EP3942084A1 - Alliage de nickel à bonne résistance à la corrosion et à résistance élevée à la traction et procédé de fabrication de demi-produits - Google Patents

Alliage de nickel à bonne résistance à la corrosion et à résistance élevée à la traction et procédé de fabrication de demi-produits

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Publication number
EP3942084A1
EP3942084A1 EP20717083.8A EP20717083A EP3942084A1 EP 3942084 A1 EP3942084 A1 EP 3942084A1 EP 20717083 A EP20717083 A EP 20717083A EP 3942084 A1 EP3942084 A1 EP 3942084A1
Authority
EP
European Patent Office
Prior art keywords
alloy
max
gamma
gas
blocks
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP20717083.8A
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German (de)
English (en)
Inventor
Julia BOTINHA
Bodo Gehrmann
Helena Alves
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
VDM Metals International GmbH
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VDM Metals International GmbH
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Filing date
Publication date
Application filed by VDM Metals International GmbH filed Critical VDM Metals International GmbH
Publication of EP3942084A1 publication Critical patent/EP3942084A1/fr
Pending legal-status Critical Current

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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
    • C22C19/055—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
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16—Remelting metals
    • C22B9/18—Electroslag remelting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16—Remelting metals
    • C22B9/20—Arc remelting
    • 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
    • C22C1/023—Alloys based on nickel
    • 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
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0433—Nickel- or cobalt-based alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/10—Formation of a green body
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0844—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid in controlled atmosphere
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/10—Inert gases
    • B22F2201/11—Argon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/15—Nickel or cobalt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Definitions

  • the invention relates to a nickel alloy with excellent resistance to hydrogen embrittlement and very good mechanical properties.
  • Age-hardenable nickel alloys have long been used in the oil and gas industry when higher strengths are required. For this area of application, good corrosion resistance, especially in H2S and oil-containing atmospheres, combined with good mechanical properties is required. Yield strength, notch impact values and strength are also important criteria for the choice of material. Examples according to the prior art are listed in Table 1.
  • the material Alloy 718 which has the following general chemical composition (in% by weight): 18.5% chromium, ⁇ 0.1% carbon, 18% iron, 0.9% titanium, 0.6% aluminum, 3% Molybdenum, 5% niobium + tantalum, the remainder Ni and melting-related
  • the alloy Alloy 718 is the material that was selected for those applications where the highest mechanical strength values are required.
  • the application temperature is not higher than approx. 200 ° C.
  • the material has good corrosion properties against hydrogen embrittlement and stress corrosion cracking and a high mechanical strength. Due to the representativeness of the use of the material Alloy 718, this alloy is regarded as the basis for further or new developments.
  • alloy Alloy 718 is a malleable and age-hardenable nickel-chromium alloy, developed by H. Eiseistein and patented in 1962 with the patent number US 3,046,108. Alloy 718 has a good combination of high strength properties and good ductility over a large area Temperature range. The material was developed for the aerospace industry and introduced a few years later in the oil & gas industry because of the combination of good corrosion resistance and good mechanical properties.
  • No. 3,160,500 discloses a matrix-reinforced nickel-chromium alloy, which later led to the development of the alloy Alloy 625, with a combination of good mechanical properties over a wide temperature range and high resistance to breakage and stress at elevated temperature. Because of its attractive combination of strength and corrosion resistance, this material has found wide application.
  • the high levels of chromium and molybdenum ensure good corrosion resistance and strength, while iron and niobium provide additional strength.
  • the aluminum and titanium additives are mainly used for metallurgical purposes and are kept low to improve weldability.
  • the alloy has the following composition: 21, 44 - 21, 68% Cr, 0.02 - 0.03% C, 0.11 - 0.12% Mn, 0.04 - 0.11% Si, 8.83 - 9.1% Mo, up to 5.32% W, 4.19-4.35% Nb, 0.16-0.23% Al, 0.13-0.20% Ti, 1.92-6.89 % Fe, up to 0.02% Mg, remainder Ni.
  • an electrode is generated by VIM
  • the electrode is subjected to a heat treatment in a temperature range between 400 and 1250 ° C for a period of 10 to 336 hours in an oven to reduce stresses and excessive aging, the electrode in air or in the oven, depending on the dimensions, in particular the diameter, to a temperature between room temperature and it is cooled below 1250 ° C, especially below 900 ° C,
  • the cooled electrode is then remelted by VAR at a remelting rate of 3.0 to 10 kg / minute to form a VAR block
  • the VAR block is heat-treated in a furnace in a temperature range between 400 and 1250 ° C. for a period of 10 to 336 hours the VAR block is cooled in air or in an oven, depending on the dimensions, in particular the diameter, to a temperature between room temperature and less than 1250 ° C, in particular less than 900 ° C,
  • VAR block is remelted again at a remelting rate of 3.0 to 10 kg / minute
  • the remelted VAR block is subjected to a heat treatment in the temperature range between 400 and 1250 ° C for a period of 10 to 336 hours,
  • the Ni-based alloy can have the following composition:
  • Alloy 625 Plus was developed based on Alloy 625 and Alloy 718. Alloy 625 Plus is a high strength alloy as an alternative to Alloy 625, with similar corrosion resistance achieved by increasing the titanium content.
  • Alloy 925 The applications for the age-hardenable alloy Alloy 925 are very similar to those for Alloy 718. They include oil well rods and tubes, gas well components, valves, collars, connector components, and packers. Alloy 925 is used when the strength requirements are slightly less than those of Alloy 718.
  • Nicorros Alloy K-500 (N05500) is a nickel-copper alloy that can be hardened through the formation of a gamma'-phase. It is used in the offshore industry, which is not heavily polluted with hydrogen sulfide. The corrosion resistance in acid gas media and the mechanical strength are lower than those of alloys such as Alloy 718 and Alloy 925.
  • Alloy 725 offers the same high strength as Alloy 718 and has a similar corrosion resistance as Alloy 625.
  • the proportion and the presence of the curing phases have a clear and direct influence on the resistance to hydrogen embrittlement.
  • materials which do not have precipitation phases and therefore cannot be hardened show a significantly better resistance to hydrogen embrittlement compared with hardenable materials which contain precipitation phases.
  • the invention is based on the object of developing an alloy based on Alloy 718 which, with improved acid gas corrosion and hydrogen embrittlement resistance, can also achieve a higher yield point and high strength, with a lower proportion of delta and gamma phase and more Proportion of gamma 'phase is preferred.
  • the invention is also based on the object of providing a method for producing an alloy based on Alloy 718, by means of which a higher yield point and high strength can be achieved, with a small proportion of delta and gamma phase and larger proportions of gamma 'Phase are given.
  • the first task is solved by a nickel alloy with (in -% by weight)
  • Nb, Ta, Al and Ti are the concentration of the respective elements in% by weight.
  • the further object is achieved on the one hand by a method for producing a powder from a nickel-based alloy by
  • the liquid melt is held for homogenization for 5 min to 2 hours,
  • a closed atomization system with a supplied gas is set to a dew point of -10 ° C to 120 ° C,
  • the melt is blown through a nozzle into a gas stream with a gas flow rate of 2 qm 3 / min to 150 qm 3 ,
  • the solidified powder particles are collected in a gas-tight container, wherein
  • the particles have a particle size of 5 pm to 250 pm
  • the particles of the powder are spherical
  • the powder has gas inclusions of 0.0 to 4% pore area (pores> 1 pm) in relation to the total area of evaluated objects,
  • the powder has a bulk density of 2 to the density of the alloy of approx. 8 g / cm 3 ,
  • the powder is packed airtight with argon under the protective gas atmosphere.
  • Nb, Ta, Al and Ti are the concentration of the respective elements in wt .-% by melting the alloy in a vacuum induction furnace (VIM) and casting it into blocks,
  • VIM blocks are subjected to stress-relief annealing in the temperature range of 500 - 1250 ° C for a period of up to 1 10 h,
  • ESR electroslag remelting process
  • VAR vacuum arc remelting process
  • the remelted blocks are homogenized annealed in the temperature range from 500 ° C to 1250 ° C for a period of up to 150 h,
  • the annealed blocks are hot and / or cold formed into semi-finished products, if necessary, at least one intermediate annealing in the temperature range from 900 ° C to 1150 ° C for a period of 0.1 to 60 h is carried out, followed by cooling in air, in a moving annealing atmosphere, inert gas, in water, in polymer or in oil.
  • the object is also achieved by a method for producing a nickel alloy with (in% by weight)
  • Nb, Ta, Al and Ti are the concentration of the elements concerned in wt .-% by openly melting the alloy, followed by treatment in a VOD or AOD plant and cast into blocks, these blocks are subjected to stress-relief annealing in the temperature range of 500 - 1250 ° C for a period of up to 110 h, if necessary,
  • the remelted blocks are homogenized annealed in the temperature range from 500 ° C to 1250 ° C for a period of up to 150 h,
  • the annealed blocks are hot and cold formed into semi-finished products
  • VIM (ESU or VAR) / possibly (ESU or VAR)
  • the alloy according to the invention can preferably be used in the product forms rod,
  • the semi-finished products / components are preferably used in the oil and gas industry and the chemical process industry.
  • the presence of each precipitated phase was analyzed and investigations were carried out in order to better understand the interaction of the hydrogen atom with the crystal structure when different positions in the unit cell are occupied by a hydrogen atom.
  • the preferred sites for trapping hydrogen in the phase boundaries or in the matrix material have been calculated, taking into account the enthalpy energy of the hydrogen when this site is occupied. Based on these results, numerical tensile tests were carried out in order to examine the bonding relationships between the metallic atoms in the vicinity of the phase boundaries.
  • the presence of a hydrogen atom in the most stable position in the gamma / gamma phase boundary has no influence on the tensile strength in comparison to a system without hydrogen atoms (FIG. 1).
  • the hydrogen atom occupies the most stable position of the gamma / gamma “phase boundary” greater atomic rearrangement occurs and the system shows a lower tensile strength compared to a system without hydrogen (Figure 2), which suggests that hydrogen embrittlement can occur.
  • Delta phase - it is not present in representative amounts in the alloy Alloy 718 for oil & gas applications - has no representative influence with regard to the mechanical effect (Figure 3).
  • Alloy 718 is available in three different variants with different requirements on the yield strength.
  • the 120K variant has a minimum yield strength of 120 ksi, which is achieved by curing at temperatures between 774 and 802 ° C.
  • the 140K variant has a minimum yield strength of 140 ksi, which is achieved by curing at temperatures between 760 and 802 ° C.
  • the 150K is the variant that is produced by a two-stage hardening at a first temperature of 700 to 750 ° C and then at a second temperature of 600 to 659 ° C and has a minimum required yield strength of 150 ksi.
  • the various heat treatment processes are able to produce a different microstructure (FIG. 4), which was investigated for comparison with the behavior against hydrogen embrittlement.
  • Gamma 'phase is excreted in the form of dot-shaped particles, while Gamma' phase shows a needle shape.
  • the resistance to hydrogen embrittlement was tested by slow stress tests under cathodic polarization according to NACE publication 3948 from 2014. Samples were tested under an inert environment (deionized water, purged with nitrogen at 40 ° C) and under an aggressive environment (0.5 M sulfuric acid solution at 40 ° C with an applied current density of 5 mA / cm 2 to obtain cathodic polarization) and determines the ratio of elongation at break between aggressive and inert environments. A higher ratio of elongation at break could be responsible for the fact that the resistance to hydrogen embrittlement is also higher.
  • the particle size of the gamma 'and gamma' precipitations can also play a role in the mechanical and corrosion properties of nickel alloys.
  • Typical conditions for the occurrence of hydrogen embrittlement are material contacts with atomic or molecular hydrogen in combination with material stresses.
  • Iron is effective in reducing metal costs, but cannot be excessively alloyed because of the deterioration in material properties.
  • Chromium is used to increase room temperature strength while ensuring general corrosion resistance. In combination with the carbon, chromium forms carbides which increase the high temperature strength.
  • the pitting corrosion resistance in media containing chloride increases with increasing molybdenum content.
  • the resistance to stress corrosion cracking at higher temperatures is also improved.
  • molybdenum can be replaced by tungsten.
  • the austenitic matrix from the gamma phase is hardened by the intermetallic precipitations Gamma ', an ordered fcc phase made of Nh (Al / Ti), and Gamma “- tetragonal NhNb phase - and therefore aluminum, titanium and niobium are added. If necessary, niobium can be substituted by tantalum. Niobium is preferred because of metal costs. Increasing the amounts of Al and Ti should lead to more gamma 'and reducing the amount of Nb should reduce the formation of gamma'.
  • Delta phase is the equilibrium phase of the precipitation hardening gamma phase (NhNb) and, according to the specifiable specification, may only be present in the structure in very small quantities, as it has a negative effect on the mechanical and corrosion properties.
  • the formation of the delta phase is avoided by using solution annealing temperatures above the delta solvus temperature.
  • the nickel alloy according to the invention has, with sufficiently high titanium, aluminum, molybdenum and niobium contents, combined with a defined heat treatment, excellent resistance to hydrogen embrittlement, but at the same time
  • the nickel content is between 50 and 55%, whereby preferred ranges can be set as follows:
  • the alloy contains cobalt with a maximum content of 3%.
  • Preferred contents can be given as follows:
  • the spread range for the element chromium is between 17 and 21%, whereby preferred ranges can be set as follows:
  • the molybdenum content is between> 0 and 9%, whereby, depending on the area of application of the alloy, preferred molybdenum contents can be set as follows:
  • the element molybdenum can, if necessary, be at least partially replaced by tungsten, provided that tungsten is not present as an independent element within the stated limits.
  • Combinations of Mo + W are also possible - depending on the application.
  • tungsten can be adjusted in contents from 0 to 9%.
  • W can be set in the alloy within the spread range as follows: > 0 - 9%
  • niobium is between 1 and 5.7%, whereby, depending on the area of application, preferred contents of the elements can be set within the following spread ranges:
  • the titanium content is between> 0 and 3.0%.
  • Ti can preferably be set in the alloy within the spread range as follows:
  • the element manganese is given in the alloy as follows:
  • the element silicon is given in the alloy as follows:
  • Copper is contained in the alloy with the following content:
  • C can be set in the alloy within the spread range as follows:
  • the alloy also contains phosphorus in contents between 0.001 and 0.02%. Preferred further contents can be given as follows:
  • the boron content is between 0.001 and 0.01%, although the following spread ranges are also conceivable:
  • Nb and Ta are the concentration of the elements concerned in% by weight.
  • Preferred areas can be set with
  • Al and Ti are the concentration of the elements in question in% by mass.
  • Preferred areas can be set:
  • Al and Ti are the concentration of the elements in question in% by weight.
  • the alloy according to the invention is preferably melted and cast in a vacuum induction furnace (VIM), followed by treatment in an electroslag remelting process (ESR) or in a vacuum arc remelting process (VAR). Possibly. the alloy is remelted again in a treatment in an electro-slag remelting process (ESR) or in a vacuum arc remelting process (VAR).
  • VIP vacuum induction furnace
  • the alloy according to the invention may be openly melted, followed by a treatment in a Vacuum Oxygen Decarburization (VOD) or Argon Oxygen Decarburization (AOD), followed by two vacuum arc remelting processes (VAR).
  • VOD Vacuum Oxygen Decarburization
  • AOD Argon Oxygen Decarburization
  • VAR vacuum arc remelting processes
  • the manufactured blocks of the alloy are heat-treated at temperatures between 500 ° C and 1250 ° C, annealing for up to 150 h, then hot and cold formed into the desired semi-finished products such as billets, rods, wires, sheets, strips and foils, if necessary with Intermediate annealing between 800 ° C and 1270 ° C for 0.05 h to 100 h.
  • the surface of the material can be removed chemically and / or mechanically (eg by peeling, turning, grinding) in between and / or at the end for cleaning.
  • solution heat treatment takes place in the temperature range from 970 ° C. to 1150 ° C. for 0.1 min to 60 h, if necessary under protective gas, such as e.g. B.
  • argon or hydrogen followed by cooling in air, possibly in the agitated annealing atmosphere, in inert gas, in water, in polymer or in oil instead.
  • This is followed by a hardening annealing in the temperature range from 600 ° C to 900 ° C for 0.1 h to 60 h, if necessary in a second stage with a further hardening annealing from 550 ° C to 900 ° C for 0.1 h to 60 h h instead of.
  • the hardening annealing is in the temperature range from 600 ° C to 900 ° C for 0.1 h to 60 h, whereby preferred ranges can be set as follows:
  • the hardening annealing takes place in a 2-stage hardening process, with a further hardening annealing from 550 ° C to 900 ° C for 0.1 h to 60 h, whereby preferred ranges can be set as follows:
  • Stage curing in the temperature range from 600 ° C to 800 ° C for 0.1 h to 60 h and 2nd stage curing in the temperature range from 550 ° C to 750 ° C for 0.1 h to 60 h
  • Stage curing in the temperature range from 600 ° C to 800 ° C for 0.1 h to 60 h and 2nd stage curing in the temperature range from 800 ° C to 900 ° C for 0.1 h to 60 h
  • the alloy according to the invention can easily be formed and used in the product forms rod, wire, strip, sheet metal, longitudinally welded tube and seamless tube.
  • the alloy can be produced and used in powder form (e.g. for additive manufacturing processes).
  • the powder is produced in a VIGA (Vacuum Induction Gas Atomiser) powder atomization system or with other methods and selected or filtered with regard to the desired range of powder particle sizes.
  • VIGA Vauum Induction Gas Atomiser
  • the alloy according to the invention should preferably be used in areas in which media containing hydrogen are provided, such as.
  • the alloy according to the invention should preferably have a proportion of gamma '/ gamma' higher than 1.3, preferably higher than 1.5. With this combination, too, the yield strength higher than 120 ksi can be achieved.
  • the phases occurring in equilibrium were calculated for different alloy variants with the JMatPro program from Thermotech.
  • the database for nickel alloys from Thermotech was used as the database for the calculations.
  • the "Heat Treatment" mode of the JMatPro software the proportions of the phases, particle size and the expected mechanical properties (e.g. yield point, tensile strength, hardness) were calculated when the material with the corresponding chemical composition is annealed at different curing temperatures. Description of properties:
  • the alloy according to the invention should also have the following properties:
  • Chemical compositions LV1, 8, 9 and 39 are examples of alloys not according to the invention.
  • the alloy can optionally be produced in the product form powder. Since the formability of an alloy does not play a role in additive manufacturing processes, there is an extended chemical composition window with regard to the aluminum content. For additive manufacturing processes, the powder can have a higher aluminum content of up to 4%. Possible chemical compositions for powder alloy are shown in Table 6.
  • Peak temperature for alloy variations (part 2).
  • Table 5.3 Chemical compositions, mechanical properties and proportions of the precipitation phases in the peak temperature for alloy variations (part 3).
  • an increase in the niobium content from approx. 3.5 to 5% can double the gamma phase content if the titanium and aluminum contents are kept constant. If the aluminum and niobium (tantalum) contents are kept constant and the titanium content is increased, more gamma phase is formed, and an improvement in the mechanical properties is expected. With an increase in aluminum, more gamma phase can be precipitated, in combination with the same or lower Ti and Nb contents (compared to Alloy 718).
  • FIGS. 5 and 6 contain phase diagrams showing the precipitation of the gamma phase below 919 ° C. and of the gamma phase below 880 ° C. for the chemical composition LB250643 (with high titanium and aluminum contents combined with low niobium - (tantalum) content).
  • phase diagram from FIG. 5 shows mathematically the formation of precipitation phases below 919 ° C. and only takes into account the thermodynamic stability. This is why no gamma "phase is taken into account in the phase diagram.
  • the delta phase is the thermodynamically most stable elimination phase, but it will form slowly due to the elimination kinetics. According to the thermodynamic calculations, the eta phase content is not essentially available for this composition.
  • the TTT (Time Temperature Transformation) diagram for the chemical composition LB250643 is shown in FIG.
  • the presence of the gamma phase is now taken into account.
  • delta and eta phases are precipitated after a longer annealing time at the hardening temperature and therefore the precipitations of these phases are influenced by the annealing time of the hardening.
  • the general behavior of the phase boundaries gamma / delta can still be critical because of the low atomic binding energy. Therefore, the annealing time of the hardening should be limited to a maximum of 60 hours in order to avoid the formation of the delta phase.
  • FIG. 8 shows the isothermal diagram for this chemical composition during curing at 650 ° C., where the maximum phase fraction of gamma 'is reached from approx. 7 hours. If the temperature is increased to 730 ° C, the time when the maximum gamma 'phase fraction is reached becomes shorter.
  • FIG. 9 shows the isothermal diagram of this chemical composition during curing at 730 ° C.
  • Table 8 Results of slow stress tests according to the publication NACE 3948 in 4 of the chemical analyzes (LB 250646: reference, LB 250647: without Nb, LB 250650: without AI, and LB 250642: with low Nb content)
  • Iron reduces the cost and should then be used. Therefore 12% is the lower limit for iron. But iron cannot be introduced excessively due to the deterioration in the properties of the material. Therefore, 24% is to be regarded as the upper limit. Iron can be substituted by cobalt if necessary.
  • a minimum content of 17% chromium increases the room temperature resistance and at the same time guarantees general corrosion resistance.
  • chromium carbides are formed which can increase the high temperature strength. Too high a chromium content worsens the phase stability of the alloy and promotes the formation of harmful phases, which has a negative impact on ductility and toughness and therefore a chromium content of 21% forms the upper limit.
  • Tungsten can be used as a substituting element for molybdenum and is then also limited to> 0 to 9%.
  • a combination of molybdenum + tungsten is also conceivable, with a W content of at least 0.01% being assumed.
  • the formation of the intermetallic hardening precipitation phase Gamma 'increases as the amount of Al + Ti increases. Therefore a minimum content of 0.4% aluminum is required. However, if the content of aluminum is too large, it aggregates and coarsens the gamma 'phase at the grain boundaries, thereby drastically deteriorating the mechanical properties and deteriorating the hot workability.
  • the Al content can be set higher for a powder alloy for additive manufacturing processes, since the associated processes do not require hot forming. Aluminum is therefore limited to 4.0%.
  • Titanium combines with aluminum and nickel to form the gamma 'phase and makes a contribution to the precipitation resistance of the alloy. Even so, if titanium is excessively incorporated, the eta phase can form, thereby impairing mechanical properties. Therefore titanium can be added up to 3.0%.
  • Niobium (or tantalum) stabilizes the gamma phase and helps increase strength. A minimum content of 1% is therefore necessary. But niobium (or tantalum) is also responsible for the formation of the gamma “phase, which is detrimental to hydrogen embrittlement resistance and must therefore be controlled. For this reason, niobium (or tantalum) is limited from 1% to 5.7%.
  • Boron and phosphorus have the effect of suppressing excessive accumulation of hydrogen at the phase and grain boundaries. This can reduce the sensitivity of hydrogen embrittlement. Even so, if boron and phosphorus are used excessively, the grain boundary segregations become too strong, and the effect of reducing hydrogen embrittlement is lost.
  • the formability can also be restricted and therefore boron becomes from 0.001% to a maximum of 0.01% and phosphorus is limited from 0.001% to a maximum of 0.02%.
  • Cobalt can substitute for nickel and improves the properties at elevated temperatures.
  • the alloy can contain up to 3% cobalt.
  • Carbon is limited to a maximum of 0.045%, as this element reduces the workability at this level due to the excessive formation of carbides.
  • the remainder of the alloy is nickel (50-55%) and it should be taken into account that the remainder contains small amounts of impurities that do not significantly change the properties of the alloy. Thus, impurities such as tailings can be present in a total amount of 0.01%. Manganese and silicon are limited to a maximum of 0.35%.
  • Precipitation phases form below 970 ° C for the possible limits of the chemical compositions and therefore the alloy is solution annealed between 0.1 min and 60 h to bring all phases into solution, depending on the dimensions of the product shapes.
  • the solution annealing temperature is limited to max. 1 150 ° C limited to limit grain growth.
  • rapid cooling in the agitated annealing atmosphere in inert gas, water, polymer or in oil is suggested.
  • a hardening annealing is then carried out in order to form the precipitation phases and to achieve good mechanical properties.
  • the material is annealed in the temperature range from 600 ° C to 900 ° C for 0.1 to 60 hours. Longer curing times lead to delta and eta phase precipitations and should be avoided.
  • curing can be carried out in a second stage in the temperature range from 550 ° C. to 900 ° C. for 0.1 h to 60 h.
  • the curing temperatures are selected depending on the application. Curing processes that optimize the mechanical properties are used for applications where higher mechanical properties are required. Curing processes that optimize the ratio of the phase proportions gamma '/ gamma' are used for applications where higher resistance to hydrogen embrittlement is required.
  • Two-stage cures can lead to different structures, with different mechanical properties, depending on the selected first-stage and second-stage temperatures.
  • the hardening leads to the higher mechanical properties, although the ratio of the phase proportions gamma '/ gamma' is lower according to the calculations.
  • a 2-stage curing with the first temperature above the peak temperature leads to medium mechanical properties.
  • the proportions of the phase proportions gamma '/ gamma' are lower in this case, so this leads to a lower resistance to hydrogen embrittlement.
  • the mechanical properties are less than the properties that can be achieved via a single-stage cure.
  • the ratio of the phase fractions gamma '/ gamma' can however be higher and therefore this heat treatment would be used for applications where the higher requirements of hydrogen embrittlement resistance are the main objective.
  • higher mechanical properties can be achieved if the first-stage temperature is below the peak temperature and the second-stage temperature is higher than the first temperature.
  • the ratio of the phase components Gamma '/ Gamma' remains at the same level.
  • the curing time must also be observed. For low-temperature curing, longer curing times are required in order to remove all precipitations, while short curing times are sufficient for higher-temperature curing.
  • the elongation at break in the acid gas test (NACE publication 3948) is above 75%, but preferably above 90%, with yield strengths in air> 100 KSI preferably 120 KSI.
  • Figure 4 SEM images of material corresponding to the 120K, 140K and

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Abstract

L'invention concerne un alliage de nickel comportant (en pourcentage en poids) 50 à 55% de Ni, 17 à 21% de Cr, >0 à 9% de Mo, 9% de W 0, 1 à 5,7% de Nb, >0 à 4,7% de Ta, 0,1 à 3,0% de Ti, 0,4 à 4,0% de AI, maximum 3,0% de Co, maximum 0,35% de Mn, maximum 0,35% de Si, maximum 0,23% de Cu, 0,001 à 0,045% de C, maximum 0,01% de S, 0,001 à 0,02% de P, 0,001 à 0,01% de B, le reste étant du Fe et les impuretés habituelles inhérentes au procédé, les relations suivantes s'appliquant, Nb + Ta 1 - 5,7% (1), AI + Ti >1,2- 5% (2), Mo + W 3 - 9% (3), où Nb, Ta, AI et Ti représentent la concentration des éléments concernés, en pourcentage en poids.
EP20717083.8A 2019-03-18 2020-03-17 Alliage de nickel à bonne résistance à la corrosion et à résistance élevée à la traction et procédé de fabrication de demi-produits Pending EP3942084A1 (fr)

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DE102019106776 2019-03-18
DE102020106433.0A DE102020106433A1 (de) 2019-03-18 2020-03-10 Nickel-Legierung mit guter Korrosionsbeständigkeit und hoher Zugfestigkeit sowie Verfahren zur Herstellung von Halbzeugen
PCT/DE2020/100210 WO2020187368A1 (fr) 2019-03-18 2020-03-17 Alliage de nickel à bonne résistance à la corrosion et à résistance élevée à la traction et procédé de fabrication de demi-produits

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TW202328465A (zh) * 2021-10-25 2023-07-16 日商山陽特殊製鋼股份有限公司 適用於積層造形之鎳系合金粉末及使用該粉末得到之積層造形體
CN114318061A (zh) * 2021-11-17 2022-04-12 华能核能技术研究院有限公司 一种用于高温或超高温气冷堆蒸汽发生器的合金及其制备方法
CN114540731B (zh) * 2022-02-23 2022-09-20 北京钢研高纳科技股份有限公司 一种gh4169合金棒材及其制备方法和紧固件
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CN113646458A (zh) 2021-11-12
JP2022526758A (ja) 2022-05-26
DE102020106433A1 (de) 2020-09-24
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BR112021012882A2 (pt) 2021-10-05
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