EP0184949B1 - Verfahren zur Wiedererzeugung von aus Nickelbasis-Superlegierung hergestellten Einzelteilen am Ende ihrer Brauchbarkeit - Google Patents

Verfahren zur Wiedererzeugung von aus Nickelbasis-Superlegierung hergestellten Einzelteilen am Ende ihrer Brauchbarkeit Download PDF

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EP0184949B1
EP0184949B1 EP85402131A EP85402131A EP0184949B1 EP 0184949 B1 EP0184949 B1 EP 0184949B1 EP 85402131 A EP85402131 A EP 85402131A EP 85402131 A EP85402131 A EP 85402131A EP 0184949 B1 EP0184949 B1 EP 0184949B1
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temperature
rejuvenation
accordance
component
fact
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EP0184949A1 (de
EP0184949B2 (de
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José Company
Alain Roger Leonnard
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Safran Aircraft Engines SAS
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Societe Nationale dEtude et de Construction de Moteurs dAviation SNECMA
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon

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  • the invention relates to a method of heat treatment for parts arriving at the end of operating potential after having undergone damage by creep in particular; the aim of the method is to make them recover their initial properties in order to prolong their lifespan. It relates to parts made of heat resistant alloy with a nickel base comprising a hardening phase -y 'and applies in particular to the moving blades of a turbomachine.
  • the blades must be able to resist creep at high temperature because they are mounted on a disc rotating between 5,000 and 20,000 rpm while being exposed to hot gases from 900 ° C to 1300 ° C and oxidants leaving the combustion.
  • the nickel-based superalloys used in aeronautics have a hardening phase -y 'whose volume fraction can reach 70%.
  • the blades subjected to such mechanical and thermal stresses undergo permanent elongation by creep which inevitably leads to their systematic scrapping after a certain number of hours of use in order to avoid the risks of catastrophic rupture.
  • the high pressure turbine blades of a certain number of engines currently have their operating potential limited to about 800 hours by creep.
  • This creep deformation process resulting in a degradation of the microcrystalline structure is the production of a heat treatment method allowing the restoration of the initial structure under conditions compatible with the geometrical criteria of the parts.
  • the invention therefore has the second objective of carrying out a heat treatment which does not require the prior operation of removing the protective layer.
  • the method of regenerating parts of heat-resistant alloy based on nickel NK15 CAT comprising in particular Co 13 to 17%, Cr 8 to 11%, Al 5 to 6%, Ti 4 to 5%, Mo 2 at 4%, Va 0.7 to 1.7%, C 0.1 to 0.2% and forming an eutectic comprising a hardening phase y ⁇ , the part having consumed at least part of its operating potential due in particular to creep damage at high temperature, consists in maintaining the part at a temperature between 1160 ° C and 1220 ° C and for a period between 1 h and 4 h to re-dissolve at least 50% of the phase ⁇ 'the method consists in cooling the part at a controlled speed to a temperature below 700 ° C corresponding to the precipitation range of the phase, this speed being chosen as a function of the desired microstructural morphology.
  • patent FR 2 292 049 describes a method for extending the duration of the secondary creep of certain alloys; it consists of an unconstrained heat treatment, carried out at a temperature lower than that of dissolution of the compounds.
  • This temperature corresponds in practice to the maximum operating temperature of the room; moreover, maintaining the temperature is quite long because, according to the hypothesis put forward, it should allow the annihilation of the lacunar networks by a diffusion process.
  • This treatment limited in temperature, is certainly ineffective for parts which have operated at high temperatures, such as 1100 ° C., since it does not allow the regeneration of the microcrystalline structure because it excludes the re-solution of the hardening compounds. .
  • its duration makes it economically uninteresting in an industrial application.
  • Patent FR 2 313 459 relates to a method for improving the service performance of metal parts which have undergone permanent elongation. It consists in subjecting these parts, before the appearance of surface cracks, to hot isostatic compression, at a temperature lower than that where a magnification of the grains occurs, then to apply a treatment of re-solution of the phases followed by 'a hardening income.
  • the major advantage of compaction lies in the fact that it closes the creep decohesions and the unclogged foundry pores. chants.
  • the IN 100 alloy of formula NK 15 CAT is a nickel-base cast alloy. Its composition is as follows: Cobalt 13 to 17%, Chromium 8 to 11%, aluminum 5 to 6%, titanium 4 to 5%, molybdenum 2 to 4%, vanadium 0.7 to 1.7%, Carbon 0.1 at 0.2% etc ...
  • the IN 100 is designed for long-term use at 1000 ° C and 1100 ° C for short periods. In all cases, its poor resistance to corrosion, in particular in a sulfurous atmosphere, requires protection, obtained for example by the vapor phase aluminization method of patent FR 1 433 497.
  • the IN 100 has a ⁇ - ⁇ 'dendritic structure decorated with eutectic aggregates and carbides.
  • the size of the basalt grain dendrites and the morphology of the hardening phase depend on the rate of cooling on casting, therefore on the local thickness of material in the part, and on the content of B and Zr. It varies from a few tenths to several mm for thicknesses ranging from 1 to 10 mm.
  • the matrix ⁇ hardened by the effect of a solid solution of Cr and Co in Ni crystallizes in the CFC system.
  • the maximum hardening comes from the precipitation of the -y 'phase, ordered, of type L1 2 (Cu 3 Au) of the same system. Crystal clear and consistent with the matrix. Its volume fraction is around 70%.
  • the approximate composition is (Ni, Co) 3 (Ti, AI).
  • the exceptional mechanical resistance when hot conferred by ⁇ 'on nickel-based superalloys comes essentially from the flow stress of this phase, which has the remarkable property of increasing when the temperature increases.
  • the alloy is rich in ⁇ - ⁇ 'eutectic islands, located in interdendritic spaces.
  • the temperature of formation of these aggregates is linked to their chemistry during the passage of the solidus, and can vary within wide proportions.
  • the thermal analysis places it between 1210 and 1275 ° C depending in particular on the carbon content.
  • the first microstructural evolution observed consists in the precipitation of secondary intergranular carbides, around the primary carbides and at the ⁇ - ⁇ 'interfaces of the eutectics, after 50 h of operation ( Figures 1 and 1A) .
  • the precipitation intensifies to become intragranular.
  • phenomena of coalescence of the ⁇ 'phase lead to the gradual disappearance of the fine precipitated ⁇ '.
  • the size of the globules -y ' reaches 3 to 4 ⁇ m and can double in the vicinity of eutectics, primary carbides and grain boundaries ( Figures 2 and 2A).
  • the examinations on thin blade show a particular arrangement of the dislocations of interface ⁇ - ⁇ 'and M23 C6 - y: tendency to an arrangement either parallel to the stress of centrifugal origin (figure 3), or in polygonization (figure 4) .
  • the microstructure at the leading edge in the middle of the blade has a dendritic appearance.
  • the interdendritic spaces are rich in eutectics and consist of precipitates ⁇ 'significantly larger than in the heart of the dendrites.
  • the geometry of certain foundry pores reveals a beginning of deformation, as already observed after 800 hours; the coalescence of the phase there causes the disappearance of the precipitated ends.
  • FIGS. 5A to D give in summary a schematic representation of the process of damage by creep of the alloy subjected to a stress of 130 MPa and a temperature of 1000 ° C., in particular observed on test pieces.
  • FIG. 5A shows the state of the structure after aluminization, there are 3 populations of ⁇ ': relatively coarse particles of interdendritic ⁇ ', fine particles of dendritic ⁇ 'and very fine particles uniformly distributed obtained during cooling after aluminization treatment.
  • the alloy is subjected to a creep potential regeneration treatment comprising a thermal cycle erasing the microstructural effects of the deformation and leading to a microstructure approaching that of the alloy before stress.
  • the part to be treated as observed, that is to say after 1000 hours of operation, is placed in an oven, preferably under vacuum in order to overcome oxidation problems. It is heated to a chosen temperature to re-dissolve a sufficient volume fraction of the hardening phase. In the present case of IN 100 alloy vanes protected by aluminization, this temperature is also determined as a function of its compatibility with maintaining the protection; in fact a too high temperature would cause the diffusion of aluminum and the dilution of the layer of nickel aluminide.
  • this temperature was chosen at 1190 ° C but may vary depending on the case between 1160 ° C and 1220 ° C.
  • the choice of temperature is also guided by the need for a sufficient margin with the melting temperature of the eutectic for industrial application.
  • Tests have shown that maintenance of less than 4 hours, preferably of the order of one hour, was sufficient to re-dissolve a volume fraction of ⁇ 'phase of at least 50%, which amounts in particular to destroying the connections between ⁇ 'globules which had developed during damage by creep.
  • the part was cooled by injecting a flow of inert gas, argon, into the oven.
  • the flow rate was controlled in order to control the cooling rate of the part to a temperature below the precipitation range of the ⁇ 'phase.
  • the set of microstructures obtained is represented in FIG. 6. It is observed that the argon coolings lead to the precipitation of two populations of -y ', and that the volume fraction of "large” ⁇ ' increases while decreases the content of fines constituents, while decreasing the cooling rate. Microstructural observation reveals a complex phenomenon of "germination-growing” and “growth-coalescence", the respective kinetics of which vary according to the local chemical composition of the matrix giving rise to ⁇ '. There is therefore a compromise between volume fractions of large ⁇ 'and a few allowing the best mechanical behavior to be obtained according to the criteria sought. Indeed, a microstructure consisting only of fine precipitates ⁇ 'is favorable to the creep behavior, but detrimental to the cold and hot ductility of the alloy.
  • Tests were also carried out on test pieces in order to characterize them in creep.
  • the IN 100 alloy test pieces underwent: 0.5%, 1% and 3% elongation under a stress of 130 MPa at 1000 ° C; in engine operating equivalent, 1% elongation is equivalent to 800 hours of operation for the above conditions.
  • the test pieces are regenerated and then reassembled in creep.
  • the test results are presented in FIG. 10. It is observed that, under the test conditions, the alloy present after regeneration of the primary and secondary creep stages, the more reduced the greater the pre-deformation.
  • the maximum gain in treatment is obtained after a pre-deformation of 0.5%.
  • the time to obtain 1% elongation is 83 ⁇ 10 hours, the time to obtain this same elongation after treatment with 0.5% elongation increases to 103 ⁇ 16 hours, ie a gain of 24% .
  • the gain is similar on the break time. It is 145 hours normally and goes to 180 hours after regeneration at 0.5% elongation.

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  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Turbine Rotor Nozzle Sealing (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Chemically Coating (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Claims (6)

1. Verfahren zur Regeneration von Einzelteilen von Turbomaschinen am Ende ihrer Brauchbarkeit verbunden mit insbesondere Beschädigungen durch plastisches Fließen aus einer Legierung auf Nickel-Guß-Basis NK15 CAT, die insbesondere aus 13 bis 17 % Cobalt, 8 bis 11 % Chrom, 5 bis 6 % Aluminium, 4 bis 5 % Titan, 2 bis 4 % Molybdän, 0,7 bis 1,7 % Vanadium, 0,1 bis 0,2 % Kohlenstoff, zusammengesetzt ist, die ein y-y' Eutektikum mit einer ausgehärteten γ'-Phase bilden, dadurch gekennzeichnet, daß das Verfahren enthält - Halten des Einzelteils auf einer Temperatur zwischen 1160 °C und 1220 °C und während einer Zeitspanne zwischen 1 h und 4 h zur überführung von wenigstens 50 % des Volumenanteils der ausgehärteten y -Phase in Lösung, - danach Abkühlen des Einzelteils unter Steuerung der Abkühlgeschwindigkeit bis zu einer Temperatur des Einzelteils unter 700 °C entsprechend dem Gefügebildungsbereich der γ'-Phase.
2. Verfahren zur Regeneration gemäß Anspruch 1, dadurch gekennzeichnet, daß die Abkühlgeschwindigkeit zwischen 600 K/h und 2500 K/h liegt und sie bis zu einer Temperatur des Einzelteils unter 700 °C geführt wird.
3. Verfahren zur Regeneration gemäß Anspruch 2, dadurch gekennzeichnet, daß die Abkühlgeschwindigkeit zwischen 1085 K/h und 1145 K/h liegt.
4. Verfahren zur Regeneration gemäß einem der vorhergehenden Ansprüche, wobei das Einzelteil einer Korrosions-Schutzbehandlung insbesondere durch Aluminisation unterzogen wird, dadurch gekennzeichnet, daß die Überführungstemperatur in Lösung niedriger gewählt ist als die für diese Schutzschicht geeignete Verdünnungstemperatur.
5. Verfahren zur Regeneration gemäß dem vorhergehenden Anspruch, dadurch gekennzeichnet, daß die überführungstemperatur in Lösung zwischen 1185 °C und 1195 °C liegt.
6. Verfahren zur Regeneration gemäß einem der vorhergehenden Ansprüche für Einzelteile, die nicht freigemachte Entfestigungen zeigen, dadurch gekennzeichnet, daß man die Einzelteile einer vorhergehenden Behandlung einer isostatischen Wärmeverdichtung unterzieht.
EP85402131A 1984-11-08 1985-11-06 Verfahren zur Wiedererzeugung von aus Nickelbasis-Superlegierung hergestellten Einzelteilen am Ende ihrer Brauchbarkeit Expired - Lifetime EP0184949B2 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8416974 1984-11-08
FR8416974A FR2572738B1 (fr) 1984-11-08 1984-11-08 Methode de regeneration de pieces en superalliage base nickel en fin de potentiel de fonctionnement

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EP0184949A1 EP0184949A1 (de) 1986-06-18
EP0184949B1 true EP0184949B1 (de) 1989-07-19
EP0184949B2 EP0184949B2 (de) 1992-08-26

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EP85402131A Expired - Lifetime EP0184949B2 (de) 1984-11-08 1985-11-06 Verfahren zur Wiedererzeugung von aus Nickelbasis-Superlegierung hergestellten Einzelteilen am Ende ihrer Brauchbarkeit

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US (1) US4753686A (de)
EP (1) EP0184949B2 (de)
JP (1) JPS61119661A (de)
CA (1) CA1275230C (de)
DE (1) DE3571650D1 (de)
FR (1) FR2572738B1 (de)
IL (1) IL76930A (de)

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5498484A (en) * 1990-05-07 1996-03-12 General Electric Company Thermal barrier coating system with hardenable bond coat
JP3069580B2 (ja) * 1995-09-08 2000-07-24 科学技術庁金属材料技術研究所長 単結晶材料の再熱処理による余寿命延長方法
JP3722975B2 (ja) * 1998-02-23 2005-11-30 三菱重工業株式会社 Ｎｉ基耐熱合金の性能回復処理方法
DE60010405T2 (de) 1999-10-23 2004-09-09 Rolls-Royce Plc Korrosionsschutzschicht für metallisches Werkstück und Verfahren zur Herstellung einer korrosionsschützenden Beschichtung auf ein metallisches Werkstück
RU2171857C2 (ru) * 2000-11-13 2001-08-10 ООО "Самаратрансгаз" Способ восстановления циклической прочности деталей газотурбинных двигателей из жаропрочных сплавов на основе никеля
EP1398393A1 (de) * 2002-09-16 2004-03-17 ALSTOM (Switzerland) Ltd Verfahren zur Wiederherstellung von Eigenschaften
RU2230822C1 (ru) * 2003-04-10 2004-06-20 Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" Способ упрочнения изделия из литейного сплава на никелевой основе
RU2258086C1 (ru) * 2003-12-17 2005-08-10 Круцило Виталий Григорьевич Способ термопластического упрочнения деталей и установка для его осуществления
RU2459885C1 (ru) * 2011-07-15 2012-08-27 Общество с ограниченной ответственностью "Производственное предприятие Турбинаспецсервис" Способ восстановительной термической обработки изделий из жаропрочных никелевых сплавов
CN105274459A (zh) * 2014-07-23 2016-01-27 中国人民解放军第五七一九工厂 真空热处理恢复镍基高温合金组织和性能的方法
US10689741B2 (en) 2015-08-18 2020-06-23 National Institute For Materials Science Ni-based superalloy part recycling method
JP2019112702A (ja) * 2017-12-26 2019-07-11 三菱日立パワーシステムズ株式会社 ニッケル基合金再生部材および該再生部材の製造方法
CN117587341B (zh) * 2023-11-24 2026-04-24 北航（四川）西部国际创新港科技有限公司 一种高温合金的恢复热处理方法
CN119574336B (zh) * 2024-12-30 2025-10-14 北京航空航天大学 一种合金蠕变试验测试装置及方法

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US3310440A (en) * 1964-10-21 1967-03-21 United Aircraft Corp Heat treatment of nickel base alloys
US3817796A (en) * 1970-06-30 1974-06-18 Martin Marietta Corp Method of increasing the fatigue resistance and creep resistance of metals and metal body formed thereby
IL46114A (en) * 1974-11-25 1977-01-31 Israel Aircraft Ind Ltd Thermal treatment method to extend the second crawling life of alloys
CH594480A5 (de) * 1975-06-03 1978-01-13 Bbc Brown Boveri & Cie
JPS52120913A (en) * 1976-04-06 1977-10-11 Kawasaki Heavy Ind Ltd Heat treatment for improving high temperature low cycle fatigue strength of nickel base cast alloy
US4161412A (en) * 1977-11-25 1979-07-17 General Electric Company Method of heat treating γ/γ'-α eutectic nickel-base superalloy body
US4328045A (en) * 1978-12-26 1982-05-04 United Technologies Corporation Heat treated single crystal articles and process
FR2503188A1 (fr) * 1981-04-03 1982-10-08 Onera (Off Nat Aerospatiale) Superalliage monocristallin a matrice a matuice a base de nickel, procede d'amelioration de pieces en ce superalliage et pieces obtenues par ce procede

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Publication number Publication date
FR2572738A1 (fr) 1986-05-09
JPS61119661A (ja) 1986-06-06
FR2572738B1 (fr) 1987-02-20
EP0184949A1 (de) 1986-06-18
EP0184949B2 (de) 1992-08-26
DE3571650D1 (en) 1989-08-24
CA1275230C (fr) 1990-10-16
IL76930A0 (en) 1986-04-29
JPH046789B2 (de) 1992-02-06
IL76930A (en) 1988-08-31
US4753686A (en) 1988-06-28

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