EP3105358B1 - Verfahren zur herstellung einer titanfreien legierung - Google Patents

Verfahren zur herstellung einer titanfreien legierung Download PDF

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Publication number
EP3105358B1
EP3105358B1 EP15716712.3A EP15716712A EP3105358B1 EP 3105358 B1 EP3105358 B1 EP 3105358B1 EP 15716712 A EP15716712 A EP 15716712A EP 3105358 B1 EP3105358 B1 EP 3105358B1
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max
alloy
titanium
weight
producing
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French (fr)
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EP3105358A1 (de
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Julia Rosenberg
Jutta KLÖWER
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VDM Metals International GmbH
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VDM Metals International GmbH
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Priority claimed from DE102014002402.4A external-priority patent/DE102014002402A1/de
Priority claimed from DE102014002693.0A external-priority patent/DE102014002693A1/de
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    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
    • 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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/004—Heat treatment of ferrous alloys containing Cr and Ni
    • 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/021—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips involving particular fabrication steps or treatments of ingots or slabs
    • 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • C21D8/0226—Hot rolling
    • 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0247—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
    • 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0247—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
    • C21D8/0263—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment following hot rolling
    • 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/10—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0081—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/08—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • 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
    • C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
    • 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
    • C22C38/004—Very low carbon steels, i.e. having a carbon content of less than 0,01%
    • 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
    • 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
    • C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
    • 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
    • C—CHEMISTRY; METALLURGY
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/20—Ferrous alloys, e.g. steel alloys containing chromium with copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon

Definitions

  • the invention relates to a method for producing a titanium-free alloy with high pitting and crevice corrosion resistance and high yield strength and strength in the work-hardened state.
  • the highly corrosion-resistant alloy Alloy 825 is mainly used in the chemical industry and offshore technology. It is marketed under the material number 2.4858 and has the following chemical composition: C ⁇ 0.025%, S ⁇ 0.015%, Cr 19.5-23.5%, Ni 28-46%, Mn ⁇ 1%, Si ⁇ 0.5% , Mo 2.5-3.5%, Ti 0.6-1.2%, Cu 1.5-3%, Al ⁇ 0.2%, Co ⁇ 1%, Fe balance.
  • the alloy Alloy 825 is a titanium-stabilized material.
  • titanium can cause problems, especially in continuous casting, since it reacts with the SiO 2 of the casting powder (Problem 3). It would be desirable to avoid the element titanium, but this leads to a significant increase in the edge crack tendency.
  • the JP 61288041 A1 refers to an alloy of the following composition: C ⁇ 0,045%, S ⁇ 0,03%, N 0,005 - 0,2%, Cr 14 - 26%, Mn ⁇ 1%, Si ⁇ 1%, Mo ⁇ 8%, Cu ⁇ 2 %, Fe ⁇ 25%, Al ⁇ 2%, B 0.001 - 0.1%, Mg 0.005 - 0.5%, remainder Ni.
  • the content of Nb is generated by a formula.
  • at least one of the elements Ti, Al, Zr, W, Ta, V, Hf may be contained in contents ⁇ 2.
  • the US 2,777,766 discloses an alloy of the following composition: C ⁇ 0.25%, Cr 18-25%, Ni 35-50%, Mo 2-12%, Nb 0.1-5%, Cu up to 2.5%, W up to 5% , Fe remainder (at least 15%).
  • GB 2123031 A is an austenitic high nickel-containing alloy of the following composition: ⁇ 0.05% C, ⁇ 0.04 N, ⁇ 1.0% Si, ⁇ 1.0% Mn, 35-45% Ni, 20-30% Cr, 4 - 7% Mo, balance iron and unavoidable impurities, where Cr + 3 Mo is at least 40%.
  • an austenitic stainless steel which has the following composition (in% by weight):> 0.05-0.15% C, ⁇ 2% Si, 0.1-3% Mn, ⁇ 0.04% P, ⁇ 0.01% S,> 20 - ⁇ 28% Cr,> 15 - 55% Ni,> 2 to 6% Cu, 0.1 - 0.8% Nb, 0.02 - 1.5% V, 0.001 - 0.1% Al,> 0.05 - 0.3% N, ⁇ 0.006% O, balance iron and impurities.
  • the EP 2163655 A1 describes a method for producing a high alloy steel pipe.
  • the following alloy is to be formed into a tube by multi-stage hot and cold forming processes: ⁇ 0.03% C, ⁇ 1.0% Si, 0.05 - 1.5% Mn, ⁇ 0.03% P, ⁇ 0.03 % S,> 22 - ⁇ 40% Ni, 20 - 30% Cr,> 0.01 - ⁇ 4.0% Mo, 0 - 4% Cu, 0.001 - 0.3% Al,> 0.05 - ⁇ 0 , 3% N, ⁇ 0.01% O, balance iron and impurities.
  • a suitable embodiment of the alloy has the following composition (in% by weight) C Max. 0.015% S Max. 0.005% N Max. 0.02% Cr 21.0 - ⁇ 23% Ni > 39.0 - ⁇ 43.0% Mn 0,5 - 0,9% Si 0.2 - ⁇ 0.5% Not a word > 4.5-6.5% Nb Max. 0.15% Cu > 1.6 - ⁇ 2.3% al 0.06 - ⁇ 0.25% Co Max. 0.5% B 0.002 - 0.004% mg 0.006 - 0.015% Fe Remainder as well as smelting-related impurities
  • the chromium content can be modified as follows: Cr > 21.5 - ⁇ 23% Cr 22.0 - ⁇ 23%
  • the molybdenum content can be modified as follows: Not a word > 5 - ⁇ 6.5% Not a word > 5 - ⁇ 6.2%
  • the content of copper can, if necessary, still be set as follows: Cu > 1.6 - ⁇ 2.0%
  • the alloy may still contain the element V in contents (in wt.) V > 0 - 1.0% V 0.2 - 0.7% be added.
  • the iron content in the alloy according to the invention should be> 22%.
  • the PRE total in terms of corrosion resistance of Alloy 825 is PRE 33 and is very low compared to other alloys.
  • Table 2 shows the active quantities PRE according to the prior art. Table 2: Sum of PRE for various prior art alloys Alloy Ni Fe Cr Not a word Other PRE Duplex 2205 5.5 rest 22 3 0.15 N 37 825 40 31 23 3.2 33 28 31 35 27 3.5 1.3 Cu 38 926 25 rest 19 6 0.16 N 47
  • Table 3 shows the results of various pitting corrosion studies.
  • the reduced titanium content has no negative influence on the pitting corrosion temperature.
  • the increased molybdenum content has positive effects.
  • Table 3 Critical pitting corrosion temperature in 6% FeCl 3 3 /% + 1% HCL, over 72 hours (ASTM G-48 Method C).
  • Figures 1 and 2 below show results of tensile tests on the one hand of the reference alloy Alloy 825 and on the other hand of alternative alloys.
  • Molybdenum has a positive effect on yield strength and strength.
  • Figures 3 and 4 illustrate the positive influence of Molydbän.
  • the alloy can also be produced by ESR / VAR remelting.
  • the inventive method is intended to be used for the production of a component in the oil and gas industry.
  • Table 6 contrasts Alloy 825 (standard) with two alloys of the present invention.

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  • Moulds For Moulding Plastics Or The Like (AREA)
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  • Arc Welding In General (AREA)

Description

  • Die Erfindung betrifft ein Verfahren zur Herstellung einer titanfreien Legierung mit hoher Lochfraß- und Spaltkorrosionsbeständigkeit sowie hoher Streckgrenze und Festigkeit im kaltverfestigten Zustand.
  • Der hochkorrosionsbeständige Werkstoff Alloy 825 wird schwerpunktmäßig in der chemischen Industrie und in der Offshore-Technik eingesetzt. Er wird unter der Werkstoffnummer 2.4858 vertrieben und hat folgende chemische Zusammensetzung: C ≤ 0,025 %, S ≤ 0,015 %, Cr 19,5 - 23,5 %, Ni 28 - 46 %, Mn ≤ 1 %, Si ≤ 0,5 %, Mo 2,5 - 3,5 %, Ti 0,6 - 1,2 %, Cu 1,5 - 3 %, Al ≤ 0,2 %, Co ≤ 1 %, Fe Rest.
  • Für neue Anwendungen in der Öl- und Gas-Industrie sind die Lochfraß- und Spaltkorrosionsbeständigkeit (Problem 1) sowie die Streckgrenze und Festigkeit (Problem 2) zu gering.
  • Im Hinblick auf den geringen Chrom- und Molybdängehalt weist Alloy 825 nur eine vergleichsweise geringe Wirksumme auf (PRE = 1 x % Cr + 3,3 x % Mo). Unter der Wirksumme PRE versteht der Fachmann Pitting Resistance Equivalent.
  • Bei der Legierung Alloy 825 handelt es sich um einen titanstabilisierten Werkstoff. Titan kann jedoch zu Problemen, insbesondere beim Strangguss führen, da es mit dem SiO2 des Gießpulvers reagiert (Problem 3). Wünschenswert wäre ein Vermeiden des Elements Titan, was allerdings zu einer signifikanten Erhöhung der Kantenrissneigung führt.
  • Die JP 61288041 A1 betrifft eine Legierung folgender Zusammensetzung: C < 0,045 %, S < 0,03 %, N 0,005 - 0,2 %, Cr 14 - 26 %, Mn < 1 %, Si < 1 %, Mo < 8 %, Cu < 2 %, Fe < 25 %, Al < 2 %, B 0,001 - 0,1 %, Mg 0,005 - 0,5 %, Rest Ni. Der Gehalt an Nb wird durch eine Formel generiert. Darüber hinaus kann mindestens eines der Elemente Ti, Al, Zr, W, Ta, V, Hf in Gehalten ≤ 2 enthalten sein.
  • Die US 2,777,766 offenbart eine Legierung folgender Zusammensetzung: C < 0,25 %, Cr 18 - 25 %, Ni 35 - 50 %, Mo 2 - 12 %, Nb 0,1 - 5 %, Cu bis 2,5 %, W bis 5 %, Fe Rest (min. 15 %).
  • Der GB 2123031 A ist eine austenitische hochnickelhaltige Legierung folgender Zusammensetzung zu entnehmen: ≤ 0,05 % C, ≤ 0,04 N, ≤ 1,0 % Si, ≤ 1,0 % Mn, 35 - 45 % Ni, 20 - 30 % Cr, 4 - 7 % Mo, Rest Eisen und unvermeidbare Verunreinigungen, wobei Cr + 3 Mo mindestens 40 % beträgt.
  • In der EP 1471158 A1 wird ein austenitischer rostfreier Stahl beschrieben, der folgende Zusammensetzung (in Gew.-%) aufweist: > 0,05 - 0,15 % C, ≤ 2 % Si, 0,1 - 3 % Mn, ≤ 0,04 % P, ≤ 0,01 % S, > 20 - < 28 % Cr, > 15 - 55 % Ni, > 2 bis 6 % Cu, 0,1 - 0,8 % Nb, 0,02 - 1,5 % V, 0,001 - 0,1 % Al, > 0,05 - 0,3 % N, ≤ 0,006 % O, Rest Eisen und Verunreinigungen.
  • Die EP 2163655 A1 beschreibt ein Verfahren zur Herstellung eines hochlegierten Stahlrohres. Nachstehende Legierung soll durch mehrstufige Warm- und Kaltverformungsprozesse zu einem Rohr umgeformt werden: ≤ 0,03 % C, ≤ 1,0% Si, 0,05 - 1,5 % Mn, ≤ 0,03 % P, ≤ 0,03 % S, > 22 - < 40 % Ni, 20 - 30 % Cr, > 0,01 - < 4,0 % Mo, 0 - 4 % Cu, 0,001 - 0,3 % Al, > 0,05 - < 0,3 % N, ≤ 0,01 % O, Rest Eisen und Verunreinigungen.
  • Durch die DE 10 2007 005 605 A1 ist eine Eisen-Nickel-Chrom-Silizium-Legierung folgender Zusammensetzung bekannt geworden: 34 - 42 % Ni, 18 - 26 % Cr, 1,0 - 2,5 % Si und Zugaben von 0,05 - 1,0 % Al, 0,01 - 1 % Mn, 0,01 - 0,26 % La, 0,0005 - 0,05 % Mg, 0,01 - 0,14 % C, 0,01 - 0,14 % N, max. 0,01 % S, max. 0,0005 % P, Rest Eisen und den üblichen verfahrensbedingten Verunreinigungen. Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren zur Herstellung einer zu Alloy 825 alternativen Legierung bereitzustellen, das den vorab aufgezeigten Problemen gerecht wird, wobei die Legierung
    • titanfrei ist,
    • eine erhöhte Lochfraß- und Spaltkorrosionsbeständigkeit aufweist,
    • eine höhere Streckgrenze im kaltverfestigten Zustand hat,
    • eine zumindest gleich gute Warmumform- und Schweißbarkeit aufweist.
  • Diese Aufgabe wird gelöst durch ein Verfahren zur Herstellung einer titanfreien Legierung mit (in Gew.-%)
    C max. 0,02 %
    S max. 0,01 %
    N max. 0,03 %
    Cr 20,0 - 23,0 %
    Ni 39,0 - 44,0 %
    Mn 0,4 - < 1,0 %
    Si 0,1 - < 0,5 %
    Mo > 4,0 - < 7,0 %
    Nb max. 0,15 %
    Cu > 1,5 - < 2,5 %
    Al 0,05 - < 0,3 %
    Co max. 0,5 %
    B 0,001 - < 0,005 %
    Mg 0,005 - < 0,015 %
    V bedarfsweise 0 - 1,0 %, insbesondere 0,2 - 0,7%
    Fe Rest sowie erschmelzungsbedingte Verunreinigungen,
    indem
    1. a) die Legierung offen im Strang- oder Blockguss erschmolzen wird,
    2. b) zur Aufhebung der durch den erhöhten Molybdängehalt verursachten Seigerungen eine Homogenisierungsglühung der erzeugten Brammen/Knüppel bei 1150-1250 °C über 15 bis 25 h durchgeführt wird, wobei
    3. c) die Homogenisierungsglühung im Anschluss an eine erste Warmumformung durchgeführt wird.
  • Eine zweckmäßige Ausgestaltung der Legierung weist folgende Zusammensetzung (in Gew.-%)
    C max. 0,015 %
    S max. 0,005 %
    N max. 0,02 %
    Cr 21,0 - < 23 %
    Ni > 39,0 - < 43,0 %
    Mn 0,5 - 0,9 %
    Si 0,2 - < 0,5 %
    Mo >4,5-6,5%
    Nb max. 0,15 %
    Cu > 1,6 - < 2,3 %
    Al 0,06 - < 0,25 %
    Co max. 0,5 %
    B 0,002 - 0,004 %
    Mg 0,006 - 0,015 %
    Fe Rest sowie erschmelzungsbedingte Verunreinigungen
  • Der Gehalt an Chrom kann bedarfsweise noch wie folgt modifiziert werden:
    Cr > 21,5 - < 23 %
    Cr 22,0 - < 23 %
  • Der Nickelgehalt kann bedarfsweise noch wie folgt modifiziert werden:
    Ni > 39, 0 - < 42 %
    Ni > 39,0 - < 41 %
  • Der Molybdängehalt kann bedarfsweise noch wie folgt modifiziert werden:
    Mo > 5 - < 6,5 %
    Mo > 5 - < 6,2 %
  • Der Gehalt an Kupfer kann bedarfsweise noch wie folgt eingestellt werden:
    Cu > 1,6 - < 2,0 %
  • Bedarfsweise kann der Legierung noch das Element V in Gehalten (in Gew.-)
    V > 0 - 1,0 %
    V 0,2 - 0,7 %
    zugesetzt werden.
  • Der Eisengehalt soll in der erfindungsgemäßen Legierung > 22 % sein.
  • Durch das Weglassen des Elements Titan entstehen - wie vorab dargelegt - beim Walzen Kantenrisse. Die Rissneigung kann durch Magnesium in der Größenordnung 50-150 ppm positiv beeinflusst werden. In der Tabelle 1 sind die dazugehörigen/untersuchten Laborschmelzen aufgeführt.
    Element in Gew-% C S N Cr Ni Mn Si Mo Ti Nb Cu Fe Al B Mg in ppm Ca in ppm Kantenrisse
    Ref825 0,002 0.0048 0,006 22,25 39,41 0,8 0,3 3,27 0,8 0,01 2 R 0,14 0 - - nein
    LB2181 0,002 0,004 0,006 22,57 39,76 0,8 0,3 3,27 0,4 0,01 2,1 R 0,12 0 - - gering
    LB2182 0,006 0,003 0,052> 22,46 39,71 0,8 0,3 3,27 - 0,01 2 R 0,11 0 - - ja
    LB2183 0,002 0,004 0,094> 22,65 39,61 0,8 0,3 3,28 - 0,01 1,9 R 0,1 0 - - ja
    LB2218 0,005 0,0031 0,048> 22.50 39,59 0,8 0,3 3,27 - 0,01 2 R 0,12 0,01 100 - nein
    LB2219 0,005 0,0021 0,043> 22,71 39,99 0,8 0,3 4,00> - 0,01 2 R 0.10 0,01 100 - nein
    LB2220 0,004 0.00202 0,042> 22,56 39,84 0,8 0.33 4,93> - 0,01 2 R 0,11 0 100 - nein
    LB2221 0,004 0,0022 0,038> 22,43 39,66 0,8 0,3 3,74> - 0,01 1,9 R 0,11 0 10 - ja
    LB2222 0,003 0,0033 0,042> 22,5 39,62 0,8 0,3 3,66> - 0,01 2 R 0,18 0 20 - ja
    LB2223 0,002 0,0036 0,041> 22.4 39,78 0,7 0,3 3,65> - 0,01 2.00 R 0,27> 0 20 - ja
    LB2234 0,003 0,005 0,007 22,57 39,77 0,8 0,3 3,26 - 0,01 2,1 R 0,15 0 80 10 nein
    LB2235 0,003 0,0034 0,006 22,56 39,67 0,8 0,3 3,28 - 0,01 2,1 R 0,12 0 150 12 nein
    LB2236 0,002 0,004 0,006 22,34 39,46 0,8 0,3 3,27 - 0,01 2 R 0,11 0 30 42 gering
    LB2317 0,001 0,0025 0.030 22.48 40,09 0,8 0,3 4,21 - 0,01( 2 R 0,16 0 100 5 nein
    LB2318 0,002 0,0036 0,038> 22,76 39,77 0,8 0,3 5,20> - 0,01 2,1 R 0,15 0 100 4 nein
    LB2319 0,002( 0,0039 0,043> 22,93> 39,79 0,8 0,3 6,06 - 0,01 2,2 R 0,12 0 100 3 nein
    LB2321 0,002 0.0051 0,040> 22,56 40,23> 0,7 0,3 6,23 - 0,01 2,1 R 0.10 0 100 4 nein
    Tabelle 1: Einfluss von Desoxidationselementen auf die Kantenrissneigung beim Warmwalzen
  • Die Wirksumme PRE im Hinblick auf die Korrosionsbeständigkeit des Alloy 825 liegt bei PRE 33 und ist im Vergleich zu anderen Legierungen sehr gering. In Tabelle 2 sind die Wirksummen PRE gemäß dem Stand der Technik abgebildet. Tabelle 2: Wirksumme PRE für verschiedene dem Stand der Technik entsprechende Legierungen
    Alloy Ni Fe Cr Mo Andere PRE
    Duplex 2205 5,5 Rest 22 3 0,15 N 37
    825 40 31 23 3,2 33
    28 31 35 27 3,5 1,3 Cu 38
    926 25 Rest 19 6 0,16 N 47
  • Durch Erhöhung des Molybdängehalts lässt sich diese Wirksumme und somit die Korrosionsbeständigkeit steigern. PRE = 1 x % Cr + 3,3 x % Mo (Pitting Resistance Equivalent).
  • Tabelle 3 zeigt die Ergebnisse diverser Lochfraßkorrosionsuntersuchungen. Der reduzierte Titangehalt hat keinen negativen Einfluss auf die Lochfraßkorrosionstemperatur. Der erhöhte Molybdängehalt hat positive Auswirkungen. Tabelle 3: Kritische Lochfraßkorrosionstemperatur in 6 % FeCl3 + 1 % HCL, über 72 h (ASTM G-48 Methode C).
    T in °C Ni Cr Mo N Ti PRE
    LB 2316 35 39,2 22,4 3,1 0,04 < 0,04 33
    LB 2317 40 40,1 22,5 4,2 0,03 < 0,04 36
    LB 2318 50 39,8 22,8 5,2 0,04 < 0,04 40
    LB 2319 55 38,8 22,9 6,1 0,04 < 0,04 43
    LB 2320 50 39 22,1 6,2 0,1 < 0,03 43
    LB 2321 50 40,2 22,6 6,2 0,04 0,4 43
    LB 2322 40 40 23,1 6,3 0,1 0,4 44
    Alloy 825 Referenz 30 40 23 3,2 < 0,02 0,8 33
  • Weitere Korrosionsuntersuchungen zeigten ebenfalls eine Verbesserung der kritischen Spaltkorrosionstemperaturen im Vergleich zum Alloy 825. Diese sind in Tabelle 4 dargestellte. Tabelle 4: Kritische Lochfraß- (CPT) und Spaltkorrosionstemperatur (CCT)
    Alloy CPT in °C CCT in °C Ni Cr Mo V Ti PRE
    825* 30 <5 33
    PV661 40 15 40 23 3,3 < 0,002 0,8 34
    PV662 50 20 40 23 5,9 < 0,002 < 0,002 42
    PV663 50 20 39 23 5,8 0,4 < 0,002 42
  • Durch 15 und 30-% Kaltverformung kann die Streckgrenze und die Festigkeit erhöht werden. In der folgenden Tabelle sind die dazugehörigen Untersuchungsergebnisse diverser Laborlegierungen aufgeführt. Tabelle 5: Zugversuche bei RT
    Zustand Alloy Rp0,2 Rm A (%) Z (%)
    Lösungsgeglüht 825 Referenz 304 646 - 51
    825 Plus (A) 389 754 39 59
    369 772 39,5 61
    825 Plus (B) 390 765 42,5 62
    383 755 40 63
    15 % KV 825 670 775 22 71
    697 793 19,5 65
    685 779 23,5 69
    825 Plus (A) 903 973 14,5 51
    893 964 13,5 50
    943 987 13,5 54
    825 Plus (B) 929 974 12,5 56
    877 964 12,5 51
    887 962 9,5 49
    30 % KV 825 852 923 14 63
    832 922 13,5 66
    842 920 17,5 64
    825 Plus (A) 979,0 1071,0 11,5 51,0
    970,0 1079,0 8,5 35,0
    996,0 1078,0 11,0 46,0
    825 Plus (B) 980,0 1078,0 11,5 47,0
    980,0 1071,0 11,0 48,0
    996,0 1083,0 10,5 48,0
  • In den nachstehenden Abbildungen 1 und 2 sind Ergebnisse von Zugversuchen, einerseits der Referenzlegierung Alloy 825 und andererseits alternativer Legierungen dargestellt.
    Figure imgb0001
  • Graphische Darstellung der Ergebnisse der Zugversuche bei Raumtemperatur (Mittelwerte) in Abhängigkeit vom Zustand.
  • Molybdän wirkt sich positiv auf die Streckgrenze und die Festigkeit aus. In den Abb. 3 und 4 wird der positive Einfluss von Molydbän verdeutlicht.
    Figure imgb0002
  • Graphische Darstellung der Ergebnisse der Zugversuche bei Raumtemperatur (Mittelwerte) in Abhängigkeit vom Molybdängehalt.
  • Mithilfe des PVR-Tests (Programmierten-Verformungs-Riss-Test) wurde die Heißrisssensibilität der Ni-Basislegierung Alloy 825 untersucht. Durch Anlegen einer linear ansteigenden Zuggeschwindigkeit während des WIG-Schweißens, wurde die kritische Zuggeschwindigkeit VKr bestimmt. In der folgenden Graphik sind die Untersuchungsergebnisse dargestellt. Je höher die Zuggeschwindigkeit und je geringer die Heißrissneigung, umso besser ist die Schweißbarkeit des Werkstoffs. Die titanfreien, hochmolybdänhaltigen Varianten (PV 506 und PV 507) zeigten weniger Risse als die Standardlegierung (PV 942).
    Figure imgb0003
    Figure imgb0004
  • Die Aufgabe wird gelöst durch ein Verfahren zur Herstellung einer Legierung, die eine Zusammensetzung gemäß einem der gegenständlichen Ansprüche aufweist, indem
    1. a) die Legierung offen im Strang- oder Blockguss erschmolzen wird,
    2. b) zur Aufhebung der durch den erhöhten Molybdängehalt verursachten Seigerungen eine Homogenisierungsglühung der erzeugten Brammen/Knüppel bei 1150-1250 °C über 15 bis 25 h durchgeführt wird, wobei
    3. c) die Homogenisierungsglühung insbesondere im Anschluss an eine erste Warmumformung durchgeführt wird.
  • Optional kann die Legierung auch durch ESU/VAR-Umschmelzen erzeugt werden. Das erfindungsgemäße Verfahren soll zur Herstellung eines Bauteils in der Öl- und Gasindustrie eingesetzt werden.
  • Als Produktformen bieten sich hierbei Bleche, Bänder, Rohre (längsnahtgeschweißt und nahtlos), Stangen oder Schmiedeteile an.
  • Tabelle 6 stellt Alloy 825 (Standard) zwei erfindungsgemäßen Legierungen gegenüber.
    Figure imgb0005
    Figure imgb0006

Claims (5)

  1. Verfahren zur Herstellung einer titanfreien Legierung mit (in Gew.-%) C max. 0,02 % S max. 0,01 % N max. 0,03 % Cr 20,0 - 23,0 % Ni 39,0 - 44,0 % Mn 0,4 - < 1,0% Si 0,1 - < 0,5 % Mo > 4,0 - < 7,0 % Nb max. 0,15 % Cu > 1,5 - < 2,5 % Al 0,05 - < 0,3 % Co max. 0,5 % B 0,001 - < 0,005 % Mg 0,005 - < 0,015 % V bedarfsweise 0 - 1,0 %, insbesondere 0,2 - 0,7% Fe Rest sowie erschmelzungsbedingte Verunreinigungen, indem
    a) die Legierung offen im Strang- oder Blockguss erschmolzen wird,
    b) zur Aufhebung der durch den erhöhten Molybdängehalt verursachten Seigerungen eine Homogenisierungsglühung der erzeugten Brammen/Knüppel bei 1150-1250 °C über 15 bis 25 h durchgeführt wird, wobei
    c) die Homogenisierungsglühung im Anschluss an eine erste Warmumformung durchgeführt wird.
  2. Verfahren nach Anspruch 1 mit (in Gew.-%) C max. 0,015 % S max. 0,005 % N max. 0,02 % Cr 21,0 - < 23 % Ni > 39,0 - < 43,0 % Mn 0,5 - 0,9 % Si 0,2 - < 0,5 % Mo > 4,5--- 6,5 % Nb max. 0,15 % Cu > 1,6 - < 2,3 % Al 0,06 - < 0,25 % Co max. 0,5 % B 0,002 - 0,004 % Mg 0,006 - 0,015 % Fe Rest sowie erschmelzungsbedingte Verunreinigungen.
  3. Verfahren nach Anspruch 1 oder 2 mit (in Gew.-%) Cr > 21,5 - < 23 % Ni > 39,0 - < 42 % Mo > 5 - < 6,5 % Cu > 1, -- < 2,2 %
  4. Verwendung des Verfahrens nach einem der Ansprüche 1 bis 3 zur Herstellung eines Bauteils in der Öl- und Gasindustrie.
  5. Verwendung nach Anspruch 4, wobei die Bauteile in den Produktionsformen Blech, Band, Rohr (längsnahtgeschweißt und nahtlos), Stangen oder als Schmiedeteil vorliegen.
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