EP3899063B1 - Matériau superausténitique - Google Patents

Matériau superausténitique Download PDF

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EP3899063B1
EP3899063B1 EP19829563.6A EP19829563A EP3899063B1 EP 3899063 B1 EP3899063 B1 EP 3899063B1 EP 19829563 A EP19829563 A EP 19829563A EP 3899063 B1 EP3899063 B1 EP 3899063B1
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superaustenitic
material according
detection limit
nitrogen
weight
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EP3899063A1 (fr
EP3899063C0 (fr
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Rainer FLUCH
Andreas KEPLINGER
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Voestalpine Boehler Edelstahl GmbH and Co KG
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Voestalpine Boehler Edelstahl GmbH and Co KG
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    • 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
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    • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
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Definitions

  • the invention relates to a super-austenitic material and a method for its production.
  • Such materials are z. B. used in chemical plant construction or in oil field or gas field technology.
  • a requirement for such materials is that they withstand corrosive attack, in particular attack in media with high chloride concentrations.
  • Such materials are, for example, from the CN 107876562A , the CN 104195446A or DE 43 42 188 known.
  • WO 02/02837 A1 is a corrosion-resistant material for use in media with a high chloride concentration in oil field technology. This is a chromium-nickel-molybdenum superaustenite that has a comparatively low nitrogen content but very high chromium and very high nickel contents.
  • the JP 2005 179733 A discloses a super austenitic material.
  • chromium-nickel-molybdenum steels usually have improved corrosion behavior compared to the previously mentioned chromium-manganese-nitrogen steels.
  • chromium manganese nitrogen steels are a more economical alloy composition that nonetheless offers an excellent combination of strength, toughness and corrosion resistance.
  • the chromium-nickel-molybdenum steels mentioned achieve significantly higher corrosion resistance than chromium manganese nitrogen steels, but are associated with significantly higher costs due to the very high nickel content.
  • PREN 16 % Cr + 3.3 x % Mo + 16 x % N.
  • MARC % Cr + 3.3 x % Mo + 20 x % N + 20 x % C - 0.25 x % Ni - 0.5 x % Mn.
  • Comparable steel grades are also known for use as shipbuilding steels for submarines, these being chromium-nickel manganese nitrogen steels which are also alloyed with niobium to stabilize the carbon, but this degrades the impact strength. These steels are generally low in manganese and therefore have relatively good corrosion resistance, but do not achieve the strength of drill collar grades.
  • the object of the invention is to create a super-austenitic, high-strength and tough material that can be produced in a comparatively simple and cost-effective manner.
  • the material is to be used, in particular in the measuring device industry and especially in the watchmaking industry, in particular as a housing for highly sensitive measuring devices and for screw support axle drives, pumps, flexible pipes, wire guides, chemical apparatus construction and seawater treatment plants. It should have a completely austenitic structure even after an optional cold forming after strain hardening the yield point should be R p0.2 >1000 MPa.
  • the alloy according to the invention has the following composition: elements preferred more preferred carbon (C) 0.01 - 0.20 0.01 - 0.1 Silicon (Si) ⁇ 0.5 ⁇ 0.5 Manganese (Mn) 4.0 - 7.0 5.0 - 6.0 Phosphorus (P) ⁇ 0.05 ⁇ 0.05 Sulfur (S) ⁇ 0.005 ⁇ 0.005 iron (Fe) rest rest Chromium (Cr) 24.0 - 28.0 26.0 - 28.0 Molybdenum (Mo) 2.5 - 3.5 2.5 - 3.5 Nickel (Ni) 12.0 - 15.5 13.0 - 15.0 vanadium (V) ⁇ 0.3 Below detection limit Tungsten (W) ⁇ 0.1 Below detection limit copper (Cu) ⁇ 0.15 Below detection limit cobalt (Co) ⁇ 0.5 Below detection limit Titanium (Ti) ⁇ 0.05 Below detection limit Aluminum (Al) ⁇ 0.1 ⁇ 0.1 niobium (Nb) ⁇ 0.025 Below detection limit boron
  • the steel according to the invention should be free of precipitation, since precipitation has a negative impact on toughness and corrosion resistance.
  • the yield point is R p0.2 >450 MPa and can easily reach values >500 MPa, with the impact work at 20°C being greater than 350 J and values of up to 440 J being reached.
  • the yield point is definitely R p0.2 >1000 MPa and values of up to 1100 MPa are achieved in practice, with strain hardened the impact work at 20°C being certainly greater than 80J, with values of 200 J being achieved in practice .
  • the notch impact work was determined according to DIN EN ISO 148-1.
  • values for the product of tensile strength Rm with notched impact strength KV of more than 100,000 MPa J, preferably >200,000 MPa J, particularly preferably >300,000 MPa J, can be achieved.
  • Carbon is contained in contents from 0.01 up to 0.25%. Carbon is an austenite former and has a favorable effect in terms of high mechanical parameters. With a view to avoiding carbidic precipitations, the carbon content should be set to between 0.01 and 0.20% by weight, in particular between 0.01 and 0.10% by weight.
  • silicon are ⁇ 0.5% by weight and are mainly used for deoxidizing the steel.
  • the specified upper limit reliably avoids the formation of intermetallic phases. Since silicon is also a ferrite former, the upper limit is also selected with a safety range in this regard. In particular, silicon can be provided in contents of 0.1-0.3% by weight.
  • Manganese is contained in amounts of 3.0 - 8.0% by weight. This is an extremely low value compared to materials according to the prior art. Up to now it has been assumed that manganese contents of more than 19% by weight, if possible more than 20% by weight, are necessary for high nitrogen solubility. Surprisingly, it has been found with the present alloy that even with the low manganese contents according to the invention, a nitrogen solubility is achieved which is above what is possible according to the prevailing expert opinion. In addition, it was previously assumed that good corrosion resistance goes hand in hand with very high manganese contents, but it has been found according to the invention that this is apparently not necessary due to unexplained synergistic effects in the present alloy.
  • the lower limit for manganese can be chosen at 3.5 or 4.0 or 4.5 or 5.0%.
  • the upper limit for manganese can be chosen at 6.0 or 6.5 or 7.0 or 7.5%.
  • Chromium levels of 17% by weight or more are found to be necessary for higher corrosion resistance. According to the invention, at least 24.0% and at most 30% chromium are included. Up to now it was assumed that contents higher than 24% by weight have an adverse effect on the magnetic permeability, because chromium is one of the ferrite-stabilizing elements. On the other hand, it was found with the alloy according to the invention that even very high chromium contents above 23% do not negatively affect the magnetic permeability in the present alloy, but the resistance to pitting and stress corrosion cracking is known to be optimally influenced.
  • the lower limit for chromium can be chosen at 25 or 26%.
  • the upper limit for chromium can be chosen at 28 or 29%.
  • Molybdenum is an element which contributes significantly to corrosion resistance in general and pitting corrosion resistance in particular, the effect of molybdenum being enhanced by nickel. According to the invention, 2.0 to 4% by weight of molybdenum are added. The lower limit for molybdenum can be chosen at 2.1 or 2.2 or 2.3 or 2.4 or 2.5%. The upper limit for molybdenum can be chosen at 3.5 or 3.6 or 3.7 or 3.8 or 3.9%. Higher molybdenum contents make an ESR treatment absolutely necessary in order to rule out segregation. Remelting processes are very complex and expensive. Therefore, according to the invention, DESU or ESU routes should be avoided.
  • tungsten is present in amounts below 0.5% and contributes to the increase in corrosion resistance.
  • the upper limit for tungsten can be chosen at 0.4 or 0.3 or 0.2 or 0.1% or below the detection limit (i.e. without any deliberate addition).
  • nickel is present in contents of 10 to 16%, as a result of which a high resistance to stress corrosion cracking is achieved in media containing chloride.
  • the lower limit for nickel can be chosen at 11 or 12 or 13%.
  • the upper limit for nickel can be chosen at 15 or 15.5%.
  • the alloying of copper is described as advantageous for the resistance in sulfuric acid, it is found according to the invention that copper at values >0.5% increases the tendency to precipitate chromium nitrides, which has a negative effect on the corrosion properties.
  • the upper limit value for copper was set at ⁇ 0.5%, preferably below 0.15%, most preferably below the detection limit.
  • Cobalt can be provided in amounts of up to 5% by weight, in particular to replace nickel.
  • the upper limit for cobalt can be chosen at 5 or 3 or 1 or 0.5 or 0.4 or 0.3 or 0.2 or 0.1% or below the detection limit (i.e. without any intentional addition).
  • Nitrogen is included at levels of 0.50 to 0.90% by weight to ensure high strength. Furthermore, nitrogen contributes to corrosion resistance and is a strong austenite former, which is why higher contents than 0.50% by weight, in particular higher than 0.52% by weight, are favorable. In order to avoid nitrogen-containing precipitates, in particular chromium nitride, the upper limit of nitrogen is limited to 0.90% by weight. It has been shown that despite the very low manganese content, in contrast to known alloys, these high nitrogen contents can be achieved in the alloy . Due to the good nitrogen solubility on the one hand and the disadvantages that are obtained with higher nitrogen contents, in particular over 0.90%, any pressure increase is even out of the question as part of a DESU route.
  • the ratio of nitrogen to carbon is greater than 15.
  • the lower limit for nitrogen can be chosen at 0.52 or 0.54 or 0.60 or 0.65%.
  • the upper limit for nitrogen can be selected at 0.80 or 0.85%.
  • boron, aluminum and sulfur can be included as further alloy components, but only optionally.
  • the alloy components vanadium and titanium are not necessarily contained in the present steel alloy. Although these elements contribute positively to the solubility of nitrogen, the high nitrogen solubility of the present invention can be provided even in their absence.
  • the alloy according to the invention should not contain niobium, since it can form precipitates which reduce toughness. Historically, niobium has only been used to bind carbon, which is not necessary in the alloy of the present invention. The niobium content is still tolerable up to 0.1%, but should not exceed the content of unavoidable impurities.
  • the components are melted under atmospheric conditions and then further treated with secondary metallurgy. Blocks are then cast, which are immediately hot-formed.
  • ESR Electroslag remelting
  • DESU pressure electroslag remelting
  • MARC opt 40 ⁇ wt%Cr + 3.3 x wt%Mo + 20 x wt%C + 20 x wt%N - 0.5 x wt%Mn
  • MARC formula is optimized by finding that the otherwise usual deduction of nickel does not apply to the system according to the invention and the limit value of 40 is necessary.
  • FIG 2 the possible process routes for the production of the alloy composition according to the invention are shown as examples.
  • a possible one is now used as an example Route described.
  • VID vacuum induction melting unit
  • melted material is simultaneously melted and treated for secondary metallurgy.
  • the melt is then poured into molds (ingot) and solidifies there into blocks.
  • molds ingot
  • These are then hot-formed in several steps. For example, pre-forged on the rotary forging machine and brought to final dimensions in the multi-line rolling mill.
  • a heat treatment step can also be carried out.
  • the cold forming step can be carried out by means of wire drawing.
  • a super-austenitic material according to the invention can not only have the described (and in particular in figure 2 illustrated) production routes are produced, the advantageous properties of the alloy according to the invention can also be achieved by a powder-metallurgical production route.
  • figure 4 are the three alloys made figure 3 produced by a method according to the invention and subjected to strain hardening.
  • R p0.2 was around 1000 MPa for all three materials and the tensile strength Rm was between 1100 MPa and 1250 MPa.
  • the impact energy was excellent at 270 J to even over 300 J (alloy C - 329.5 J).
  • the advantage of the invention is that an austenitic, high-strength material with increased corrosion resistance and a low nickel content is created, which at the same time shows high strength and paramagnetic behavior.
  • a completely austenitic structure is also present after cold forming, so that it has been possible to combine the positive properties of a cost-effective CrMnNi steel with the outstanding technical properties of a CrNiMo steel.
  • a special feature of the invention is that, due to the high nitrogen content, the work hardening rate is higher than with other super austenites in order to be able to achieve tensile strengths (R m ) of 2500 MPa.
  • R m tensile strengths
  • Typical areas of application for the materials according to the invention are shipbuilding and here in particular submarine construction, chemical apparatus construction, seawater treatment plants, the paper industry, screws and bolts, flexible pipes, so-called wirelines, completion tools, springs, valves, umbilicals, axle drives, pumps. Depending on the area of application, there may be minor alloy adjustments which figure 5 are shown.
  • the strength can be further increased by cold forming, as already described.

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Claims (24)

  1. Matériau superausténitique constitué d'un alliage comprenant les éléments d'alliage suivants, toutes les proportions étant exprimées en % en poids ainsi que les impuretés inévitables :
    Éléments Carbone (C) 0,01 - 0,25 Silicium (Si) < 0,5 Manganèse (Mn) 3,0 - 8,0 Phosphore (P) < 0,05 Soufre (S) < 0,005 Fer (Fe) le reste étant Chrome (Cr) 24,0 - 30,0 Molybdène (Mo) 2,0 - 4,0 Nickel (Ni) 12,0 - 16,0 Vanadium (V) < 0,5 Tungstène (W) < 0,5 Cuivre (Cu) < 0,5 Cobalt (Co) < 5,0 Titane (Ti) < 0,1 Aluminium (Al) < 0,2 Niobium (Nb) < 0,1 Bore (B) < 0,01 Azote (N) 0,50 - 0,90.
  2. Matériau superausténitique selon la revendication 1, caractérisé en ce que l'alliage est constitué des éléments suivants ainsi que d'impuretés inévitables, toutes les proportions étant exprimées en % en poids :
    Éléments Carbone (C) 0,01 - 0,20 Silicium (Si) < 0,5 Manganèse (Mn) 4,0 - 7,0 Phosphore (P) < 0,05 Soufre (S) < 0,005 Fer (Fe) le reste étant Chrome (Cr) 24,0 - 28,0 Molybdène (Mo) 2,5 - 3,5 Nickel (Ni) 12,0 - 15,5 Vanadium (V) < 0,3 Tungstène (W) < 0,1 Cuivre (Cu) < 0,15 Cobalt (Co) < 0,5 Titane (Ti) < 0,05 Aluminium (Al) < 0,1 Niobium (Nb) < 0,025 Bore (B) < 0,005 Azote (N) 0,52 - 0,80
  3. Matériau superausténitique selon la revendication 1 ou 2, caractérisé en ce que l'alliage est constitué des éléments suivants ainsi que d'impuretés inévitables, toutes les proportions étant exprimées en % en poids :
    Éléments Carbone (C) 0,01 - 0,1 Silicium (Si) < 0,5 Manganèse (Mn) 5,0 - 6,0 Phosphore (P) < 0,05 Soufre (S) < 0,005 Fer (Fe) le reste étant Chrome (Cr) 26,0 - 28,0 Molybdène (Mo) 2,5 - 3,5 Nickel (Ni) 13,0 - 15,0 Vanadium (V) Inférieur à la limite de détection Tungstène (W) Inférieur à la limite de détection Cuivre (Cu) Inférieur à la limite de détection Cobalt (Co) Inférieur à la limite de détection Titane (Ti) Inférieur à la limite de détection Aluminium (Al) < 0,1 Niobium (Nb) Inférieur à la limite de détection Bore (B) < 0,005 Azote (N) 0,54 - 0,80.
  4. Matériau superausténitique selon l'une des revendications précédentes,
    caractérisé en ce que
    le matériau est obtenu par traitement métallurgique secondaire de la masse fondue, coulée en lingots, directement suivie d'un formage à chaud, éventuellement d'un formage à froid et éventuellement d'un traitement mécanique ultérieur.
  5. Matériau superausténitique selon l'une des revendications précédentes,
    caractérisé en ce que
    la limite d'élasticité Rp0,2>500 Mpa est de préférence > 750 MPa.
  6. Matériau superausténitique selon l'une des revendications précédentes,
    caractérisé en ce que
    la résilience à température ambiante en orientation longitudinale est de Av > 300 J.
  7. Matériau superausténitique selon l'une des revendications précédentes,
    caractérisé en ce que
    le matériau est entièrement austénitique après le formage à froid, c'est-à-dire qu'il est exempt de martensite de déformation.
  8. Matériau superausténitique selon l'une des revendications précédentes,
    caractérisé en ce que
    le soufre en tant qu'impureté ne dépasse pas 0,005 % en poids.
  9. Matériau superausténitique selon l'une des revendications précédentes,
    caractérisé en ce que
    en ce que le phosphore est présent en tant qu'impureté à raison de 0,05 % en poids au maximum.
  10. Matériau superausténitique selon l'une des revendications précédentes,
    caractérisé en ce que
    le manganèse présente comme valeur limite supérieure 6,0 % ou 6,5 % ou 7,0 % ou 7,5 % ou 7,9 %, et
    comme valeur limite inférieure 3,1 % ou 3,5 % ou 4,0 % ou 4,5 % ou 5,0 %.
  11. Matériau superausténitique selon l'une des revendications précédentes, caractérisé en ce que le chrome présente comme valeur limite supérieure 28 % ou 29 % ou 29,8 % et comme valeur limite inférieure 24,0 % ou 25 % ou 26 %.
  12. Matériau superausténitique selon l'une des revendications précédentes, caractérisé en ce que le molybdène présente comme valeur limite supérieure 3,5 % ou 3,6 % ou 3,7 % ou 3,8 % ou 3,9 % ou 3,95 % et
    comme valeur limite inférieure 2,05 % ou 2,1 % ou 2,2 % ou 2,3 % ou 2,4 % ou 2,5 %.
  13. Matériau superausténitique selon l'une des revendications précédentes, caractérisé en ce que le nickel présente comme valeur limite supérieure 15 % ou 15,5 % ou 15,8 % et comme valeur limite inférieure 12,0 % ou 13 %.
  14. Matériau superausténitique selon l'une des revendications précédentes, caractérisé en ce que l'azote présente comme valeur limite supérieure 0,80 % ou 0,85 % ou 0,88 % et comme valeur limite inférieure 00,51 % ou 0,52 % ou 0,55 %.
  15. Matériau superausténitique selon l'une des revendications précédentes, caractérisé en ce que le cobalt est à < 5 % ou < 1 % ou < 0,5 % ou < 0,4 % ou < 0,3 % ou < 0,2 % ou < 0,1 % ou inférieur à la limite de détection.
  16. Matériau superausténitique selon l'une des revendications précédentes, caractérisé en ce que le cuivre est à < 0,3 % ou < 0,1 % ou inférieur à la limite de détection.
  17. Matériau superausténitique selon l'une des revendications précédentes, caractérisé en ce que le tungstène est à < 0,5 % ou < 0,3 % ou < 0,2 % ou < 0,1 % ou inférieur à la limite de détection.
  18. Procédé de fabrication d'un matériau superausténitique selon l'une des revendications précédentes, caractérisé en ce que l'alliage est constitué des éléments suivants ainsi que d'impuretés inévitables, toutes les proportions étant exprimées en % en poids :
    Éléments Carbone (C) 0,01 - 0,25 Silicium (Si) < 0,5 Manganèse (Mn) 3,0 - 8,0 Phosphore (P) < 0,05 Soufre (S) < 0,005 Fer (Fe) le reste étant Chrome (Cr) 24,0 - 30,0 Molybdène (Mo) 2,0 - 4,0 Nickel (Ni) 12,0 -16,0 Vanadium (V) < 0,5 Tungstène (W) < 0,5 Cuivre (Cu) < 0,5 Cobalt (Co) < 5,0 Titane (Ti) <0,1 Aluminium (Al) < 0,2 Niobium (Nb) < 0,1 Bore (B) < 0,01 Azote (N) 0,50 - 0,90
    est fondu puis soumis à un traitement métallurgique secondaire, l'alliage ainsi obtenu est ensuite coulé en lingots et laissé se solidifier, puis directement chauffé et déformé à chaud, les produits étant notamment soumis à une nouvelle déformation à froid suivie d'un usinage mécanique.
  19. Procédé de fabrication d'un matériau superausténitique selon la revendication 18, caractérisé en ce que l'alliage est constitué des éléments suivants ainsi que d'impuretés inévitables, toutes les proportions étant exprimées en % en poids :
    Éléments Carbone (C) 0,01 - 0,20 Silicium (Si) <0,5 Manganèse (Mn) 4,0 - 7,0 Phosphore(P) < 0,05 Soufre (S) < 0,005 Fer (Fe) le reste étant Chrome (Cr) 24,0 - 28,0 Molybdène (Mo) 2,5 - 3,5 Nickel (Ni) 12,0 - 15,5 Vanadium (V) < 0,3 Tungstène (W) < 0,1 Cuivre (Cu) < 0,1 Cobalt (Co) < 0,5 Titane (Ti) < 0,05 Aluminium (Al) < 0,1 Niobium (Nb) < 0,025 Bore (B) < 0,005 Azote (N) 0,52 - 0,80
  20. Procédé de fabrication d'un matériau superausténitique selon la revendication 18 ou 19, caractérisé en ce que l'alliage est constitué des éléments suivants ainsi que d'impuretés inévitables, toutes les proportions étant exprimées en % en poids :
    Éléments Carbone (C) 0,01 - 0,10 Silicium (Si) < 0,5 Manganèse (Mn) 5,0 - 6,0 Phosphore (P) < 0,05 Soufre (S) < 0,005 Fer (Fe) le reste étant Chrome (Cr) 26,0 - 28,0 Molybdène (Mo) 2,5 - 3,5 Nickel (Ni) 13,0 - 15,0 Vanadium (V) Inférieur à la limite de détection Tungstène (W) Inférieur à la limite de détection Cuivre (Cu) < 0,1 Cobalt (Co) Inférieur à la limite de détection Titane (Ti) Inférieur à la limite de détection Aluminium (Al) < 0,1 Niobium (Nb) Inférieur à la limite de détection Bore (B) < 0,005 Azote (N) 0,54 - 0,80.
  21. Procédé selon l'une des revendications 18 à 20, caractérisé en ce que le formage à chaud s'effectue en plusieurs étapes partielles.
  22. Procédé selon l'une quelconque des revendications 18 à 21, caractérisé en ce qu'entre les étapes partielles de déformation à chaud, le produit est à nouveau chauffé, et après la dernière étape de déformation à chaud, un recuit de mise en solution est effectué si nécessaire.
  23. Procédé selon l'une des revendications 18 à 22, caractérisé en ce qu'après la dernière étape de déformation à chaud ainsi que le recuit de mise en solution optionnel, une étape de déformation à froid est effectuée pour obtenir une résistance à la traction Rm > 2000 MPa en particulier Rm > 2500 MPa notamment du produit de Rm * KV > 100000 MPa J.
  24. Utilisation d'un matériau superausténitique selon l'une des revendications 1 à 17, en particulier fabriqué par un procédé selon l'une des revendications 18 à 23 pour des composants et en particulier des boîtiers d'instruments de mesure et/ou de montres et/ou d'axes porteurs de vis et/ou d'entraînements d'axes et/ou de pompes et/ou de tuyaux flexibles et/ou de câbles mécaniques et/ou pour la construction d'appareils chimiques et/ou d'installations de traitement de l'eau de mer et/ou pour la construction navale et/ou des vis et/ou des boulons et/ou des outils de complétion.
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US20240052469A2 (en) 2024-02-15
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EP3899063C0 (fr) 2023-08-30
PL3899064T3 (pl) 2023-11-20
CN113544295A (zh) 2021-10-22
US20230332282A1 (en) 2023-10-19
EP3899064C0 (fr) 2023-08-30
US20220145436A1 (en) 2022-05-12
EA202191412A1 (ru) 2021-09-28
BR112021011849A2 (pt) 2021-09-08
JP2022522092A (ja) 2022-04-14
WO2020127789A1 (fr) 2020-06-25
JP2022514920A (ja) 2022-02-16

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