WO2018221648A1 - Procédé de production d'un superalliage résistant à la chaleur à base de ni - Google Patents

Procédé de production d'un superalliage résistant à la chaleur à base de ni Download PDF

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Publication number
WO2018221648A1
WO2018221648A1 PCT/JP2018/020939 JP2018020939W WO2018221648A1 WO 2018221648 A1 WO2018221648 A1 WO 2018221648A1 JP 2018020939 W JP2018020939 W JP 2018020939W WO 2018221648 A1 WO2018221648 A1 WO 2018221648A1
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forging
phase
heating
temperature
forging material
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PCT/JP2018/020939
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English (en)
Japanese (ja)
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昂平 小林
洋一 菅
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日立金属株式会社
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Priority to JP2019521297A priority Critical patent/JP6663575B2/ja
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J1/00—Preparing metal stock or similar ancillary operations prior, during or post forging, e.g. heating or cooling
    • B21J1/02—Preliminary treatment of metal stock without particular shaping, e.g. salvaging segregated zones, forging or pressing in the rough
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J1/00—Preparing metal stock or similar ancillary operations prior, during or post forging, e.g. heating or cooling
    • B21J1/06—Heating or cooling methods or arrangements specially adapted for performing forging or pressing operations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • 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
    • 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

Definitions

  • the present invention relates to a method for producing a Ni-base superalloy using radial forging.
  • An alloy representative of Alloy 718 (hereinafter referred to as 718 alloy) is a typical Ni-based superheat-resistant alloy in which a delta phase (hereinafter referred to as ⁇ phase) precipitates in the metal structure.
  • This alloy is widely used as a member that requires high reliability in the aircraft and energy fields.
  • the ⁇ phase uses the pinning effect to make the crystal grain size of the alloy finer, and various proposals for making the ⁇ phase appropriate have been made.
  • Patent Document 1 a hot forging material composed of a Ni-based alloy containing Nb is subjected to a heat treatment at a temperature of 915 ⁇ 10 ° C.
  • a step of precipitating in the parent phase a step of finishing forging at a forging ratio of 2 or higher at a temperature of 900 ° C. or less to the treated material to obtain a forging material in which the cut pieces of the ⁇ phase are dispersed in the mother phase;
  • There is an invention of a method for producing a Ni-based alloy material comprising a step of performing a solution treatment on a forged material.
  • Patent Document 2 describes Ni: 50 to 55%, Cr: 17 to 21%, Al: 0.2 to 0.8%, Ti: 0.6 by mass%. -1.2%, Nb: 4.7-5.6%, Mo: 2.8-3.3%, Co: ⁇ 1.0%, C + Si + Mn + P + S + Cu + B: ⁇ 1.1%, balance Fe
  • a free forging method of a Ni-base heat-resistant alloy member that obtains a Ni-base heat-resistant alloy member having crystal grains refined by performing the following steps on a forged material made of a Ni-base heat-resistant alloy.
  • the to-be-forged material is subjected to a ⁇ -phase precipitation treatment for precipitating the ⁇ -phase in a needle shape, and then the to-be-formed material to which the ⁇ -phase precipitation has been performed is heated at 920 to less than 1025 ° C. for 1 to 36 hours. Then, the precipitated needle-like ⁇ phase is partially solid-solved with separation, and an initial amount adjustment treatment of the ⁇ phase for adjusting the amount of precipitation of the ⁇ phase is performed.
  • a finishing forging process is performed in which free forging and reheating are performed at least once in a stroke at a total rolling reduction of 33% or more.
  • a product using a material obtained by radially forging 718 alloy has a problem that it is difficult to obtain desired mechanical characteristics, and the 0.2% yield strength may be particularly low.
  • the cause was investigated, it was found that the amount of ⁇ phase precipitation and the crystal structure had an effect on the 0.2% proof stress.
  • the manufacturing conditions such as heat treatment are strictly controlled and restricted in applications in the energy field such as aircraft components and turbines where 718 alloy is used, so the optimum metal structure of the forged material that is the material before heat treatment Need to be done.
  • Patent Document 2 the initial amount adjustment process of the ⁇ phase for adjusting the precipitation amount of the ⁇ phase is performed, and further, free forging and reheating are repeated one or more times, but the solution treatment (1050 ° C. to 1120 ° C. ) - ⁇ phase precipitation treatment (800-1200 ° C.)-Initial treatment for adjusting the initial amount of ⁇ phase (920-1025 ° C.) is performed before free forging.
  • the object of the present invention is to produce a Ni-base superalloy having a fine grain structure capable of obtaining a high 0.2% proof stress by one heat treatment using radial forging and one heat forging. Is to provide a method.
  • the present invention has been made in view of the above-described problems. That is, the present invention includes a forging material heating step of heating a forging material made of a Ni-base superheat-resistant alloy to a temperature equal to or higher than the ⁇ -phase solid solution temperature of the Ni-base superheat-resistant alloy; The forging is repeated at a temperature of 880 ° C. or more, and the forging is repeated by rotating the forging material in the circumferential direction and pressing the entire length for extending the entire length.
  • This is a Ni-based superalloy manufacturing method including a hot forging process in which forging is completed in one heat by radial forging.
  • the heating temperature in the forging material heating step is 1010 to 1050 ° C. More preferably, it is a method for producing a Ni-base superalloy having a visual field area ratio of the ⁇ phase found in the metal structure after forging in a visual field of 10,000 ⁇ m 2 of 0.8 to 1.5%.
  • Ni-based superalloy capable of forming fine crystal grains capable of obtaining a high 0.2% proof stress by one-heat forging using radial forging.
  • productivity can be improved by applying radial forging capable of high-speed forging (forging and forging).
  • the ⁇ phase is dissolved as much as possible in the forging material heating step described later.
  • the temperature at which the fine ⁇ phase is precipitated is selected, and the amount of fine ⁇ phase that is found in the hot forged material obtained in the hot forging process is thereby determined. make low.
  • the growth of the ⁇ phase is suppressed, and only the fine ⁇ phase is precipitated to reduce the amount of precipitation.
  • the fine ⁇ phase can be expected to promote the nucleation of recrystallized grains because it becomes a transition starting point.
  • the heat treatment at the time of die forging into a product shape performed thereafter causes a fine ⁇ phase to precipitate at the crystal grain boundary and increase the starting point for recrystallization at the grain boundary.
  • the crystal grains of the final product can be refined. Therefore, the application of the manufacturing method of the Ni-base superalloy according to the present invention can be applied to products having a heat history in which the heating temperature of the die forging after the hot forging process, which will be described later, and the solution heat treatment is less than the ⁇ phase solution temperature. Application is preferred. The present invention is described in detail below.
  • the “Ni-based super heat-resistant alloy” referred to in the present invention is a precipitation strengthening type alloy containing Ni of 50% by mass or more and containing an appropriate amount of Nb or the like of a ⁇ phase generating element.
  • the forging material for example, a prismatic or columnar material suitable for radial forging may be prepared.
  • the composition of a typical Ni-based superalloy used in the present invention is known as Inconel (R) 718 alloy (Inconel is a registered trademark of Special Metal Corporation).
  • C 0.08% or less
  • Si 0.35% or less
  • Mn 0.35% or less
  • P 0.015% or less
  • S 0.015% or less
  • Ni 50.0 to 55.0%
  • Cr 17.0 to 21.0%
  • Mo 2.8 to 3.3%
  • Cu 0.30% or less
  • Al 0.20 to 0.80%
  • Ti 0.65 to 1.15%
  • Nb + Ta 4.
  • alloy having a composition of 75 to 5.50%, B: 0.006% or less, and the balance of Fe and inevitable impurities.
  • This Ni-based superalloy is made by vacuum melting to produce a consumable electrode, and the consumable electrode is used to remelt the vacuum to form an ingot, which is then formed into a forging material by hot plastic working such as hot forging or hot pressing. To do. If necessary, for example, the consumable electrode or ingot may be subjected to a homogenization heat treatment at 1100 ° C. or higher.
  • the conditions for forming and hot working on the forging material can be used in a conventional manner, but the crystal grain size of the forging material is adjusted to, for example, 4.0 to 8.0 by ASTM grain size number. It is preferable to keep it.
  • the above forging material is heated to a temperature equal to or higher than the ⁇ phase solid solution temperature of the Ni-base superalloy (the first pre-forging heating in FIG. 1 may be referred to as a forging material heating step).
  • the heating temperature of the forging material heating process is set to be higher than the ⁇ phase solid solution temperature of the Ni-base superalloy.
  • the ⁇ phase is dissolved before forging and the fine ⁇ phase is forged after forging. This is for precipitating.
  • a preferable temperature range of the forging material heating step is 1010 to 1050 ° C.
  • the heating temperature in the forging material heating process for the forging material is less than 1010 ° C.
  • the ⁇ phase precipitated during forming of the forging material using a press or the like does not sufficiently dissolve, becomes coarse, and becomes fine ⁇ A phase may not be obtained.
  • the heating temperature in the forging material heating step exceeds 1050 ° C.
  • the crystal structure of the forging material becomes coarse, and it becomes difficult to obtain a fine structure after radial forging. Therefore, the heating temperature of the preferable forging material heating step for the forging material is set to 1010 to 1050 ° C. By setting the temperature of the forging material to 1010 ° C.
  • the ⁇ phase can be surely dissolved once, and the fine ⁇ phase can be precipitated in the subsequent forging process. It will be easier to achieve this.
  • the upper limit of the heating temperature of a preferable forging raw material heating process is 1030 degreeC.
  • the heating time is not particularly limited, but approximately 1.0 to 6.0 hours is sufficient.
  • radial forging is used. While radial forging has the advantage that it can be forged at high speed, it is difficult to apply strain near the center of the diameter of the forged material. Therefore, when producing a forging material, it is preferable to apply a strain in advance to a location that becomes the center of the diameter of the forged material by hot pressing or the like. For this purpose, for example, it is preferable that the hot pressing temperature is set to 1010 to 1050 ° C. and the forging ratio is 0.6 to 1.2. Further, before starting forging in the hot forging process described later, a glass lubricant may be coated for the purpose of suppressing the temperature drop of the forging material, and the temperature may be raised to the above heating temperature. The coated glass lubricant functions as a temperature decrease suppressing layer, and can suppress the temperature decrease of the forging material until the first pass is completed.
  • ⁇ Hot forging process> forging of the heated forging material from four directions is started.
  • the forging ratio per pass in intermittent pressing from one end to the other is set to 1.05 to 1.25, and this is preferably repeated for 6 to 10 passes.
  • radial forging is applied in which the forging material is pressed from four directions and rotated in the circumferential direction, and the operation of extending the entire length is repeated by pressing over the entire length.
  • Radial forging is applied by stretching the forging material in the longitudinal direction while pressing the forging material at a high speed and pressing in four directions, so that the crystal structure in the circumferential direction and the amount of ⁇ phase precipitates.
  • Ni-base heat-resistant alloy members are often used in rotating parts of aircraft engine parts, it is desirable that the mechanical properties be uniform in the circumferential direction. Therefore, the above-mentioned radial forging is preferable.
  • forging can be completed with one heat.
  • “1 heat” means that the hot forging process is not interrupted and the forging material is not reheated.
  • the forging end temperature is set to 880 ° C. or higher. This is because if the temperature is lower than 880 ° C., the hot forged material may break.
  • the ⁇ phase found in the metal structure of the hot forged material after forging is 0.8 to 1.5 at a field area ratio of 10,000 ⁇ m 2 so that the 0.2% proof stress can be increased. % Is preferable.
  • the field area ratio of 10,000 ⁇ m 2 is set to 0.8 to 1.5% because fine heating is performed in this range by performing pre-forging heating (heating before second forging in FIG. 1) —finish forging. This is because a crystal structure can be obtained. If the ⁇ phase found in the visual field area of 10000 ⁇ m 2 is less than 0.8%, the pinning effect of the ⁇ phase does not work during the heating before the second forging, and the crystal grains may become coarse.
  • the ⁇ phase found in the field area of 10,000 ⁇ m 2 exceeds 1.5%, the fine ⁇ phase may not precipitate at the grain boundaries during the heating before the second forging.
  • a preferable lower limit of the visual field area ratio of the ⁇ phase is 0.9%, and a preferable upper limit of the visual field area ratio of the ⁇ phase is 1.3%.
  • the ⁇ phase may be measured and observed using a scanning electron microscope (SEM). Further, the viewing area of measuring the viewing area ratio in the present invention was 10000 2 is excessively can cause field area results in a slight variation in the narrow and the measurement results, whereas, excessively wide viewing area than 10000 2 Even so, there is no significant change in the measurement results.
  • the test piece to be measured is taken from the position of D / 4 (1/4 of the diameter D) of the hot forging material, and measurement is performed from a cross section along the longitudinal direction.
  • the crystal grains can be refined by applying die forging to the final product shape and subsequent solution heat treatment.
  • it is most suitable for application to a product having a thermal history below the ⁇ phase solid solution temperature. If the temperature is raised above the ⁇ phase solution temperature by die forging or solution heat treatment, the amount and size of the ⁇ phase of the hot forged material will change, and there is a risk that crystal grain refinement cannot be obtained. is there.
  • the forging materials of the present invention example (forging material A) and the comparative example (forging material B), which were the same up to the step of obtaining the forging material were prepared.
  • the prepared forging material is a Ni-based super heat-resistant alloy having a composition equivalent to 718 alloy, an ingot to which vacuum melting and vacuum remelting are applied, and an octagon having a cross section of 220 mm diagonally by hot forging. Is a columnar forging material having a length of 1500 mm.
  • the crystal grain of the forging material was ASTM grain size number of about 5.0.
  • the ⁇ phase solid solution temperature corresponding to 718 alloy is approximately 1010 ° C.
  • This forging material was forged to a cross-sectional diameter of 130 mm.
  • For the forging material A a radial forging machine capable of forging with one heat was used. The forging ratio per pass during the forging process was 1.09 to 1.21 during confirmation, and finished in 8 passes.
  • For the forging material B a normal hot forging device forging from two directions requiring a plurality of heat numbers was used.
  • FIG. 1 shows a process outline diagram, and Table 1 shows a heating temperature, a forging start temperature, a forging end temperature, and the number of heats in the forging material heating process.
  • the visual field area ratio of 10000 ⁇ m 2 in the ⁇ phase after the hot forging process is also shown. The method for measuring the visual field area ratio was performed under the conditions described above.
  • FIG.2 and FIG.3 shows the structure
  • the visual field area ratio of the ⁇ phase is in the range of 0.8 to 1.5%.
  • the comparative example is 3.71%, and it can be seen that the amount of precipitation of ⁇ phase is small in the present invention.
  • the crystal grains were about 8.0 in terms of ASTM grain size number.
  • the average diameter of the ⁇ phase was as fine as 1.0 ⁇ m or less.
  • the number of ⁇ phases per visual field area is 146 to 204 in the example of the present invention of 1.0 ⁇ m or less, and 48 to 62 in the example of more than 1.0 ⁇ m, and the number of ⁇ phases of 1 ⁇ m or less is approximately 250. The number below 1 and over 1 ⁇ m was approximately 70 or less.
  • the number of ⁇ phases of 1.0 ⁇ m or less is 294 to 352, the number of ⁇ phases exceeding 1.0 ⁇ m is 156 to 197, the number of ⁇ phases themselves is large, and 1 ⁇ m
  • the excess ⁇ phase was about twice or more. Thereafter, die forging heating (heating before second forging) was performed at 980 ° C.
  • the structure was observed for some parts without forging. 4 and 5 show the structure after die forging heating (heating before second forging).
  • a fine ⁇ phase having a diameter of 1.0 ⁇ m or less was precipitated at the grain boundary.
  • the precipitation state of the ⁇ phase was hardly changed from that before the heating, and the ⁇ phase having a diameter of 1.5 to 2.0 ⁇ m remained as it was.
  • Die forging (finish forging) and solution heat treatment were performed using the hot forging material that had been subjected to die forging heating (heating before second forging).
  • Table 2 shows the heating temperature, forging temperature, and solution treatment temperature during die forging.
  • FIG. 6 shows the organization state. As shown in FIG. 6, it can be seen that those using the forging material A of the present invention have fine crystal grains.
  • the 0.2% proof stress was measured according to JIS Z2441.
  • 0.2% proof stress measurement required specimens were collected from those subjected to 12 die forgings and solution heat treatments shown in Table 2 and subjected to aging heat treatment. Thereafter, the variation was examined by a tensile test.
  • the Ni-based super heat-resistant alloy manufacturing method of the present invention applied the 0.2% proof stress of 1178 MPa or more and the variation was within standard deviation ⁇ 18. The lowest value was 1040 MPa, the variation was the standard deviation ⁇ 31, and the characteristics varied greatly.
  • fine crystal grains capable of obtaining a high 0.2% proof stress can be obtained by one-heat forging using radial forging. Moreover, productivity can be improved by applying radial forging capable of high-speed forging (forging and forging).

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  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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Abstract

L'invention concerne un procédé de production d'un superalliage résistant à la chaleur à base de Ni qui peut être à grain fin et qui permet d'obtenir une limite conventionnelle d'élasticité à 0,2 % élevée dans un forgeage par étirage à chaud à 1 traitement thermique à l'aide d'un forgeage radial. Le procédé de production d'un superalliage résistant à la chaleur à base de Ni comprend : une étape de chauffage de matériau de forgeage par étirage permettant de chauffer un matériau de forgeage par étirage composé d'un superalliage résistant à la chaleur à base de Ni jusqu'à au moins la température de solubilité de la phase δ du superalliage résistant à la chaleur à base de Ni ; et une étape de forgeage par étirage à chaud dans laquelle le forgeage par étirage du matériau de forgeage par étirage est terminé à une température supérieure ou égale à 880 °C, le forgeage par étirage étant terminé en 1 traitement thermique par forgeage radial dans lequel une opération de pressage du matériau de forgeage par étirage sur toute la longueur de celui-ci pour étendre toute la longueur de celui-ci est répétée tout en faisant tourner le matériau de forgeage par étirage dans la direction circonférentielle.
PCT/JP2018/020939 2017-05-31 2018-05-31 Procédé de production d'un superalliage résistant à la chaleur à base de ni WO2018221648A1 (fr)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110331352A (zh) * 2019-08-20 2019-10-15 太原钢铁(集团)有限公司 一种控制镍基合金碳化物分布的径锻方法
CN114632901A (zh) * 2022-03-18 2022-06-17 西安聚能高温合金材料科技有限公司 一种超超临界火电机组用高温合金自由锻棒坯制备方法
CN115161502A (zh) * 2022-07-14 2022-10-11 江苏以豪合金有限公司 一种电热元件用镍基高电阻电热合金丝的制备工艺

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11342443A (ja) * 1998-05-29 1999-12-14 Daido Steel Co Ltd ニッケル基耐熱合金の加工方法
JP6079294B2 (ja) * 2013-02-22 2017-02-15 大同特殊鋼株式会社 Ｎｉ基耐熱合金部材の自由鍛造加工方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11342443A (ja) * 1998-05-29 1999-12-14 Daido Steel Co Ltd ニッケル基耐熱合金の加工方法
JP6079294B2 (ja) * 2013-02-22 2017-02-15 大同特殊鋼株式会社 Ｎｉ基耐熱合金部材の自由鍛造加工方法

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110331352A (zh) * 2019-08-20 2019-10-15 太原钢铁(集团)有限公司 一种控制镍基合金碳化物分布的径锻方法
CN114632901A (zh) * 2022-03-18 2022-06-17 西安聚能高温合金材料科技有限公司 一种超超临界火电机组用高温合金自由锻棒坯制备方法
CN114632901B (zh) * 2022-03-18 2024-05-17 西安聚能高温合金材料科技有限公司 一种超超临界火电机组用高温合金自由锻棒坯制备方法
CN115161502A (zh) * 2022-07-14 2022-10-11 江苏以豪合金有限公司 一种电热元件用镍基高电阻电热合金丝的制备工艺

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