US20230212716A1 - Nickel-base precipitation hardenable alloys with improved hydrogen embrittlement resistance - Google Patents

Nickel-base precipitation hardenable alloys with improved hydrogen embrittlement resistance Download PDF

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US20230212716A1
US20230212716A1 US18/091,576 US202218091576A US2023212716A1 US 20230212716 A1 US20230212716 A1 US 20230212716A1 US 202218091576 A US202218091576 A US 202218091576A US 2023212716 A1 US2023212716 A1 US 2023212716A1
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equal
plastic strain
nickel
alloy
precipitation hardenable
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Brian DeForce
Brian A. Baker
Edward Francis Damm, III
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Huntington Alloys Corp
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Huntington Alloys Corp
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Assigned to HUNTINGTON ALLOYS CORPORATION reassignment HUNTINGTON ALLOYS CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: DAMM, EDWARD FRANCIS, III, BAKER, BRIAN, DEFORCE, Brian
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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%
    • 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
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon

Definitions

  • the present disclosure relates to nickel-base precipitation hardenable alloys, and particularly to nickel-base precipitation hardenable alloys with improved hydrogen embrittlement resistance.
  • Nickel-base precipitation hardenable alloys are used for the manufacture of critical down-hole components in oil field equipment. Such alloys are known to be resistant to chloride-ion stress corrosion cracking, sulfide stress corrosion cracking, and galvanically-induced hydrogen stress corrosion cracking. However, ever increasing resistance to hydrogen embrittlement (HE) is desired. Resistance to hydrogen embrittlement may be evaluated by determining a plastic strain ratio and a plastic strain to failure. As used herein, the phrases “plastic strain to failure” and “plastic strain ratio” refer to the plastic strain to failure and plastic strain ratio as established in NACE Standard TM0198. This standard provides a slow strain rate test for evaluation of Ni-based alloys for resistance to hydrogen-induced stress corrosion cracking (SCC) in simulated oil field production environments at elevated temperatures.
  • SCC hydrogen-induced stress corrosion cracking
  • plastic strain to failure is the maximum plastic deformation in the material before the material breaks.
  • a projection of an elastic line through the stress and strain value at failure is used to determine the amount of strain attributed to sample plastic deformation as the total strain at failure minus the equivalent elastic strain at the failure point.
  • the HE plastic strain ratio is the plastic strain to failure determined from a sample tested in acid divided by the plastic strain to failure determined from a sample tested in an inert environment.
  • the present disclosure addresses the issue of improved HE resistance of nickel-base precipitation hardenable alloys and other issues related to nickel-base precipitation hardenable alloys for use in oil field environments.
  • a Ni-based precipitation hardenable alloy has a composition, in wt.% of Cr from about 18.0% to about 23.0%, Fe from about 7.0% to about 12.0%, Mo from about 6.5% to about 9.5%, Nb from about 3.2% to about 5.2%, Ti from about 0.3% to about 1.3%, Al up to about 0.4%, and balance Ni and incidental impurities, a yield strength greater than or equal to 120 ksi, a plastic strain ratio greater than 0.35, and a plastic strain to failure greater than or equal to 9.0%.
  • the alloy has a Ti content about 0.8% to about 1.1% and an Fe content between about 9.0% to about 12.0%.
  • the alloy has a Ti content between about 0.8% to about 1.0% and an Fe content between about 10.0% to about 12.0%.
  • the alloy has a Ti content between about 0.4% to about 0.8% and an Fe content between about 10.0% to about 12.0%.
  • the alloy in one form has a desired plastic strain ratio, i.e., greater than or equal to 0.35, and a plastic strain to failure greater than or equal to 9.0%
  • the alloy also maintains a desired strength, i.e., greater than or equal to 120 ksi (827 MPa).
  • the alloy has an HE plastic strain ratio greater than or equal to 0.35, a plastic strain to failure greater than 9.0% and the yield strength is between about 120 ksi (827 MPa) and 150 ksi (1034 MPa).
  • the alloy has a plastic strain ratio greater than or equal to 0.40 and a plastic strain to failure greater than or equal to 10.0%.
  • the plastic strain ratio is greater than or equal to 0.50 and the plastic strain to failure is greater than or equal to 12.0%.
  • a Ni-based precipitation hardenable alloy has a composition, in wt.% of Cr from about 18.0% to about 23.0%, Fe from about 9.0% to about 16.0%, Mo from about 4.5% to about 7.5%, Nb from about 3.2% to about 5.2%, Ti from about 0.4% to about 1.3%, Al up to about 0.4%, and balance Ni and incidental impurities, a yield strength greater than or equal to 120 ksi, a plastic strain ratio greater than or equal to 0.30, and a plastic strain to failure greater than or equal to 8.5%.
  • the alloy has a Ti content about 0.8% to about 1.1% and an Fe content between about 11.0% to about 16.0%.
  • the alloy has a Ti content between about 0.8% to about 1.0% and an Fe content between about 12.0% to about 16.0%.
  • the alloy has a Ti content between about 0.5% to about 0.8% and an Fe content between about 12.0% to about 16.0%.
  • the alloy in this form has a desired plastic strain ratio, i.e., greater than or equal to 0.30, the alloy still maintains a desired strength, i.e., greater than or equal to 120 ksi (827 MPa).
  • a desired strength i.e., greater than or equal to 120 ksi (827 MPa).
  • the alloy has a plastic strain ratio greater than or equal to 0.30, a plastic strain to failure greater than or equal to 8.5% and the yield strength is between about 120 ksi (827 MPa) and 150 ksi (1034 MPa).
  • the alloy has a plastic strain ratio greater than or equal to 0.35 and a plastic strain to failure greater than or equal to 9.0%.
  • the plastic strain ratio is greater than or equal to 0.45 and the plastic strain to failure is greater than or equal to 10.0%.
  • a Ni-based precipitation hardenable alloy has a composition, in wt.% of Cr from about 18.0% to about 23.0%, Fe from about 15.0% to about 21.0%, Mo from about 3.0% to about 4.5%, Nb from about 3.2% to about 5.2%, Ti from about 0.5% to about 1.3%, Al up to about 0.4%, Cu from about 0.5% to about 3.0%, and balance Ni and incidental impurities.
  • This alloy has a yield strength greater than or equal to 140 ksi, a plastic strain ratio greater than or equal to 0.30, and a plastic strain to failure greater than or equal to 8.0%.
  • the Ti content is about 0.8% to about 1.1% and the Fe content is between about 16.0% to about 21.0%.
  • the alloy has a Ti content between about 0.8% to about 1.0% and an Fe content between about 17.0% to about 20.0%.
  • the alloy has a Ti content between about 0.5% to about 0.8% and an Fe content between about 18.0% to about 21.0%.
  • this alloy has a desired plastic strain ratio, i.e., greater than or equal to 0.5, the alloy still maintains a desired strength, i.e., greater than or equal to 140 ksi (965 MPa).
  • the alloy has a plastic strain ratio greater than or equal to 0.30, a plastic strain to failure greater than or equal to 8.0% and the yield strength is between about 140 ksi (965 MPa) and 170 ksi (1172 MPa).
  • this alloy has a plastic strain ratio greater than or equal to 0.35 and a plastic strain to failure greater than or equal to 9.0%.
  • the plastic strain ratio is greater than or equal to 0.45 and the plastic strain to failure is greater than or equal to 10.0%.
  • Unified Numbering System (UNS) composition specifications for nine (9) nickel-based (Ni-base) precipitation hardenable alloys are shown.
  • Manganese (Mn) 0 - 0.2 0 - 0.35 0 - 0.35 0 - 1 0 - 1 0 - 1 0 - 0.5 0 - 0.5
  • the alloys shown in Table 1 are known to be used in a variety of industries and applications, some of which include down-hole components in oil field equipment, and for which enhanced HE resistance is desired. Alloys falling within the UNS specifications shown in Table 1 were subjected to HE testing (see Paper No. 13284, CORROSION 2019 Conference Proceedings; incorporated herein by reference). Also, the inventors performed a statistical analysis of the compositions of the alloys in Table 1 and discovered that the HE resistance of these alloys showed a trend of enhanced HE resistance as a function of decreasing Ti content and increasing Fe content. Particularly, the plastic strain ratio for the alloys was discovered to obey the following relationship based on statistical modeling:
  • Plastic strain ratio 0 .3461 + 0 .016572*Fe - 0 .2022*Ti
  • Table 2 four Ni-based alloys with varying amounts of chromium, iron, molybdenum, niobium, titanium and aluminum are shown. Particularly, specific alloys generally falling within the UNS N07716, UNS N07718, UNS N09925, and UNS N09945 composition ranges are shown in Table 2. It should be understood that the compositions of the alloys shown in Table 2 were obtained from Paper No. 4248 in the CORROSION 2014 Conference Proceedings (incorporated herein by reference) and may not include all of the alloying elements in the UNS specifications listed in the table.
  • the alloys in Table 2 were subjected to HE testing (see Paper No. 4248, CORROSION 2014 Conference Proceedings). Also, a statistical analysis of the compositions of the alloys in Table 2 and the HE resistance of these alloys similarly showed a trend of enhanced HE resistance as a function of decreased Ti content and increased Fe content. Particularly, the reduction in area ratio for testing in an HE environment to testing in an inert environment was discovered to obey the following relationship based on statistical modeling:
  • Ni-based precipitation hardenable alloys with varying amounts of chromium, iron, molybdenum, niobium, titanium and aluminum are shown. Particularly, specific alloys generally falling within the UNS N07725, UNS N07716, and UNS N07718 composition ranges are shown in Table 3. It should be understood that the compositions and names of the alloys shown in Table 3 were obtained from Paper No. 11114 in the CORROSION 2018 Conference Proceedings (incorporated herein by reference) and may not include all of the alloying elements provided in a corresponding UNS specification.
  • the alloys in Table 3 were subjected to HE testing (see Paper No. 11114, CORROSION 2018 Conference Proceedings). Also, a statistical analysis of the compositions of the alloys in Table 3 and the HE resistance of these alloys similarly showed a trend of enhanced HE resistance as a function of decreasing Ti content. Particularly, the reduction in fracture load for the alloys testing in an HE environment versus testing in an inert environment was discovered to obey the relationship based on statistical modeling:
  • the laboratory melted alloys in Table 4 were fabricated from 4-inch diameter 50-pound vacuum induction (VIM) melted ingots in the form of 0.625′′ diameter hot-rolled rod product.
  • the homogenized and hot-rolled rod samples were annealed at 1900° F.
  • Age-hardening was performed at 1350° F. for 8 hours with a furnace cool at 100° F. per hour to 1150° F. with a hold for 8 hours followed by air cooling.
  • Production melted alloys were fabricated from commercial VIM-melted material.
  • VIM electrodes at 18′′ diameter were vacuum arc re-melted (VAR) to 20′′ diameter and forged to finished diameter between 5 and 10′′ in diameter with a gyro-rotational forging machine (GFM).
  • VAR vacuum arc re-melted
  • the finished rods were annealed between 1850-1900° F.
  • Age-hardening was performed at between 1300-1365° F. for 5.5-8 hours with furnace cool at 50-100° F. per hour to 1150° F. with hold for 5.5-12 hours followed by air cooling.
  • the alloys in Table 5 were further subjected to HE resistance testing.
  • the HE resistance of each variant was tested per NACE TM0198 Method C slow strain rate testing procedure.
  • the slow strain rate test incorporates a slow, dynamic strain applied at a constant extension rate. It evaluates resistance to hydrogen induced stress cracking.
  • Table 7 summarizes the HE resistance average test results per heat. (Blank or no values indicate no test was completed for that alloy).
  • Ti content, Fe content, and yield strength each have an influence in HE resistance.
  • yield strength range of 120-170 ksi lower Ti content and higher Fe content correspond with increased HE resistance.
  • Table 8 shows a summary of composition ranges, plastic strain ratios and yield strengths for the new alloys according to the present disclosure.
  • a Ni-based precipitation hardenable alloy has a composition, in wt.% of Cr from about 18.0% to about 23.0%, Fe from about 7.0% to about 12.0%, Mo from about 6.5% to about 9.5%, Nb from about 3.2% to about 5.2%, Ti from about 0.3% to about 1.3%, Al up to about 0.4%, and balance Ni and incidental impurities and a plastic strain ratio greater than or equal to 0.35 or a plastic strain to failure of greater than or equal to 9.0 percent.
  • the alloy has a Ti content between about 0.8% to about 1.1%, while in other variations the alloy has a Ti content between about 0.8% to about 1.0%.
  • the alloys has a Ti content about 0.8% to about 1.1% and an Fe content between about 9.0% to about 12.0%.
  • the alloy has a Ti content between about 0.8% to about 1.0% and an Fe content between about 10.0% to about 12.0%.
  • additional alloying elements such as B, C, Co, Mn, P, Si, and S can be present in amounts corresponding to the UNS N07725 specification and/or normal melting practices for making Ni-based precipitation hardenable alloys while remaining within the scope of the present disclosure.
  • the alloy has a desired plastic strain ratio, i.e., greater than or equal to 0.35, the alloy also maintains a desired strength, i.e., greater than or equal to 120 ksi (827 MPa). That is, even with Ti reduced to lower levels within or below the Ti range for UNS N07725, the alloy still has a desired yield strength for down-hole components in oil field production.
  • the alloy has a plastic strain ratio is greater than or equal to 0.35 and the yield strength is between about 120 ksi (827 MPa) and 150 ksi (1034 MPa).
  • the alloy has a plastic strain ratio is greater than or equal to 0.3 and the yield strength is between about 130 ksi (896 MPa) and 150 ksi (1034 MPa). In another form, the alloy has a plastic strain ratio greater than or equal to 0.35, a plastic strain ratio greater than or equal to 9.0% and the yield strength is between about 140 ksi (965 MPa) and 150 ksi (1034 MPa). Also, in some variations the alloy has a plastic strain ratio greater than or equal to 0.40 and a plastic strain to failure greater than or equal to 10.0%. For example, in at least one variation, the plastic strain ratio is greater than or equal to 0.50 and the plastic strain to failure is greater than or equal to 12.0%.
  • a Ni-based precipitation hardenable alloy has a composition, in wt.% of Cr from about 18.0% to about 23.0%, Fe from about 9.0% to about 16.0%, Mo from about 4.5% to about 7.5%, Nb from about 3.2% to about 5.2%, Ti from about 0.4% to about 1.3%, Al up to about 0.4%, and balance Ni and incidental impurities and a plastic strain ratio greater than or equal to 0.3 or a plastic strain to failure of greater than or equal to 8.5 percent.
  • the alloy has a Ti content between about 0.8% to about 1.1%, while in other variations the alloy has a Ti content between about 0.8% to about 1.0%.
  • the alloy has a Ti content about 0.8% to about 1.1% and an Fe content between about 14.0% to about 17.0%. In still another form, the alloy has a Ti content between about 0.8% to about 1.0% and an Fe content between about 15.0% to about 17.0%. Also, additional alloying elements such as B, C, Co, Mn, P, Si, and S can be present in amounts corresponding to normal melting practices for making Ni-based precipitation hardenable alloys while remaining within the scope of the present disclosure.
  • the alloy has a desired plastic strain ratio, i.e., greater than or equal to 0.30, the alloy still maintains a desired strength, i.e., greater than or equal to 120 ksi (827 MPa).
  • the alloy has a plastic strain ratio greater than or equal to 0.30, a plastic strain to failure greater than or equal to 8.5% and the yield strength is between about 120 ksi (827 Mpa) and 150 ksi (1034 Mpa).
  • the alloy has a plastic strain ratio greater than or equal to 0.30, a plastic strain to failure greater than or equal to 8.5%, and the yield strength is between about 130 ksi (896 Mpa) and 150ksi (1034 Mpa).
  • the alloy has a plastic strain ratio greater than or equal to 0.30, a plastic strain to failure greater than or equal to 8.5% and the yield strength is between about 140 ksi (965 Mpa) and 150 ksi (1034 Mpa).
  • the alloy has an HE plastic strain ratio greater than or equal to 0.35 and a plastic strain to failure greater than or equal to 9.0%.
  • the plastic strain ratio is greater than or equal to 0.45 and the plastic strain to failure is greater than or equal to 10.0%.
  • a Ni-based precipitation hardenable alloy has a composition, in wt.% of Cr from about 18.0% to about 23.0%, Fe from about 15.0% to about 21.0%, Mo from about 3.0% to about 4.5%, Nb from about 3.2% to about 5.2%, Ti from about 0.5% to about 1.3%, Al up to about 0.4%, Cu from about 0.5% to about 3.0%, and balance Ni and incidental impurities and a plastic strain ratio greater than or equal to 0.3 or a plastic strain to failure of greater than or equal to 8.0 percent.
  • the alloy has a Ti content between about 0.8% to about 1.1%, while in another form, the alloy has a Ti content between about 0.8% to about 1.0%. In at least one variation, the alloy has a Ti content about 0.8% to about 1.1% and an Fe content between about 19.0% to about 22.0%. In yet another form, the alloy has a Ti content between about 0.8% to about 1.0% and an Fe content between about 20.0% to about 22.0%. Also, additional alloying elements such as B, C, Co, Mn, P, Si, and S can be present in amounts corresponding to the UNS N09946 specification and/or normal melting practices for making Ni-based precipitation hardenable alloys while remaining within the scope of the present disclosure.
  • additional alloying elements such as B, C, Co, Mn, P, Si, and S can be present in amounts corresponding to the UNS N09946 specification and/or normal melting practices for making Ni-based precipitation hardenable alloys while remaining within the scope of the present disclosure.
  • the alloy has a desired plastic strain ratio, i.e., greater than or equal to 0.3, the alloy still maintains a desired strength, i.e., greater than or equal to 140 ksi (965 MPa).
  • the alloy has a plastic strain ratio greater than or equal to 0.30, a plastic strain to failure greater than or equal to 8.0% and the yield strength is between about 140 ksi (965 MPa) and 170 ksi (1172 MPa).
  • the alloy has a plastic strain ratio greater than or equal to 0.30, a plastic strain to failure greater than or equal to 8.0%, and the yield strength is between about 145 ksi and 170 ksi (1172 MPa).
  • the alloy has a plastic strain ratio greater than or equal to 0.30, a plastic strain to failure greater than or equal to 8.0% and the yield strength is between about 150 ksi (1034 MPa) and 170 ksi (1172 MPa).
  • the alloy has a plastic strain ratio greater than or equal to 0.35 and a plastic strain to failure greater than or equal to 9.0%.
  • the plastic strain ratio is greater than or equal to 0.45 and the plastic strain to failure is greater than or equal to 10.0%.
  • HE resistance measures i.e. plastic strain to failure or plastic strain ratio
  • strengths i.e., yield strengths
  • a critical range of Ti is desired. That is, a critical range of Ti in the alloys has been discovered such that a desired HE resistance is provided or exceeded, while a desired level of yield strength is provided or exceeded.
  • the alloys have an undesirable (e.g., low) yield strength and for Ti levels greater than the maximum values shown in Table 8, the alloys have an undesirable (e.g., low) HE resistance.
  • a critical range of Ti and a critical range of Fe are desired. That is, a critical range of Ti and a critical range of Fe in the alloys have been discovered such that a desired HE resistance is provided or exceeded, a desired level of yield strength is provided or exceeded, and alloying elements such as Mo and Cr remain generally in solid solution, i.e., undesirable Mo- and/or Cr-rich precipitates (e.g., sigma phase) are not present in the new alloys.
  • compositions of the alloys shown in Table 8 include all incremental values between the minimum alloying element composition and maximum alloying element composition values listed above. That is, a minimum alloying element composition value for any of the alloys shown in Table 8 can range from the minimum value to the maximum value shown in the table. Likewise, the maximum alloying element composition value for any of the alloys shown in Table 8 can range from the maximum value shown to the minimum value shown in the table.
  • the minimum Ti content for the A- New Alloy 725 can be 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, or 1.3, and any value between these incremental values
  • the maximum Ti content for the A- New Alloy 725 can be 1.3, 1.2, 1.1, 1.0, 0.9, 0.8, 0.7, 0.6, 0.5, 0.4, or 0.3, and any value between these incremental values.
  • the yield strength of the alloys shown in Table 8 include all incremental values between the minimum yield strength and maximum yield strength values listed above. That is, a minimum yield strength value for any of the alloys shown in Table 8 can range from the minimum yield strength value to the maximum yield strength value shown in the table. Likewise, the maximum yield strength value for any of the alloys shown in Table 8 can range from the maximum yield strength value shown to the minimum yield strength value shown in the table.
  • the plastic strain ratio of the alloys shown in Table 8 include all incremental values between the minimum plastic strain ratio and maximum plastic strain ratio values listed above. That is, a minimum plastic strain ratio value for any of the alloys shown in Table 8 can range from the minimum plastic strain ratio value to the maximum plastic strain ratio value shown in the table.
  • the HE plastic strain of the alloys shown in Table 8 include all incremental values between the minimum plastic strain to failure and maximum plastic strain to failure values listed above. That is, a minimum plastic strain value for any of the alloys shown in Table 8 can range from the minimum plastic strain value to the maximum plastic strain value shown in the table.
  • the phrase at least one of A, B, and C should be construed to mean a logical (A OR B OR C), using a non-exclusive logical OR, and should not be construed to mean “at least one of A, at least one of B, and at least one of C.”

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IL82587A0 (en) * 1986-05-27 1987-11-30 Carpenter Technology Corp Nickel-base alloy and method for preparation thereof
WO2000003053A1 (fr) * 1998-07-09 2000-01-20 Inco Alloys International, Inc. Traitement thermique pour alliages a base de nickel
US9017490B2 (en) * 2007-11-19 2015-04-28 Huntington Alloys Corporation Ultra high strength alloy for severe oil and gas environments and method of preparation
US10253382B2 (en) * 2012-06-11 2019-04-09 Huntington Alloys Corporation High-strength corrosion-resistant tubing for oil and gas completion and drilling applications, and process for manufacturing thereof

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