EP1270754B1 - Two-step aging treatment for Ni-Cr-Mo alloys - Google Patents

Two-step aging treatment for Ni-Cr-Mo alloys Download PDF

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Publication number
EP1270754B1
EP1270754B1 EP02014216A EP02014216A EP1270754B1 EP 1270754 B1 EP1270754 B1 EP 1270754B1 EP 02014216 A EP02014216 A EP 02014216A EP 02014216 A EP02014216 A EP 02014216A EP 1270754 B1 EP1270754 B1 EP 1270754B1
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EP
European Patent Office
Prior art keywords
alloy
hours
temperature
alloys
cooling
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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EP02014216A
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German (de)
English (en)
French (fr)
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EP1270754A1 (en
Inventor
Lee M. Pike, Jr.
Dwaine L. Klarstrom
Michael F. Rothman
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Haynes International Inc
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Haynes International Inc
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Priority claimed from US09/894,179 external-priority patent/US6544362B2/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
    • 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
    • C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
    • 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 invention relates to heat treatment processes for nickel-chromium molybdenum-alloys having a chromium content of from 12 to 23.5 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% 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 482°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 improved age-hardening process involves an alloy with this P value that has been given an age hardening treatment at about 704°C for at least 8 hours and preferably for about 12 to 20 hours, furnace cooling to a temperature from about 538°C to about 718°C and holding the material at that temperature for at least 8 hours and preferably for about 28 to 36 hours, followed by air cooling to room temperature.
  • a Ni-Cr-Mo alloy having 12% to 23.5% chromium and treated with this two-step heat treatment or age-hardening process shows improved or comparable tensile strength to the standard aging process used in the lower chromium level 242 alloy. Because of the combination of high yield strength and ductility properties, the alloy and two-step aging process significantly increase affordability of this alloy for applications requiring such properties.
  • This age hardening process involves aging the alloy at about 691°C to about 760°C for from 8 to 20 hours, cooling the alloy to a temperature of at from about 538°C to about 718°C, maintaining the alloy within that temperature range for at least 8 hours and preferably for from 24 to 36 hours and cooling the alloy to room temperature.
  • Ni-Cr-Mo commercial alloys whose compositions are set forth in Table 1.
  • the commercial alloys were HASTELLOY S sheet, HASTELLOY C-276 plate, HASTELLOY C-4 plate, Alloy 59 sheet and INCONEL alloy 686 sheet.
  • 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 H to 26.06% for alloy P. Molybdenum ranged from 9.91% in alloy G to 23.89% in alloy S. All of the alloys contained similar amounts of aluminum, cobalt, iron, and manganese. Tungsten was present within a range of 0.11% 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 12.7mm plate at annealing temperatures in the range of 1038°C to 1093°C for thirty minutes. The commercial alloys were cut from sheets and plates available from the manufacturer.
  • 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 23.5% and a P value within the range of 31.2 to 35.9.
  • the test results for Alloy M indicate that the first step should be at least about 8 hours long at a temperature ranging from about 691°C to about 760°C while the second step should be at least about 24 hours long at a temperature ranging from about 538°C to about 691°C.
  • the data also indicates that when a higher temperature is used for the first step then a lower temperature can be used for the second step. While first step temperatures of up to 927°C were found to be useful in age hardening the alloy, microstructural examination revealed that an undesirable grain boundary precipitation occurred when the first step temperature was 760°C or greater. This precipitation would be expected to degrade corrosion resistance.
  • Ni 2 (Mo,Cr) age hardening begins with short range ordering followed by creation of precipitates that impart the hardening property. Upon continued heating a solvus temperature will be reached at which the precipitates will go back into solution.
  • the short range ordering is also related to time and temperature. Both the short range ordering and the solvus temperature vary from one- alloy composition to another. To provide age hardening any two-step aging treatment must involve a selection of times and temperatures that provides either the necessary short range ordering or the initial precipitation of the hardening phase in the first step and avoids the solvus during the second step. This can be seen in the data for Alloy M in Table 3.
  • Alloy K has higher molybdenum and lower chromium than Alloys M, N and O. Alloy K was tested at 704°C, 732°C and 760°C for 8, 16 and 32 hours as shown in Table 4. The data shows that the first treatment could be 8 hours at 760°C when the second step was conducted for 40 hours at 704°C or 718°C but not at 732°C. The second step could be run for 8 hours at 704°C when the first step was conducted for 32 hours at 732°C. From this data we conclude that higher temperatures can be used in the second step for alloys having higher molybdenum and lower chromium. Moreover, either step can be as short as 8 hours when the other step is 32 to 40 hours.
  • an acceptable age hardening response can be obtained when the first step is at least about 8 hours long at a temperature ranging from about 691°C to about 760°C and the second step is at least about 8 hours long at a temperature of from about 538°C to about 718°C.
  • the two-step age-hardening treatment here disclosed can 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 from 40 to 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)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Heat Treatment Of Steel (AREA)
  • Turbine Rotor Nozzle Sealing (AREA)
  • Heat Treatment Of Articles (AREA)
  • Heat Treatment Of Nonferrous Metals Or Alloys (AREA)
EP02014216A 2001-06-28 2002-06-26 Two-step aging treatment for Ni-Cr-Mo alloys Expired - Lifetime EP1270754B1 (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US165650 1988-03-08
US894179 2001-06-28
US09/894,179 US6544362B2 (en) 2001-06-28 2001-06-28 Two step aging treatment for Ni-Cr-Mo alloys
US10/165,650 US6638373B2 (en) 2001-06-28 2002-06-07 Two step aging treatment for Ni-Cr-Mo alloys

Publications (2)

Publication Number Publication Date
EP1270754A1 EP1270754A1 (en) 2003-01-02
EP1270754B1 true EP1270754B1 (en) 2012-04-25

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EP (1) EP1270754B1 (enExample)
JP (1) JP4206229B2 (enExample)
KR (1) KR20030003017A (enExample)
CN (1) CN1246490C (enExample)
AU (1) AU785025B2 (enExample)
CA (1) CA2391903C (enExample)
GB (1) GB2377944B (enExample)
MX (1) MXPA02006453A (enExample)
TW (1) TWI224146B (enExample)

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KR20030003016A (ko) * 2001-06-28 2003-01-09 하이네스인터내셔널인코포레이티드 Ｎｉ-Ｃｒ-Ｍｏ합금의 에이징 처리방법 및 결과의 합금
US6860948B1 (en) * 2003-09-05 2005-03-01 Haynes International, Inc. Age-hardenable, corrosion resistant Ni—Cr—Mo alloys
RU2321653C1 (ru) * 2006-05-31 2008-04-10 Юлия Алексеевна Щепочкина Сплав на основе никеля
US7785532B2 (en) 2006-08-09 2010-08-31 Haynes International, Inc. Hybrid corrosion-resistant nickel alloys
RU2330083C1 (ru) * 2006-10-09 2008-07-27 Юлия Алексеевна Щепочкина Сплав на основе никеля
JP4816950B2 (ja) * 2006-11-10 2011-11-16 三菱マテリアル株式会社 耐食性および耐摩耗性に優れたＮｉ基合金およびそのＮｉ基合金からなるコンダクターロール
CN101333613B (zh) * 2008-08-06 2010-06-09 钢铁研究总院 一种中温平板式固体氧化物燃料电池金属连接体用镍基膨胀合金
DE102011013091A1 (de) * 2010-03-16 2011-12-22 Thyssenkrupp Vdm Gmbh Nickel-Chrom-Kobalt-Molybdän-Legierung
US9761883B2 (en) * 2011-11-03 2017-09-12 Johnson Controls Technology Company Battery grid with varied corrosion resistance
CN103740983B (zh) * 2013-12-19 2015-11-04 重庆材料研究院有限公司 高强韧耐腐蚀时效强化型镍基合金及直接时效热处理方法
JP5725630B1 (ja) * 2014-02-26 2015-05-27 日立金属Ｍｍｃスーパーアロイ株式会社 熱間鍛造性および耐食性に優れたＮｉ基合金
EP3574541A1 (en) 2017-01-27 2019-12-04 CPS Technology Holdings LLC Battery grid
RU2672647C1 (ru) * 2017-08-01 2018-11-16 Акционерное общество "Чепецкий механический завод" Коррозионностойкий сплав
WO2021045183A1 (ja) * 2019-09-06 2021-03-11 日立金属株式会社 Ｎｉ基合金、Ｎｉ基合金粉末、Ｎｉ基合金部材、およびＮｉ基合金部材を備えた製造物
CN114045452A (zh) * 2021-11-15 2022-02-15 贵州航宇科技发展股份有限公司 一种Haynes242合金锻件的锻造及热处理方法
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
CN116083755A (zh) * 2023-02-28 2023-05-09 广东博盈特焊技术股份有限公司 一种激光熔覆用耐高温腐蚀合金粉末及其制备方法和用途
CN116716518B (zh) * 2023-06-30 2024-02-09 江西宝顺昌特种合金制造有限公司 一种哈氏合金c-4管板及其制备方法
CN120119193B (zh) * 2025-04-01 2025-08-26 内蒙古电力(集团)有限责任公司内蒙古电力科学研究院分公司 一种gh4169高温合金加速老化方法

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TWI224146B (en) 2004-11-21
CN1246490C (zh) 2006-03-22
GB0214712D0 (en) 2002-08-07
GB2377944A (en) 2003-01-29
CN1412331A (zh) 2003-04-23
MXPA02006453A (es) 2004-05-05
EP1270754A1 (en) 2003-01-02
AU5064502A (en) 2003-01-02
GB2377944B (en) 2005-03-23
AU785025B2 (en) 2006-08-24
JP4206229B2 (ja) 2009-01-07
JP2003027163A (ja) 2003-01-29
CA2391903A1 (en) 2002-12-28
KR20030003017A (ko) 2003-01-09
GB2377944A9 (en) 2003-03-13
CA2391903C (en) 2009-09-29

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