WO2015020007A1 - Superalliage à base de ni type renforcé à dispersion de particules d'oxyde - Google Patents

Superalliage à base de ni type renforcé à dispersion de particules d'oxyde Download PDF

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Publication number
WO2015020007A1
WO2015020007A1 PCT/JP2014/070501 JP2014070501W WO2015020007A1 WO 2015020007 A1 WO2015020007 A1 WO 2015020007A1 JP 2014070501 W JP2014070501 W JP 2014070501W WO 2015020007 A1 WO2015020007 A1 WO 2015020007A1
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mass
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oxide
phase
high temperature
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Japanese (ja)
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原田　広史
月峰 谷
知 石原
忠晴 横川
敏治 小林
裕 小泉
鉄井　利光
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National Institute for Materials Science
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National Institute for Materials Science
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Priority to US14/909,799 priority Critical patent/US20160160323A1/en
Priority to JP2015530883A priority patent/JPWO2015020007A1/ja
Priority to EP14834221.5A priority patent/EP3031939B1/fr
Publication of WO2015020007A1 publication Critical patent/WO2015020007A1/fr
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/057—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%
    • 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
    • C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent

Definitions

  • the present invention relates to an oxide particle dispersion strengthened Ni-base superalloy.
  • Ni-base superalloys generally exhibit excellent characteristics based on the solid solution strengthening and precipitation strengthening mechanisms of the ⁇ ′ phase. Many excellent single crystal cast alloys based on such a strengthening mechanism have already been developed. However, improvement of the service temperature by these strengthening mechanisms becomes increasingly difficult as the temperature rises. On the other hand, in addition to these strengthening mechanisms, based on a dispersion strengthening mechanism using oxide fine particles, an oxide particle dispersion strengthened Ni-base superalloy that is considered to be able to improve the service temperature is expected.
  • Oxide particle dispersion strengthened Ni-base superalloy has a structural feature that a large number of fine oxide particles generally having a particle size of 1 ⁇ m or less are dispersed in a matrix phase in which other elements are dissolved in Ni. There is. In addition to oxide particles, depending on the alloy composition, precipitates such as ⁇ 'phase may be dispersed.
  • Patent Documents 1 to 3, Non-patent Document 1, TMO-2 alloy, and the like have been developed (Patent Documents 4 to 5, Non-Patent Documents).
  • Patent Document 2). These alloys are basically produced by solidifying an alloy powder produced by a mechanical alloying method by a method such as hot extrusion.
  • the added amount of tungsten (W) or tantalum (Ta) is increased with respect to the MA6000 alloy to realize a superior high temperature strength.
  • Patent Document 6 an oxide dispersion strengthened Ni-base superalloy has been proposed (Patent Document 6).
  • the high temperature corrosion and high temperature oxidation of a yttria particle dispersion strengthened alloy are also examined and reported (nonpatent literature 3).
  • the TMO-2 alloy described above is excellent in high temperature strength, but contains 12% by mass or more of W in order to increase the high temperature strength.
  • the inclusion of such a large amount of W is effective for improving mechanical properties, but may reduce high temperature corrosion resistance.
  • an object of the present invention is to provide a new oxide particle dispersion strengthened Ni-base superalloy which is excellent in high temperature corrosion resistance and can improve mechanical properties such as high temperature strength.
  • the present inventors proceeded with examination of the alloy composition of an oxide particle dispersion-strengthened Ni-base superalloy, and contained ruthenium (Ru) in an amount of 0.1% by mass or more and 14.0% by mass. It has been found that by containing it in the following range, high-temperature corrosion resistance is good and mechanical properties such as high-temperature strength can be improved.
  • the present invention has been completed based on such findings.
  • the oxide particle dispersion-strengthened Ni-base superalloy of the present invention has 0.1 to 14.0% by weight of Ru, 0.1% to 14.0% by weight, together with Ni, in the composition. Al and inevitable impurities are contained, and 0.01 to 3.0% by mass of oxide particles in the entire amount are dispersed in the crystal structure.
  • the oxide particle dispersion-strengthened Ni-base superalloy of the present invention containing Ru in the range of 0.1% by mass or more and 14.0% by mass or less the high temperature corrosion resistance is good, the high temperature strength, etc.
  • the mechanical properties after heating in the range of 1260 ° C. to 1300 ° C. can be remarkably improved.
  • the oxide particle dispersion-strengthened Ni-base superalloy of the present invention has 0.1 to 14.0% by weight of Ru, 0.1% to 14.0% by weight, together with Ni. It is characterized by containing aluminum (Al) inevitable impurities in an amount of mass% or less and oxide particles in an amount of 0.01 mass% or more and 3.0 mass% or less of the total amount being dispersed in the crystal structure.
  • Ru is one of the elements that characterize the invention of this application, and is dissolved in the ⁇ phase as a parent phase and improves the high-temperature strength by solid solution strengthening. Moreover, precipitation of the TCP phase produced
  • the Ru content is preferably in the range of 0.1 to 14.0% by mass, and more preferably in the range of 1.0 to 14.0% by mass. If the Ru content is less than 0.1% by mass, the TCP phase precipitates at high temperatures, and high high-temperature strength cannot be ensured. On the other hand, if the content of Ru exceeds 14% by mass, the ⁇ phase is precipitated and the high-temperature strength decreases, which is not preferable. In addition, since Ru is expensive as much as 200 to 300 times the price of Ni compared to Ni, etc., it is preferable that Ru be as small as possible within the range of improving high temperature strength by solid solution strengthening.
  • the upper limit is preferably 8.0% by mass.
  • the addition of Al precipitates the ⁇ 'phase and contributes to the improvement of strength by precipitation strengthening.
  • the Al content is preferably in the range of 0.1 to 14.0% by mass. If the Al content is less than 0.1% by mass, precipitation strengthening is insufficient and the desired high-temperature strength cannot be ensured, and if it exceeds 14.0% by mass, a coarse ⁇ ′ phase is formed. This is because it is formed in a large amount and deteriorates mechanical properties.
  • the amount of oxide particles added for dispersion strengthening is desirably 0.01% by mass to 3.0% by mass.
  • the type of oxide particles is not particularly limited, but yttrium oxide having high chemical stability even at a high temperature is particularly preferable. However, when high purity yttrium oxide is added, some elements in the alloy may react with yttrium oxide to form a composite oxide during production or use at a high temperature. Therefore, a composite oxide of yttrium oxide and aluminum oxide such as Y 4 Al 2 O 9 is also preferable instead of yttrium oxide.
  • alloy additive elements include 0.1 mass% or more and 14.0 mass% or less Re, 0.1 mass% or more and 20.0 mass% or less Co, 0.1 mass% or more and 20 mass% or more depending on the application.
  • composition More preferable composition (mass%) is exemplified as follows.
  • Ru 1.0 to 8.0 Al: 1.0 to 10.0 Cr: 1.0 to 10.0 Co: 1.0-10.0 Mo: 0.1 to 4.0 W: 1.0 to 8.0 Ta: 1.0 to 10.0 Hf: 0.05 to 5.0 Zr: 0.05 to 5.0 Ti: 0.1 to 5.0 Nb: 0.1 to 5.0 Re: 0.1 to 8.0 V: 0.1 to 2.0 Pt: 0.1 to 6.0 Pd: 0.1 to 6.0 Ir: 0.1 to 6.0 B: 0.005 to 0.05 C: 0.005 to 0.05 Oxide particles: 0.1 to 3.0 Re dissolves in the ⁇ phase, which is the parent phase, and improves high-temperature strength by solid solution strengthening. It also has the effect of improving corrosion resistance.
  • the content is more preferably in the range of 0.1 to 14.0% by mass.
  • the Re content is less than 0.1% by mass, the solid solution strengthening of the ⁇ phase is insufficient and the desired high-temperature strength cannot be ensured, so the Re content is preferably 14.0% by mass. Exceeding this is not preferable because the TCP phase precipitates at a high temperature and a high high-temperature strength cannot be secured.
  • Cr is an element with excellent oxidation resistance and improves high temperature corrosion resistance.
  • the Cr content is less than 0.1% by mass, the high temperature corrosion resistance cannot be improved. If the Cr content exceeds 20.0 mass%, precipitation of the ⁇ 'phase is suppressed and harmful phases such as the ⁇ phase and the ⁇ phase are generated, and the high-temperature strength is lowered.
  • Co increases the solid solubility limit of Al, Ta, and other parent phases at high temperatures, precipitates ⁇ 'phase, and improves high temperature strength.
  • the Co content is less than 0.1% by mass, the ⁇ ′ phase is not sufficiently precipitated, and the high temperature strength cannot be improved. If the Co content exceeds 20.0% by mass, the balance with other elements such as Al, Ta, Mo, W, Hf, and Cr is lost, and a harmful phase is precipitated to lower the high-temperature strength. .
  • Mo dissolves in the matrix ⁇ phase to increase the high temperature strength and contributes to the high temperature strength by precipitation hardening. If the Mo content is less than 0.1% by mass, these effects are not sufficient, and the high temperature strength cannot be improved. If the Mo content exceeds 15.0% by mass, the high temperature corrosion resistance is lowered, which is not preferable.
  • W improves the high-temperature strength by the action of solid solution strengthening and precipitation hardening in the presence of Mo and Ta.
  • the W content is preferably 20.0% by mass or less. This is because if the W content exceeds 20.0 mass%, the high temperature corrosion resistance may be reduced.
  • each element needs a content of 0.1% by mass.
  • the content is preferably 10.0% by mass or less, particularly preferably 6.0% by mass or less. Good.
  • Ta, Ti, and Nb contribute to precipitation strengthening by substituting Al sites in the ⁇ 'phase. Further, the high temperature strength is improved by the action of solid solution strengthening and precipitation strengthening in the presence of Mo and W.
  • the content of Ta is preferably 15.0% by mass or less. This is because if the Ta content exceeds 15.0% by mass, the ⁇ phase and the ⁇ phase are formed and the high temperature strength is lowered.
  • the contents of Ti and Nb are each less than 0.1% by mass, precipitation strengthening and solid solution strengthening in the presence of Mo and W cannot be obtained.
  • the contents of Ti and Nb are each preferably 10.0% by mass or less. This is because if the content of Ti or Nb exceeds 10.0% by mass, a harmful phase is formed and the high-temperature strength decreases.
  • V is an element that dissolves in the ⁇ ′ phase and strengthens the ⁇ ′ phase. If the V content is less than 0.1% by mass, these effects cannot be obtained.
  • the content of V is preferably 5.0% by mass or less. This is because if the V content exceeds 5.0% by mass, the creep strength is lowered.
  • Hf is a grain boundary segregation element and segregates at the grain boundaries of the ⁇ phase and ⁇ ′ phase to strengthen the grain boundaries, thereby improving the high temperature strength.
  • Hf needs to be 0.01% by mass or more. If the content of Hf exceeds 10.0% by mass, it is not preferable because local melting may occur and the high-temperature strength may be reduced.
  • B is an element that reinforces the grain boundary, thereby improving the high temperature strength. In order to obtain these effects, B must be 0.001% by mass or more. If the B content exceeds 1.0% by mass, harmful carbides are precipitated at the grain boundaries, which is not preferable.
  • composition of the composition elements of the oxide particle dispersion-strengthened Ni-base superalloy according to the present invention include the following, including the examples described later.
  • Ni-Ru-Al-Re-Co-Cr-Mo-W-Ta-Hf-oxide particles Ni-Ru-Al-Re-Co-Cr-Mo-W-Ta-Hf- (B, C) -Oxide particles
  • an alloy powder produced by a mechanical alloying method can be enclosed in a can and solidified by a method such as a hot extrusion method.
  • the alloy powder can be solidified by a method such as a hot isostatic pressing (HIP) method or a hot pressing method. Or after solidifying alloy powder by these methods, it can produce by performing a hot extrusion process or a hot rolling process.
  • HIP hot isostatic pressing
  • a combination of a base material element and an additive element, which are constituent elements, is determined depending on the intended use and economy of a heat resistant alloy.
  • a turbine disk is required to have a high temperature strength in a temperature range of 400 to 500 ° C.
  • a member such as a combustor, a nozzle, a turbine blade, and a shroud has a temperature range of about 800 to 1000 ° C. High strength and high temperature corrosion resistance are required.
  • the strengthening effect by the dispersed particles that is, the effect of preventing the dislocation motion that causes deformation by the oxide particles is increased when the particles are finer and the particle interval is short.
  • the dispersion particle size distribution is preferably 0.001 ⁇ m to 5 ⁇ m in consideration of particle aggregation during production.
  • the distribution is preferably 1 ⁇ m or less.
  • the amount of oxide particles is particularly preferably 0.5 to 3.0% of the total amount in order to obtain strength at a high temperature of 800 ° C. or higher.
  • the upper limit of the particle size distribution of the alloy and metal powder used is, for example, 250 ⁇ m, the efficiency of mechanical alloying and sintering for solidification can be improved.
  • the ratio of the mixed powder weight to the steel ball weight is 1/10 to 1 in the attritor. / 20, 1-5 to 1/10 for planetary ball mills, and the rotation speed of the ball mill is preferably 50 to 400 rpm, depending on the scale of the ball mill.
  • the alloying treatment time is desirably 20 hours or longer.
  • pre-alloying treatment it is preferable to replace the inside of the ball mill container with an inert atmosphere such as Ar (argon) in consideration of oxygen contamination during alloying.
  • Solidification of the dispersed alloyed powder by sintering is performed by hot extrusion or HIP method after filling the powder in a mild steel container according to the powder metallurgy method.
  • the sintering is preferably performed in a temperature range of 1000 to 1300 ° C. for Ni-based alloys in consideration of diffusion fusion between powders, densification, further solidification of alloy atoms, and high temperature stability of oxide particles.
  • the vacuum treatment in the container performed as a pretreatment here is to prevent oxygen from being contained in the dispersed alloy as much as possible at the time of sintering, and to prevent formation of a strong oxide on the powder surface.
  • the purpose is to remove moisture, oxygen and other contaminants present or adsorbed on the powder surface, and the scale of the equipment at a temperature of 100 ° C. to 600 ° C. in a vacuum of 10 ⁇ 1 to 10 ⁇ 3 torr. However, heat treatment for 10 minutes to 10 hours is preferable.
  • Example 1 Extruded material of Ni-6.4Co-4.5Cr-1.1Mo-4.0W-5.8Al-7.5Ta-0.1Hf-6.3Re-4.9Ru-1.1Y 2 O 3 composition (each numerical value is% by mass) as follows Produced.
  • the raw material powder was blended so as to achieve the target composition as a whole, and mechanical alloying treatment was performed using an attritor.
  • the treated alloy powder was put into a can, vacuum-processed and sealed, and solidified by a hot isostatic press (HIP) method at a heating temperature of 1180 ° C. and a pressing force of 118 MPa.
  • This HIP material was subjected to hot extrusion under conditions of a heating temperature of 1200 ° C. and an extrusion ratio of 5 to obtain a round bar extruded material.
  • HIP hot isostatic press
  • FIG. 1 is a diagram comparing the result of X-ray diffraction of this extruded material with the result of mechanical alloying powder.
  • the X-ray diffraction pattern (A in the figure) of the mechanical alloying powder mainly consisted of (111) and (200) diffraction peaks of Ni solid solution.
  • the (110) diffraction peak of the ⁇ ′ phase was observed. That is, it can be seen that this extruded material mainly consists of a Ni solid solution ( ⁇ ) phase, on which the ⁇ ′ phase is precipitated.
  • FIG. 2 shows the structure of the extruded material observed with a transmission electron microscope. Arrows in the figure indicate oxide particles. In this structure, a large number of fine oxide particles of about several tens of nm were dispersed in the crystal grains.
  • a small piece was cut out from the extruded material and subjected to isothermal heating treatment at a temperature of 1260 ° C. to 1300 ° C. for 1 hour.
  • This heat treatment is generally performed at a temperature such that the oxide particle dispersion strengthened Ni-base superalloy is manufactured as a hot-extrusion material or a hot-rolling material, and further processed into a member having a desired size and shape. This is because the hot forging process or the like may be performed.
  • the micro Vickers hardness of each sample after the heat treatment was 598 at 1260 ° C. and 585 at 1290 ° C.
  • the high temperature corrosion resistance of this alloy was evaluated by a molten salt corrosion test.
  • the extruded material was cut into a cylindrical shape with a diameter of 6 mm and a height of 4.5 mm so that the axial direction coincided with the extrusion direction, immersed in molten salt, and heated at a temperature of 800 ° C. for 4 hours.
  • the molten salt used as the corrosive medium was a 3: 1 mixed salt of sodium sulfate and sodium chloride.
  • An amount of the mixed salt in which the cylindrical sample was completely immersed was put in a crucible and heated in advance to 800 ° C. in a heating furnace, and after the temperature was sufficiently stabilized, the cylindrical sample was immersed in the molten salt. As a result of calculating the decrease rate of the sample diameter before and after the test, it was 0.17%.
  • Ni-5.9Co-3.8Cr-0.9Mo-3.9W-6.1Al-8.6Ta-0.2Hf-5.3Re-4.6Ru-1.2Y 4 Al 2 O 9 composition (each numerical value is% by mass) It produced as follows.
  • the raw material powder was blended so as to achieve the target composition as a whole, and mechanical alloying treatment was performed using an attritor.
  • the treated alloy powder was put into a can, vacuum-processed and sealed, and subjected to hot extrusion under the conditions of a heating temperature: 1050 ° C. and an extrusion ratio: 15, to obtain a round bar extruded material.
  • a small piece was cut out from the extruded material and subjected to isothermal heating treatment at a temperature of 1260 ° C. to 1300 ° C. for 1 hour.
  • the micro Vickers hardness of each sample after the heat treatment was 626 at 1260 ° C. and 585 at 1290 ° C.
  • the high temperature corrosion resistance of this alloy was evaluated by a molten salt corrosion test under the same conditions as in Example 1.
  • the sample was immersed in molten salt and heated at a temperature of 800 ° C. for 4 hours, and the reduction rate of the sample diameter before and after the test was calculated. As a result, it was 0.17%.
  • Ni-6.1Co-3.8Cr-0.9Mo-4.2W-6.3Al-9.2Ta-0.2Hf-5.0Re-4.7Ru-1.2Y 4 Al 2 O 9 composition (each value is% by mass) It produced as follows.
  • the raw material powder was blended so as to achieve the target composition as a whole, and mechanical alloying treatment was performed using an attritor.
  • the treated alloy powder was put into a can, vacuum-processed and sealed, and subjected to hot extrusion under the conditions of a heating temperature: 1050 ° C. and an extrusion ratio: 15, to obtain a round bar extruded material.
  • a small piece was cut out from the extruded material and subjected to isothermal heating treatment at a temperature of 1260 ° C. to 1300 ° C. for 1 hour.
  • the micro Vickers hardness of each sample after the heat treatment was 664 at 1260 ° C. and 596 at 1290 ° C.
  • the high temperature corrosion resistance of this alloy was evaluated by a molten salt corrosion test under the same conditions as in Examples 1 and 2.
  • the sample was immersed in molten salt and heated at a temperature of 800 ° C. for 4 hours, and the reduction rate of the sample diameter before and after the test was calculated. As a result, it was 0.17%.
  • Non-Patent Document 2 discloses a test result of micro Vickers hardness after isothermal heat treatment of an extruded material of TMO-2 alloy.
  • the alloy composition of the extruded material in this test is Ni-9.8Co-5.9Cr-2.0Mo-12.4W-4.2Al-4.7Ta-0.8Ti-0.05Zr-0.05C-0. 01B-1.1Y 2 O 3 (the numerical value is mass%).
  • this alloy has about 3 times the content of W compared with the alloy composition of an Example.
  • Non-patent document 3 discloses the results of the molten salt corrosion test of this alloy under the same conditions as in Examples 1 to 3. The diameter reduction rate of this extruded material was 29.0%.
  • FIG. 3 shows a comparison of the micro Vickers hardness after the isothermal heat treatment (1 hour) in Examples 1 to 3 and the comparative example as a graph arranged by the heat treatment temperature.
  • the white circles are the results of Example 1
  • the triangles are the results of Example 2
  • the diamonds are the results of Example 3
  • the black circles are the results of the comparative example.
  • the oxide particle dispersion-strengthened Ni-base superalloy of the present invention improves the mechanical properties after heating in the range of 1260 ° C to 1300 ° C even if the W content is greatly reduced by containing Ru. Is shown.
  • the results of the molten salt corrosion test show that the diameter reduction rate of each of Examples 1 to 3 is 0.17%, whereas the diameter reduction rate of the Example is 29.0%. It is shown that the high temperature corrosion resistance is remarkably improved. This is presumably because the alloys of Examples 1 to 3 significantly reduce the W content as compared with the alloys of Examples.

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Abstract

Le superalliage à base de Ni type renforcé à dispersion de particule d'oxyde de l'invention, comprend, avec un Ni, au moins 0,1% en masse et au plus 14,0% en masse de Ru, au moins 0,1% en masse et au plus 14,0% en masse de Al, et des impuretés inévitables. Au moins 0,01% en masse et au plus 3,0% en masse de particules d'oxyde de la masse totale, sont dispersées à l'intérieur d'une composition cristalline.
PCT/JP2014/070501 2013-08-05 2014-08-04 Superalliage à base de ni type renforcé à dispersion de particules d'oxyde Ceased WO2015020007A1 (fr)

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US14/909,799 US20160160323A1 (en) 2013-08-05 2014-08-04 Oxide particle dispersion-strengthened ni-base superalloy
JP2015530883A JPWO2015020007A1 (ja) 2013-08-05 2014-08-04 酸化物粒子分散強化型Ｎｉ基超合金
EP14834221.5A EP3031939B1 (fr) 2013-08-05 2014-08-04 Superalliage à base de ni type renforcé à dispersion de particules d'oxyde

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JP2013162525 2013-08-05

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EP3211111A3 (fr) * 2016-02-24 2017-11-29 MTU Aero Engines GmbH Procédé de traitement thermique pour des composants constitués de super-alliages à base de nickel
WO2021066142A1 (fr) * 2019-10-03 2021-04-08 東京都公立大学法人 Alliage résistant à la chaleur, poudre d'alliage résistant à la chaleur, article moulé en alliage résistant à la chaleur et son procédé de production
US11359638B2 (en) 2017-10-31 2022-06-14 Hitachi Metals, Ltd. Alloy article, method for manufacturing said alloy article, product formed of said alloy article, and fluid machine having said product

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