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EP1270755B1 - Procédé de vieillissement d'alliages Ni-Cr-Mo - Google Patents

Procédé de vieillissement d'alliages Ni-Cr-Mo Download PDF

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Publication number
EP1270755B1
EP1270755B1 EP02014217.0A EP02014217A EP1270755B1 EP 1270755 B1 EP1270755 B1 EP 1270755B1 EP 02014217 A EP02014217 A EP 02014217A EP 1270755 B1 EP1270755 B1 EP 1270755B1
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Prior art keywords
alloy
alloys
hours
chromium
molybdenum
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EP02014217.0A
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German (de)
English (en)
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EP1270755A1 (fr
Inventor
Lee M. Pike, Jr.
Dwaine L. Klarstrom
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Haynes International Inc
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Haynes International Inc
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Priority claimed from US09/894,353 external-priority patent/US6579388B2/en
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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
    • 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
    • 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%

Definitions

  • the invention relates to heat treatment processes for nickel-chromium molybdenum-alloys having a chromium content of from 12 to 19 weight percent.
  • Ni-Cr-Mo alloys and particularly those with chromium content of 15 to 24% have been popular for use in corrosive environments such as encountered in the chemical and petrochemical industries.
  • Age-hardening is a process used in the metallurgical industry to give an alloy composition higher strength, as measured by its yield strength, tensile strength, and by notched stress rupture tests typically used in the art.
  • Various applications demand a combination of high tensile strength and low thermal expansion properties.
  • One such application is in the aerospace industry.
  • Another application is seal rings used in land-based gas turbines.
  • a combination of high tensile strength and ductility is also very useful for bolts. Because of the demanding operating conditions and performance parameters for metal products in these applications, various methods of age-hardening have been used.
  • One common technique is to heat the alloy to a selected high temperature, hold the alloy at that temperature for a period of time and then cool the alloy to room temperature.
  • the alloy may be heated to one temperature, cooled, heated again to a second temperature and cooled. Examples of these processes are disclosed in United States Patent No. 3,871,928 .
  • the temperatures and time periods used to age harden an alloy depend upon the composition of the alloy. For all age-hardenable commercial alloys there are established times and temperatures used that have become standard in the industry because they are known to produce the desired properties. For Ni-Cr-Mo alloys having high chromium content, that is chromium greater than 12%, the general view in the art is that heat treatment beyond the initial annealing in an effort to improve mechanical properties would be impractical due to the lengthy required times (hundreds to thousands of hours) and such treatments simply have not been done.
  • Ni-Cr-Mo alloys and nickel-molybdenum (Ni-Mo) alloys are widely utilized for commercial applications in the chemical industry, for example.
  • alloys such as these are not usually considered responsive to heat treatment, and are therefore used in the annealed condition.
  • HAYNES® 242TM alloy which will be discussed later.
  • Ni-Cr-Mo and Ni-Mo alloys are not commercially age-hardenable does not mean that they do not exhibit any metallurgical response to thermal exposure at intermediate temperatures.
  • alloys of this type can exhibit complex secondary phase reactions when exposed in the temperature range from about 538°C to 871°C.
  • the phases which form can often be deleterious to both alloy ductility and other aspects of service performance. This is particularly observed with Ni-Mo alloys containing about 25 to 30 % molybdenum. In such materials, exposure at temperatures from about 538°C to 871°C can result in the rapid formation of embrittling Ni 3 Mo or Ni 4 Mo phases in the microstructure. This can be a problem for both component manufacturing and for component performance.
  • Ni-Cr-Mo alloys with about 16 % molybdenum and 16 % chromium weight percent content
  • the occurrence of these particular intermetallic phases is not usually observed after short term thermal exposures.
  • Ni 2 (Mo,Cr) is evidenced in the microstructure.
  • a long-range-ordered phase, with structure similar to that of Pt 2 Mo, the Ni 2 (Mo,Cr) phase serves to significantly increase the strength of these materials without a severe loss of ductility.
  • the one major drawback is the prolonged aging time required to produce this phase.
  • United States Patent No. 4,818,486 discloses a low thermal expansion nickel based alloy that contains 5% to 12% chromium and 10% to 30% molybdenum.
  • the patent teaches that the aging times typically required to obtain desired hardness without deleterious phases being formed is well over 1000 hours at temperatures of 649°C to 816°C for most Ni-Mo-Cr alloys.
  • the aging time to harden the alloy composition disclosed in the '486 patent is as little as 24 hours at 649°C.
  • the alloy of this patent has been marketed under the trademarks 242 alloy and HAYNES 242 alloy.
  • HAYNES 242 alloy has been sold for applications requiring high tensile strength and a low coefficient of thermal expansion. Other beneficial properties of the 242 alloy include good thermal stability, good low cycle fatigue resistance, and excellent containment capabilities due to its tensile strength and ductility.
  • HAYNES 242 alloy consists of about 8 % (weight percent) chromium, about 20-30 % molybdenum, about 0.35 % to up to about 0.5 % aluminum, up to 0.03 % carbon, up to about 0.8 % manganese, up to about 0.8 % silicon, up to about 2 % iron, up to about 1 % cobalt, up to about 0.006 % boron, and the balance weight percent being nickel.
  • Ni-Cr-Mo alloy is disclosed in United States Patent No. 5,019,184 to Crum et al. That alloy contains 19% to 23% chromium and 14 to 17.5% molybdenum.
  • the patent discloses homogenization heat treatment at temperatures ranging from 1149°C to 1260°C for periods of from 5 to 50 hours. The purpose of the treatment is to produce a corrosion resistant alloy having a desired microstructure rather than to strengthen the alloy. No tensile strength data is given for any of these samples disclosed in the patent.
  • the alloy of this patent has been commercialized under the designation INCONEL® alloy 686.
  • Ni-Cr-Mo alloy Yet another corrosion resistant Ni-Cr-Mo alloy is disclosed in United States Patent No. 4,906,437 to Heubner et al. This alloy contains 22% to 24% chromium and 15% to 16.5% molybdenum. There is no disclosure of any heat treatment or age hardening of this alloy. The alloy disclosed in this patent has been commercialized under the designation VDM NICROFER 923 h Mo or Alloy 59.
  • Ni-Cr-Mo alloy A high yield strength Ni-Cr-Mo alloy is disclosed in United States Patent No. 4,129,464 to Matthews et al. This alloy contains 13% to 18% chromium and 13% to 18% molybdenum. The patent says that the alloy could be aged using a single step aging treatment of at least 50 hours at 480°C to 593°C, but all examples are aged 168 hours or more. The statement that at least 50 hours is required was an extrapolation of the results obtained from a 168 hours aging treatment. The patent reports data for three alloys numbered 1, 2 and 3. Alloy 1 is commercially available under the trademark HASTELLOY® C-276 alloy. Alloy 2 is commercially available as HASTELLOY C-4 alloy. Alloy 3 is commercially available as HASTELLOY S alloy. Further nickel-chromium-molybdenum age hardenable alloys are disclosed in WO 98/55661 or EP499969 .
  • the alloys are aged at about 593°C to 718°C for at least 4 and preferably 48 hours and then air cooled. When so treated the alloys will have tensile properties suitable for use in applications requiring high tensile strength and ductility.
  • high chromium content nickel based alloys having a combination of high yield strength and ductility properties can be made at lower cost than other alloys having such properties. Consequently, the present alloy is a more affordable alloy for applications requiring such properties.
  • Ni-Cr-Mo commercial alloys whose compositions are set forth in Table 1.
  • the commercial alloys were HASTELLOY S sheet, HASTELLOY C-276 sheet, and HASTELLOY C-4 sheet and plate. The thickness of each sheet was 3.2 mm and the plate was 9.5 mm thick. The designation "n.m.” in Table 1 indicates that the presence of an element was not measured. Table 1 also reports the P value for each alloy.
  • the chromium content of the test alloys ranged from 11.56% for alloy 6 to 22.28% for alloy 10. Molybdenum ranged from 14.73% in alloy 10 to 23.89% in alloy 13. All of the alloys contained similar amounts of aluminum, cobalt, iron, and manganese. Tungsten was present within a range of 0.13% to 0.34%. The alloys also contained small amounts of boron, carbon, cerium, copper, magnesium, phosphorus, sulfur, silicon, and vanadium. The test alloys were annealed after hot rolling to 12.7 mm plate at annealing temperatures in the range of 1038°C to 1093°C for thirty minutes and water quenched. The commercial alloys were cut from sheets or plate available from the manufacturer.
  • test alloys were treated with a single-step aging treatment in which they were aged at 649°C for 48 hours. Then they were air cooled to room temperature.
  • the commercial alloys HASTELLOY S, HASTELLOY C-276 and HASTELLOY C-4 alloys were aged at 593°C for 50 hours. Then they were air cooled to room temperature. This 50 hour treatment corresponds to the treatment proposed for those alloys by Matthews et al. in United States Patent No. 4,129,464 .
  • alloy 12 To be acceptable an alloy must have elongation values greater than 40 percent and yield strengths greater than 500 MPa. Alloys 1, 2, 3, 8 and 9 all had acceptable properties. Alloys 12 and 13 did not possess enough tensile ductility as measured by the percent elongation. Alloys 4, 5, 6, 7, 10 and 11 did not possess a high enough yield strength. Since the chromium content and molybdenum content of alloy 12 is within the range of chromium content and molybdenum content of the acceptable alloys it is clear that neither chromium content nor molybdenum content is the sole predictor of acceptable tensile properties in this class of alloys. We concluded that it is the interaction of nearly all of the alloying elements that is the predictor of such properties.
  • Figure 1 is a graph of the tested alloys based upon the P value of the alloy and the chromium content. Each alloy that had acceptable tensile properties is plotted with a dot. An X is used to plot those alloys whose tensile properties were not acceptable after the alloy was subjected to the two-step aging treatment. A box has been drawn around the acceptable alloys. It is readily apparent from Figure 1 that the acceptable alloys have a chromium content of 12% to 19% and a P value within the range of 31.2 to 35.9.
  • Figure 2 is a graph similar to Figure 1 but plots the P value of the alloy against the molybdenum content. As shown in Figure 2 , the acceptable alloys contain from 18% to 23% molybdenum. The fact that Alloy 4 did not pass the tensile property requirements even though its chromium content is within the desired range indicates that molybdenum content is also critical. Alloy 4 had only 17% molybdenum.
  • a sample was determined to have age hardened if it had a Rockwell C (Rc) hardness value of more than 20.0.
  • Rc Rockwell C
  • a sample in the unaged condition confirmed that the material started out with a hardness of less than 20.0.
  • All samples given aging treatments at 649°C for about 24 to 48 hours were found to strongly age harden.
  • the samples of Alloy 2 aged at 677°C and 704°C for 48 hours did not harden.
  • samples of Alloy 8 did age harden when treated at 677°C and 704°C for 48 hours. Indeed, Alloy 8 age hardened when treated at 677°C for times ranging from 4 hours to 48 hours.
  • Alloy 8 age hardening did not occur in Alloy 8 at 8 or 12 hours, but did occur when the treatment time was 16 and 48 hours. Furthermore, Alloy 8 age hardened when treated at 718°C for 48 hours. The difference between the responses of Alloys 2 and 8 to heat treatment times and temperatures can be attributed to the fact that Alloy 8 has higher molybdenum and lower chromium than Alloy 2. The test results indicate that the alloy should be age hardened for at least about 4 hours at a temperature ranging from about 593°C to about 718°C. Even though the longest aging time used in our tests was 48 hours longer aging times could be used.
  • the age-hardening treatment here disclosed be done in a total time of less than 100 hours and preferably less than 50 hours. Indeed we prefer to complete the process in 48 hours. By using heat treatments totaling less than 100 hours, and preferably not greater than 50 hours, one can produce lower cost, high chromium, Ni-Cr-Mo alloys that have desirable tensile properties. While the process here disclosed may also work when total aging times exceed 100 hours, the energy costs associated with such treatments make the process less desirable and commercially impractical.

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  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Heat Treatment Of Steel (AREA)
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Claims (8)

  1. Alliage de nickel-chrome-molybdène durci par vieillissement, ayant une valeur de dureté Rc supérieure à 20 Rockwell et ayant une limite d'élasticité supérieure constitué en pourcentage en poids de 12 % à 19 % de chrome, de 18 % à 23 % de molybdène ; jusqu'à 3 % de fer ; jusqu'à 0,5 % d'aluminium ; jusqu'à 0,015 % de bore ; jusqu'à 0,02 % de carbone ; jusqu'à 2,5 % de cobalt ; jusqu'à 1,5 % de manganèse ; jusqu'à 1,25 % de niobium ; jusqu'à 0,75 % de silicium ; jusqu'à 2,2 % de tantale ; jusqu'à 0,7 % de titane ; jusqu'à 4,5 % de tungstène ; jusqu'à 2,0 % de cuivre ; jusqu'à 0,035 % de vanadium ; éventuellement jusqu'à 0,1 % d'un élément des terres rares ; éventuellement jusqu'à 0,03 % de soufre ; éventuellement jusqu'à 0,04 % de phosphore ; et
    un complément de nickel plus des impuretés; l'alliage ayant une valeur P de 31,2 à 35,9, P étant définie comme : P = 2 , 46 Al + 0 , 19 Co + 0 , 83 Cr - 0 , 16 Cu + 0 , 39 Fe + 0 , 59 Mn + 1 , 0 Mo + 0 , 81 Zr + 2 , 15 Si Si + 1 , 06 V + 0 , 39 W + 0 , 68 Nb + 0 , 52 Hf + 0 , 45 Ta + 1 , 35 Ti
    Figure imgb0009
    et l'alliage étant durci par vieillissement à une température de 593°C à 718°C pendant au moins 4 heures, puis refroidi à température ambiante.
  2. Alliage de nickel-chrome-molybdène durci par vieillissement, ayant une valeur de dureté Rc supérieure à 20 Rockwell et ayant une limite d'élasticité supérieure, constitué en pourcentage en poids de 12 % à 19 % de chrome, de 18 % à 23 % de molybdène ; de 0,12 % à 0,2 % d'aluminium ; de 0,002 % à 0,006 % de carbone ; de 0,30 % à 0,34 % de manganèse ; de 1,0 % à 1,7 % de fer ; de 0,05 % à 0,8 % de cobalt ; de 0,10 % à 0,34 % de tungstène ; et de 0,002 % à 0,005 % de bore ;
    l'alliage comprenant également éventuellement :
    de 0,005 % à 0,009 % de cérium, et
    de 0,01 % à 0,06 % de cuivre, et
    de 0,001 % à 0,004 % de magnésium, et
    de 0,002 à 0,005 % de phosphore, et
    de 0,001 % à 0,004 % de soufre ; et
    de 0,01 % à 0,02 % de vanadium ;
    et un complément de nickel plus des impuretés;
    l'alliage ayant une valeur P de 31,2 à 35,9, P étant définie comme : P = 2 , 46 Al + 0 , 19 Co + 0 , 83 Cr - 0 , 16 Cu + 0 , 39 Fe + 0 , 59 Mn + 1 , 0 Mo + 0 , 81 Zr + 2 , 15 Si + Si + 1 , 06 V + 0 , 39 W + 0 , 68 Nb + 0 , 52 Hf + 0 , 45 Ta + 1 , 35 Ti
    Figure imgb0010
    et l'alliage étant durci par vieillissement à une température de 593°C à 718°C pendant au moins 4 heures, puis refroidi à température ambiante.
  3. Alliage selon l'une quelconque des revendications précédentes, l'alliage étant durci par vieillissement en pas plus de 50 heures.
  4. Alliage selon l'une quelconque des revendications précédentes, l'alliage étant durci par vieillissement à environ 649°C pendant 48 heures.
  5. Méthode de traitement d'un alliage de nickelchrome-molybdène durci par vieillissement ayant une valeur de dureté Rc supérieure à 20 Rockwell et ayant une limite d'élasticité supérieure, constitué en pourcentage en poids de 12 % à 19 % de chrome, de 18 % à 23 % de molybdène ; jusqu'à 0,5 % d'aluminium ; jusqu'à 0,015 % de borne ; jusqu'à 0,02 % de carbone ; jusqu'à 2,5 % de cobalt ; jusqu'à 3 % de fer ; jusqu'à 1,5 % de manganèse ; jusqu'à 1,25 % de niobium ; jusqu'à 0,75 % de silicium ; jusqu'à 2,2 % de tantale ; jusqu'à 0,7 % de titane ; jusqu'à 4,5 % de tungstène ; jusqu'à 2,0 % de cuivre ; jusqu'à 0,035 % de vanadium ; éventuellement jusqu'à 0,1 % d'un élément des terres rares ; éventuellement jusqu'à 0,03 % de soufre ; éventuellement jusqu'à à 0,04 % de phosphore ; et le complément de nickel plus des impuretés; l'alliage ayant une valeur P de 31,2 à à 35,9, P étant définie comme : P = 2 , 46 Al + 0 , 19 Co + 0 , 83 Cr - 0 , 16 Cu + 0 , 39 Fe + 0 , 59 Mn + 1 , 0 Mo + 0 , 81 Zr + 2 , 15 Si + Si + 1 , 06 V + 0 , 39 W + 0 , 68 Nb + 0 , 52 Hf + 0 , 45 Ta + 1 , 35 Ti
    Figure imgb0011
    la méthode comprenant : le durcissement par vieillissement de l'alliage à une température de 593°C à 718°C pendant au moins 4 heures ;
    et le refroidissement de l'alliage à température ambiante.
  6. Méthode selon la revendication 5, dans laquelle l'alliage est durci par vieillissement en pas plus de 50 heures.
  7. Méthode selon la revendication 5, dans laquelle l'alliage est durci par vieillissement à 649°C pendant 48 heures.
  8. Méthode selon la revendication 5, dans laquelle l'alliage est durci par vieillissement en pas plus de 24 heures.
EP02014217.0A 2001-06-28 2002-06-26 Procédé de vieillissement d'alliages Ni-Cr-Mo Expired - Lifetime EP1270755B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US894353 2001-06-28
US09/894,353 US6579388B2 (en) 2001-06-28 2001-06-28 Aging treatment for Ni-Cr-Mo alloys
US10/165,649 US6610155B2 (en) 2001-06-28 2002-06-07 Aging treatment for Ni-Cr-Mo alloys
US165649 2002-06-07

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EP1270755B1 true EP1270755B1 (fr) 2014-03-26

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JP (1) JP4977302B2 (fr)
KR (1) KR20030003016A (fr)
CN (1) CN1249260C (fr)
AU (1) AU784826B2 (fr)
CA (1) CA2391909C (fr)
GB (1) GB2377945B (fr)
MX (1) MXPA02006451A (fr)
TW (1) TWI226906B (fr)

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CN114182139B (zh) * 2021-12-10 2022-12-02 西北工业大学 一种析出强化镍基高温合金及其制备方法

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AU784826B2 (en) 2006-06-29
AU5064602A (en) 2003-01-02
JP4977302B2 (ja) 2012-07-18
EP1270755A1 (fr) 2003-01-02
GB0214715D0 (en) 2002-08-07
MXPA02006451A (es) 2005-02-03
CN1407124A (zh) 2003-04-02
JP2003064436A (ja) 2003-03-05
CA2391909C (fr) 2006-01-10
CA2391909A1 (fr) 2002-12-28
KR20030003016A (ko) 2003-01-09
CN1249260C (zh) 2006-04-05
TWI226906B (en) 2005-01-21
GB2377945A (en) 2003-01-29

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