EP0184949B2 - 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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Publication number
EP0184949B2
EP0184949B2 EP85402131A EP85402131A EP0184949B2 EP 0184949 B2 EP0184949 B2 EP 0184949B2 EP 85402131 A EP85402131 A EP 85402131A EP 85402131 A EP85402131 A EP 85402131A EP 0184949 B2 EP0184949 B2 EP 0184949B2
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Prior art keywords
temperature
rejuvenation
cooling
creep
nickel
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EP85402131A
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English (en)
French (fr)
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EP0184949B1 (de
EP0184949A1 (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

Definitions

  • 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 chamber .
  • the nickel-based superalloys used in aeronautics have a hardening phase y ′, the volume fraction of which 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%, Ai 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 yy 'comprising a hardening phase y', the part having consumed at least part of its operating potential at cause in particular of damage by creep 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 phase y ′, the method consists in subsequently cooling the part at a controlled speed to a temperature below 700 ° C. corresponding to the precipitation range of phase y ′, this speed being chosen as a function
  • 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 having operated at high temperatures, such as 1100 ° C., because 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 non-opening foundry pores.
  • 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-term. 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 y-y 'decorated by 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 y 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 phase y ', ordered, of type L1 2 (Cu 3 Au) of the same crystalline system and consistent with the matrix. Its volume fraction is around 70%.
  • the approximate composition is (Ni, Co) 3 (T, AI).
  • the exceptional mechanical resistance when hot gives y 'to 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 flows y-y ', 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 new dawn presents at the leading edge as at the trailing edge a structure y-y 'rich in eutectics and primary carbides.
  • y' coarse 'of size close to 2 f..lm precipitating shortly after the solidification of the alloy
  • fine of size close to 0.2 f .. lm precipitating during cooling following the protective treatment.
  • the primary carbides precipitating while the alloy is not fully solidified, are repelled in the interdendritic sites where the grain boundaries are located, which are essentially distinguished by the difference in orientation of the y 'between 2 contiguous grains.
  • the first microstructural evolution observed consists in the precipitation of secondary intergranular carbides, around the primary carbides and at the interfaces y-y 'of the eutectics, after 50 h of operation (FIGS. 1 and 1 A).
  • the precipitation intensifies to become intragranular.
  • phenomena of coalescence of the phase y ' cause the gradual disappearance of the precipitated ends y'.
  • the size of the globules reaches 3 to 4 ⁇ m there and can double in the vicinity of eutectics, primary carbides and grain boundaries ( Figures 2 and 2A).
  • the microstructure at the leading edge in the middle of the blade has a dendritic appearance.
  • the interdendritic spaces are rich in eutectic and consist of precipitates y 'substantially 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 y 'phase causes the disappearance of the fine precipitates.
  • 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 y ′: relatively coarse particles of interdendritic y ′, fine particles of y ′ dendritic and very fine particles uniformly distributed obtained during cooling after aluminization treatment.
  • the invention relates to a known type of process in which 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 eutecti than for industrial application.
  • the part was cooled by injecting a flow of inert gas, argon, into the oven. We controlled the flow in order to control the cooling rate of the room.
  • the part is cooled by controlling the cooling rate to a temperature below 700 ° C corresponding to the precipitation range of phase y '.
  • 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” y' increases while the content of fine constituents decreases , 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 y '. There is therefore a compromise between the volume fractions of large y 'and of fine y' allowing the best mechanical behavior to be obtained as a function of the criteria sought.
  • the cooling rate is controlled between 1085 ° C / h and 1145 ° C / h which leads to the microstructure of Figure 9. Under these conditions, it is no longer possible to differentiate a new blade ( Figure 7) of a regenerated blade (FIG. 9) by the sole examination of their microstructure: distribution of ⁇ - ⁇ 'identical in the two cases, absence of secondary carbides, the latter having been dissolved during the treatment.
  • 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 shown in FIG. 10. It is observed that, under the test conditions, the alloy present after regeneration of the primary and secondary cloud stages, the smaller 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)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Chemically Coating (AREA)

Claims (4)

1. Verfahren zum Regenerieren am Ende der Brauchbarkeit, das insbesondere mit Fließchäden verbunden ist, von Einzelteilen von Turbomaschinen aus einer Gußlegierung auf Nickelbasis vom Typ NK 15 CAT, welche besonders aus 13 bis 17% Co, 8 bis 11 % Cr, 5 bis 6 % Al, 4 bis 5 % Ti, 2 bis 4 % Mo, 0,7 bis 1,7 % V und 0,1 bis 0,2 % C zusammengesetzt ist und ein y-y'-Eutektikum mit der hartmachenden y'-Phase bildet, umfassend eine erste Stufe mit dem Halten des Einzelteils auf einer Temperatur zwischen 1160 °C bis 1220 °C während einerzeit zwischen 1 und 4 Stunden zur Überführung von wenigstens 50 % des Volumenanteils der hartmachenden y'-Phase in Lösung,
dadurch gekennzeichnet,
daß noch eine zweite Stufe vorgesehen ist, die besteht aus dem Abkühlen des Einzelteils unter Regelung der Abkühlgeschwindigkeit bis auf eine Temperatur des Einzelteils unterhalb von 700 °C entsprechend dem Bereich der Phasenausscheidung für die Phase y' bei einer Abkühlgeschwindigkeit zwischen 1085 K/h und 1145 K/h.
2. Verfahren zum Regenerieren gemäß dem vorangehenden Anspruch unter Einsatz eines Einzelteils, das eine Korrosionsschutzbehandlung, insbesondere durch Aluminieren durchgemacht hat,
dadurch gekennzeichnet,
daß die Überführungstemperatur niedriger gewählt ist als die für diese Schutzbehandlung eigentümliche Verdünnungstemperatur.
3. Verfahren gemäß dem vorangehenden Anspruch,
dadurch gekennzeichnet,
daß die Überführungstemperatur in die Lösung zwischen 1185 °C und 1195 °C liegt.
4. Verfahren zum Regenerieren gemäß einem der vorangehenden Ansprüche unter Einsatz eines Einzelteils mit nicht herauskommenden Entefestigungen,
dadurch gekennzeichnet,
daß man das Einzelteil einer vorangehenden 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

Publications (3)

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EP0184949A1 EP0184949A1 (de) 1986-06-18
EP0184949B1 EP0184949B1 (de) 1989-07-19
EP0184949B2 true 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 (13)

* 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
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
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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
IL76930A (en) 1988-08-31
US4753686A (en) 1988-06-28
CA1275230C (fr) 1990-10-16
DE3571650D1 (en) 1989-08-24
JPS61119661A (ja) 1986-06-06
JPH046789B2 (de) 1992-02-06
FR2572738B1 (fr) 1987-02-20
EP0184949B1 (de) 1989-07-19
IL76930A0 (en) 1986-04-29
EP0184949A1 (de) 1986-06-18

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