US20100000636A1 - Duplex stainless steel - Google Patents

Duplex stainless steel Download PDF

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US20100000636A1
US20100000636A1 US12/305,014 US30501407A US2010000636A1 US 20100000636 A1 US20100000636 A1 US 20100000636A1 US 30501407 A US30501407 A US 30501407A US 2010000636 A1 US2010000636 A1 US 2010000636A1
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steel
hot
rolled
bar
weight
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Bernard Bonnefois
Jerome Peultier
Mickael Serriere
Jean-Michel Hauser
Eric Chauveau
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Ugitech SA
Industeel Creusot
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Ugitech SA
Industeel Creusot
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Assigned to INDUSTEEL CREUSOT, UGITECH reassignment INDUSTEEL CREUSOT ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HAUSER, JEAN-MICHEL, CHAUVEAU, ERIC, BONNEFOIS, BERNARD, PEULTIER, JEROME, SERRIERE, MICKAEL
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    • C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
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Definitions

  • the present invention relates to a duplex stainless steel more particularly intended for the manufacture of structural components for material production installations (chemical, petrochemical, paper and offshore industries) or energy production installations, without in any way being limited thereto, and also to the process for manufacturing plate, strip, bar, rod, wire or sections from this steel.
  • this steel may be used as a substitute for a 304L type stainless steel in many applications, for example in the above industries or in the agri-foodstuff industry, including parts produced from formed rod or wire (welded grids, etc.), sections (strainers, etc.), shafts, etc. It is also possible to produce castings and forgings.
  • stainless steel grades of 304 type and 304L type which, in the annealed state, have an essentially austenitic microstructure. In the cold-worked state they may furthermore contain a variable proportion of martensite.
  • these steels include large additions of nickel, the cost of which is generally prohibitive.
  • these grades may pose problems from a technical standpoint in certain applications, as they have poor tensile properties in the annealed state, especially as regards the yield strength, and a rather low stress corrosion resistance.
  • Austenitic-ferritic stainless steels are also known, which are composed mainly of a mixture of ferrite and austenite, such as the steels 1.4362, 1.4655, 1.4477, 1.4462, 1.4507, 1.4410, 1.4501 and 1.4424 according to the EP10088 standard, which all contain more than 3.5% nickel. These steels are particularly resistant to corrosion and to stress corrosion.
  • Ferritic or ferritic-martensitic stainless steel grades are also known, the microstructure of which, for a defined range of heat treatments, is composed of two constituents—ferrite and martensite—preferably in a 50/50 ratio, such as the 1.4017 grade according to the EN10088 standard. These grades, with a chromium content generally less than 20%, have high tensile mechanical properties but do not have satisfactory corrosion resistance.
  • the object of the present invention is to remedy the drawbacks of the steels and manufacturing processes of the prior art by providing a stainless steel exhibiting good mechanical properties and in particular a tensile yield strength greater than 400 or even 450 MPa in the annealed or solution-treated state, a high corrosion resistance, in particular the same or better than that of 304L, good microstructural stability and good toughness of welded zones, without adding expensive addition elements, and also providing a process for manufacturing plate, strip, bar, rod, wire or sections from this steel which is simpler to implement.
  • the first subject of the invention is a duplex stainless steel, the composition of which consists of, in % by weight:
  • I LCR % Cr+3.3 ⁇ % Mo+16 ⁇ % N+2.6 ⁇ % Ni ⁇ 0.7 ⁇ % Mn.
  • the steel according to the invention may also include the following optional features, taken individually or in combination:
  • the proportion of ferrite is between 35 and 55% by volume
  • the chromium content is between 22 and 24% by weight
  • the manganese content is less than 1.5% by weight
  • the calcium content is less than 0.03% by weight
  • the molybdenum content is greater than 0.1% by weight.
  • a second subject of the invention consists of a process for hot-rolled plate, strip or coil made of steel according to the invention, in which:
  • said ingot or slab is hot-rolled at a temperature between 1150 and 1280° C. in order to obtain plate, strip or coil.
  • said ingot or slab is hot-rolled at a temperature between 1150 and 1280° C. in order to obtain what is called quarto plate; a heat treatment is then carried out at a temperature between 900 and 1100° C.; and said plate is cooled by an air quench.
  • a third subject of the invention consists of a process for manufacturing hot-rolled bar or rod made of steel according to the invention, in which:
  • said ingot or bloom is hot-rolled from a temperature between 1150 and 1280° C. in order to obtain bar, which is air-cooled, or a coil of wire stock which is water-cooled; and then, optionally:
  • a heat treatment is carried out at a temperature between 900 and 1100° C.
  • said bar or a coil of wire stock is quench-cooled.
  • a cold-drawing operation is carried out on said bar or a die-drawing operation is carried out on said rod, after being cooled.
  • the invention also covers a process for manufacturing a steel section, in which a cold-forming operation is carried out on a hot-rolled bar obtained according to the invention, and also a process for manufacturing a steel forging, in which a hot-rolled bar obtained according to the invention is cut up into slugs and then a forging operation is carried out on said slugs between 1100° C. and 1280° C.
  • the invention furthermore covers various products that can be obtained by the processes according to the invention and also their uses, such as:
  • the duplex stainless steel according to the invention comprises the contents defined below.
  • the carbon content of the grade is equal to or less than 0.05%, preferably less than 0.03%, by weight. This is because too high a content of this element degrades the localized corrosion resistance by increasing the risk of chromium carbides precipitating in the heat-affected zones of welds.
  • the chromium content of the grade is between 21 and 25% by weight, preferably between 22 and 24% by weight, so as to obtain good corrosion resistance, which is at least equivalent to that obtained with type 304 or 304L grades.
  • the nickel content of the grade is between 1 and 2.95%, preferably equal to or less than 2.7%, or even 2.5%, by weight.
  • This austenite-forming element is added so as to obtain good crevice corrosion resistance.
  • contents of greater than 1% and preferably greater than 1.2% by weight it has a favourable effect in combating the initiation of pitting corrosions.
  • its content is limited since above 2.95% by weight a degradation in the resistance to pitting propagation is observed.
  • Addition of nickel also makes it possible to obtain a good tough-ness/ductility compromise since it has the benefit of translating the toughness transition curve towards low temperatures, this being particularly advantageous for the manufacture of thick quarto plate, for which the toughness properties are important.
  • the nickel content in the steel according to the invention is limited, it has been found to be necessary, in order to obtain an appropriate austenite content after heat treatment between 900° C. and 1100° C., to add other austenite-forming elements in unusually high amounts and to limit the contents of ferrite-forming elements.
  • the nitrogen content of the grade is between 0.16 and 0.28% by weight, which generally means that the nitrogen is added to the steel during smelting.
  • This austenite-forming element firstly makes it possible to obtain ferrite-austenite two-phase duplex steel containing an appropriate proportion of austenite exhibiting good stress corrosion resistance, and also to obtain metal with high mechanical properties. It also makes it possible to have good microstructural stability in the heat-affected zones of welds. Its maximum content is limited since, above 0.28%, a solubility problem may be observed: formation of blisters during solidification of slabs, blooms, ingots, castings or welds.
  • the content of manganese which is also an austenite-forming element below 1150° C., is kept below 2.0% by weight, and preferably below 1.5% by weight, because of the deleterious effects of this element on many counts.
  • manganese which is also an austenite-forming element below 1150° C.
  • Additions of ferro-manganese normally used to bring the grade to composition also contain appreciable amounts of phosphorus and also selenium, which elements it is not desirable to introduce into the steel and are difficult to remove when refining the grade.
  • Manganese also disturbs this refining, by limiting the possibility of decarburation. It also poses a problem further downstream in the process, as it impairs the corrosion resistance of the grade because of the formation of manganese sulphides (MnS) and of oxidized inclusions.
  • MnS manganese sulphides
  • This element is conventionally added to grades that it is desired to enrich with nitrogen, so as to increase the solubility of that element in the grade. Without a sufficient manganese content, it was therefore not possible to achieve such a nitrogen level in the steel.
  • the inventors have found that it is possible to limit the addition of manganese in the steel according to the invention, while still adding sufficient nitrogen in order to obtain the desired effect on the ferrite-austenite balance of the base metal and to stabilize the heat-affected zones of welds.
  • Molybdenum a ferrite-forming element
  • tungsten is maintained with a content of less than 0.15% by weight.
  • the contents of these two elements are such that the sum Mo+W/2 is less than 0.50% by weight, preferably less than 0.4% by weight and even more preferably less than 0.3% by weight. This is because the present inventors have found that, by maintaining these two elements, and with the sum of their contents below the values indicated, no precipitation of embrittling intermetallics is observed, thereby making it possible in particular to relax the process for manufacturing steel plate or strip by permitting said plate or strip to be air-cooled after heat treatment or hot processing.
  • Copper an austenite-forming element
  • This element improves the corrosion resistance in a reducing acid medium.
  • its content is limited to 0.50% by weight in order to prevent the formation of epsilon-phases, which it is desirable to avoid, since these result in hardening of the ferritic phase and embrittlement of the duplex alloy.
  • the oxygen content is preferably limited to 0.010% by weight, so as to improve its forgeability.
  • Boron is an optional element that may be added to the grade according to the invention in an amount of between 0.0005% and 0.01% by weight, preferably between 0.0005% and 0.005% and even more preferably between 0.0005% and 0.003% by weight, so as to improve its hot conversion.
  • Silicon a ferrite-forming element
  • aluminium is present with a content of less than 1.4% by weight.
  • Aluminium, a ferrite-forming element is present with a content of less than 0.05% by weight and preferably between 0.005% and 0.040% by weight, so as to obtain low-melting-point calcium aluminate inclusions.
  • the maximum aluminium content is also limited, so as to avoid excessive formation of aluminium nitrides.
  • Cobalt an austenite-forming element
  • Cobalt is maintained with a content of less than 0.5% by weight, preferably less than 0.3% by weight.
  • This element is a residual element provided by the raw materials. In particular, it is limited because of handling problems that it may pose after irradiation of components in nuclear power plants.
  • Rare earth metals may be added to the composition in an amount of 0.1% by weight, preferably less than 0.06% by weight. Mention may in particular be made of cerium and lanthanum. The contents of these two elements are limited, as they are liable to form undesirable intermetallics.
  • Vanadium a ferrite-forming element
  • Vanadium may be added to the grade in an amount of 0.5% by weight and preferably less than 0.2%, so as to improve the crevice corrosion resistance of the steel.
  • Niobium a ferrite-forming element
  • Niobium may be added to the grade in an amount of 0.3% by weight and preferably less than 0.050% by weight. It helps to improve the tensile strength of the grade, thanks to the formation of fine niobium nitrides. Its content is limited, so as to limit the formation of coarse niobium nitrides.
  • Titanium a ferrite-forming element
  • Titanium may be added to the grade in an amount of 0.1% by weight and preferably less than 0.02% by weight, in order to limit the formation of titanium nitrides formed in particular in the liquid steel.
  • the grade according to the invention it is also possible to add calcium to the grade according to the invention, in order to obtain a calcium content of less than 0.03% by weight and preferably greater than 0.0002% or even greater than 0.0005% by weight, so as to control the nature of the oxide inclusions and improve machinability.
  • the content of this element is limited, as it is liable to form, with sulphur, calcium sulphides which degrade the corrosion resistance properties.
  • the calcium content is limited to less than 0.0005%, preferably less than 0.0002%, by weight.
  • Sulphur is maintained with a content of less than 0.010% by weight and preferably with a content of less than 0.003% by weight.
  • this element forms sulphides with manganese or calcium, the presence of sulphides being deleterious to the corrosion resistance. Sulphur is considered as an impurity.
  • An addition of magnesium in an amount with a final content of 0.1% may be made so as to modify the nature of the sulphides and the oxides.
  • Selenium is preferably maintained at less than 0.005% by weight because of its deleterious effect on the corrosion resistance. This element is in general introduced into the grade as impurities of ferrite and manganese ingots.
  • Phosphorus is maintained with a content of less than 0.040% by weight, and is considered as an impurity.
  • the balance of the composition consists of iron and impurities.
  • these impurities may also be zirconium, tin, arsenic, lead or bismuth.
  • Tin may be present with a content of less than 0.100% by weight and preferably less than 0.030% by weight in order to prevent welding problems.
  • Arsenic may be present with a content of less than 0.030% by weight and preferably less than 0.020% by weight.
  • Lead may be present with a content of less than 0.002% by weight and preferably less than 0.0010% by weight.
  • Bismuth may be present with a content of less than 0.0002% by weight and preferably less than 0.00005% by weight.
  • Zirconium may be present in an amount of 0.02%.
  • the present inventors have found that, when the percentages by weight of chromium, molybdenum, nitrogen, nickel and manganese satisfy the relationship below, the grades in question exhibit good localized corrosion resistance, that is to say resistance to the formation of pits or crevices:
  • I LCR % Cr+3.3 ⁇ % Mo+16 ⁇ % N+2.6 ⁇ % Ni ⁇ 0.7 ⁇ % Mn ⁇ 30.5.
  • the microstructure of the steel according to the invention in the annealed state, is composed of austenite and ferrite, which phases are preferably, after treatment for 1 h at 1000° C., present with a ferrite proportion of 35 to 65% by volume and more particularly preferably 35 to 55% by volume.
  • I F 6 ⁇ (% Cr+1.32 ⁇ % Mo+1.27 ⁇ % Si) ⁇ 10 ⁇ (% Ni+24 ⁇ % C+16.15 ⁇ % N+0.5 ⁇ % Cu+0.4 ⁇ % Mn) ⁇ 6.17.
  • the ferrite index I F must be between 40 and 70.
  • the microstructure does not contain other phases that would be deleterious to its mechanical properties, especially such as the sigma-phase and other intermetallic phases.
  • part of the austenite may have been converted to martensite, depending on the actual temperature of deformation and the amount of cold deformation applied.
  • the steel according to the invention may be smelted and manufactured in the form of hot-rolled plate, again called quarto plate, but also in the form of hot-rolled strip, from slabs or ingots, and also in the form of cold-rolled strip from hot-rolled strip. It may also be hot-rolled in the form of bar or rod stock or sections or forgings. These products may then be hot-converted by forging or cold-converted into bar or drawn sections or die-drawn wire.
  • the steel according to the invention may also be processed by casting, whether followed by heat treatment or not.
  • This ingot, slab or bloom is generally obtained by melting the raw materials in an electric furnace followed by vacuum remelting of the AOD or VOD type with decarburization.
  • the grade can then be cast in the form of ingots, or in the form of slabs or blooms by continuous casting in a bottomless mould. It is also conceivable to cast the grade directly in the form of thin slabs, in particular by continuous casting between counter-rotating rolls.
  • this may optionally be reheated so as to reach a temperature between 1150 and 1280° C., but it is also possible to work directly on the slab immediately on being continuously cast, while still hot.
  • the slab or ingot is then hot-rolled in order to obtain a quarto plate generally having a thickness between 5 and 100 mm.
  • the reduction ratios generally employed at this stage vary between 3 and 30%.
  • This plate then undergoes a heat treatment to put the precipitates, formed at this stage, back into solution by reheating to a temperature between 900 and 1100° C., and is then cooled.
  • the process according to the invention provides for air-quench cooling, which is easier to implement than the conventionally used cooling for this type of grade, which is more rapid cooling, using water. However, it remains possible to carry out a water-cooling operation, if so desired.
  • This slow air cooling is particular made possible thanks to the limited nickel and molybdenum content of the composition according to the invention, which is not subject to the precipitation of intermetallic phases detrimental to its usage properties.
  • This cooling may in particular be carried out at a rate ranging from 0.1 to 2.7° C./s.
  • the quarto plate After being hot-rolled, the quarto plate may be leveled, cut and pickled if it is desired to deliver it in this state.
  • rod with a diameter of 13 mm or less When rod with a diameter of 13 mm or less is manufactured, it may be cooled by a water quench in the form of turns spread out on a conveyor after said turns have passed along a conveyor for 2 to 5 minutes through a solution treatment furnace at a temperature between 850° C. and 1100° C.
  • a subsequent furnace heat treatment between 900° C. and 1100° C. may optionally be carried out on this bar or coil, already treated after the hot-rolling, if it is desired to complete the recrystallization of the structure and slightly reduce the tensile properties.
  • the bar may undergo a cold-drawing operation or the rod may undergo a die-drawing operation, after being cooled.
  • the hot-rolled bar may also be cold-formed or parts may be manufactured after the bar has been cut up into slugs and then forged.
  • FIGS. 1 to 5 show:
  • FIG. 1 A correlation between % ferrite after treatment at 1100° C. and I F for as-processed products
  • FIG. 2 A relative diametral change ⁇ as a function of the deformation temperature
  • FIG. 3 Pitting potentials E1 and E2, determined on forged bars, as a function of the index I LCR ;
  • FIG. 4 The uniform corrosion rate V, determined on forged bars, as a function of the index I LCR ;
  • FIG. 5 Critical temperatures T CC and T CP , determined on forged bars, as a function of the index I LCR .
  • An industrial heat according to the invention of 150 tonnes referenced 8768 was produced. This grade was smelted by melting in an electric furnace then vacuum-refined with decarburization in order to achieve the intended carbon level. It was then continuously cast into slabs measuring 220 ⁇ 1700 mm in cross section before being hot-rolled, after reheating to 1200° C., into quarto plates with thicknesses of 7, 12 and 20 mm. The plates thus obtained then underwent a heat treatment at around 1000° so as to put the various precipitates present at this stage back into solution. After the heat treatment, the plates were water-cooled, then leveled, cut and pickled.
  • compositions in percentages by weight of the various grades smelted on a laboratory scale or an industrial scale are given in Table 1, together with the compositions of the various industrial products or semi-finished products smelted in an electric furnace, followed by AOD refining and cast into ingots or continuously cast, these being mentioned for comparison.
  • Specimens ranging from 1 to 8 cm 3 in volume were cut from these laboratory heats in the as-cast state or from industrial products in the as-cast state, and heat treatments for 30 minutes at various temperatures were carried out on these specimens, in a salt bath, followed by an end-of-treatment water quench, in order to determine the proportion of ferrite at high temperature. Since ferrite is magnetic, unlike austenite, carbides and nitrides possibly present, an assaying method was used in which the saturation magnetization was measured. The ferrite contents thus determined are given in Table 2 and plotted in FIG. 1 .
  • FIG. 1 shows that there is a good correlation between the index I F and the ferrite contents measured on the base metal after treatments at 1100° C.
  • heat 14441 according to the invention has, below 1300° C., a ferrite content appropriate to hot transformation to a duplex structure. Furthermore, after heat treatment in the 950° C. to 1100° C. range, it has a ferrite content appropriate for stress corrosion resistance.
  • the ferrite content was also measured by the grid method (according to ASTM E 562 standard) on forged bars after heat treatment at 1030° C. and in heat-affected zones of weld beads deposited by a coated electrode with a constant energy resulting in cooling rates at 700° C. of 20° C./s.
  • the results (ferrite contents of the base metal and of the heat-affected zone) are given in Table 3. This shows that heats 14441 and 14604 according to the invention have a ferrite content in the base metal and in the heat-affected zone that is favourable to localized corrosion resistance and to stress corrosion resistance, and also favourable to toughness (cf. Table 5),
  • Ingot 14439 exhibited blisters and was unusable. To avoid this phenomenon during casting in air at atmospheric pressure, it proved necessary to limit the nitrogen content of the heats according to the invention to less than 0.28% by weight.
  • the hot-deformability was evaluated using hot tensile tests carried out on test specimens, the calibrated part of which, having a diameter of 8 mm and a length of 5 mm, was heated by Joule heating for 80 seconds at 1280° C. and then cooled at 2° C. per second down to the test temperature, which varied between 900 and 1280° C. When this temperature was reached, the rapid tensile test was immediately started, at the rate of 73 mm/s; after fracture, the necking diameter at the break was measured.
  • heat 14441 according to the invention has a hot-deformability comparable to that of comparative reference heat 14382.
  • the tensile properties R e0.2 and R m were determined according to the NFEN 10002-1 standard.
  • the toughness K V was determined at various temperatures according to the NF EN 10045 standard.
  • the toughness values determined at 20° C. for the laboratory heats 14441 and 14604 and for the industrial heat 8768, all three according to the invention, are all greater than 200 J, this being satisfactory taking into account the yield strength level of these grades.
  • the toughness values at 20° C. are below 100 J. This confirms the need for a sufficient addition of nitrogen in order to obtain a satisfactory toughness level.
  • Corrosion resistance tests were carried out both on the forged bars from laboratory heats and on coupons removed from hot-rolled plates coming from the industrial heats.
  • the critical pitting temperature in a ferric chloride medium (6% FeCl 3 ) was also determined according to the ASTM G48-00 standard, method C.
  • the arrangement favouring floating crevice corrosion was in accordance with the recommendations given in the ASTM G78-99 standard.
  • the critical crevice temperature is the minimum temperature for which crevices with a depth of greater than 25 ⁇ m are observed.
  • I LCR localized corrosion resistance index
  • Heats 14383 and 14660 not according to the invention having I LCR indices equal to 28.7 and 29.8, exhibit an inferior corrosion behaviour than a steel of AISI 304L type.
  • Heats 14604 and 14441 according to the invention having an I LCR of 30.9 and 33, behave at least as well as 304L type steel.
  • the steels according to the invention must preferably have an I LCR of greater than 30.5 and preferably greater than 32.
  • Uniform corrosion was characterized by evaluating the corrosion rate by loss of weight after 72 hours' immersion in a 2% dilute sulphuric acid solution heated to 40° C.
  • the steel specimens were polished under water using SiC paper up to 1200 and then aged for 24 hours in air.
  • the cyclic polarization test in a chloride medium was carried out by starting with measurement of the floating potential for 15 min, followed by cyclic dynamic polarization at 100 mV/min starting from the floating potential up to the potential for which the current reached an intensity of 300 ⁇ A/cm 2 , followed by return to the potential for which the current is zero.

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TWI463020B (zh) 2014-12-01
RU2009101139A (ru) 2010-07-27
WO2007144516A2 (fr) 2007-12-21
ES2401601T3 (es) 2013-04-23
EP2038445A2 (fr) 2009-03-25
BRPI0713673A2 (pt) 2012-10-23
CA2656946A1 (fr) 2007-12-21
US20150167135A1 (en) 2015-06-18
KR20090031864A (ko) 2009-03-30
TW200815613A (en) 2008-04-01
KR101169627B1 (ko) 2012-07-30
RU2406780C2 (ru) 2010-12-20
DK2038445T3 (da) 2013-04-08
ZA200810587B (en) 2009-11-25
EP2038445B1 (fr) 2012-12-26
SI2038445T1 (sl) 2013-06-28
PL2038445T3 (pl) 2013-09-30
AU2007259069B2 (en) 2011-04-28
CN101501234B (zh) 2012-01-04
BRPI0713673B1 (pt) 2014-11-25
AU2007259069A1 (en) 2007-12-21
US20190226068A1 (en) 2019-07-25
CA2656946C (fr) 2012-01-24
WO2007144516A3 (fr) 2008-04-10

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