimensions (up to several tens of centimeters in height) of industrial gas turbines.
  • This superalloy must also show good microstructural stability with respect to the precipitation of chromium-rich brittle intermetallic phases during long-term high temperature holdings.
  • the superalloy according to the invention capable of monocrystalline solidification, has the following weight composition: Co: 4.75 at 5.25% Cr: 11.5 at 12.5% MB: 0.8 at 1.2% W: 3.75 at 4.25% al: 3.75 at 4.25% Ti: 4 at 4.8% Your: 1.75 at 2.25% VS: 0.006 at 0.04% B: ⁇ 0.01% Zr: ⁇ 0.01% Hf: ⁇ 1% Nb: ⁇ 1% Ni and possible impurities: 100% complement.
  • the alloy according to the invention has an excellent compromise between creep resistance and hot corrosion resistance. It is suitable for the manufacture of monocrystalline parts, that is to say made of a single metallurgical grain. This particular structure is obtained for example by means of a conventional method of solidification directed in a thermal gradient, using a helical or baffled grain selection device or a monocrystalline seed.
  • the invention also relates to an industrial turbine blade made by monocrystalline solidification of the superalloy above.
  • Figures 1 and 2 are graphs illustrating the properties of different superalloys.
  • SCB444 An alloy according to the invention called SCB444 was developed with reference to the nominal composition shown in Table I. In this table are also reported the nominal concentrations of major elements of the reference alloys IN939, IN738, IN792 and SC16. Table I: Concentrations by weight in major elements (%) Alloy Or Co Cr MB W A1 Ti Your Nb IN939 Based 19 22.5 - 2 1.9 3.7 1.4 1 IN738 Based 8.5 16 1.7 2.6 3.4 3.4 1.7 0.9 IN792 Based 9 12.4 1.9 3.8 3.1 4.5 3.9 - SC16 Based - 16 3 - 3.5 3.5 3.5 - SCB444 Based 5 12 1 4 4 4.4 2 -
  • Chromium has a beneficial and preponderant effect on the resistance to hot corrosion of nickel-based superalloys.
  • the experiment thus showed that a concentration close to 12% by weight was necessary and sufficient in the alloy of the invention to obtain a resistance to hot corrosion equivalent to that of the reference alloy IN792 under the conditions hot corrosion tests described below, which are representative of the environment created by the combustion gases of certain industrial turbines.
  • a higher chromium content would not make it possible to reach the volume fraction of the ⁇ 'phase necessary for the good creep resistance of the alloy up to 1000 ° C., without the alloy becoming unstable with respect to the precipitation of Fragile intermetallic phases rich in chromium in the ⁇ matrix.
  • a lower concentration of chromium would not match the resistance to hot corrosion of the reference alloy IN792.
  • Chromium also participates in the hardening of the ⁇ matrix in which this element is distributed preferentially.
  • Molybdenum strongly hardens the matrix ⁇ in which this element is distributed preferentially.
  • the amount of molybdenum that can be introduced into the alloy is however limited because this element has a detrimental effect on the hot corrosion resistance of nickel-based superalloys.
  • a concentration close to 1% by weight in the alloy of the invention is not detrimental to its resistance to corrosion and significantly contributes to its hardening.
  • Cobalt also participates in solid solution hardening of the ⁇ matrix.
  • the cobalt concentration has an influence on the solution temperature of the hardening phase ⁇ '(solvus temperature ⁇ '). It is thus advantageous to increase the cobalt concentration to lower the solvus temperature of the ⁇ 'phase and to facilitate the homogenization of the alloy by heat treatment without risk of causing a start of melting. Moreover, it may also be advantageous to reduce the cobalt concentration in order to increase the solvus temperature of the ⁇ 'phase and thus to benefit from greater stability of the ⁇ ' phase at high temperature, which is favorable to the creep resistance.
  • the concentration of 5% by weight of cobalt in the alloy of the invention leads to an optimal compromise between good homogenization ability and good creep resistance.
  • the tungsten whose concentration is around 4% by weight in the alloy of the invention is distributed substantially equally between the ⁇ and ⁇ 'phases and thus contributes to their respective hardenings. His concentration in the alloy is however limited because this element is heavy, and has a negative effect on the resistance to hot corrosion.
  • the concentration of aluminum is around 4% by weight in the alloy of the invention.
  • the presence of this element causes the precipitation of the hardening phase ⁇ '.
  • Aluminum also promotes resistance to oxidation.
  • the titanium and tantalum elements are added to the alloy of the invention in order to reinforce the ⁇ 'phase in which they substitute for the aluminum element.
  • the respective concentrations of these two elements in the alloy of the invention are close to 4.4% by weight for titanium and 2% by weight for tantalum. Under the conditions described below for hot corrosion tests, corresponding to the intended application, experience has shown that the presence of titanium is more favorable to the resistance to hot corrosion than that of tantalum. .
  • the titanium concentration has however been limited on the one hand by the fact that this element can have a negative effect on the oxidation resistance, and on the other hand because a too high concentration of titanium can cause a destabilization of the ⁇ 'phase.
  • the sum of the concentrations of tantalum, titanium and aluminum roughly defines the hardening phase volume fraction ⁇ '.
  • the concentrations of these three elements have been adjusted in such a way as to optimize the ⁇ 'phase volume fraction, while keeping the stable ⁇ and ⁇ ' phases during the long-term hold at high temperature, and taking into account that the Chromium concentration was set at about 12% by weight so as to achieve the desired corrosion resistance.
  • Alloy SCB444 was developed as ⁇ 001> orientation monocrystals. The density of this alloy was measured and found to be 8.22 g.cm -3 .
  • the alloy After directed solidification, the alloy consists essentially of two phases: the austenitic matrix ⁇ , a nickel-based solid solution, and the ⁇ 'phase, an intermetallic compound whose basic formula is Ni 3 Al, which precipitates most of it within the ⁇ matrix in the form of fine particles smaller than one micrometer in the course of solid state cooling.
  • ⁇ 'phase an intermetallic compound whose basic formula is Ni 3 Al, which precipitates most of it within the ⁇ matrix in the form of fine particles smaller than one micrometer in the course of solid state cooling.
  • a small fraction of ⁇ 'phase is also found in massive particles resulting from a liquid eutectic transformation -> ⁇ + ⁇ ' at the end of solidification.
  • the eutectic phase volume fraction ⁇ / ⁇ ' is close to 1.4%.
  • the SCB444 alloy was subjected to a homogenization heat treatment at a temperature of 1270 ° C. for 3 hours with cooling in air. This temperature is greater than the solvus temperature of the ⁇ 'phase (solution dissolution temperature of the ⁇ ' phase precipitates), which is equal to 1253 ° C., and lower than the melting start temperature, equal to 1285 ° C. vs.
  • This treatment aims to dissolve all the ⁇ 'phase precipitates whose size distribution is very extensive in the raw state of solidification directed, to eliminate massive particles of eutectic ⁇ / ⁇ ' and reduce heterogeneities related to the dendritic solidification structure.
  • the cooling following the homogenization treatment described above was carried out by quenching in air.
  • the speed of this cooling must be sufficiently high so that the size of the particles having precipitated during this cooling is less than 500 nm.
  • the homogenization heat treatment procedure that has just been described is an example that makes it possible to obtain the desired result, ie a homogeneous distribution of fine ⁇ 'phase particles whose size does not exceed 500 nm.
  • the SCB444 alloy was tested after being subjected to a homogenization treatment as described above, and then to two income treatments making it possible to stabilize the size and the volume fraction of the ⁇ 'phase precipitates.
  • a first treatment of income was to heat the alloy at 1100 ° C for 4 hours with cooling in air which has the effect of stabilizing the size of ⁇ phase precipitates.
  • a second treatment of income at 850 ° C for 24 hours, followed by cooling in air, optimizes the volume fraction of phase ⁇ '. This ⁇ 'phase volume fraction is estimated at 57% in the SCB444 alloy.
  • the ⁇ 'phase precipitated in the form of cuboidal particles whose size is between 200 and 500 nm.
  • Hot cyclic corrosion tests were carried out at 900 ° C on the SCB444 alloy in an industrial corrosion bench with burner.
  • the cycle was as follows: 1 hour at 900 ° C in the corrosive atmosphere produced by the burner, then 15 minutes out of the oven at room temperature.
  • the burner operated with 0.20% sulfur fuel.
  • a saline solution at 0.5 gl -1 NaCl was vaporized on the sample at a rate of 2.2 m 3 ⁇ h -1 .
  • the sample was coated every 100 hours with a deposition of 0.5 mg.cm -2 Na 2 SO 4 .
  • alloys IN738 and IN792 were tested simultaneously.
  • the corrosion resistance criterion is the number of cycles for which the first pits of corrosion appear on the surface of the sample.
  • the graph in FIG. 2 makes it possible to compare the creep rupture times obtained for alloys SCB444, IN738, IN792 and SC16.
  • On the abscissa is the applied stress.
  • On the ordinate is the value of the Larson-Miller parameter.
  • T is the creep temperature in Kelvin
  • t the break time in hours.

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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)

Claims (2)

  1. Superlegierung auf Nickelbasis, geeignet für die monokristalline Erstarrung, dadurch gekennzeichnet, dass die Gewichtszusammensetzung wie folgt ist: Co: 4,75 bis 5,25% Cr: 11,5 bis 12,5 % Mo: 0,8 bis 1,2 % W: 3,75 bis 4,25 % Al: 3,75 bis 4,25 % Ti: 4 bis 4,8 % Ta: 1,75 bis 2,25 % C: 0,006 bis 0,04 % B: ≤ 0.01% Zr: ≤ 0,01 % Hf ≤ 1 % Nb ≤ 1 % Ni und mögliche Verunreinigungen: Ergänzung auf 100 %.
  2. Industrielle Turbinenschaufel erhalten durch die monokristalline Erstarrung einer Superlegierung nach Anspruch 1.
EP00403362A 2000-11-30 2000-11-30 Superlegierung auf Nickelbasis für Einkristallturbinenschaufeln von industriellen Turbinen mit hoher Beständigkeit gegen Heisskorrosion Expired - Lifetime EP1211336B1 (de)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP00403362A EP1211336B1 (de) 2000-11-30 2000-11-30 Superlegierung auf Nickelbasis für Einkristallturbinenschaufeln von industriellen Turbinen mit hoher Beständigkeit gegen Heisskorrosion
DE60035052T DE60035052T2 (de) 2000-11-30 2000-11-30 Superlegierung auf Nickelbasis für Einkristallturbinenschaufeln von industriellen Turbinen mit hoher Beständigkeit gegen Heisskorrosion
US10/008,745 US20030047252A1 (en) 2000-11-30 2001-11-30 Nickel-based superalloy having high resistance to hot-corrosion for monocrystalline blades of industrial turbines
JP2001365810A JP2002194467A (ja) 2000-11-30 2001-11-30 産業用タービンの単結晶ブレードのための高い耐高温腐食性をもつニッケル系超合金
US10/636,024 US20040069380A1 (en) 2000-11-30 2003-08-07 Nickel-based superalloy having high resistance to hot-corrosion for monocrystalline blades of industrial turbines

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP00403362A EP1211336B1 (de) 2000-11-30 2000-11-30 Superlegierung auf Nickelbasis für Einkristallturbinenschaufeln von industriellen Turbinen mit hoher Beständigkeit gegen Heisskorrosion

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EP1211336A1 EP1211336A1 (de) 2002-06-05
EP1211336B1 true EP1211336B1 (de) 2007-05-30

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EP00403362A Expired - Lifetime EP1211336B1 (de) 2000-11-30 2000-11-30 Superlegierung auf Nickelbasis für Einkristallturbinenschaufeln von industriellen Turbinen mit hoher Beständigkeit gegen Heisskorrosion

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Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060182649A1 (en) * 2005-02-16 2006-08-17 Siemens Westinghouse Power Corp. High strength oxidation resistant superalloy with enhanced coating compatibility
EP2103700A1 (de) * 2008-03-14 2009-09-23 Siemens Aktiengesellschaft Legierung auf Nickelbasis und Verwendung, Turbinenblatt oder -schaufel und Gasturbine
FR3057880B1 (fr) * 2016-10-25 2018-11-23 Safran Superalliage a base de nickel, aube monocristalline et turbomachine
FR3097879B1 (fr) * 2019-06-28 2021-05-28 Safran Aircraft Engines Procede de fabrication d’une piece en superalliage monocristallin

Family Cites Families (12)

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Publication number Priority date Publication date Assignee Title
DE3109293C2 (de) * 1980-03-13 1985-08-01 Rolls-Royce Ltd., London Verwendung einer Nickellegierung für einkristalline Gußstücke
US5399313A (en) * 1981-10-02 1995-03-21 General Electric Company Nickel-based superalloys for producing single crystal articles having improved tolerance to low angle grain boundaries
US5154884A (en) * 1981-10-02 1992-10-13 General Electric Company Single crystal nickel-base superalloy article and method for making
US4885216A (en) * 1987-04-03 1989-12-05 Avco Corporation High strength nickel base single crystal alloys
GB2234521B (en) * 1986-03-27 1991-05-01 Gen Electric Nickel-base superalloys for producing single crystal articles having improved tolerance to low angle grain boundaries
US5403546A (en) * 1989-02-10 1995-04-04 Office National D'etudes Et De Recherches/Aerospatiales Nickel-based superalloy for industrial turbine blades
US5395584A (en) * 1992-06-17 1995-03-07 Avco Corporation Nickel-base superalloy compositions
US6355117B1 (en) * 1992-10-30 2002-03-12 United Technologies Corporation Nickel base superalloy single crystal articles with improved performance in air and hydrogen
JPH07286503A (ja) * 1994-04-20 1995-10-31 Hitachi Ltd 高効率ガスタービン
EP1038982A1 (de) * 1999-03-26 2000-09-27 Howmet Research Corporation Einkristalline Superlegierungskörpern mit verminderter Rekristallisierung der Körnern
EP1054072B1 (de) * 1999-05-20 2003-04-02 ALSTOM (Switzerland) Ltd Nickel-Basis-Superlegierung
DE50006694D1 (de) * 1999-07-29 2004-07-08 Siemens Ag Hochtemperaturbeständiges bauteil und verfahren zur herstellung des hochtemperaturbeständigen bauteils

Non-Patent Citations (1)

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US20040069380A1 (en) 2004-04-15
DE60035052D1 (de) 2007-07-12
DE60035052T2 (de) 2008-01-24
EP1211336A1 (de) 2002-06-05
US20030047252A1 (en) 2003-03-13
JP2002194467A (ja) 2002-07-10

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