EP3117017B1 - Alliage à base nickel à durcissement structural, pièce en cet alliage et son procédé de fabrication - Google Patents

Alliage à base nickel à durcissement structural, pièce en cet alliage et son procédé de fabrication Download PDF

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Publication number
EP3117017B1
EP3117017B1 EP15709520.9A EP15709520A EP3117017B1 EP 3117017 B1 EP3117017 B1 EP 3117017B1 EP 15709520 A EP15709520 A EP 15709520A EP 3117017 B1 EP3117017 B1 EP 3117017B1
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Prior art keywords
alloy
trace amounts
temperature
phase
traces
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German (de)
English (en)
French (fr)
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EP3117017A1 (fr
Inventor
Coraline CROZET
Alexandre Devaux
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Aubert and Duval SA
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Aubert and Duval SA
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/02—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling heavy work, e.g. ingots, slabs, blooms, or billets, in which the cross-sectional form is unimportant ; Rolling combined with forging or pressing
    • B21B1/026—Rolling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D7/00—Casting ingots, e.g. from ferrous metals
    • B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
    • 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
    • C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
    • 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
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper

Definitions

  • the invention relates to alloys based on nickel (superalloys), and more precisely those intended for the manufacture of parts to be used at high temperatures. Typically, this is the case of the elements of terrestrial, aeronautical and other turbines.
  • NiCo20Cr20MoTi alloy (AFNOR standard) known as "C263” is known whose composition is typically Ni, Cr (19-21%), Co (19-21%), Mo (5,6- 6.1%), Ti (1.9-2.4%), Al ( ⁇ 0.6%). The percentages are percentages by weight, as will be the case for all the compositions indicated thereafter.
  • the alloy known as INCO 617 Ni, Cr (20-24%), Co (10-15%), Mo (8-10%), Al (0.8-1.5%), Ti (0-0.6 %)
  • INCO 617 Ni, Cr (20-24%), Co (10-15%), Mo (8-10%), Al (0.8-1.5%), Ti (0-0.6 %)
  • the alloy known as RENE 41 Ni, Cr (18-20%), Co (10-12%), Mo (9-10.5%), Al (1.4-1.6%) , Ti (3-3.3%)
  • RENE 41 Ni, Cr (18-20%), Co (10-12%), Mo (9-10.5%), Al (1.4-1.6%) , Ti (3-3.3%)
  • WASPALOY Ni, Cr (18-21%), Co (12-15%), Mo (3.5-5%), Al (1.2-1.6%), Ti (2.75-3.25%).
  • JP 61-235529 discloses an alloy for a continuous casting machine support roll, having a high resistance to heat and oxidation. It contains 14-25% Cr; 5-25% Co; 0.1-7% of W; 0.1-3% Ti; 0.1-3% Al with Ti + Al ⁇ 4%; ⁇ 0.01% of O; ⁇ 0.03% of N; ⁇ 0.06% C; ⁇ 1.0% Mn; ⁇ 0.5% Si; ⁇ 0.03% of P; ⁇ 0.03% of S; the rest being Ni.
  • Ni base alloys for high temperature applications typically 700-900 ° C having both a good microstructural stability at the temperatures of use, good mechanical properties at these same temperatures , and simultaneously a good forgeability and good weldability allowing the manufacture of said parts in the desired configurations and their integration in the devices for which they are intended.
  • ⁇ 'phase fraction is preferably between 5 and 20%.
  • the solvus temperature of its ⁇ 'phase is preferably less than or equal to 980 ° C.
  • the subject of the invention is also a process for manufacturing a nickel-based alloy part, characterized in that an ingot having the previously defined composition is prepared and homogenized at a temperature of at least 1150 ° C. for 24 to 72 hours, it is hot worked by forging or rolling in a supersolvus temperature range, it is dissolved at a temperature of 1100 to 1200 ° C for 1 to 4 hours, it is cooled to at least 1 ° C / min, for example in water, is aged at a temperature of 750 to 850 ° C for 7 to 10 hours, and is cooled, for example in calm air, or in an enclosure.
  • the invention also relates to a turbine element land or aeronautical alloy nickel-based, characterized in that it was prepared according to the above method.
  • a first condition for optimizing the equilibrium between Al and Ti is that the phase formation ⁇ is avoided at the temperatures of use of the alloy during its preferred uses, that is to say at temperatures of 700-900 ° C, typically of the order of 750 ° C.
  • the formation of the ⁇ phase is directly related to the Ti and Al contents present in the alloy and to their ratio. It is thus necessary to determine the ranges of contents in these elements which make it possible to avoid it with 700-900 ° C, considering the remainder of the composition of the alloy.
  • the forging is carried out in a temperature range where there is no ⁇ 'phase precipitation which would make the metal too hard and subject to the appearance of defects, such as cracks, during deformations. It is therefore performed at a temperature above the solvus temperature of this phase. This temperature is therefore advantageous not to be too high, for a forging is possible in industrial conditions. More precisely, the solvus temperature of the ⁇ 'phase must be as low as possible in order to avoid the precipitation of this phase during the inevitable cooling of the product during the forging.
  • the Cr content is between 18 and 22%, preferably 18 to 20%. Cr is important to ensure resistance to corrosion and oxidation, and to establish the resistance of the alloy to the effects of the environment at high temperatures. An excessively high content favors the obtaining of undesirable fragile phases, such as the ⁇ phase, and the limit of 22% by weight is set accordingly.
  • the content of Co is between 18 and 22%, preferably 19 to 21%.
  • a high Co content is necessary in order to improve the forgeability of the grade by decreasing the solvus temperature of the ⁇ 'phase, however, it must be limited, mainly, for cost reasons.
  • the sum of the contents in Mo and W must be between 4 and 8%, preferably 5.5 to 7.5%. These two elements are substitutable for each other.
  • the lower limit of 4% guarantees structural hardening and good creep resistance, and the upper limit of 8% prevents the formation of harmful phases.
  • the Zr content is between traces (in other words, a lack of voluntary addition, the residual content of possible Zr resulting only from the melting of the raw materials and the elaboration, with the associated impurities) and 0.06%. .
  • the content of B is between traces and 0.03%, preferably 0.003 to 0.01%.
  • the content of C is between traces and 0.1%, preferably 0.04 to 0.06%.
  • the Fe content is limited to 1% maximum. Beyond, it may form phases harmful to the properties of the alloy.
  • Nb and Ta are both limited to 0.01% maximum. These elements are expensive and have a strong tendency to segregate without these segregations having advantages that could offset their disadvantages (contrary to what can happen for Zr, B and C).
  • S, P, Mn and Si must also be limited so as not to reduce the hot ductility.
  • An excess of Si would also cause a precipitation of Laves phases during solidification, and it will be difficult to put them back in solution during subsequent heat treatments. Resilience would be degraded.
  • an ingot having the above composition is prepared by double or triple melting, thus involving at least one of the ESR and VAR processes, and homogenized at a temperature of at least 1150.
  • it is hot-worked by forging or rolling in a supersolvus temperature range, dissolved at a temperature of 1100 to 1200 ° C for 1 to 4 hours, cooled rapidly to room temperature. minus 1 ° C / min, for example in water, it is aged at 750 to 850 ° C for 7 to 10 hours, and is cooled, for example in calm air, or in an enclosure.
  • variations can be made to this process, by not performing some of these steps or by adding others. They can be followed in particular by machining or any other operation of final dimensioning of the part.
  • Table 1 Compositions of the samples tested Ech. Or% Cr% Co% Mo% W% B% C% % Zr al% Ti% O ppm N ppm (1) (2) (3) (4) AT 51,60 19.71 20.15 5.98 traces 0.005 0,051 0.02 0.77 1.50 3.5 17 1.06 2.57 0.45 2.66 B 47.50 20.86 20.49 5.96 1.43 0,010 0,050 0.02 1.95 1.13 3.1 18 0.58 3.31 0.17 4.06 C 51,00 19.79 20,12 6.13 traces 0,010 0,050 0.01 2.64 0.22 3.4 15 0.08 2.90 0.41 4.18 D 51.50 19.74 20.00 6.20 traces traces 0,052 0.01 0.42 2.24 3.1 22 5.33 3.11 0.24 2.87 E 50,40 19.60 20.00 5.97 traces 0,002 0.049 0,003 3.00 0.252 3 16 0.08 3.30 0.30 4.75 F 48,20 19.52 20.60 4.22 3.48 0,
  • Samples A, B and C correspond to the invention, the other samples are reference alloys which do not comply with at least one of the conditions (1) to (4) previously defined because of their Al and Ti contents.
  • Sample B corresponds to the version of the invention considered optimal, where the contents of all the elements are in the preferred ranges.
  • the reference sample D corresponds to a conventional C263 type alloy which does not respect the relation (1).
  • Sample E and sample F do not respect relationship (3).
  • Sample G does not respect relationships (3) and (4).
  • Sample H does not respect relationship (2). This shows that the respect of all relations (1) to (4) is necessary to obtain the desired results.
  • the samples tested were made by VIM-VAR double melting (that is, as is conventional, by melting the raw materials in a vacuum induction furnace, followed by casting and solidification of an electrode, the latter being refined by vacuum reflow in an arc furnace), to obtain ingots of 200 kg.
  • This method is commonly used for the manufacture of ingots for forming forged or laminated parts of high purity inclusionary and low levels of residual elements, especially gaseous. It is however not necessarily used to develop the alloys of the invention, if they are intended for the production of parts that do not have very high requirements on these points. In these cases, less complex conventional methods of preparation can be used, provided that they make it possible to reach the necessary low levels on certain residual elements, in particular by a suitable choice of raw materials.
  • This heat treatment is typical of the C263 alloy for its usual applications such as turbine elements.
  • the THERMOCALC software does not provide any phase appearance ⁇ for these samples in their treatment conditions, except for sample D.
  • micrographs were made on portions of said samples which had undergone overaging at 750 ° C for 3000 h to simulate a use of the corresponding alloys at high temperature.
  • Field electron microscopy micrographs are shown on the figures 1 (sample D), 2 (sample A), 3 (sample B), 4 (sample C), 5 (sample E), 6 (sample F), 7 (sample G) and 8 (sample H).
  • sample D representative of a conventional C263 alloy
  • the figure 9 shows the results of mechanical tensile tests on these same samples for the measurement of Rm, carried out between ambient and 800 ° C.
  • the figure 10 shows the measurement results of Rp 0.2
  • the figure 11 shows the results of measurement of elongation at break A%
  • the figure 12 shows the results of Z% necking tests carried out under the same conditions.
  • alloys B and C according to the invention have tensile results (Rm and Rp 0.2 ) similar to those of the reference alloy D.
  • the tensile results of the alloy A according to FIG. The invention is slightly degraded with respect to those of alloy D but remains satisfactory.
  • the hot ductility of alloy A is the best of all, which can be a benefit for some uses. The invention therefore makes it possible to optimally optimize or preserve all of these mechanical properties with respect to the reference alloy C263.
  • Alloys E, F and G have very good results in traction, especially hot. But their loss of hot ductility is very important, which can be attributed to a poor balancing of the contents of Al and Ti.
  • the figure 13 shows the results of breaking creep tests at 750 ° C: the breaking stress in MPa is given according to the Larson-Miller parameter (PLM) as is conventional to proceed.
  • PLM Larson-Miller parameter
  • the alloys A, B, C according to the invention, and the reference alloys F and G have longer rupture times than that of the reference alloy D. This shows that, from this point of view too, the invention provides an improvement in the performance of the alloy D which is closest thereto.
  • the alloy E has a short life because of its insufficient hot ductility, and the tests could not be prolonged beyond a PLM of 23.4. Alloy H is, again, very clearly unsatisfactory.
  • the figure 14 shows the results of resilience tests conducted on several test specimens of the alloys A according to the invention and D of reference, firstly after treatment heat treatment solution and then aging as described above, secondly after over-aging of 3000 h at 750 ° C following the previous heat treatment, again to simulate the evolution of the alloy in use.
  • the results are clear: the resilience Kv is practically unaffected by the over-aging of the sample A, whereas it drops very substantially for the sample D. This confirms that the phase ⁇ formed during a high use
  • the temperature of the conventional C263 alloy has a strong embrittling effect, and the invention overcomes this problem.
  • the figure 15 shows the alloy A being forged at about 1100 ° C and no crack is actually visible.
  • the figure 16 shows the alloy E being forged at the same temperature, and slight cracks are visible.
  • the figure 17 shows the F alloy being forged at the same temperature, and the cracks are much deeper than in the previous cases.
  • the figure 18 shows the G alloy being forged at the same temperature, and again deep coves are visible. The good forgeability of the alloys according to the invention is thus confirmed, and is attributed to a lower proportion of ⁇ 'phase than for the reference samples E, F and G.
  • a preferred application of the invention is the manufacture of terrestrial and aeronautical turbine elements, but it is, of course, not exclusive.
EP15709520.9A 2014-03-14 2015-03-13 Alliage à base nickel à durcissement structural, pièce en cet alliage et son procédé de fabrication Active EP3117017B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL15709520T PL3117017T3 (pl) 2014-03-14 2015-03-13 Stop na bazie niklu o utwardzeniu dyspersyjnym, element z tego stopu i sposób jego wytwarzania

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1452157A FR3018525B1 (fr) 2014-03-14 2014-03-14 Alliage a base nickel a durcissement structural, piece en cet alliage et son procede de fabrication.
PCT/EP2015/055346 WO2015136094A1 (fr) 2014-03-14 2015-03-13 Alliage à base nickel à durcissement structural, pièce en cet alliage et son procédé de fabrication

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EP3117017A1 EP3117017A1 (fr) 2017-01-18
EP3117017B1 true EP3117017B1 (fr) 2019-05-08

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US (1) US20170002449A1 (zh)
EP (1) EP3117017B1 (zh)
JP (1) JP2017514998A (zh)
CN (1) CN106133161A (zh)
BR (1) BR112016021062A2 (zh)
CA (1) CA2942604A1 (zh)
FR (1) FR3018525B1 (zh)
PL (1) PL3117017T3 (zh)
RU (1) RU2016136763A (zh)
WO (1) WO2015136094A1 (zh)

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RU2685908C1 (ru) * 2018-09-20 2019-04-23 Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" (ФГУП "ВИАМ") Жаропрочный литейный сплав на основе никеля и изделие, выполненное из него
CN109967674B (zh) * 2019-03-22 2020-12-08 上海电气上重铸锻有限公司 核电蒸汽发生器用高温合金锻件的制造方法
WO2020195049A1 (ja) * 2019-03-26 2020-10-01 日立金属株式会社 Ｎｉ基超耐熱合金の製造方法およびＮｉ基超耐熱合金
CN110616354B (zh) * 2019-11-12 2022-03-04 湖南人文科技学院 一种用于激光近净成形的镍基高温合金粉末及其制备方法与应用
KR20220115419A (ko) * 2021-02-10 2022-08-17 창원대학교 산학협력단 대형 초내열합금 잉곳의 단조 특성 향상을 위한 균질화 열처리 방법
CN117340173B (zh) * 2023-12-06 2024-03-08 成都先进金属材料产业技术研究院股份有限公司 抑制镍铜合金锻造过程中开裂的方法

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JPS61235529A (ja) * 1985-04-10 1986-10-20 Hitachi Zosen Corp 連続鋳造設備に使用するロ−ル材料
JP3132602B2 (ja) * 1991-09-28 2001-02-05 大同特殊鋼株式会社 摩擦圧接バルブの製造方法
WO2011071054A1 (ja) * 2009-12-10 2011-06-16 住友金属工業株式会社 オーステナイト系耐熱合金
JP5899806B2 (ja) * 2011-10-31 2016-04-06 新日鐵住金株式会社 Ｈａｚにおける耐液化割れ性に優れたオーステナイト系耐熱合金
EP2860272B1 (en) * 2012-06-07 2017-10-04 Nippon Steel & Sumitomo Metal Corporation Ni-BASED ALLOY

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Publication number Publication date
US20170002449A1 (en) 2017-01-05
RU2016136763A3 (zh) 2018-10-24
BR112016021062A2 (pt) 2017-08-15
FR3018525B1 (fr) 2017-05-26
RU2016136763A (ru) 2018-03-16
CA2942604A1 (fr) 2015-09-17
PL3117017T3 (pl) 2019-11-29
CN106133161A (zh) 2016-11-16
EP3117017A1 (fr) 2017-01-18
WO2015136094A1 (fr) 2015-09-17
JP2017514998A (ja) 2017-06-08
FR3018525A1 (fr) 2015-09-18

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