EP2889387B1 - Alliage à base de ni ayant une excellente résistance à la fragilisation par l'hydrogène et un procédé de fabrication d'une matière d'alliage à base de ni - Google Patents

Alliage à base de ni ayant une excellente résistance à la fragilisation par l'hydrogène et un procédé de fabrication d'une matière d'alliage à base de ni Download PDF

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Publication number
EP2889387B1
EP2889387B1 EP13831112.1A EP13831112A EP2889387B1 EP 2889387 B1 EP2889387 B1 EP 2889387B1 EP 13831112 A EP13831112 A EP 13831112A EP 2889387 B1 EP2889387 B1 EP 2889387B1
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Prior art keywords
based alloy
hydrogen
hydrogen embrittlement
less
temperature
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German (de)
English (en)
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EP2889387A1 (fr
EP2889387A4 (fr
Inventor
Kouichi Takasawa
Eiji Maeda
Shinya Sato
Takashi Hatano
Tatsuya Takahashi
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Japan Steel Works Ltd
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Japan Steel Works Ltd
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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
    • C22C19/056—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
    • 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
    • C22C30/00—Alloys containing less than 50% by weight of each constituent

Definitions

  • the present invention relates to a Ni-based alloy having excellent hydrogen embrittlement resistance and a method for producing a Ni-based alloy material.
  • ammonothermal method has been known as a kind of single crystal growing method and the ammonothermal method has been, for example, applied to single crystal growth of gallium nitride that is a nitride semiconductor for a blue light emitting diode.
  • Gallium nitride has been expected to be utilized as an optical device such as a high-brightness LED and a semiconductor laser, and an electronic device for use in a transistor for electric vehicle, an amplifier for mobile phone base station, or the like.
  • an optical device such as a high-brightness LED and a semiconductor laser
  • an electronic device for use in a transistor for electric vehicle, an amplifier for mobile phone base station, or the like For the application to these devices, it is necessary to enlarge the size of the gallium nitride single crystal and a size of 2 inches or more to 6 inches or more, further a size larger than that has been desired.
  • a vapor-phase growth method has been a main stream for the growth of the gallium nitride single crystal.
  • the method is being replaced by the ammonothermal method in which a crystal is grown in high-temperature and high-pressure ammonia. Since a temperature of 600 to 650°C and a pressure of 200 to 250 MPa are generally used as synthetic conditions in the ammonothermal method, application of a Ni-Fe-based alloy is attempted as a pressure vessel material having high strength under a high-temperature environment.
  • Patent Document 1 discloses a technique relating to an Fe-Ni-based alloy having high strength and excellent hydrogen embrittlement resistance, which is used as a high-pressure hydrogen piping material for hydrogen station.
  • the document presents a two-layer structure piping material consisting of an outer layer having high strength imparted thereto by aging and an inner layer having hydrogen embrittlement resistance imparted thereto.
  • Patent Document 2 discloses a Ni-Fe alloy in which high strength and hydrogen embrittlement resistance are exhibited by controlling particle size of the ⁇ ' phase and fractions of individual precipitation phases.
  • Patent Document 3 discloses a technique dealing with hydrogen embrittlement resistance and the like at high temperature.
  • Patent Document 4 discloses a Ni-Fe based forging superalloy, which is excellent in high-temperature strength and high-temperature ductility, the superalloy comprising 30 to 40 wt% of iron, 14 to 16 wt% of chromium, 1.2 to 1.7 wt% of titanium, 1.1 to 1.5 wt% of aluminum, 1.9 to 2.7 wt% of niobium, 0.05 wt% or less of carbon, and the remainder being nickel and inevitable impurities, wherein the ⁇ -phase (Ni 3 Al) having an initial mean particle size of 50 to 100 nm is precipitated.
  • the superalloy comprising 30 to 40 wt% of iron, 14 to 16 wt% of chromium, 1.2 to 1.7 wt% of titanium, 1.1 to 1.5 wt% of aluminum, 1.9 to 2.7 wt% of niobium, 0.05 wt% or less of carbon, and the remainder being nickel and inevitable impurities, wherein
  • Patent Documents 1 and 2 the temperature at which the alloys have high strength and excellent hydrogen embrittlement resistance is room temperature in Patent Documents 1 and 2 and it is unclear whether these characteristics may be assured or not under high temperature and high pressure.
  • Patent Document 3 deals with a high Ni-based alloy having high strength and excellent hydrogen embrittlement resistance, which is usable at 200 to 500°C, it is considered that characteristics at 600 to 650°C, which are problems of the present invention, cannot be secured in the alloy and also characteristics under high pressure cannot be assured at all.
  • any of the conventional Ni-Fe-based alloys having high strength and excellent hydrogen embrittlement resistance cannot assure those characteristics under the conditions dealt with in the present invention.
  • the present invention has been made based on the above circumstances and an object thereof is to provide a Ni-based alloy having high strength and excellent hydrogen embrittlement resistance even in a high-temperature and high pressure environment, such as 600 to 650°C and 200 to 250 MPa, and a method for producing a Ni-based alloy material.
  • the present inventors have found that a Ni-based alloy having high strength and excellent hydrogen embrittlement resistance even under high temperature and high pressure is obtained by restricting the composition of the Ni-based alloy to a specific range and thus they have accomplished the present invention.
  • the gist of the invention lies on the following ⁇ 1> to ⁇ 7>.
  • Ni-based alloy having good hydrogen embrittlement resistance at such a high temperature as 600°C or higher and excellent creep properties in such a higher-temperature region as 700°C. Furthermore, as a secondary effect, application of the Ni-based alloy to a pressure vessel material for an ammonothermal method enables production of a pressure vessel capable of coping with a higher-temperature and higher-pressure environment and thus, for example, it is expected that enlargement, mass production, and cost reduction of a gallium nitride single crystal useful as an electronic device may be remarkably advanced.
  • the Ni-based alloy according to the invention consists of, in terms of mass ratios, Fe: 30 to 40%, Cr: 14 to 16%, Ti: 1.2 to 1.7%, Al: 1.1 to 1.5%, Nb: 1.9 to 2.7%, and P: 40 to 150 ppm, and optionally Mg: 0.01% or less, Zr: 0.1% or less, with the remainder being Ni and unavoidable impurities.
  • the Ni-based alloy further includes at least either one of Mg: 0.01% or less and Zr: 0.1% or less.
  • Fe is effective for cost reduction of the alloy when the content thereof increases but a Laves phase forms when Fe is excessively incorporated together with Nb incorporation and the formation invites deterioration of material characteristics, such as an increase in hydrogen embrittlement susceptibility. Therefore, the content of Fe is controlled to 30 to 40%. For the same reason, it is preferable to determine the lower limit thereof to 33% and the upper limit thereof to 38%.
  • Cr is an element necessary for enhancing oxidation resistance, corrosion resistance, and strength. Also, it combines with C to form a carbide, thereby enhancing high-temperature strength. However, too large content thereof invites destabilization of matrix and promotes the formation of harmful TCP phases such as a ⁇ phase and ⁇ -Cr, resulting in adverse influences on ductility and toughness. Also, there is a concern that the ⁇ phase acts as a hydrogen accumulation site in the alloy to enhance the hydrogen embrittlement susceptibility. Therefore, the content of Cr is limited to 14 to 16%.
  • Ti mainly forms a MC carbide to suppress crystal grain coarsening of the alloy and also combines with Ni to precipitate a ⁇ ' phase, thereby contributing to precipitation strengthening of the alloy.
  • the stability of the ⁇ ' phase at high temperature is lowered and an ⁇ phase is formed, thereby impairing strength, ductility, toughness, and high-temperature long-term structural stability.
  • the ⁇ phase also acts as a hydrogen accumulation site in the alloy to enhance the hydrogen embrittlement susceptibility. Therefore, the content of Ti is limited to the range of 1.2 to 1.7%.
  • Al combines with Ni to precipitate a ⁇ ' phase, thereby contributing to precipitation strengthening of the alloy.
  • the ⁇ ' phase aggregates at grain boundaries and is coarsened, thereby drastically impairing mechanical properties at high temperature and also lowering hot workability. Therefore, the content of Al is limited to 1.1 to 1.5%.
  • Nb is an element that stabilizes the ⁇ ' phase and contributes to strength enhancement but when Nb is exceedingly incorporated, the precipitation of the ⁇ phase, the ⁇ phase, and the Laves phase that are harmful phases is promoted, thereby remarkably lowering the structural stability and enhancing the hydrogen embrittlement susceptibility. Therefore, the content of Nb is limited to 1.9 to 2.7%.
  • P is considered to have an effect of suppressing excessive accumulation of hydrogen at grain boundaries by increasing consistency of the grain boundaries and lowering the hydrogen embrittlement susceptibility, so that P is incorporated.
  • a P content of 40 ppm or more is necessary.
  • P has effects of lengthening the creep rupture time and decreasing the minimum creep rate.
  • the content of P is limited to 40 to 150 ppm. For the same reason, it is preferable to determine the lower limit thereof to 45 ppm and the upper limit thereof to 140 ppm.
  • Mg mainly combines with S to form a sulfide and enhances hot workability, so that Mg is incorporated as desired.
  • the content of Mg is preferably controlled to 0.01% or less.
  • the lower limit of the Mg content is more preferably controlled to 0.0005% or more.
  • Zr segregates at grain boundaries to contribute to an improvement in high-temperature characteristics, so that Zr is incorporated as desired.
  • the hot workability of the alloy is lowered, so that the content of Zr is preferably controlled to 0.1% or less.
  • Mg and Zr are contained in the above ranges but it is more preferable to contain both of Mg and Zr in view of securing good hot workability.
  • the remainder in the Ni-based alloy according to the invention is Ni and unavoidable impurities.
  • the unavoidable impurities mean elements which are initially contained in raw materials of the alloy or are unavoidably mixed in during the smelting of the alloy, and examples thereof include O, N and S.
  • the content of the unavoidable impurities in the whole Ni-based alloy is preferably as low as possible and is more preferably 50 ppm or less in view of high purification of the alloy.
  • the Ni-based alloy of the invention has excellent hydrogen embrittlement resistance and can be suitably used as a material to be exposed to a hydrogen atmosphere. Also, it is excellent in high strength characteristic at high temperature and can be suitably used as an ammonothermal pressure vessel material.
  • the Ni-based alloy of the invention can be smelted by a usual method and, as the invention, the smelting method is not particularly limited.
  • the Ni-based alloy of the invention can be subjected to processing such as forging as desired and can be subjected to a solution treatment or a thermal treatment by aging (aging treatment).
  • the solution treatment can be performed, for example, under conditions of 1,040 to 1,140°C for 4 to 10 hours.
  • the aging treatment is preferably a treatment performed in at least two stages.
  • the aging treatment can be performed twice at a temperature of 825 to 855°C and at a temperature of 710 to 740°C.
  • the treatment is preferably performed first at a temperature of 825 to 855°C (first stage) and subsequently at a temperature of 710 to 740°C (second stage) in this order.
  • the time for the aging treatment is more preferably from 4 to 10 hours at the first stage and from 4 to 24 hours at the second stage.
  • tensile strength at room temperature and high tensile strength at a high temperature of 600°C or higher can be secured and a Ni-based alloy material having excellent hydrogen embrittlement resistance can be obtained.
  • the resulting tensile strength is preferably 1,000 MPa or more at room temperature and 820 MPa or more at 625°C.
  • M 23 C 6 type carbide precipitates in excess when the temperature at the second stage of the aging treatment is lower than 710°C, and MC type carbide is coarsened when the temperature is higher than 740°C. Thereby, there is a concern that adverse influences such as a decrease in high-temperature ductility are caused in both cases.
  • the hydrogen charge is simulated by intrusion of a hydrogen quantity of 50 ppm.
  • Ni-based alloys obtained in the above more preferred is also the Ni-based alloy affording such a high-temperature creep property that a creep rupture time at 700°C and 333 MPa is 1,500 hours or more.
  • Ni-based alloys obtained in the above more preferred is also the Ni-based alloy affording such a high-temperature creep property that a minimum creep rate at 700°C and 333 MPa is 1 ⁇ 10 -8 s -1 or less.
  • the Ni-based alloy having the above-mentioned hydrogen embrittlement index and high-temperature creep properties can be obtained by satisfying the compositional requirements mentioned above, and particularly containing P in an amount of 40 ppm or more.
  • the material using the Ni-based alloy according to the invention can be used for any desired uses capable of exhibiting the hydrogen embrittlement resistance through plastic working or machining, and particularly can be suitably used as an ammonothermal pressure vessel material. Thereby, it becomes possible to realize the enlargement, mass production, and cost reduction of a gallium nitride single crystal, for example.
  • test materials invention materials P1, P2 and comparative materials 1, 2.
  • test materials were machined to form tensile test pieces for evaluation of hydrogen embrittlement resistance and creep test pieces.
  • Test material Chemical composition of test material (% by mass; ppm by mass for P, S, N, and O) C Si Mn P (ppm) S (ppm) Ni Cr Al Ti Nb Fe Mg Zr N (ppm) O (ppm) Invention material (P1) 0.011 0.01 0.01 45 2 41.40 15.41 1.26 1.45 2.05 38.26 0.0015 0.030 13 16 Invention material (P2) 0.012 0.01 0.01 130 2 41.37 15.40 1.26 1.44 2.06 38.30 0.0015 0.030 12 15 Comparative material 1 0.011 0.01 0.02 33 ⁇ 1 41.66 15.10 1.11 1.68 2.06 38.20 ⁇ 0.0005 ⁇ 0.010 31 7 Comparative material 2 0.011 0.01 0.01 8 3 41.39 15.40 1.24 1.41 2.08 38.24 0.0012 0.036 7 16
  • the hydrogen charging conditions are set so as to simulate 50 ppm that is a hydrogen quantity which is assumed to intrude into the material in an actual ammonothermal method.
  • a tensile test was performed at 625°C and a tensile strength and a reduction of area were measured.
  • a smaller value of the hydrogen embrittlement index indicates more excellent hydrogen embrittlement resistance.
  • test temperature was 700°C
  • test stress was 333 MPa and 275 MPa in the rupture test and was 333 MPa in the rate test.
  • Table 2 shows the tensile strength, reduction of area, and hydrogen embrittlement index of each of the hydrogen charged materials and the hydrogen non-charged materials at 625°C. Incidentally, the hydrogen embrittlement index of the invention material P1 became negative but this is indicated as 0.00 for convenience sake in Table 2.
  • FIG. 1 shows a relationship between the hydrogen embrittlement index of each of the invention materials P1 and P2 (hereinafter sometimes collectively referred to as “invention material”) and the comparative materials 1 and 2 (hereinafter sometimes collectively referred to as “comparative material”) at 625°C and the P content in each Ni-based alloy.
  • the hydrogen embrittlement index of the invention material is remarkably small as compared with that of the comparative material and thus it is realized that the invention material is extremely excellent in the hydrogen embrittlement resistance at high temperature.
  • the hydrogen embrittlement index decreases to 0.1 or less and the hydrogen embrittlement susceptibility reduces to such a degree that the influence of hydrogen can be almost ignored. From the results, it is realized that P has effects of suppressing excessive accumulation of hydrogen at grain boundaries by increasing the consistency of the grain boundaries and lowering the hydrogen embrittlement susceptibility and a P content of 40 ppm or more is necessary for improving the hydrogen embrittlement resistance by increasing the P content.
  • FIG. 2 and FIG. 3 show results of the creep rupture test and results of the creep rate test, respectively.
  • the rupture time of the invention material is greatly longer than that of the comparative material.
  • the rupture time of the invention material in the case where the test stress is 333 MPa is at least ten times that of the comparative material 1 and the rupture time is about 1,500 hours in the case of the invention material P1 and is about 2,000 hours in the case of the invention material P2.
  • the minimum creep rate of the invention material is at least one fourth or less as compared with that of the comparative material 2 and the value is 1 ⁇ 10 -8 s -1 (3.6 ⁇ 10 -5 h -1 ) or less.

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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)
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  • Pressure Vessels And Lids Thereof (AREA)
  • Heat Treatment Of Steel (AREA)

Claims (7)

  1. Alliage à base de Ni constitué, en termes de rapports massiques, de Fe : 30 à 40 %, Cr : 14 à 16 %, Ti : 1,2 à 1,7 %, Al : 1,1 à 1,5 %, Nb : 1,9 à 2,7 % et P : 40 à 150 ppm, et éventuellement Mg : 0,01 % ou moins, Zr : 0,1 % ou moins, le reste étant du Ni et des impuretés inévitables.
  2. Alliage à base de Ni selon la revendication 1, qui comprend en outre au moins l'un de Mg : 0,01 % ou moins et Zr : 0,1 % ou moins en termes de rapports massiques.
  3. Alliage à base de Ni selon la revendication 1 ou 2, dans lequel un indice de fragilisation par l'hydrogène EI défini par EI = (RAA - RAH)/RAA quand une réduction surfacique d'un matériau chargé d'hydrogène et une réduction surfacique d'un matériau non chargé d'hydrogène lors d'un essai de traction sont respectivement désignées RAH et RAA, vaut 0,1 ou moins à 625 °C.
  4. Alliage à base de Ni selon l'une quelconque des revendications 1 à 3, dans lequel un temps de rupture par fluage à 700 °C et 333 MPa est de 1500 heures ou plus.
  5. Alliage à base de Ni selon l'une quelconque des revendications 1 à 4, dans lequel un taux de fluage minimum à 700 °C et 333 MPa est de 1 × 10-8 s-1 ou moins.
  6. Alliage à base de nickel selon l'une quelconque des revendications 1 à 5, qui est utilisé en tant que matériau pour récipient sous pression ammono-thermique.
  7. Procédé de production d'un matériau allié à base de Ni, ledit procédé comprenant la soumission de l'alliage à base de Ni selon la revendication 1 ou 2 à un traitement de mise en solution puis deux fois à un traitement de vieillissement à une température de 825 à 855 °C et à une température de 710 à 740 °C.
EP13831112.1A 2012-08-24 2013-08-22 Alliage à base de ni ayant une excellente résistance à la fragilisation par l'hydrogène et un procédé de fabrication d'une matière d'alliage à base de ni Active EP2889387B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2012184966A JP5599850B2 (ja) 2012-08-24 2012-08-24 耐水素脆化特性に優れたＮｉ基合金および耐水素脆化特性に優れたＮｉ基合金材の製造方法
PCT/JP2013/072431 WO2014030705A1 (fr) 2012-08-24 2013-08-22 Alliage à base de ni ayant une excellente résistance à la fragilisation par l'hydrogène et un procédé de fabrication d'une matière d'alliage à base de ni

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EP2889387A1 EP2889387A1 (fr) 2015-07-01
EP2889387A4 EP2889387A4 (fr) 2016-04-27
EP2889387B1 true EP2889387B1 (fr) 2018-05-02

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US (1) US20150225827A1 (fr)
EP (1) EP2889387B1 (fr)
JP (1) JP5599850B2 (fr)
KR (1) KR101704312B1 (fr)
CN (1) CN104583432B (fr)
WO (1) WO2014030705A1 (fr)

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JP6176665B2 (ja) * 2014-02-20 2017-08-09 株式会社日本製鋼所 Ｎｉ−Ｆｅ基合金およびＮｉ−Ｆｅ基合金材の製造方法
US12023643B1 (en) * 2023-12-14 2024-07-02 First Ammonia Motors, Inc. System and method for heating gas in a continuous focused path within an electric catalyst unit

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JPS57149441A (en) * 1981-03-12 1982-09-16 Res Inst Electric Magnetic Alloys Elinver type alloy for high temperature and preparation thereof
JPH05255788A (ja) 1992-03-12 1993-10-05 Sumitomo Metal Ind Ltd 耐水素脆化高Ｎｉ基合金およびその製造方法
JP3058794B2 (ja) * 1993-08-19 2000-07-04 日立金属株式会社 Ｆｅ−Ｎｉ−Ｃｒ基超耐熱合金、エンジンバルブおよび排ガス触媒用ニットメッシュ
JP2003164946A (ja) * 2001-11-29 2003-06-10 Daido Steel Co Ltd ニッケル基超合金のインゴットを製造する方法
JP4123064B2 (ja) * 2003-06-13 2008-07-23 株式会社日立製作所 蒸気タービンロータおよび蒸気タービンプラント
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JP5147037B2 (ja) * 2006-04-14 2013-02-20 三菱マテリアル株式会社 ガスタービン燃焼器用Ｎｉ基耐熱合金
JP4261562B2 (ja) * 2006-08-25 2009-04-30 株式会社日立製作所 高温強度と高温延性の優れたＮｉ−Ｆｅ基鍛造超合金とその製造法および蒸気タービンロータ
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JP2010174360A (ja) 2009-02-02 2010-08-12 Hitachi Ltd 耐水素脆化材料及びその製造方法
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JP5633883B2 (ja) * 2010-08-26 2014-12-03 三菱日立パワーシステムズ株式会社 蒸気タービン用鍛造合金、それを用いた蒸気タービンロータ

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Publication number Publication date
KR20150034282A (ko) 2015-04-02
CN104583432A (zh) 2015-04-29
JP5599850B2 (ja) 2014-10-01
EP2889387A1 (fr) 2015-07-01
JP2014043597A (ja) 2014-03-13
US20150225827A1 (en) 2015-08-13
CN104583432B (zh) 2017-05-24
EP2889387A4 (fr) 2016-04-27
WO2014030705A1 (fr) 2014-02-27
KR101704312B1 (ko) 2017-02-07

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