EP1840232A1 - Legierung auf Nickelbasis - Google Patents

Legierung auf Nickelbasis Download PDF

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Publication number
EP1840232A1
EP1840232A1 EP07105258A EP07105258A EP1840232A1 EP 1840232 A1 EP1840232 A1 EP 1840232A1 EP 07105258 A EP07105258 A EP 07105258A EP 07105258 A EP07105258 A EP 07105258A EP 1840232 A1 EP1840232 A1 EP 1840232A1
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EP
European Patent Office
Prior art keywords
alloy
equal
contents
temperature
workpiece
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Granted
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EP07105258A
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English (en)
French (fr)
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EP1840232B1 (de
Inventor
Isabelle Augustins Lecallier
Pierre Caron
Jean-Yves Guedou
Didier Locq
Loeïz Naze
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Association pour la Recherche et le Developpement des Methodes et Processus Industriels
Office National dEtudes et de Recherches Aerospatiales ONERA
Safran Aircraft Engines SAS
Original Assignee
Association pour la Recherche et le Developpement des Methodes et Processus Industriels
Office National dEtudes et de Recherches Aerospatiales ONERA
SNECMA SAS
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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%
    • 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
    • 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 alloys, or superalloys, based on nickel (Ni) intended more particularly for the production of turbine disks or turbine engine compressor, according to powder metallurgy processes.
  • the turbomachines concerned can be aeronautical (turbojet engine, turboprop engine) or terrestrial (gas turbine dedicated to the production of energy).
  • the compressor and turbine disks respectively located upstream and downstream of the combustion chamber of a turbojet engine are subjected in service to mechanical stresses comparable to traction, creep and fatigue, at temperatures up to 800 ° C. However, it is desired that the operating lifetimes of these disks reach several thousand hours. These discs must therefore be made of an alloy having, at high temperatures, a high resistance to tensile stresses, a very good creep resistance, as well as a good resistance to the propagation of cracks.
  • these discs can be made of Ni-based alloys according to powder metallurgy processes, these processes limiting chemical segregation phenomena and promoting good microstructural homogeneity of the alloy.
  • This alloy example is part of the two-phase alloys which comprise: a so-called gamma phase formed by a nickel-based solid solution, which constitutes the matrix of the metallurgical grains, and a phase called gamma prime, whose structure is based on the Ni 3 Al ordered intermetallic compound.
  • the gamma prime phase forms several populations of inter or intra-granular precipitates that appear at different stages of the thermomechanical history of the alloy and have different roles. distinct in the mechanical behavior of the alloy.
  • the intergranular precipitate population limits the growth of the gamma matrix grains during a recrystallization heat treatment.
  • the population of intergranular precipitates and thus the size of said grains is controlled.
  • the maximum temperature reached during this heat treatment is greater (treatment said supersolvus) or lower (so-called subsolvus treatment) at the dissolution temperature (or solvus temperature) of the intergranular precipitates of gamma prime phase, the recrystallization results in a high grain size (for a supersolvus treatment) or a small grain size (for a subsolvus treatment).
  • the two-phase alloys are thermomechanically treated to present either a fine grain microstructure (small grains), that is to say having a grain size of about 5 at 15 .mu.m (that is to say, indices ASTM 12 to 9, according to the "American Society for Testing and Material” standard), ie a coarse-grained microstructure, that is to say having a size of grain of the order of 20 to 180 microns (that is to say, ASTM indices 8 to 2).
  • the grain reinforcement is ensured by the presence of different populations of intra-granular precipitates of the gamma prime Ni 3 Al base phase and it is generally accepted that the tensile strength, when hot, of these alloys increases with the volume fraction of the gamma prime phase, this fraction up to 60%.
  • the N18 alloy whose volume fraction of gamma prime phase is about 55%, is mainly subjected to subsolvus treatments, because it is desired to obtain a fine-grained microstructure. Indeed, the fatigue and tensile strength of this alloy is generally preferred over its creep resistance, due to a temperature of use often less than 650 ° C, that is to say relatively moderate.
  • the purpose of the invention is to propose Ni-based alloys for which it is possible to carry out a subsolvus treatment, but also a supersolvus treatment on an industrial scale and which preferably have high temperature mechanical characteristics, in particular a creep resistance, at least equivalent, and preferably greater than that of the alloy N18.
  • the Applicant has established that the elemental composition of alloy N18 allowed, during the maintenance of temperature at more than 650 ° C for sufficiently long periods, the development of topologically compact phases, generally referred to as sigma and mu phases, which are harmful. the high temperature behavior of a disc in operation.
  • composition of the alloys of the invention is chosen so as to precipitate a limited volume fraction of gamma prime phase.
  • alloys of the invention are thus less rich than the alloy N18 gamma prime phase, they have against all expectations, in their microstructural small grain, tensile characteristics and creep resistance greater than those of this reference alloy. It also appears that these alloys exhibit fatigue cracking rates equivalent to or even lower than those of alloy N18.
  • the high resistance to tensile stresses is particularly favorable to the bursting behavior of these discs that may occur during an accidental overspeed regime. This high resistance also makes it possible to anticipate good properties in oligocyclic fatigue and adequate lifetimes.
  • the reduction, relative to the N18 alloy, of the gamma prime phase volume fraction is favorable for producing discs having a coarse-grained microstructure and therefore a high resistance to creep at high temperature (ie ie for temperatures greater than or equal to 700 ° C).
  • This creep resistance associated with very good mechanical characteristics in traction and in propagation of cracks in fatigue-creep allows the use of these discs at higher temperatures than in the current turbomachines, which allows access to better thermal efficiency and to reduce the specific consumption of turbomachines.
  • this coarse-grained microstructure is further facilitated by the comfortable temperature range between the solvus temperature of the gamma prime phase and the melting start temperature of the alloy.
  • the compositions of the alloys of the invention are such that the width of this range is greater than or equal to 35 ° C. This allows the industrial production of heat treatments beyond the solvus temperature, without the risk of burning of the alloy.
  • the ability to develop one or other of the large and small grains microstructures and the good mechanical properties corresponding to each of these two microstructures is a definite advantage of the alloys of the invention compared to those used for this purpose. day and, in particular, alloy N18.
  • this ability allows for dual structure disks. Indeed, by carrying out a heat treatment under a temperature gradient, a coarse grain structure is developed in the peripheral zone of the disk, where the temperatures in service are the highest and where creep plays a significant role in the damage of the material. , and a small-grain structure in the central zone of the disk (near the hub), colder, where the damage results essentially from the traction forces and cyclic stresses.
  • the alloys of the invention have a relatively low density, preferably less than or equal to 8. , 3 kg / dm 3 , which makes it possible to limit the mass of the disk and the stresses resulting from the centrifugal force.
  • the elemental compositions of the alloys of the invention provide them with good microstructural stability with regard to the appearance of the sigma and mu phases, which is delayed beyond 500 hours of maintenance at 750 ° C.
  • the compositions of the alloys of the invention have a limited gamma prime phase volume fraction and, preferably, less than or equal to 50%.
  • the gamma prime phase must nevertheless be in sufficient proportion, the volume fraction of gamma prime phase is preferably between 40 and 50%.
  • the sum of the contents of Al, Ti and Nb, in atomic percentages is greater than or equal to 10.5% and less than or equal to 13%, ie: 10.5% ⁇ Al + Ti + Nb ⁇ 13%.
  • the precipitation of the gamma prime phase in Ni-based alloys depends exclusively on the presence of Al in sufficient concentration
  • the elements Ti and Nb, which, by substituting for Al, constitute this phase are, like this one, considered as favorable elements for the formation of the gamma prime phase and are called gamma prime-genes.
  • the value of the volume fraction of the gamma prime phase is therefore a function of the sum of the atomic concentrations of Al, Ti and Nb.
  • tantalum (Ta) is also a gamma primegen element but that it has not been retained in the composition of the alloys of the invention. Indeed, Ta is an element of high atomic mass, which necessitates complex composition adjustments in order to maintain the density of the alloy under a reasonable limit (preferably less than or equal to 8.3 kg / dm 3 ). In addition, the cost of Ta is high and its beneficial role on crack resistance could not be clearly established. Finally, its enhancement effect of the gamma prime phase does not appear to be greater than that of the elements Ti and Nb. It has even been found that the resistance of the alloys of the invention was at least equivalent to that of the alloys containing Ta.
  • the Al, Ti and Nb contents, in atomic percentages in the alloys of the invention are such that the ratio between the sum of the contents of Ti and Nb, and the Al content, is greater than or equal to 0.9 and less than or equal to 1.1, ie: 0.9 ⁇ [(Ti + Nb) / Al] ⁇ 1.1.
  • the Al-substituted Ti and Nb atoms in the Ni 3 Al base gamma prime phase have the effect of reinforcing it by mechanisms similar to those of solid solution hardening. This hardening is even higher than the ratio [(Ti + Nb) / Al] is high.
  • the ordered phase eta Ni 3 Ti precipitates in the form of elongated platelets which have a detrimental effect on the mechanical behavior, especially on the ductility of the alloys which contain them.
  • the concentration of Nb must be limited because an excessive content of Nb is detrimental to the resistance to the propagation of cracks in this type of alloys.
  • the contents in W, Mo, Cr and Co, in atomic percentages are such that the sum of the contents in W, Mo, Cr and Co is greater than or equal to 30% and less than or equal to at 34%, and such that the sum of the contents in W and Mo is greater than or equal to 3% and less than or equal to 4.5%, namely: 30% ⁇ W + Mo + Cr + Co ⁇ 34%; and 3% ⁇ W + Mo ⁇ 4.5%.
  • the elements which essentially substitute for Ni in the gamma solid solution are Cr, Co, Mo and W.
  • Cr is essential for the resistance to oxidation and corrosion of the alloy and participates, as a solid solution, in the hardening of the gamma matrix.
  • Co improves the resistance of these alloys to creep at high temperatures.
  • the increase in Co concentration within the limits of the stability of the gamma phase structure, makes it possible to lower the solvus temperature of the gamma prime phase and thus to facilitate the implementation of heat treatments. partial or total solution of solution thereof.
  • Mo and W provide a strong hardening of the gamma matrix by the effect of solid solution.
  • these elements have high atomic masses and their substitution with Ni (in particular the substitution of W for Ni) results in a significant increase in the density of the alloy.
  • the contents of Cr, Mo, Co and W in the alloys of the invention must therefore be carefully adjusted with respect to each other to obtain the desired effects, in particular optimum curing of the gamma matrix, without thereby risking causing the premature appearance of the phases of fragile intermetallic compounds, sigma and mu. These phases, when they develop in excessive amounts, can indeed cause a significant reduction in the ductility and mechanical strength of the alloys.
  • minor elements C, B and Zr form segregations mainly at the grain boundaries, for example in the form of carbides or borides. They contribute to increase the strength and ductility of alloys by changing the chemistry of grain boundaries and their absence would be detrimental.
  • an excess content of these elements leads to a reduction of the melting temperature beginning and excessive precipitation of carbides and borides which consumes alloy elements that no longer participate in the hardening of the alloy.
  • the concentrations of carbon, boron and zirconium are therefore adjusted, in particular with non-zero minimum levels of carbon and boron, in order to obtain at high temperature optimum mechanical strength and ductility for the alloys of the invention.
  • Hf is also present in moderate amounts because this element improves resistance to intergranular hot cracking.
  • the subject of the invention is also a method for manufacturing a part, more particularly a turbomachine part such as a compressor or turbine disk, characterized in that a blank of said part is produced, or the part itself from a powder of an alloy according to the invention, by a powder metallurgy technique.
  • said blank or said part is subjected to a recrystallization heat treatment according to which the blank or part is brought, either at a temperature below the solvus temperature of the gamma prime phase of said alloy, or at a temperature of less than a temperature greater than the solvus temperature of the gamma prime phase of said alloy, and less than the melting start temperature of this alloy, so as to promote the development of a grain size microstructure adapted to the stress conditions.
  • the parts made from the alloys according to the invention are preferably manufactured by powder metallurgy techniques.
  • the rate of cooling following the dissolution treatment makes it possible to control the distribution of the intragranular precipitates of gamma prime phase.
  • One or more treatments of income make it possible to control the size of the tertiary precipitates of phase gamma prime and to relax the internal stresses which result from the quenching.
  • the alloy A is the alloy N18 and the alloy B is sold under the reference Rene-88DT.
  • a partial solution treatment of the gamma prime phase was performed at a temperature below the solvus temperature (Tsolvus) of the gamma prime phase (at about Tsolvus - 25 ° C).
  • the cooling rate was of the order of 100 ° C./min after dissolution. This treatment was followed by an income of 24 hours at 750 ° C and air cooling.
  • a treatment of total dissolution of the gamma prime phase was performed at a temperature above the solvus gamma prime (at about Tsolvus + 15 at 20 ° C).
  • the cooling rate was of the order of 140 ° C./min after the dissolution. This treatment was followed by an 8 hour income at 760 ° C and air cooling.
  • Tables III and IV are presented some results of mechanical tests carried out in tension, in creep and in crack propagation, respectively for alloys having received a subsolvus treatment (Table III) and a supersolvus treatment (Table IV).
  • the creep tests were carried out in air at 700 ° C. under an initial stress of 550 MPa (650 MPa for the C1 alloy).
  • the data t 0.2% is the holding time in hours to reach a plastic deformation of 0.2%.
  • the load cycle is as follows: load increase in 10 seconds, hold time of 300 seconds at maximum load and discharge in 10 seconds with a load ratio (minimum load / maximum load) equal to 0.05.
  • the data V f35 is the crack propagation velocity, measured at a delta K value equal to 35 MPa.m 1/2 .
  • microstructural examinations were performed on subsolvus-treated alloys A and C1 to detect the appearance of topologically compact phases (i.e., fragile intermetallic compounds) after an aging heat treatment of 500 hours at 750 ° C.
  • the observations were made by scanning electron microscopy, backscattered electron contrast, on untouched samples.
  • the severe aging of 500 hours at 750 ° C causes, in alloy A, the inter and intra-granular formation of phases rich in heavy elements. These phases appear in clear contrast (white edging) at the grain boundaries in Figure 1.
  • These phases when formed in excessive amounts, can cause a significant reduction in the ductility and mechanical strength of the alloys.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
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EP07105258A 2006-03-31 2007-03-29 Legierung auf Nickelbasis Active EP1840232B1 (de)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR0651145A FR2899240B1 (fr) 2006-03-31 2006-03-31 Alliage a base de nickel

Publications (2)

Publication Number Publication Date
EP1840232A1 true EP1840232A1 (de) 2007-10-03
EP1840232B1 EP1840232B1 (de) 2009-05-13

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US (1) US20070227630A1 (de)
EP (1) EP1840232B1 (de)
JP (1) JP5398123B2 (de)
CA (1) CA2583140C (de)
DE (1) DE602007001092D1 (de)
FR (1) FR2899240B1 (de)
RU (1) RU2433197C2 (de)

Cited By (4)

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CN104561662A (zh) * 2014-11-17 2015-04-29 江苏环亚电热仪表有限公司 一种粉末合金及其生产工艺
FR3098849A1 (fr) * 2019-07-16 2021-01-22 Safran Aircraft Engines Carter amélioré de module d’aéronef
WO2021116607A1 (fr) 2019-12-11 2021-06-17 Safran Superalliage a base de nickel
WO2023175266A1 (fr) 2022-03-17 2023-09-21 Safran Superalliage a base de nickel.

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WO2018216067A1 (ja) * 2017-05-22 2018-11-29 川崎重工業株式会社 高温部品及びその製造方法
US10577679B1 (en) 2018-12-04 2020-03-03 General Electric Company Gamma prime strengthened nickel superalloy for additive manufacturing
FR3130294B1 (fr) 2021-12-15 2025-05-16 Safran Alliage à base de nickel
FR3130292B1 (fr) 2021-12-15 2024-06-14 Safran Alliage à base de nickel exempt de cobalt
FR3130293A1 (fr) 2021-12-15 2023-06-16 Safran Alliage à base de nickel comprenant du tantale
EP4506478A4 (de) * 2022-05-02 2025-08-13 Proterial Ltd Legierung, legierungspulver, legierungselement und verbundelement
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CN117327946B (zh) * 2023-10-09 2026-01-06 中国科学院金属研究所 一种镍基铸造高温合金及其制备方法
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CN119387473B (zh) * 2024-11-08 2025-10-31 南昌航空大学 双组织钛合金叶盘的可控应变等温模锻成形模具及方法
CN119703085B (zh) * 2024-11-28 2025-09-09 西安欧中材料科技股份有限公司 一种制备高性能gh4079盘环件的方法及航空发动机用盘环件

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104561662A (zh) * 2014-11-17 2015-04-29 江苏环亚电热仪表有限公司 一种粉末合金及其生产工艺
FR3098849A1 (fr) * 2019-07-16 2021-01-22 Safran Aircraft Engines Carter amélioré de module d’aéronef
WO2021116607A1 (fr) 2019-12-11 2021-06-17 Safran Superalliage a base de nickel
FR3104613A1 (fr) 2019-12-11 2021-06-18 Safran Superalliage a base de nickel
US12180565B2 (en) 2019-12-11 2024-12-31 Safran Nickel-based superalloy
WO2023175266A1 (fr) 2022-03-17 2023-09-21 Safran Superalliage a base de nickel.
FR3133623A1 (fr) 2022-03-17 2023-09-22 Safran Superalliage à base de nickel

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FR2899240A1 (fr) 2007-10-05
JP5398123B2 (ja) 2014-01-29
JP2007277721A (ja) 2007-10-25
US20070227630A1 (en) 2007-10-04
EP1840232B1 (de) 2009-05-13
CA2583140C (fr) 2015-03-17
RU2433197C2 (ru) 2011-11-10
RU2007111861A (ru) 2008-10-10
DE602007001092D1 (de) 2009-06-25
CA2583140A1 (fr) 2007-09-30
FR2899240B1 (fr) 2008-06-27

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