US3660177A - Processing of nickel-base alloys for improved fatigue properties - Google Patents

Processing of nickel-base alloys for improved fatigue properties Download PDF

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US3660177A
US3660177A US38227A US3660177DA US3660177A US 3660177 A US3660177 A US 3660177A US 38227 A US38227 A US 38227A US 3660177D A US3660177D A US 3660177DA US 3660177 A US3660177 A US 3660177A
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alloy
eta
precipitate
temperature
phase
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Edgar E Brown
Raymond C Boettner
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Raytheon Technologies Corp
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United Aircraft Corp
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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 fatigue p base alloys such as lnconel 718, lncoloy 901 and Waspaloy, are significantly improved by a thermomechanical processing .143 L5 R, 48/115 F 43/123 technique involving the generation of an intermetallic pinning 22 1/10 phase, such as a spheriodal eta phase or an overaged gamma 148/115 R H 5 F 12 7 prime phase, with subsequent recrystallization to provide a uniform microstructure having a grain size of ASTM 10-1 3 or finer.
  • the present invention relates in general to the nickel-base alloys and, more particularly, to a novel fabrication process therefor to provide improved physical properties including increased fatigue resistance.
  • nickel-base alloys of the type typified by lnconel 718, lncoloy 901 and Waspaloy representative chemistries for these alloys being as follows:
  • This invention contemplates the processing of certain precipitation hardened nickel-base alloys to provide improved fatigue resistance thereto. It is applicable to those nickel-base alloys precipitating intermetallic compounds, such as an eta (Ni cb, Ni Til or overaged gamma prime (Ni Al, Ti), which are stable above the alloy recrystallization temperature and which may be produced in the microstructure below the alloy recrystallization temperature. These are hereinafter collectively referred to as pinning phases.
  • the alloys are thermodynamically processed to provide a uniform dispersion of a fine pinning phase and subsequently recrystallized.
  • the uniform dispersion of the pinning phase may be provided in a number of ways including: cold or warm working the alloy and subsequently heat treating the as-worked structure to precipitate a spheroidal eta or overaged gamma prime phase; warm working at a temperature sufficient to induce precipitation of the pinning phase during deformation; or establishment of a conventional needle-like eta phase and subsequent thermomechanical processing to effect a conversion to the desired pinning phase such as the line spheroidal eta.
  • the alloy is first subjected to heat treatments to minimize alloy heterogeneity and to precipitate the conventional needle-like eta; then warm worked to effect a conversion of the eta to a uniform fine dispersion of the desired spheroidal eta; and subsequently recrystallized to form a microstructure having a grain size of ASTM 10-13 or finer.
  • the conventional aging heat treatments are thereafter applied for strengthening purposes.
  • FIG. 1 is a photomicrograph of conventionally processed 1nconel 718 bar stock revealing a comparatively coarse grain size (ASTM 4-5) with the absence of any significant amount of the eta phase. l50 before reduction).
  • FIG. 2 is a photomicrograph of an lnconel 718 pancake processed according to the present invention and illustrating a fine grain size (ASTM 12). (250Xbefore reduction).
  • FIG. 3 is a photomicrograph, at greater magnification, of the sample of FIG. 2 showing a uniform distribution of spherical eta particles refining grain size. 1 ,000Xbefore reduction).
  • FIG. 4 is a graph plotting the fatigue resistance of lncoloy 901 as a function of grain size.
  • grain size refinement can be achieved through precipitation of an eta phase prior to recrystallization.
  • Eta in this alloy is an orthorhombic Ni Cb phase which is typically precipitated in this alloy in the l,600"-l ,700" F. temperature range and which is stable above the alloy recrystallization temperature.
  • eta is allowed to precipitate in fully annealed alloy, it nucleates at grain boundaries and grows preferentially along (111) crystallographic planes, forming long straight needles traversing each grain. Inasmuch as in this form it does not contribute significantly to the strength of the alloy and in fact competes for the elements forming the hardening gamma prime precipitate, most of the literature has concluded that the eta phase should be avoided.
  • the eta precipitate is forced to precipitate in a material which has been deformed below the alloy recrystallization temperature or otherwise properly processed, it may be provided in a uniform dispersion throughout the matrix, appearing metallographically as generally spheroidal particles 1-3 microns in size. This may be seen in FIG. 3. If the alloy is then recrystallized with the uniform dispersion of fine spheroidal eta present, the newly formed grain boundaries incorporate the eta, effectively inhibiting grain growth. The result is a much finer, more uniform grain size than that achieved by conventional processing, which may readily be observed by a comparison of the microstructures of FIGS. 1 and 2.
  • Recrystallization is a process whereby cold-worked material i l di lo e omm] f th forging or other def ation reverts to a strain-free structure by the nucleation and growth variables. IQ of new grains. In the precipitation; hardened, nickel-base al- Experience has demonstrated that a number of criteria must loys recrystallization is conducted above the solvus tempera be satisfied for effective results.
  • the pinning precipitate must t re of the hardening phase or phases.
  • the pinning precipitate must ture above the gamma prime solvus but below that of the precipitate profusely at temperatures below the recrystalliza- P l P can of wl'paioy as conventionally temperature d i n b digpefnd nif ly mulated, the pinning precipitate and the hardening phase are throughout the microstructure. And recrystallisation must 20 essentially identical chemically and metallurgicslly, the prints occur subsequent to the formation and dispersion of the ry difference residing in the size of the precipitate. However, pinning precipitate.
  • Retardation of grain growth by a eta andthe gamma prime hardening phases in the lnconel 718 uniform dispersion of spheroidal eta has also been accomand lncoloy 90l alloys.
  • the fine grain structures processed according to the present invention exhibiting grainsizes of ASTM l0 0.0002 inch diameter) or finer display superior fatigue and tensile strength properties. Tensile and yield strengths are increased by a factor of about 10-20 percent, and the smooth high cycle fatigue (HCF) life is increased by a factor of 40 percent.
  • lncoloy 90l does present somewhat of a practical processing problem. Whereas lnconel 7 I 8 exhibits a 50-75 F. temperature differential between the eta solvus and the recrystallization temperature, the differential for lncoloy 901 is only about l5'-25 F. Due to this very narrow differential, processing difficulties are increased with these alloys. it is, of course, possible to resolve this problem by certain modifications in alloy composition. Eta solvus temperatures were detennined for several such modifications as detailed in Table I.
  • eta precipitates in the lnconel 7 l 8 and lncoloy 901 alloys at the nominal chemistry in the l,500-l,700 F. range. If fully annealed material is exposed to heat treatment in this temperature range, eta precipitation will occur as a needle-like phase whereas the desired grain size refinement is dependent upon the presence of eta as a uniform distribution of spheroidal particles.
  • Spheroidal eta precipitation may be caused to occur under either of two processing conditions: l heat treatment of cold worked alloys of this type in the l,600- l ,700' F. temperature range, or (2) warm working below the recrystallization temperature )l,7$0 F.). in addition, spheroidal eta may be provided by warm working the alloys containing the needle-like eta below the alloy recrystallization temperature.
  • 8 and Hunts 0114 lncoloy 901 alloys is as follows: (a) homogenization, and eta precipitation heat treatment at l,650-1,700' F. for 4-8 hours, (b) forging at a 50-65 percent reduction at or below the eta solvus temperature (1,825 P. and 1,750 E, respectively, for the above alloys) and (c) solution heat treatment with recrystallization 2$-50 F. below the eta solvus. The latter heat treatment for 1 hour is sufficient to induce recrystallization without substantial grain growth. Short time reheats in excess of those described are tolerable provided that the eta structure is not adversely affected and no substantial grain growth occurs.
  • the alloys prior to use are subjected to the usual aging heat treatment for strengthening through precipitation of the hardening gamma prime phase.
  • this comprises holding at 1,325 F. for 8 hours, and 1.150 F. for 8 hours.
  • the aging comprises heat treatment at 1,325 F. for 6 hours and 1,200 F. for 12 hours. Cooling rates are generally equivalent to air cool or faster.
  • the preferred processing involves: (a) an initial heat treatment at l,800-i,825 F. for 24-48 hours to form the overaged gamma prime precipitate; forging to the desired configuration using a preheat temperature of 1,800-l ,850' F. and reductions of 30 percent or more; and heat treatment at 1,800-1,850 F. for 2-4 hours for recrystallization, providing a grain size of ASTM 10 or finer.
  • a sustained temperature of 1,850 F. cannot be exceeded during any stage of the process subsequent to the formation of the overaged gamma prime pinning precipitate because of its instability above this temperature.
  • a final stabilization heat treatment at about l,550 F. for 4 hours and aging at about 1,400 F. for 16 hours will provide a full hardness response.
  • Stross rupture data for line gruln lncoloy U01 harstock material By providing a fine uniform dispersion of a pinning precipitate, such as the spheroidal eta phase or the overaged gamma prime, prior to recrystallization, and effecting recrystallization in the presence of the pinning phase to control the grain size, it is possible to provide dramatic improvements in the fatigue resistance of nickel-base alloys of the type typified by lnconel 718, lncoloy 901 and Waspaloy.
  • a pinning precipitate such as the spheroidal eta phase or the overaged gamma prime
  • the method of improving the fatigue resistance of the precipitation hardenable, nickel-base alloys capable of precipitating inter-metallic compounds which are stable above the alloy recrystallization temperature which comprises:
  • the intermetallic pinning precipitate is a spheroidal eta phase or an overaged gamma prime phase.
  • the intermetallic pinning precipitate has an average particle size of about 0.1-1 micron.
  • thermomechanical processing comprises cold working of the alloy followed by heat treatment near but below the alloy recrystallization temperature to precipitate the spheroidal eta phase.
  • thermomechanical processing comprises warm working the alloy near but below the alloy recrystallization temperature to precipitate the spheroidal eta phase.
  • thermomechanical processing comprises homogenization of the alloy and precipitation of a needle-like eta phase followed by warm working near but below the alloy recrystallization temperature to convert the needle-like eta phase to the spheroidal eta phase.
  • the method of improving the fatigue resistance of the below the eta phase solvus to a grain size of ASTM [D or lncoloy 90l alloy which comprises:

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  • Engineering & Computer Science (AREA)
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Cited By (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4362578A (en) * 1980-10-16 1982-12-07 Teledyne Industries, Inc. Method of hot working metal with induction reheating
US4375375A (en) * 1981-10-30 1983-03-01 United Technologies Corporation Constant energy rate forming
US5415712A (en) * 1993-12-03 1995-05-16 General Electric Company Method of forging in 706 components
FR2722510A1 (fr) * 1994-07-13 1996-01-19 Societe Nationale D Etude Et De Construction De Mo Procede d'elaboration de toles en alliage 718 et de formage superplastique de ces toles
FR2755040A1 (fr) * 1996-10-31 1998-04-30 Aerospatiale Procede de fabrication par fluotournage a froid d'une piece en alliage inconel 718
CN1058757C (zh) * 1996-05-09 2000-11-22 沈阳黎明发动机制造公司 一种镍基高温合金锻件和棒材获得均匀超细晶粒的方法
US6193823B1 (en) 1999-03-17 2001-02-27 Wyman Gordon Company Delta-phase grain refinement of nickel-iron-base alloy ingots
US6334912B1 (en) * 1998-12-31 2002-01-01 General Electric Company Thermomechanical method for producing superalloys with increased strength and thermal stability
US6447624B2 (en) * 2000-04-11 2002-09-10 Hitachi Metals, Ltd. Manufacturing process of nickel-based alloy having improved hot sulfidation-corrosion resistance
US20020159911A1 (en) * 2001-04-25 2002-10-31 Koenigsmann Holger J. Nickel-titanium sputter target alloy
EP1293583A1 (de) * 2001-09-18 2003-03-19 Honda Giken Kogyo Kabushiki Kaisha Nickelbasislegierung, Herstellungsverfahren und Schmiedewerkzeug
EP1325965A1 (de) * 2001-12-21 2003-07-09 Hitachi Metals, Ltd. Ni-Legierung mit verbesserte Oxidation Widerstand, Warmfestigkeit and Warmbearbeitbarkeit
US6605164B2 (en) 1994-06-24 2003-08-12 Ati Properties, Inc. Nickel-based alloy having high stress rupture life
US20040084118A1 (en) * 2002-10-31 2004-05-06 Raymond Edward Lee Quasi-isothermal forging of a nickel-base superalloy
US20040221927A1 (en) * 2002-07-19 2004-11-11 Raymond Edward Lee Isothermal forging of nickel-base superalloys in air
US20060000715A1 (en) * 2000-01-25 2006-01-05 Whitcher Forrest D Manufacturing medical devices by vapor deposition
US20090104040A1 (en) * 2007-10-19 2009-04-23 Shinya Imano Nickel Based Alloy for Forging
CN100500881C (zh) * 2007-03-05 2009-06-17 贵州安大航空锻造有限责任公司 Gh4169合金近等温锻造用细晶环坯的制坯方法
CN102652179A (zh) * 2009-12-10 2012-08-29 斯奈克玛 一种制造铬镍铁耐热蚀合金718型镍超级合金的方法
CN101412066B (zh) * 2007-10-17 2012-10-03 沈阳黎明航空发动机(集团)有限责任公司 一种gh4169合金盘的锤锻工艺
US8608877B2 (en) 2010-07-27 2013-12-17 General Electric Company Nickel alloy and articles
US20140090753A1 (en) * 2012-09-28 2014-04-03 United Technologies Corporation Method for solution heat treated alloy components
US8910409B1 (en) 2010-02-09 2014-12-16 Ati Properties, Inc. System and method of producing autofrettage in tubular components using a flowforming process
US9217619B2 (en) 2011-03-02 2015-12-22 Ati Properties, Inc. Composite gun barrel with outer sleeve made from shape memory alloy to dampen firing vibrations
US9551053B2 (en) 2011-06-23 2017-01-24 United Technologies Corporation Method for limiting surface recrystallization
US9662740B2 (en) 2004-08-02 2017-05-30 Ati Properties Llc Method for making corrosion resistant fluid conducting parts
US10118259B1 (en) 2012-12-11 2018-11-06 Ati Properties Llc Corrosion resistant bimetallic tube manufactured by a two-step process
CN114226620A (zh) * 2021-10-20 2022-03-25 中国航发沈阳黎明航空发动机有限责任公司 一种细化gh2907合金环形锻件晶粒度的方法
US11441217B2 (en) 2017-12-14 2022-09-13 Vdm Metals International Gmbh Method for producing semi-finished products from a nickel-based alloy
US11951528B2 (en) 2020-08-20 2024-04-09 Rolls-Royce Corporation Controlled microstructure for superalloy components

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JPS58174538A (ja) * 1982-04-02 1983-10-13 Hitachi Ltd 原子炉用隙間構造部材に用いられる耐応力腐食割れ性に優れたＮｉ基合金製部材
US4957567A (en) * 1988-12-13 1990-09-18 General Electric Company Fatigue crack growth resistant nickel-base article and alloy and method for making
FR2691983B1 (fr) * 1992-06-03 1994-07-22 Snecma Procede de traitement thermique d'un superalliage a base de nickel.
FR2941962B1 (fr) 2009-02-06 2013-05-31 Aubert & Duval Sa Procede de fabrication d'une piece en superalliage a base de nickel, et piece ainsi obtenue.
CN111575620B (zh) * 2020-07-01 2021-11-16 中南大学 一种获得gh4169合金超细晶锻件的方法
CN112410618B (zh) * 2020-11-19 2021-10-22 中国第二重型机械集团德阳万航模锻有限责任公司 Gh4698高温合金模具制备方法

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US3519503A (en) * 1967-12-22 1970-07-07 United Aircraft Corp Fabrication method for the high temperature alloys

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JPS5511823B2 (de) * 1972-06-06 1980-03-27

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3420716A (en) * 1965-11-04 1969-01-07 Curtiss Wright Corp Method of fabricating and heat-treating precipitation-hardenable nickel-base alloy
US3519503A (en) * 1967-12-22 1970-07-07 United Aircraft Corp Fabrication method for the high temperature alloys

Cited By (46)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4362578A (en) * 1980-10-16 1982-12-07 Teledyne Industries, Inc. Method of hot working metal with induction reheating
US4375375A (en) * 1981-10-30 1983-03-01 United Technologies Corporation Constant energy rate forming
US5415712A (en) * 1993-12-03 1995-05-16 General Electric Company Method of forging in 706 components
US6605164B2 (en) 1994-06-24 2003-08-12 Ati Properties, Inc. Nickel-based alloy having high stress rupture life
US6328827B1 (en) 1994-07-13 2001-12-11 Societe Nationale d'Etude et de Construction de Moteurs d'Aviation “SNECMA” Method of manufacturing sheets made of alloy 718 for the superplastic forming of parts therefrom
FR2722510A1 (fr) * 1994-07-13 1996-01-19 Societe Nationale D Etude Et De Construction De Mo Procede d'elaboration de toles en alliage 718 et de formage superplastique de ces toles
CN1058757C (zh) * 1996-05-09 2000-11-22 沈阳黎明发动机制造公司 一种镍基高温合金锻件和棒材获得均匀超细晶粒的方法
EP0841107A1 (de) * 1996-10-31 1998-05-13 AEROSPATIALE Société Nationale Industrielle Verfahren zur Herstellung eines Werkstückes aus Inconel 718-Legierung durch Kaltfliessdrücken
FR2755040A1 (fr) * 1996-10-31 1998-04-30 Aerospatiale Procede de fabrication par fluotournage a froid d'une piece en alliage inconel 718
US6334912B1 (en) * 1998-12-31 2002-01-01 General Electric Company Thermomechanical method for producing superalloys with increased strength and thermal stability
EP1177324A1 (de) * 1999-03-17 2002-02-06 Wyman Gordon Company Delta-phasen kornfeinung von blöcken aus nickel-eisen-basis legierungen
US6193823B1 (en) 1999-03-17 2001-02-27 Wyman Gordon Company Delta-phase grain refinement of nickel-iron-base alloy ingots
EP1177324A4 (de) * 1999-03-17 2002-09-18 Wyman Gordon Co Delta-phasen kornfeinung von blöcken aus nickel-eisen-basis legierungen
US20060000715A1 (en) * 2000-01-25 2006-01-05 Whitcher Forrest D Manufacturing medical devices by vapor deposition
US8460361B2 (en) * 2000-01-25 2013-06-11 Boston Scientific Scimed, Inc. Manufacturing medical devices by vapor deposition
US6447624B2 (en) * 2000-04-11 2002-09-10 Hitachi Metals, Ltd. Manufacturing process of nickel-based alloy having improved hot sulfidation-corrosion resistance
US6478895B1 (en) * 2001-04-25 2002-11-12 Praxair S.T. Technology, Inc. Nickel-titanium sputter target alloy
WO2002088408A1 (en) * 2001-04-25 2002-11-07 Praxair S.T. Technology, Inc. Nickel-titanium sputter target alloy
US20020159911A1 (en) * 2001-04-25 2002-10-31 Koenigsmann Holger J. Nickel-titanium sputter target alloy
EP1293583A1 (de) * 2001-09-18 2003-03-19 Honda Giken Kogyo Kabushiki Kaisha Nickelbasislegierung, Herstellungsverfahren und Schmiedewerkzeug
US20060081315A1 (en) * 2001-09-18 2006-04-20 Honda Giken Kogyo Kabushiki Kaisha Method for producing Ni based alloy and forging die
US6997994B2 (en) 2001-09-18 2006-02-14 Honda Giken Kogyo Kabushiki Kaisha Ni based alloy, method for producing the same, and forging die
EP1325965A1 (de) * 2001-12-21 2003-07-09 Hitachi Metals, Ltd. Ni-Legierung mit verbesserte Oxidation Widerstand, Warmfestigkeit and Warmbearbeitbarkeit
US6852177B2 (en) 2001-12-21 2005-02-08 Hitachi Metals Ltd. Ni-based alloy improved in oxidation-resistance, high temperature strength and hot workability
US6908519B2 (en) * 2002-07-19 2005-06-21 General Electric Company Isothermal forging of nickel-base superalloys in air
US20040221927A1 (en) * 2002-07-19 2004-11-11 Raymond Edward Lee Isothermal forging of nickel-base superalloys in air
US20040084118A1 (en) * 2002-10-31 2004-05-06 Raymond Edward Lee Quasi-isothermal forging of a nickel-base superalloy
US6932877B2 (en) * 2002-10-31 2005-08-23 General Electric Company Quasi-isothermal forging of a nickel-base superalloy
US9662740B2 (en) 2004-08-02 2017-05-30 Ati Properties Llc Method for making corrosion resistant fluid conducting parts
CN100500881C (zh) * 2007-03-05 2009-06-17 贵州安大航空锻造有限责任公司 Gh4169合金近等温锻造用细晶环坯的制坯方法
CN101412066B (zh) * 2007-10-17 2012-10-03 沈阳黎明航空发动机(集团)有限责任公司 一种gh4169合金盘的锤锻工艺
US8956471B2 (en) * 2007-10-19 2015-02-17 Mitsubishi Hitachi Power Systems, Ltd. Nickel based alloy for forging
US9567656B2 (en) 2007-10-19 2017-02-14 Mitsubishi Hitachi Power Systems, Ltd. Nickel based alloy for forging
US20090104040A1 (en) * 2007-10-19 2009-04-23 Shinya Imano Nickel Based Alloy for Forging
CN102652179A (zh) * 2009-12-10 2012-08-29 斯奈克玛 一种制造铬镍铁耐热蚀合金718型镍超级合金的方法
CN102652179B (zh) * 2009-12-10 2015-11-25 斯奈克玛 一种制造铬镍铁耐热蚀合金718型镍超级合金的方法
US8910409B1 (en) 2010-02-09 2014-12-16 Ati Properties, Inc. System and method of producing autofrettage in tubular components using a flowforming process
US8608877B2 (en) 2010-07-27 2013-12-17 General Electric Company Nickel alloy and articles
US9562276B2 (en) 2010-07-27 2017-02-07 General Electric Company Nickel alloy and articles
US9217619B2 (en) 2011-03-02 2015-12-22 Ati Properties, Inc. Composite gun barrel with outer sleeve made from shape memory alloy to dampen firing vibrations
US9551053B2 (en) 2011-06-23 2017-01-24 United Technologies Corporation Method for limiting surface recrystallization
US20140090753A1 (en) * 2012-09-28 2014-04-03 United Technologies Corporation Method for solution heat treated alloy components
US10118259B1 (en) 2012-12-11 2018-11-06 Ati Properties Llc Corrosion resistant bimetallic tube manufactured by a two-step process
US11441217B2 (en) 2017-12-14 2022-09-13 Vdm Metals International Gmbh Method for producing semi-finished products from a nickel-based alloy
US11951528B2 (en) 2020-08-20 2024-04-09 Rolls-Royce Corporation Controlled microstructure for superalloy components
CN114226620A (zh) * 2021-10-20 2022-03-25 中国航发沈阳黎明航空发动机有限责任公司 一种细化gh2907合金环形锻件晶粒度的方法

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DE2124580A1 (de) 1971-12-02
BE767327A (fr) 1971-10-18
JPS572143B1 (de) 1982-01-14
CA941717A (en) 1974-02-12
DE2124580C2 (de) 1982-03-11
CH538545A (fr) 1973-06-30
IL36403A0 (en) 1971-05-26
IL36403A (en) 1974-01-14
FR2089069A5 (de) 1972-01-07
SE379557B (de) 1975-10-13
GB1320442A (en) 1973-06-13

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