US3046108A - Age-hardenable nickel alloy - Google Patents

Age-hardenable nickel alloy Download PDF

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US3046108A
US3046108A US773702A US77370258A US3046108A US 3046108 A US3046108 A US 3046108A US 773702 A US773702 A US 773702A US 77370258 A US77370258 A US 77370258A US 3046108 A US3046108 A US 3046108A
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alloy
nickel
age
strength
alloys
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Herbert L Eiselstein
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Huntington Alloys Corp
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International Nickel Co Inc
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Priority to US773702A priority patent/US3046108A/en
Priority to GB36942/59A priority patent/GB897464A/en
Priority to CH8047559A priority patent/CH401485A/fr
Priority to BE584632A priority patent/BE584632A/fr
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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
    • C22C19/055—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%

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  • the present invention relates to a malleable and agehardenable nickel-chromium base alloy and, more particularly, to a malleable nickel-chromium base alloy having a particularly high combination of strength properties and ductility over the temperature range extending from room temperature to approximately 1400 F.
  • Another object of the invention is to provide an improved nickel-chromium base alloy of specially controlled composition which exhibits a high rupture life at elevated temperatures.
  • the invention also contemplates providing an improved age-hardenable nickel-chromium base alloy having a yield strength representing a very high proportion of the tensile strength in the age-hardened condition while at the same time displaying a very high elongation.
  • Another object of the invention is to provide an improved age-hardenable nickeLchromium base alloy which is readily producible in usual mill forms such as sheet, rod, tubing, shapes, etc.
  • the present invention particularly contemplates a nickel-base alloy containing about 4.0% to about 8.0% columbium, about 2% to 4% molybdenum, about 15% to about 23% chromium, about 0.2% to about 2% aluminum, about 0.2% to about 2% titanium, not more than 0.5 silicon, with the sum of the aluminum and titanium contents not exceeding about 2%, up to about 0.1% carbon, up to about 0.5% zirconium, about 0.005% to about 0.015% boron, up to about 1% manganese, up to about 30% iron, and the balance essentially metal from the group consisting of nickel and cobalt, said balance being about 45% to about 58% or 60% of the alloy with the cobalt content being up to about 30% and with the nickel content being at least 30% of the alloy.
  • alloys are characterized by a very high combination of tensile strength and ductility as measured in the room temperature tensile test and will provide a yield strength (0.2% set) in the annealed and age-hardened condition of at least about 100,000 p.s.i. coupled with a high elongation which will usually be at least about 20%.
  • these alloys will provide very high rupture strength in the age-hardened condition at temperatures on the order of about l200 F. to about 1350 F. or 1400 F.
  • the age'hardened alloys will usually provide a rupture life of at least about hours under a stress of 90,000 psi. at 1200 F.
  • a preferred alloy contemplated in accordance with the invention contains about 0.03% carbon, about 0.18% manganese, about 0.27% silicon, about 53% nickel, about 21% chromium, about 0.6% aluminum, about 0.6% titanium, about 4% columbium, about 3% molybdenum, about 0.009% boron and the balance essentially iron.
  • the sum of the columbium and molybdenum contents preferably is at least about 7%.
  • Aluminum and titanium in small amounts impart malleability, age hardenability and high strength to the alloy and must be present in amounts of at least about 0.2% each.
  • Molybdenum in the alloy contributes to the strength properties thereof at elevated temperatures but does not contribute age hardenability to the alloy.
  • the molybdenum content of the alloy may be replaced by an equal weight amount of tungsten while retaining substantially the same properties although the hot malleabillty of the alloy is reduced thereby.
  • columbium in the alloy may be replaced in part with tantalum in the amount of up to 4% of the alloy without materially changing the properties of the alloy.
  • Tantalumfree alloys and/or alloys wherein not more than 50% of the columbium content is replaced by tantalum are notchductile at elevated temperatures. Boron in an amount exceeding about 0.001% and up to about 0.02%, e.g., about 0.005% to about 0.015%, contributes to the strength of the alloy over the temperature range from about atmospheric temperature to about 1400 F. Boron contributes particularly to high strength and ductility in the stress-rupture test at elevated temperatures.
  • the alloy may also contain up to about 0.5% zirconium, e.g., about 0.05% to about 0.3% zirconium. Zirconium functions as a malleabilizer and deoxidizer and contributes to age hardening.
  • the alloys are soft and ductile in the annealed or solution-treated condition, i.e., after a heat treatment at a temperature of at least about l550 or 1600" F. up to about 2200 F. for a period of about 1 hour.
  • the alloys respond readily to age hardening in the temperature range a of about 1200 to 1350 F. for periods of time of at least about 4 hours and up to 24 hours, e.g., 16 hours.
  • the alloys may be solution treated or annealed prior to aging or may be aged directly from the as-forged or hot rolled alloys defined in Table I were subjected to tensile tests at room temperature with the results set forth in the following Table III.
  • alloys described hereinbefore develop high stress-rupture properties at 1200 F. when directly aged from the hot rolled or asforged state without a solution anneal.
  • the alloy in the as-cast condition is readily wrought using commercial hot working operations such as rolling, forging, extrusion, etc.
  • a number of alloys having the compositions set forth 4, in the above Table I were melted in an induction furnace open to the air and were cast into graphite molds to form 4-inch diameter round ingots.
  • the ingots were forged to bars approximately /a of an inch square using a series of forging and reheating steps.
  • the ingots were forged without difliculty.
  • the alloy contributes to elevated temperature strength and -treating temperatures. butes to the elevated gth properties thereof but does not con- 5 tribute age hardenability to the allo permits the use of lower solution Molybdenum in the alloy c-ontri temperature stren y.
  • the molybdenum may be replaced in whole or in part amount of tungsten while retaining me properties although the hot malyL h P re as W u u do me m w my. 610
  • the alloy should be solution treated or annealed prior to aging.
  • This solution treatment involves a heating in the te about 1800 F. to about 2000 is the criterion, conmperature range of F. for a period of time tains about 4% to about 8% colurnbium, about 13% to about 23% chromium denum, about 0.2%
  • test specimens employed were machined from forgings and were subjected to a heat treatment prior to testing, which treatment comprised a heating at 1900-2000 F. for one hour, a quench in water, and a reheating at 1300-1350 F. for sixteen hours, followed by air cooling.
  • the curves labeled A and B show, respectively, the tensile and yield (0.2% offset) strengths for the alloys at room temperature.
  • the curves labeled C, D and E show, respectively, the 100-hour rupture strength for the alloys at 1200 F., 1300 F. and 1400 F.
  • the data presented in the drawin demonstrate that the maximum room temperature strength is obtained in the alloys at about 53% nickel and that increasing the nickel content beyond 53% increases the rupture strength for the alloys at elevated temperatures.
  • the present invention is directed to age hardenable nickel alloys containing about to about 25% chromium, up to about 7% molydenum, about 3% to about 8% columbium, about 0.2% to about 2% titanium, about 0.2% to about 2% aluminum, with the sum of aluminum and titanium not exceeding about 2.5%, not more than about 0.2% carbon, up to about 0.02% boron, up to about 40% iron, and the balance essentially a metal from the group consisting of cobalt and nickel with the sum of the nickel and cobalt contents being about 45% to about 80% of the alloy and the cobalt content being up to about 40% of the alloy and the nickel content being at least 30%.
  • the sum of the columbium and molybdenum contents be at least about 9% and up to about and that the amount of columbium be at least about 4%.
  • Aluminum and titanium in small amounts are essential to provide malleability, additional age hardenability and high strength in the alloy and must be present in amounts of at least about 0.2% each. It is important that alloys within the invention have contents of columbium plus tantalum, aluminum plus titanium, chromium and nickel as related according to the following formulae:
  • the alloy may be substantially or entirely copper free or may contain up to about 4% copper, preferably not over about 0.15% copper.
  • Cobalt in the alloy is beneficial from the standpoint of improving properties at elevated temperature and, in addition, cobalt enables the use of lower annealing or solution-treating temperatures.
  • Molybdenum in the alloy contributes to the elevated temperature strength properties thereof but does not contribute age hardenability to the alloy.
  • the molybdenum content of the alloy may be replaced in whole or in part by an equal weight amount of tungsten while retaining substantially the same properties although the hot malleability of the alloy is reduced thereby.
  • Columbium in the alloy may be replaced in part with tantalum in the amount of up to about 4% of the alloy without materially changing the properties of the alloy.
  • Tantalum-free alloys and/or alloys wherein not more than 50% of the columbium content is replaced by tantalum are notchductile at elevated temperatures. Since commerciallyavailable columbium contains about 10% tantalum, the values reported herein for columbium include about 10% by weight of tantalum. Boron in an amount exceeding 0.001% and up to about 0.02%, e.g., about 0.005% to about 0.015%, contributes to the strength of the alloy over the temperature range from about atmospheric temperature to about 1400 F. Boron contributes particularly to high strength and ductility in the stress-rupture test at elevated temperatures.
  • the alloy may also contain up to about 0.5% Zirconium, e.g., about 0.05% to about 0.3% zirconium, which functions as a malleabilizer and deoxidizer and contributes to age hardening.
  • the balance of the alloy is metal from the group consisting of nickel and cobalt, it is to be understood that the balance will include small amounts of impurities and incidental elements which do not materially change the properties of the alloy.
  • impurities such as sulfur and phosphorus in a total amount up to about 0.05% may be present in the alloy.
  • the alloy may contain up to about 1% silicon, but the silicon content should not exceed this amount as otherwise forgeability of the alloy is impaired.
  • silicon does not exceed 0.5% to secure best properties at elevated temperatures.
  • Manganese in an amount up to about 1% may be present in the alloy.
  • the alloy is readily age hardenable when heated in the temperature range of about 1200 to about 1350 F.
  • the alloy may be aged to develop high strength either directly from the as-forged or hot rolled condition or after a solution treatment at a temperature of about 1550 F. to about 2200 F. for a period of about 1 hour. In the aged condition, the alloys are strong and ductile and do not develop brittleness after long exposure to stress at elevated temperature.
  • alloys contemplated in accordance with the invention possess a very high combination of strength and ductility.
  • these alloys generally will provide a room temperature yield strength of at least. 100,000 p.s.i. or much hi her along with a substantial elongation which usually isat least 20%.
  • many of the alloys contemplated in accordance with the invention will provide a 10"-hour rupture strength of at least about 110,000 p.s.i., or much higher,.at 1200" F.
  • alloy No. 25 displayed a rupture life of 482.8 hours at 1200 F. and 100,000 p.s.i.
  • Alloys within the invention are strongly age hardenable and will provide a room temperature yield strength in the aged condition which is at least 50% or or more than the room temperature yield strength for the same alloy in the solution annealed condition.
  • the small content of aluminum and titanium required in the allo which advantageously is a total of at least about 0.75%, contributes very importantly to the age hardena-bility of the alloy and to the development of high strength in the alloy at elevated temperature.
  • an alloy outside the scope of the invention and containing about 0.07% carbon, about 18.26% iron, about 53.42% nickel, about 20.95% chromium, about 0.024% aluminum, about 0.041% titanium, about 2.08% molybdenum and about 4.59% columbium was essentially non-age hardenable and developed a room temperature yield strength (0.2% set) of only 68,000 psi. and had a 100-hour rupture strength at 1200 F. of only about 75,000 p.s.i.
  • comparable alloys Nos. 9 and 8 developed room temperature yield strengths (0.2% set) in the aged condition of 167,500 p.s.i. and 190,000 p.s.i., respectively, and were character- 0 ized by 100-hour rupture strengths at 1200 in the aged condition of 100,000 psi. and 105,000 p.s.i., respectively.
  • the sum of aluminum and itanium does not exceed about 2.5% or, more advantageously, about 2%, as greater amounts of these elements reduce the rupture strength of the alloy at elevated temperatures and also greatly reduce forgeability of the alloy.
  • a commercial-scale melt weighing about 5000 pounds was air melted in a commercial induction furnace.
  • This melt contained about 4.29% colum- 11 bium, about 2.45% molybdenum, about 20.81% chromium, about 17.66% iron, about 53.02% nickel, about 0.009% boron, about 0.39% aluminum, about 0.64% titanium, about 0.39% silicon, about 0.05% carbon and
  • the fatigue strength (endurance limit at 10 cycles) at room temperature of hot-rolled, heat-treated bar stock made from this metal was 80,000 p.s.i. after aging at 1300 F. for 16 hours and 97,500 p.s.i. after aging at about 0.29% manganese.
  • Hot-rolled sheet 0.082 inch thick and cold-rolled sheet 0.30% manganese and about 0.03% carbon The ingots 0.070 inch thick made [from the alloy were aged by heatwere overhauled to remove surface defects and were ing for 16 hours at 1300 F.
  • cold-rolled 20 heated and forged to billets.
  • the billets were reheated sheet 0.060 inch thick made from the alloy was annealed and hot rolled to various mill forms, including hot-rolled at 1800 F. in a production gas-fired continuous annealrounds about inch in diameter.
  • Alloys contemplated in accordance with the invention may be produced by melting the required ingredients together in a furnace satisfactory for melting high-nickel alloys. Additions of aluminum, titanium, columbium and boron are made late in the melting cycle. Additional deoxidation with magnesium or calcium may be employed.
  • the alloys produced in accordance with the invention are characterized by the fact that they provide high strength properties as reflected in the stress-rupture test at elevated temperatures of about 1200 F. to 1400 F. in the as-rolled and aged condition.
  • the alloys within the invention are characterized by an essentially featureless microstructure even after prolonged exposure to the deleterious eifects of combined stress and temperature.
  • the alloys within the invention are characterized by high fatigue strength over a range of temperatures up to about 1400 F.
  • the microstructure displays clean grain boundaries and shows no precipitate other than carbides at usual optical magnifications in the aged condition.
  • the alloy can be produced in the usual hot-worked mill forms, including sheet, strip, rods, bars, tubing, etc.
  • the alloy is useful in a wide variety of applications as a structural member in air frames, missiles, rockets and the like. It is also useful for compressor and turbine rotors in gas turbines. It is also useful as compressor and turbine blading in gas turbines and as turbine blading in steam turbines.
  • the alloy may also be used in a variety of forms such as sheet and tubing in applications such as pressure vessels, steam lines, high-temperature piping and the like.
  • the alloy may also be used in hightemperature bolts such as those used in aircraft gas turbines, stationary gas turbines and steam turbines and it is also useful in the form of springs subjected in use to elevated temperatures. The corrosion resistance of the alloy is good.
  • the alloy provides a very high ratio of strength to density (the Shapiro index).
  • the alloy is non-magnetic.
  • An age-hardenable, hot-workable nickel-base alloy consisting essentially of about 21% chromium, about 3% molybdenum, about 4% of metal from the group consisting of columhium and tantalum wherein the tantalum content does not exceed about 50% of the colu-mbium, about 0.6% titanium, about 0.6% aluminum, about 0.03% carbon, about 0.27% silicon, about 0.18% manganese, about 0.009% boron, about 53% nickel, and the balance essentially iron, said alloy being characterized in the age-hardened condition by a yield strength (0.2% oifset) of at least about 100,000 pounds per square inch at room temperature and by a -hour rupture strength of at least about 90,000 psi. at 1200 F.
  • An age-hardenable, hot-workable nickel alloy consisting essentially of about 15% to about 23% chromium, about 2% to about 4% molybdenum, about 4% to about 8% of metal from the group consisting of columbium and tantalum wherein the tantalum content does not exceed about 50% of the eolumbiurn, aluminum and titanium each in a small amount of at least about 0.2%, with the total aluminum plus titanium content not exceeding about 2%, not more than about 0.1% carbon, not more than about 0.5% silicon, about 0.001% to about 0.02% boron, up to about 30% iron, up to about 1% manganese, and the balance essentially nickel,
  • nickel content being about 45 to about 60% of the alloy, said alloy being characterized in the agehardened condition by a yield strength (0.2% offset) of at least about 100,000 pounds per square inch at room temperature and by a l-hour rupture strength of at least about 90,000 p.s.i. at 1200 F.
  • An age-hardenable, hot-workable nickel alloy consisting essentially of about 15% to about 23% chromium, about 2% to about 4% molybdenum, about 4% to about 8% of metal from the group consisting of columbium and tantalum wherein the tantalum content does not exceed :about 50% of the columbium, aluminum plus titanium each in a small amount of at least about 0.2%, with the total aluminum plus titanium content not exceeding about 2%, not more than about 0.1% carbon, not more than about 0.5% silicon, about 0.005 to about 0.015% boron, up to about 30% iron, up to about 1% manganese, and the balance essentially metal from the group consisting of nickel and cobalt, with the sum of the nickel and cobalt contents being about 51% to about 56% of the alloy and the nickel content being at least about 30% of the alloy, said alloy beingcharacterized in the agehardened condition by a yield strength (0.2% offset) of at least about 100,000 pounds per square inch at room temperature'and by high rupture strength at temperatures up to about 1
  • An age-hardenable, hot-workable nickel-base alloy consisting essentially of about 13% to about 23% chromium, about 2% to about 5% molybdenum, about 4% to about 8% of metal from the group consisting of columbium and tantalum wherein the tantalum content does not exceed about 50% of the columbium, aluminum and titanium each in a small amount of at least about 0.2%, with the total aluminum plus titanium content not exceeding about 2%, not more than about 0.1% carbon, not more than about 0.5% silicon, about 0.001% to about 0.02% boron, up to about 20% iron, up to about 1% manganese, and the balance essentially metal from the group consisting of nickel and cobalt, with the sum of the nickel and cobalt contents being about 60% to about 75% of the alloy, with the nickel content being at least about 30% of the alloy, and with the cobalt content being up to about 40% of the alloy, said alloy being characterized in the age-hardened condition by a yield strength (0.2% offset) of at least about 100,000
  • An age-hardenable, hot-workable nickel alloy consisting essentially of about chromium, about 3% molybdenum, about 7.5% of metal from the group consisting of columbium and tantalum wherein the tantalum content does not exceed about 50% of the colum-bium, about 0.7% titanium, about 0.7% aluminum, about 0.04% carbon, about 0.3% silicon, about 0.005% boron, about 8% iron, about 0.3% manganese, and the balance essentially nickel, said alloy being characterized in the agehardened condition by a yield strength (0.2% offset) of at least about 100,000 pounds per square inch at room temperature and by a 100-hour rupture strength at 1200 F. of at least about 100,000 pounds per square inch.
  • An age-'hardenable, hot-workable nickel alloy consisting essentially of about 10% to about 25% chromium, about 2% to about 7% of metal from the group consisting of molybdenum and tungsten, more than 3% and up to about 9% of metal from the group consisting of columbium and tantalum with the tantalum content not exceeding about 50% of the columbium, aluminum and titanium each in a small amount of at least about 0.2%, with the total aluminum plus titanium content not exceeding about 2.5%, not more than 0.2% carbon, not more than 0.5 silicon, about 0.001% to about 0.02% boron, up to about 30% iron, up to about 1% manganese, and the balance essentially metal from the group consisting of nickel and cobalt, with the sum of the nickel and cobalt contents being about 45% to about of the alloy, with the nickel content being at least about 30% and with the cobalt content being up to about 40% of the alloy, said alloy being characterized in that when the nickel content is at least 50%, the contents of columbium plus tant
  • An age-hardenable, hot-workable nickel alloy consisting essentially of about 10% to about 25% chromium, about 2% to about 7% of metal from the group consisting of molybdenum and tungsten, more than 3% and up to about 9% of metal from the group consisting of columbi-um and tantalum wherein the tantalum content does not exceed 50% of the columbium, aluminum plus titanium each in a small amount of at least about 0.2%, with the total aluminum plus titanium content not exceeding about 2.5%, not more than 0.2% carbon, not more than 1% silicon, about 0.001% to about 0.02% boron, up to about 0.5% zirconium, up to about 1% manganese, up to about 30% iron and the balance essentially nickel, said alloy being characterized after hot working and aging by a yield strength (0.2% offset) of at least about 100,000 pounds per square inch at room temperature and by a 100-hour rupture strength of at least about 90,000 p.s.i. at 1200 F.
  • An age-hardenable, bot-workable nickel alloy consisting essentially of about 10% to about 25% chromium, about 2% to about 7% molybdenum, about 4% to about 9% of metal from the group consisting of columbium and tantalum wherein the tantalum content does not exceed about 50% of the columbium, about 0.75% to about 2% of metal from the group consisting of aluminum and titanium, not more than about 0.1% carbon, not more than about 0.5 silicon, about 0.001% to about 0.

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DENDAT1250642D DE1250642B (enrdf_load_stackoverflow) 1958-11-13
US773702A US3046108A (en) 1958-11-13 1958-11-13 Age-hardenable nickel alloy
GB36942/59A GB897464A (en) 1958-11-13 1959-10-30 Improvements relating to nickel-chromium alloys
CH8047559A CH401485A (fr) 1958-11-13 1959-11-11 Alliage nickel-chrome
BE584632A BE584632A (fr) 1958-11-13 1959-11-13 Perfectionnements aux alliages de nickel et de chrome.

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US3466171A (en) * 1965-07-20 1969-09-09 Int Nickel Co Nickel-chromium-niobium alloy
US3486886A (en) * 1965-09-30 1969-12-30 Mitsubishi Heavy Ind Ltd Cobalt base alloy
US3493366A (en) * 1965-11-12 1970-02-03 Int Nickel Co Alloy for service in petrochemical and hydrocarbon processing
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US3619183A (en) * 1968-03-21 1971-11-09 Int Nickel Co Nickel-base alloys adaptable for use as steam turbine structural components
US3871928A (en) * 1973-08-13 1975-03-18 Int Nickel Co Heat treatment of nickel alloys
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US4225363A (en) * 1978-06-22 1980-09-30 The United States Of America As Represented By The United States Department Of Energy Method for heat treating iron-nickel-chromium alloy
DE3019931A1 (de) * 1979-07-27 1981-12-03 Westinghouse Electric Corp., 15222 Pittsburgh, Pa. Verfahren zur waermebehandlung einer eisen-nickel-chromlegierung
US4359349A (en) * 1979-07-27 1982-11-16 The United States Of America As Represented By The United States Department Of Energy Method for heat treating iron-nickel-chromium alloy
EP0066361A3 (en) * 1981-04-17 1983-01-19 Huntington Alloys, Inc. Corrosion resistant high strength nickel-based alloy
US4415530A (en) * 1980-11-10 1983-11-15 Huntington Alloys, Inc. Nickel-base welding alloy
US4487743A (en) * 1982-08-20 1984-12-11 Huntington Alloys, Inc. Controlled expansion alloy
US4578130A (en) * 1979-07-27 1986-03-25 The United States Of America As Represented By The United States Department Of Energy Iron-nickel-chromium alloy having improved swelling resistance and low neutron absorbence
JPS62130252A (ja) * 1985-11-26 1987-06-12 ユナイテツド・テクノロジ−ズ・コ−ポレイシヨン ニツケル基超合金
US4685978A (en) * 1982-08-20 1987-08-11 Huntington Alloys Inc. Heat treatments of controlled expansion alloy
US4685977A (en) * 1984-12-03 1987-08-11 General Electric Company Fatigue-resistant nickel-base superalloys and method
US4689279A (en) * 1982-10-12 1987-08-25 Westinghouse Electric Corp. Composite containing nickel-base austenitic alloys
EP0234172A2 (en) 1985-12-30 1987-09-02 United Technologies Corporation High-strength nickel-base superalloy for castings, treated by means of hot isostatic pressing
US4731117A (en) * 1986-11-04 1988-03-15 Crucible Materials Corporation Nickel-base powder metallurgy alloy
US4750944A (en) * 1985-12-30 1988-06-14 United Technologies Corporation Laves free cast+hip nickel base superalloy
US4761190A (en) * 1985-12-11 1988-08-02 Inco Alloys International, Inc. Method of manufacture of a heat resistant alloy useful in heat recuperator applications and product
US4765956A (en) * 1986-08-18 1988-08-23 Inco Alloys International, Inc. Nickel-chromium alloy of improved fatigue strength
US4788036A (en) * 1983-12-29 1988-11-29 Inco Alloys International, Inc. Corrosion resistant high-strength nickel-base alloy
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