US20230265545A1 - Aluminum alloy material and hydrogen embrittlement inhibitor for aluminum alloy materials - Google Patents

Aluminum alloy material and hydrogen embrittlement inhibitor for aluminum alloy materials Download PDF

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US20230265545A1
US20230265545A1 US18/007,616 US202118007616A US2023265545A1 US 20230265545 A1 US20230265545 A1 US 20230265545A1 US 202118007616 A US202118007616 A US 202118007616A US 2023265545 A1 US2023265545 A1 US 2023265545A1
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aluminum alloy
alloy composition
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Hiroyuki Toda
Kazuyuki Shimizu
Ibaraki YAMAGUCHI
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Japan Atomic Energy Agency
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Japan Atomic Energy Agency
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/10—Alloys based on aluminium with zinc as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C22C21/08—Alloys based on aluminium with magnesium as the next major constituent with silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C22C21/16—Alloys based on aluminium with copper as the next major constituent with magnesium

Definitions

  • the present invention relates to an aluminum alloy material and to a hydrogen embrittlement inhibitor for aluminum alloy materials.
  • Aluminum alloy materials which have a wide range of applications, suffer from the problem of hydrogen embrittlement cracks, and proposals have been made to solve this problem (see PTL 1 to 4).
  • PTL 1 discloses an aluminum alloy material for a high pressure gas vessel, which has an aluminum alloy composition that contains, in terms of mass%, 4.0 to 6.7% of Zn, 0.75 to 2.9% of Mg, 0.001 to 2.6% of Cu, 0.05 to 0.40% of Si, 0.005 to 0.20% of Ti and 0.01 to 0.5% of Fe, and contains one or two or more of 0.01 to 0.7% of Mn, 0.02 to 0.3% of Cr, 0.01 to 0.25% of Zr and 0.01 to 0.10% of V so as to satisfy the relationship 1.0% ⁇ Fe+Mn+Cr+Zr+V ⁇ 0.1%, with the remainder comprising Al and unavoidable impurities, and in which the relationship between electrical conductivity (%IACS) and the total content of Fe, Mn, Cr, Zr and V satisfies the following relationship: electrical conductivity (%) ⁇ -4.9 ⁇ (Fe+Mn+Cr+Zr+V)+40.0, and which has a 0.2% proof stress of 275 MPa
  • PTL 2 discloses a method for producing a thick aluminum alloy thick plate having excellent strength and ductility, in which a thick plate in which the total area ratio of intermetallic compounds having an equivalent circle diameter of more than 5 ⁇ m is controlled to 2% or less is obtained by using an Al-Zn-Mg-Cu-based aluminum alloy, which contains 5.0 to 7.0% of Zn, 1.0 to 3.0% of Mg and 1.0 to 3.0% of Cu, also contains a total of 0.05 to 0.5% of one or two or more of 0.05 to 0.3% of Cr, 0.05 to 0.25% of Zr, 0.05 to 0.40% of Mn and 0.05 to 0.35% of Sc, and further contains 0.25% or less of Si and 0.25% or less of Fe as impurities, with the remainder comprising Al and unavoidable impurities, subjecting an ingot of this alloy to a homogenizing treatment by holding the ingot at a temperature of 450 to 520° C.
  • PTL 3 discloses a method for producing a high strength Al-Zn-Mg-based aluminum alloy forging material having excellent resistance to stress corrosion cracking by regulating the Fe content in the alloy to 0.15 wt% or less when an aluminum alloy, which contains 4.5 to 8.5 wt% of Zn, 1.5 to 3.5 wt% of Mg and 0.8 to 2.6 wt% of Cu and further contains at least one of Mn, Cr, Zr, V and Ti, with the remainder comprising Al and impurities, is molded into a forging material having an H-section by forging.
  • PTL 4 discloses a high strength aluminum alloy for welded structures, which exhibits excellent stress corrosion cracking resistance and which contains 5 to 8 wt% of Zn, 1.2 to 4.0 wt% of Mg, more than 1.5 wt% and not more than 4.0 wt% of Cu, 0.03 to 1.0 wt% of Ag, 0.01 to 1.0 wt% of Fe, 0.005 to 0.2 wt% of Ti and 0.01 to 0.2 wt% of V, and further contains one or two or more of 0.01 to 1.5 wt% of Mn, 0.01 to 0.6 wt% of Cr, 0.01 to 0.25 wt% of Zr, 0.0001 to 0.08 wt% of B and 0.03 to 0.5 wt% of Mo, with the remainder comprising aluminum and unavoidable impurities.
  • the problem to be solved by the present invention is to provide: an aluminum alloy material that can effectively prevent or inhibit hydrogen embrittlement; and a hydrogen embrittlement inhibitor for aluminum alloy materials.
  • the composition of invention example 6 in table 1 in PTL 1 contains 0.21 mass% of Si, 0.28 mass% of Fe, and the like
  • the composition of alloy A in table 1 on page 11 of PTL 2 contains 0.21 mass% of Si, 0.28 mass% of Fe, and the like
  • the composition of sample 4 in table 1 on page 4 of PTL 3 contains 0.10 mass% of Si, 0.19 mass% of Fe, and the like
  • the composition of comparative alloy 10 in table 1 on page 4 of PTL 4 contains 0.10 mass% of Si, 0.20 mass% of Fe, and the like, but these compositions all fall outside the scope of the aluminum alloy material of the present invention.
  • An aluminum alloy material which has an aluminum alloy composition of any one of aluminum alloy compositions (1) to (7) below.
  • a hydrogen embrittlement inhibitor for aluminum alloy materials which comprises Al 7 Cu 2 Fe particles and can prevent hydrogen embrittlement of aluminum alloy materials.
  • the present invention is capable of providing: an aluminum alloy material that can effectively prevent or inhibit hydrogen embrittlement; and a hydrogen embrittlement inhibitor for aluminum alloy materials.
  • FIG. 1 is a virtual cross section of a tomographic image of a microstructure of a (High Fe) aluminum alloy material of Working Example 1.
  • FIG. 2 is a virtual cross section of a tomographic image of a fracture surface of the (High Fe) aluminum alloy material of Working Example 1.
  • FIG. 3 is a virtual cross section of a tomographic image of a (Low Fe) aluminum alloy material of Reference Example 2.
  • FIG. 4 is a virtual cross section of a tomographic image of a fracture surface of the (Low Fe) aluminum alloy material of Reference Example 2.
  • FIG. 5 is a schematic diagram of separation at ⁇ /Al interfaces as a result of hydrogen trapping.
  • FIG. 6 is a number line diagram of hydrogen trapping energies of microstructures in an aluminum alloy material.
  • FIG. 7 is a schematic diagram of the crystal structure (space group P4/mnc) of Al 7 Cu 2 Fe particles.
  • FIG. 8 is a bar chart showing trapped hydrogen amounts at sites in the aluminum alloy materials of Working Example 1 (High Fe) and Reference Example 2 (Low Fe).
  • FIG. 9 is a graph that shows the relationship between hydrogen distribution to IMC (Al 7 Cu 2 Fe) particles (H at IMC), hydrogen distribution to a semi-coherent precipitate interface (H at ⁇ 2 ), and hydrogen embrittlement (quasi-cleavage creak) area fraction QCF.
  • the aluminum alloy composition is any one of aluminum alloy compositions (1) to (7) below.
  • the aluminum alloy material of the present invention can effectively prevent or inhibit hydrogen embrittlement.
  • it is possible to effectively prevent or inhibit hydrogen embrittlement to the extent required in the aerospace industry.
  • the hydrogen embrittlement inhibitor for aluminum alloy materials of the present invention which is described later, comprises Al 7 Cu 2 Fe particles having the hydrogen trapping sites mentioned above.
  • hydrogen embrittlement cracks include grain boundary cracks and quasi-cleavage cracks, and quasi-cleavage cracks in particular can be effectively prevented or inhibited in the present invention.
  • the aluminum alloy composition is any one of aluminum alloy compositions (1) to (7) above.
  • the aluminum alloy composition is preferably aluminum alloy composition (3) above in the present invention.
  • the aluminum alloy material of the present invention preferably has an Fe content of more than 0.12 mass%, more preferably more than 0.15 mass%, particularly preferably more than 0.25 mass%, and yet more preferably 0.30 mass% or more, relative to the entire aluminum alloy material.
  • the volume ratio of the second phase particles preferably Al 7 Cu 2 Fe particles
  • the number density of the second phase particles, and the particle diameter of the second phase particles can also be increased.
  • the upper limit of the amount of Fe is not particularly limited.
  • the amount of Fe relative to the entire aluminum alloy material can be, for example, 1.0 mass% or less, 0.8 mass% or less, or 0.6 mass% or less. If the amount of Fe is less than these upper limits, the volume ratio, number density and particle size of the second phase particles are reduced to a certain extent, meaning that it is easier to inhibit deterioration of material properties caused by aggregation and localization of second phase particles.
  • the aluminum alloy material of the present invention contains aluminum as a primary component, and preferably contains 0.50 mass% or more of aluminum.
  • Aluminum alloy composition (1) is as shown below.
  • the content of Fe is preferably more than 0.35 mass% and not more than 1.0 mass%, and more preferably more than 0.35 mass% and not more than 0.6 mass%.
  • Aluminum alloy composition (2) is as shown below.
  • the content of Fe is preferably more than 0.15 mass% and not more than 1.0 mass%, and more preferably more than 0.15 mass% and not more than 0.6 mass%.
  • Aluminum alloy composition (3) is as shown below.
  • the content of Fe is preferably more than 0.25 mass% and not more than 1.0 mass%, and more preferably more than 0.25 mass% and not more than 0.6 mass%.
  • Aluminum alloy composition (4) is as shown below.
  • the content of Fe is preferably more than 0.55 mass% and not more than 1.0 mass%, and more preferably more than 0.55 mass% and not more than 0.6 mass%.
  • Aluminum alloy composition (5) is as shown below.
  • the content of Fe is preferably more than 0.35 mass% and not more than 1.0 mass%, and more preferably more than 0.35 mass% and not more than 0.6 mass%.
  • Aluminum alloy composition (6) is as shown below.
  • the content of Fe is preferably more than 0.12 mass% and not more than 1.0 mass%, and more preferably more than 0.12 mass% and not more than 0.6 mass%.
  • Aluminum alloy composition (7) is as shown below.
  • the content of Fe is preferably more than 0.50 mass% and not more than 1.0 mass%, and more preferably more than 0.50 mass% and not more than 0.6 mass%.
  • the shape of the aluminum alloy material of the present invention is not particularly limited.
  • the aluminum alloy material may be bulky or particulate, but is preferably bulky.
  • the aluminum alloy material of the present invention preferably contains second phase particles having a higher hydrogen trapping energy than that of a semi-coherent precipitate interface.
  • second phase particles means particles having a composition that is different from the constituent composition of a parent phase.
  • the second phase particles in the aluminum alloy material are particles having a composition that is different from that of Al or the aluminum alloy material.
  • Second phase particles having a higher hydrogen trapping energy than that of a semi-coherent precipitate interface are not particularly limited. Second phase particles having a higher hydrogen trapping energy than that of a semi-coherent precipitate interface can be determined using first principle calculations.
  • the term “first principle calculations” means theoretically representing an electronic state by mathematically solving the Schrodinger equation (without using experimental data or empirical parameters). The distribution of hydrogen at each trapping site can be calculated from the density of other hydrogen trapping sites, such as grain boundaries, precipitates and lattices, and the binding energy with hydrogen.
  • the internal plastic strain distribution can be determined by means of 3D mapping. From the 3D strain distribution, geometrically required dislocations, statistically required dislocations, and concentration distributions of atomic vacancies can be calculated.
  • second phase particles having a hydrogen trapping energy higher than that of a semi-coherent precipitate interface are preferably Al 7 Cu 2 Fe particles.
  • similar effects can be expected from particles having an Al:Cu:Fe atomic ratio that deviates from the stoichiometric composition of 7:2:1 by approximately 30% (for example, Al 7 Cu 2 Fe 0.7 particles).
  • the hydrogen trapping energies of the microstructures in the aluminum alloy material that of Al 7 Cu 2 Fe particles is 0.56 eV.
  • preferred second phase particles or microstructures other than Al 7 Cu 2 Fe particles having hydrogen trapping energies that are higher than that of a semi-coherent precipitate interface (0.55 eV) are not yet known.
  • the shape of the second phase particles includes a variety of shapes, such as spherical, elliptical, square cylinder-shaped, cylindrical, cubic, rectangular parallelepiped-shaped and scaly, but is preferably spherical or elliptical.
  • the volume ratio of the second phase particles is preferably 0.05 to 10.0%, more preferably 0.1 to 5.0%, and particularly preferably 0.5 to 2.0%.
  • the volume ratio of the second phase particles can be calculated as the volume of the second phase particles relative to the volume of the aluminum alloy material by means of, for example, 3D analysis using X-Ray tomography (CT).
  • the number density of the second phase particles is preferably 6.5 ⁇ 10 12 /m 3 to 100 ⁇ 10 12 /m 3 , more preferably 10 ⁇ 10 12 /m 3 to 50 ⁇ 10 12 /m 3 , and particularly preferably 20 ⁇ 10 12 /m 3 to 40 ⁇ 10 12 /m 3 .
  • the number density of the second phase particles can be calculated by means of, for example, 3D analysis using high resolution X-Ray tomography (CT) having a spatial resolution of up to 1 ⁇ m.
  • CT X-Ray tomography
  • the average particle diameter of the second phase particles is preferably 0.5 to 20 ⁇ m.
  • the upper limit of the average particle diameter of the second phase particles is preferably 10 ⁇ m or less, and particularly preferably 5.0 ⁇ m or less.
  • the average particle diameter of the second phase particles can be calculated as an arithmetic mean value by means of, for example, 3D analysis using X-Ray tomography (CT).
  • the method for producing the aluminum alloy material is not particularity limited.
  • the hydrogen embrittlement inhibitor for aluminum alloy materials which comprises Al 7 Cu 2 Fe particles, inside a raw material aluminum alloy material, it is possible to prevent hydrogen embrittlement in the aluminum alloy material.
  • Al 7 Cu 2 Fe particles it is possible to add Al 7 Cu 2 Fe particles to the raw material aluminum alloy material, or to add Fe at the time of production to form Al 7 Cu 2 Fe particles, and ultimately use the Al 7 Cu 2 Fe particles as a hydrogen embrittlement inhibitor.
  • the raw material aluminum alloy material may be a raw material mixture before a metal such as Al or a metal compound is alloyed.
  • the aluminum alloy material can be produced by subjecting the raw material aluminum alloy material (which may be a raw material mixture) to a well-known process such as a heat treatment, rolling, forging and/or casting.
  • a heat treatment such as a heat treatment, rolling, forging and/or casting.
  • the hydrogen embrittlement inhibitor for aluminum alloy materials of the present invention comprises Al 7 Cu 2 Fe particles and can prevent hydrogen embrittlement of aluminum alloy materials.
  • Al 7 Cu 2 Fe particles may be contained in an existing aluminum alloy material, but such a product was not known to be a hydrogen embrittlement inhibitor for aluminum alloy materials.
  • the raw material aluminum alloy material in which hydrogen embrittlement is to be prevented may be the aluminum alloy material of the present invention or a conventional aluminum alloy material.
  • the hydrogen embrittlement inhibitor for aluminum alloy materials of the present invention is preferable for the hydrogen embrittlement inhibitor for aluminum alloy materials of the present invention to be able to prevent hydrogen embrittlement of an aluminum alloy material having aluminum alloy composition (A) below.
  • the hydrogen embrittlement inhibitor for aluminum alloy materials of the present invention is preferable for the hydrogen embrittlement inhibitor for aluminum alloy materials of the present invention to be able to prevent hydrogen embrittlement in an aluminum alloy material having any one of aluminum alloy compositions (1) to (7) above.
  • the hydrogen embrittlement inhibitor for aluminum alloy materials of the present invention is able to prevent hydrogen embrittlement in an aluminum alloy material having any one of aluminum alloy compositions (A1) to (A7) below.
  • Aluminum alloy compositions (A1) to (A7) are summarized in Table 1 below. “Alloy number” in Table 1 means the alloy number in JIS H 4100: 2014 “Aluminum and aluminum alloy plates and strips”.
  • an aluminum alloy material (High Fe) of Working Example 1 in which content of Fe was 0.30 mass%, was prepared as an aluminum alloy material that satisfies aluminum alloy composition (3).
  • This aluminum alloy material is an Al-Zn-Cu alloy which contains 50 mass% or more of Al as a primary component, with the component having the next highest content being Zn, followed by Cu.
  • FIG. 1 shows a virtual cross section of a tomographic image of a microstructure of the (High Fe) aluminum alloy material of Working Example 1.
  • FIG. 2 shows a virtual cross section of a tomographic image of a fracture surface of the (High Fe) aluminum alloy material of Working Example 1.
  • QCF means Area fraction of Quasi-cleavage creak.
  • FIG. 3 shows a virtual cross section of a tomographic image of the (Low Fe) aluminum alloy material of Reference Example 2.
  • FIG. 4 shows a virtual cross section of a tomographic image of a fracture surface of the (Low Fe) aluminum alloy material of Reference Example 2.
  • the hydrogen amount (H at IMC) in a microstructure and the hydrogen amount (H at ⁇ 2 ) in a semi-coherent precipitate ( ⁇ 2 , semi-coherent) were determined using a calculation process.
  • the hydrogen trapping energies of microstructures in the aluminum alloy material were calculated using first principle calculations. The obtained results are shown in FIG. 6 .
  • spiral dislocations (Screw disl.), solute Mg atoms (Solute Mg), edge dislocations (Edge disl.), grain boundaries (GB), vacancies (Vac.), coherent precipitate interfaces ( ⁇ 1 , coherent), semi-coherent precipitate interfaces ( ⁇ 2 , semi-coherent), Al 7 Cu 2 Fe particles (IMCp), pore surface (Pore (surface H), and molecular hydrogen in the pore (Pore (H 2 )) are shown in order from the left.
  • the crystal structure (space group P4/mnc) of the Al 7 Cu 2 Fe particles is shown in FIG. 7 (see Bown et al., Acta Cryst., 9 (1956), 911). From FIG. 7 , it can be confirmed that there is a hydrogen trapping site that can strongly trap H inside the Al 7 Cu 2 Fe particles.
  • the hydrogen distribution state in the aluminum alloy material was analyzed.
  • FIG. 8 amounts of hydrogen trapped in microstructures of lattices (Lattice), solute Mg atoms (Mg), pores (V), grain boundaries ( ⁇ ), Al 7 Cu 2 Fe particles (IMCp), coherent precipitate interfaces (coherent), semi-coherent precipitate interfaces (semi-coherent) and pores (Pore), respectively, are shown in order from the left.
  • the left hand bar shows a case where the amount of Fe is 0.30 mass% (High Fe), which corresponds to Working Example 1
  • the right hand bar shows a case where the amount of Fe is 0.01 mass% (Low Fe), which corresponds to Reference Example 2.
  • results for a case where the amount of Fe is 0.05 mass% (Mid Fe), which corresponds to Reference Example 1 are not shown in FIG. 8 .
  • FIG. 9 is a graph that shows the relationship between hydrogen distribution to IMC (Al 7 Cu 2 Fe) particles (H at IMC), hydrogen distribution to a semi-coherent precipitate interface (H at ⁇ 2 ), and hydrogen embrittlement (quasi-cleavage creak) area fraction QCF.
  • the horizontal axis shows the amount of Fe in the aluminum alloy materials of Working Example 1, Reference Example 1 and Reference Example 2.
  • the aluminum alloy material effectively functions as a hydrogen brittle inhibitor even in a case where a material for casting an aluminum alloy material having a conventional well-known composition specified in JIS H 4100: 2014 is used, because Al 7 Cu 2 Fe particles are formed inside the material as second phase particles.

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JP2020096333A JP2021188102A (ja) 2020-06-02 2020-06-02 アルミニウム合金材およびアルミニウム合金材の水素脆化防止剤
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PCT/JP2021/020104 WO2021246267A1 (ja) 2020-06-02 2021-05-27 アルミニウム合金材およびアルミニウム合金材の水素脆化防止剤

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CA2091355A1 (en) * 1990-08-22 1992-02-23 James Christopher Mohr Aluminium alloy suitable for can making
JP6198479B2 (ja) * 2013-06-25 2017-09-20 株式会社神戸製鋼所 溶接構造部材用アルミニウム合金鍛造材およびその製造方法
JP6298640B2 (ja) * 2014-01-21 2018-03-20 株式会社Ｕａｃｊ押出加工 二輪車及び三輪車用アンダーブラケット並びにその製造方法
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