WO2021254028A1 - Acier inoxydable à trempe secondaire martensitique, à ultra-haute résistance et renforcé par précipitation cohérente de nanoparticules b2 et son procédé de préparation - Google Patents

Acier inoxydable à trempe secondaire martensitique, à ultra-haute résistance et renforcé par précipitation cohérente de nanoparticules b2 et son procédé de préparation Download PDF

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WO2021254028A1
WO2021254028A1 PCT/CN2021/092941 CN2021092941W WO2021254028A1 WO 2021254028 A1 WO2021254028 A1 WO 2021254028A1 CN 2021092941 W CN2021092941 W CN 2021092941W WO 2021254028 A1 WO2021254028 A1 WO 2021254028A1
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stainless steel
strength
alloy
maraging stainless
maraging
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王清
王镇华
董闯
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大连理工大学
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26—Methods of annealing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • C21D8/0236—Cold rolling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/54—Ferrous alloys, e.g. steel alloys containing chromium with nickel with boron
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/008—Martensite

Definitions

  • the invention belongs to the field of high-strength stainless steel, and particularly relates to a BCC-based ultra-high-strength maraging stainless steel strengthened by the coherent precipitation of B2 nanoparticles and a preparation method thereof.
  • the strength exceeds 2.0 GPa and the elongation exceeds 8.0%.
  • maraging steel As an ultra-high-strength steel, maraging steel is widely used in cutting-edge fields such as aviation, aerospace and military, and has high engineering application value and scientific research significance.
  • Traditional maraging steel is based on ultra-low carbon (or carbon-free) lath martensite (BCC-based) with high density of dislocations. After aging treatment, it forms a variety of non-coherent or semi-coherent with the matrix. Intermetallic compounds (Ni 3 Ti, Ni 3 Mo and Fe 2 (Mo,Ti)) are strengthened. These precipitated phases often have a large interface energy with the matrix, have a high nucleation barrier, and are easy to nucleate at defects such as grain boundaries, resulting in low density and uneven precipitation of the strengthening phase.
  • the precipitated phases are easy to grow along the direction of low mismatch degree, which is easy to be coarsened, which makes the alloy extremely sensitive to the process; and there is a large lattice distortion between the precipitated phase and the matrix. It is easy to produce stress concentration in the process of misalignment, which induces crack initiation, resulting in extremely poor uniform plastic deformation ability of the alloy. And in order to increase the density of the precipitated phases, such steels are usually added with higher content of Ni and Co elements, which further increases the use cost of the steel. Therefore, traditional maraging steel has certain limitations.
  • the maraging steel with coherent precipitation strengthening of B2-NiAl nanoparticles avoids these limitations.
  • the lattice constant (0.2887nm) of the ordered superstructure of BCC B2-NiAl phase is similar to that of ⁇ -Fe (0.2866nm).
  • the coherent precipitated phase has lower interfacial energy and requires less nucleation work .
  • the present invention provides a new ultra-high-strength maraging stainless steel with good corrosion resistance and strong plastic matching with coherent precipitation strengthening of B2 nanoparticles, the strength of which exceeds 2.0 GPa, and the elongation is greater than 8.0%.
  • the present invention designs and develops a B2 nano particle coherent precipitation strengthening ultra-high-strength maraging stainless steel.
  • the purpose of the present invention is to realize uniform and coherent precipitation of high-density B2 nanoparticles on the martensite matrix, thereby designing a maraging stainless steel with ultra-high strength, good plasticity and corrosion resistance.
  • An ultra-high strength maraging stainless steel with coherent precipitation strengthening of B2 nanoparticles including Fe, Cr, Ni, Al, Mo, W, Nb, C, B elements, Si, Mn, S, P, O, N It is an impurity element, and the mass percentage (wt.%) of its alloy composition is as follows, Cr: 4.0 ⁇ 6.0, Ni: 13.0 ⁇ 15.0, Al: 3.0 ⁇ 4.0, Mo: 1.0 ⁇ 2.0, W: 0.3 ⁇ 0.7, Nb: 0.2 ⁇ 0.4, C: 0.03 ⁇ 0.05, B: 0.004 ⁇ 0.008, Si ⁇ 0.20, Mn ⁇ 0.20, S ⁇ 0.01, P ⁇ 0.02, O ⁇ 0.005, N ⁇ 0.02, Fe: balance; and Nb/C atom The percentage ratio is 1:1, and the atomic percentage ratio of Cr/(Mo+W) is 8:1.
  • the maraging stainless steel has a specific microstructure: high-density (>10 24 m -3 ) B2 phase nanoparticles (3-5 nm) are uniformly and coherently precipitated on the lath martensite matrix, making the The strength of steel is higher than 2.0GPa.
  • a preparation method of ultra-high-strength maraging stainless steel with coherent precipitation strengthening of B2 nanoparticles including the following contents: firstly, each alloy component is smelted at least four times in a vacuum arc according to its mass percentage to obtain an alloy ingot; Secondly, use a muffle furnace to homogenize the alloy ingot, the treatment temperature is 1250°C, the treatment time is 2h, and then it is cold rolled with multiple passes, the total deformation is about 70%; finally, annealing is carried out at 950°C Treat for 15min, and carry out aging treatment at 500°C for 4 ⁇ 48h.
  • the idea for realizing the above technical solution is to use the applicant's cluster composition design method to design the composition of maraging stainless steel.
  • the composition design method is based on the "cluster + connecting atom" structure model, and the stable solid solution structure is divided into clusters and connecting atoms.
  • the cluster is the nearest neighbor coordination polyhedron formed by a certain atom as the center.
  • the clusters in the FCC structure are cubic octahedrons with a coordination number of CN12, and the connecting atoms are placed in the gaps of the cluster stacking, usually located in the next adjacent shell of the cluster.
  • a simple cluster composition formula [cluster] (connecting atom) x can be determined, that is, a cluster matches x connecting atoms.
  • This cluster composition design method has been successfully applied to the design of high-temperature austenitic stainless steels, low-elastic ⁇ -Ti alloys and other engineering alloys, providing new ideas and methods for the composition design of high-performance engineering alloys.
  • austenite is directly related to the Ni equivalent and Cr equivalent of the alloy.
  • the addition of Mo element and W element not only plays a solid solution strengthening effect, but also improves the pitting corrosion resistance of steel. And in the Fe-Cr-Ni-Al quaternary system, the addition of Mo can also increase the lattice constant of the BCC matrix, thereby reducing the lattice mismatch between the BCC matrix and the precipitated phase B2, which is more conducive to the coherence of the B2 phase Precipitate out. Therefore, the addition of Mo and W is based on the atomic ratio of Cr/(Mo+W) of 8:1 instead of the Cr element in the cluster formula.
  • MC-type carbides can not only refine the original austenite grains, but also play a role of strengthening the second phase, but the excessive addition of C will cause the welding performance of the alloy to decrease, and at the same time reduce the plasticity of the steel. Therefore, the addition of C element is controlled between 0.03 and 0.05wt.%. At the same time, in order to suppress the precipitation of coarse and large Cr 23 C 6 carbides, it is necessary to add the same atomic percentage of Nb element. The addition of trace element B (0.004 ⁇ 0.008wt.%) can increase the grain boundary bonding force, thereby improving the plasticity of steel.
  • composition of the ultra-high-strength maraging stainless steel with coherent precipitation strengthening of B2 nanoparticles which is Fe-(4.0 ⁇ 6.0)Cr-(13.0 ⁇ 15.0)Ni-(3.0 ⁇ 4.0)Al-(1.0 ⁇ 2.0)Mo-(0.3 ⁇ 0.7)W-(0.2 ⁇ 0.4)Nb-(0.03 ⁇ 0.05)C-(0.004 ⁇ 0.008)B
  • Si, Mn, S, P, O, N are impurity elements: Si ⁇ 0.20 , Mn ⁇ 0.20, S ⁇ 0.01, P ⁇ 0.02, O ⁇ 0.005, N ⁇ 0.02 (wt.%).
  • the preparation method of the present invention is as follows: high-purity metal material is used, and ingredients are carried out according to mass percentage.
  • a vacuum non-consumable arc smelting furnace is used to melt the ingredients at least four times under the protection of an argon atmosphere to obtain an alloy ingot with a uniform composition and a mass of about 100g, and the mass loss during the smelting process does not exceed 0.1%.
  • the alloy ingot was homogenized with a muffle furnace. The homogenization temperature was 1250°C and the time was 2h. Subsequently, cold rolling is performed in multiple passes, and the reduction in each pass does not exceed 0.2 mm, and the total deformation is about 70%, and a plate sample with a thickness of about 3 mm is obtained.
  • the alloy sheet is annealed, the annealing temperature is 950°C, the annealing time is 15min, and finally the aging treatment is carried out at 500°C for 4 ⁇ 48h.
  • Use metallographic microscope (OM), scanning electron microscope (SEM), transmission electron microscope (TEM) and X-ray diffractometer (XRD, Cu K ⁇ radiation, ⁇ 0.15406nm) to detect alloy structure and structure; use HVS-1000 dimension
  • the hardness tester is used to test the hardness of a series of alloys under different heat treatment conditions; the UTM5504 electronic universal tensile testing machine is used to test the tensile mechanical properties at room temperature; the CS350 electrochemical workstation is used to test the corrosion resistance of the alloy in 3.5wt.% NaCl aqueous solution .
  • the present invention is an ultra-high-strength maraging stainless steel strengthened by the coherent precipitation of B2 nanoparticles.
  • the mass percentage (wt.%) of the alloy composition is Cr: 4.0 ⁇ 6.0, Ni: 13.0 ⁇ 15.0, Al: 3.0 ⁇ 4.0, Mo: 1.0 ⁇ 2.0, W: 0.3 ⁇ 0.7, Nb: 0.2 ⁇ 0.4, C: 0.03 ⁇ 0.05, B: 0.004 ⁇ 0.008, Si ⁇ 0.20, Mn ⁇ 0.20, S ⁇ 0.01, P ⁇ 0.02, O ⁇ 0.005, N ⁇ 0.02, Fe: balance; and the atomic percentage ratio of Nb/C is 1: 1.
  • the atomic percentage ratio of Cr/(Mo+W) is 8:1.
  • the alloy is aged at 500°C (4 ⁇ 48h) After that, high-density (>10 24 m -3 ) B2 phase nanoparticles (3-5 nm) are uniformly and coherently precipitated on the lath martensite matrix.
  • the present invention designs and develops an ultra-high-strength maraging stainless steel with coherent precipitation strengthening of B2 nanoparticles based on our self-developed cluster composition method.
  • the present invention adopts the new concept of coherent precipitation strengthening, through the coherent precipitation of high-density B2 phase nanoparticles on the martensite matrix ,
  • the uniform precipitation and the coherent phase interface brought by the coherent precipitation coupled with the high density of movable dislocations in the lath martensite, hinder the initiation of cracks , Improve the uniform plastic deformation ability of the new horse-aged stainless steel.
  • the new maraging stainless steel uses cheap Al, Cr and other elements to replace the expensive elements Co and Ti in traditional maraging steels, and adds the C element avoided by traditional maraging steels.
  • the preparation process is simple. Material costs are greatly reduced.
  • a B2 nano-particle coherent precipitation-strengthened ultra-high-strength maraging stainless steel has been developed, and the mass percentage (wt.%) of the alloy composition is Cr: 4.0-6.0, Ni: 13.0 ⁇ 15.0, Al: 3.0 ⁇ 4.0, Mo: 1.0 ⁇ 2.0, W: 0.3 ⁇ 0.7, Nb: 0.2 ⁇ 0.4, C: 0.03 ⁇ 0.05, B: 0.004 ⁇ 0.008, Si ⁇ 0.20, Mn ⁇ 0.20, S ⁇ 0.01, P ⁇ 0.02, O ⁇ 0.005, N ⁇ 0.02, Fe: margin;
  • This new type of maraging stainless steel uses cheap Al, Cr and other elements to replace the expensive elements Co and Ti in traditional maraging steel.
  • the new maraging stainless steel has a strength higher than 2.0 through the coherent precipitation strengthening of high-density B2 phase particles. GPa's ultra-high strength, good uniform plastic deformation ability, and excellent corrosion resistance.
  • Fig. 1 is a TEM structure morphology of the alloy prepared in Example 1. High-density B2 phase nanoparticles are coherently precipitated on the martensite matrix.
  • Example 1 Fe-5.30Cr-13.47Ni-3.10Al-1.22Mo-0.50W-0.23Nb-0.03C-0.005B (wt.%) alloy
  • High-purity metal materials are used, and ingredients are carried out in accordance with mass percentage.
  • a vacuum non-consumable arc smelting furnace is used to melt the ingredients at least four times under the protection of an argon atmosphere to obtain an alloy ingot with a uniform composition and a mass of about 100g. The mass loss during the smelting process does not exceed 0.1%.
  • Use a muffle furnace to homogenize the alloy ingot at 1250°C/2h. Subsequently, cold rolling is performed in multiple passes, and the reduction in each pass does not exceed 0.2 mm, and the total deformation is about 70%, and a plate sample with a thickness of about 3 mm is obtained. After that, the alloy sheet is annealed at 950°C/15min, and finally aging at 500°C/8h.
  • Step 2 Alloy structure and mechanical properties and corrosion resistance test
  • High-purity metal materials are used, and ingredients are carried out in accordance with mass percentage.
  • a vacuum non-consumable arc smelting furnace is used to melt the ingredients at least four times under the protection of an argon atmosphere to obtain an alloy ingot with a uniform composition and a mass of about 100g, and the mass loss during the smelting process does not exceed 0.1%.
  • Use a muffle furnace to homogenize the alloy ingot at 1250°C/2h.
  • cold rolling is performed in multiple passes, and the reduction in each pass does not exceed 0.2 mm, and the total deformation is about 70%, and a plate sample with a thickness of about 3 mm is obtained.
  • the alloy sheet is annealed at 950°C/15min, and finally aged at 500°C/12h.
  • Step 2 Test the alloy structure and mechanical properties
  • OM, SEM, and XRD were used to detect the structure and structure of the alloy after stabilization.
  • the results showed that the alloy of the present invention was a lath martensite structure, and high-density B2 phase nanoparticles were co-precipitated on the martensite matrix.
  • Example 3 Fe-6.0Cr-13.0Ni-4.0Al-2.0Mo-0.50W-0.40Nb-0.05C-0.008B (wt.%) alloy
  • a vacuum non-consumable arc smelting furnace is used to melt the ingredients at least four times under the protection of an argon atmosphere to obtain an alloy ingot with a uniform composition and a mass of about 100g, and the mass loss during the smelting process does not exceed 0.1%.
  • Use a muffle furnace to homogenize the alloy ingot at 1250°C/2h.
  • cold rolling is performed in multiple passes, and the reduction in each pass does not exceed 0.2 mm, and the total deformation is about 70%, and a plate sample with a thickness of about 3 mm is obtained.
  • the alloy sheet is annealed at 950°C/15min, and finally aging at 500°C/48h.
  • Step 2 Alloy structure and mechanical properties and corrosion resistance test
  • the alloy of the present invention is a lath martensite structure, and high-density B2 phase nanoparticles are co-precipitated on the martensite matrix.

Abstract

La présente invention concerne un acier inoxydable à trempe secondaire martensitique, à ultra-haute résistance et renforcé par précipitation cohérente de nanoparticules B2, et son procédé de préparation, qui relèvent du domaine de l'acier inoxydable à haute résistance. L'acier inoxydable à trempe secondaire martensitique contient les éléments Fe, Cr, Ni, Al, Mo, W, Nb, C et B, Si, Mn, S, P, O et N étant des éléments d'impuretés. Le pourcentage en masse (% en poids) des composants de l'alliage est Cr : de 4,0 à 6,0, Ni : de 13,0 à 15,0, Al : de 3,0 à 4,0, Mo : de 1,0 à 2,0, W : de 0,3 à 0,7, Nb : de 0,2 à 0,4, C : de 0,03 à 0,05, B : de 0,004 à 0,008, Si ≤ 0,20, Mn ≤ 0,20, S ≤ 0,01, P ≤ 0,02, O ≤ 0,005, N ≤ 0,02, Fe : le reste. Le rapport des pourcentages atomiques de Nb/C est égal à 1:1. Le rapport des pourcentages atomiques de Cr/(Mo+W) est égal à 8:1. D'après la présente invention, une précipitation cohérente et uniforme de nanoparticules de phase B2 à haute densité sur une matrice de martensite est obtenue au moyen d'une conception des composants d'un alliage telle que l'alliage présente une résistance ultra-haute, supérieure à 2,0 GPa, une capacité de déformation plastique uniforme satisfaisante et une excellente résistance à la corrosion. De plus, le processus de préparation est simple, le coût des matériaux est considérablement réduit et un nouvel acier inoxydable à trempe secondaire martensitique à ultra-haute résistance est obtenu.
PCT/CN2021/092941 2020-06-17 2021-05-11 Acier inoxydable à trempe secondaire martensitique, à ultra-haute résistance et renforcé par précipitation cohérente de nanoparticules b2 et son procédé de préparation WO2021254028A1 (fr)

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CN202010555730.3A CN111593260B (zh) 2020-06-17 2020-06-17 一种b2纳米粒子共格析出强化的超高强度马氏体时效不锈钢及制备方法
CN202010555730.3 2020-06-17

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