Classifications

• • C—CHEMISTRY; METALLURGY
  • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
  • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
  • C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
  • C25F1/02—Pickling; Descaling
  • C25F1/04—Pickling; Descaling in solution
  • C25F1/06—Iron or steel
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
  • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
• • C—CHEMISTRY; METALLURGY
  • C21—METALLURGY OF IRON
  • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
  • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
  • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
• • C—CHEMISTRY; METALLURGY
  • C21—METALLURGY OF IRON
  • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
  • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
  • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
  • C21D8/0205—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips of ferrous alloys
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
  • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
  • C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
  • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
  • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
  • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
  • C22C38/46—Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
  • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
  • C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum

Definitions

• the present invention relates to an austenitic stainless steel strip, having an elastic limit Rp 0.2 greater than or equal to 600 MPa, an upper tensile load Rm greater than or equal to 800 MPa, an elongation A 80 greater than or equal to 40%, and a glossy surface appearance, of annealing-gloss type.
• the invention also relates to a continuous manufacturing process for this austenitic stainless steel strip.
• austenitic stainless steels are used in a wide range of end applications such as for example the manufacture of mechanical parts, cooking utensils, and tubes.
• the strip of austenitic stainless steel is subjected to a heat treatment and a final etching which, according to the conditions of implementation, gives it either a surface appearance having a high gloss, interesting by example for platerie, an aspect of matte surface interesting for the manufacture of building facades.
• gloss means a surface having a gloss greater than 50
• a “matte surface appearance” means a surface having a gloss of less than 20.
• the gloss corresponds to measuring the reflectivity of the surface and is measured at an angle of 60 °.
• the austenitic stainless steel strip is cold-rolled beforehand with rolls which impart a glossy surface appearance to the strip.
• the cold rolled strip is then degreased and rinsed, and then undergoes a heat treatment in a vertical furnace called "bright annealing" in which there is a reducing atmosphere.
• the strip travels in the oven consisting of an enclosure completely isolated from the outside atmosphere, comprising three zones in which a neutral or reducing gas circulates.
• This gas is chosen for example, from hydrogen, nitrogen or a mixture of hydrogen and nitrogen (HNX gas), and has a dew point of between -60 and -45 ° C.
• the strip is first heated in the first zone of the oven at a temperature of between 1050 and 1150 ° C, and at a heating rate of 30 to 60 ° C / sec. Then, it is maintained at this temperature in the second zone of the oven for a time sufficient to allow the recrystallization of the steel and the restoration of the mechanical properties. Finally, it is cooled in the third zone of the oven to a temperature of the order of 150 ° C to prevent re-oxidation of the surface of the strip with the oxygen of the air, when the band leaves the oven enclosure.
• the glossy surface appearance imparted to the strip during cold rolling is maintained, because the oxide film which formed during the annealing is very thin, of a thickness of the order of 10 angstrom.
• Another means of manufacturing an austenitic stainless steel strip having a glossy surface appearance is to subject the strip to a final treatment of the annealing-pickling type, which gives it an annealed-stripped surface appearance; to say a matte surface appearance, then to proceed to an operation of either polishing the surface of the strip, or skin-pass of the strip.
• the procedure is as follows.
• the previously cold-rolled strip undergoes continuous annealing at a temperature of the order of 1100 ° C, for about 1 min, in an oven where the thermal energy is generated by combustion of hydrocarbons which regulates the air supply to the burner so as to obtain an oxidizing atmosphere.
• a reducing atmosphere that is to say an atmosphere containing an excess of hydrocarbons, to avoid degradation of the corrosion resistance of the strip by re-carburation of steel by hydrocarbons.
• the annealed strip then undergoes air cooling and / or forced cooling by spraying water outside the oven.
• the pickling is generally carried out in several pickling tanks containing acid solutions capable of removing this oxide layer, such as a mixture of nitric acid and hydrofluoric acid.
• the strip is subjected to either a skin-pass operation or a polishing operation until the desired glossy surface appearance is obtained.
• the skin-pass is made with so-called mirror-polishing cylinders, ie cylinders having an arithmetic average roughness Ra of between 0.05 and 0.08 ⁇ m which give the steel strip a surface appearance. gloss.
• the austenitic stainless steel strips obtained according to these two processes have insufficient mechanical characteristics, since their elastic limit Rp 0.2 is between 250 and 350 MPa, and their load at break Rm is between 600 and 700 MPa, for an elongation A 80 of between 50 and 60%.
• the operation of skin-pass or polishing is an additional step.
• the polishing operation is a long and delicate operation.
• the present invention therefore aims to avoid the disadvantages of the processes of the prior art, and to provide a method for conferring on an austenitic stainless steel strip treated in a hydrocarbon combustion furnace, an appearance of glossy surface, an elastic limit Rp 0.2 of 600 MPa and a tensile strength Rm of 800 MPa associated with elongation A 80 greater than or equal to 40%.
• the strip of steel according to the invention also advantageously has a surface whose arithmetic average roughness is less than or equal to 0.08 ⁇ m, which gives the strip a smooth surface and therefore an even brighter surface appearance.
• the invention also relates to a continuous manufacturing process for this austenitic stainless steel strip.
• the remainder of the composition is iron and other elements usually expected to be found as impurities resulting from the processing of stainless steel, in proportions that do not affect the properties sought.
• the slab After being cast, the slab is hot rolled in a strip train to form a hot rolled strip which is annealed and optionally etched.
• the hot-rolled strip then undergoes various treatments, so as to obtain a strip having both excellent mechanical characteristics and a glossy surface appearance, without having recourse to either annealing in a bright annealing furnace, or a final polishing of the surface of the strip or a final skin-pass operation.
• the installation used to manufacture the strip according to the invention comprises a cold rolling device of strips, consisting of a band train comprising working rolls between which scrolls the austenitic stainless steel strip of composition according to the invention.
• the working rolls have an arithmetic mean roughness Ra of less than or equal to 0.15 ⁇ m, and preferably less than or equal to 0.10 ⁇ m.
• the diameter of the working rolls of the belt gear is between 50 and 100 mm, to minimize the rolling forces for the high reduction rates, that is to say from 75% reduction.
• the band train not only reduces the thickness of the band, but also to help crush the asperities from the previously hot rolled strip.
• the installation comprises a hydrocarbon combustion furnace comprising an open enclosure through which the band passes, and means for introducing a gas mixture of hydrocarbon and air.
• the open enclosure comprises, in the running direction of the band shown, two successive zones, a first heating zone and a second temperature maintenance.
• the first heating zone is equipped with powerful heating means (not shown) capable of rapidly heating the strip at a heating rate V1, up to a holding temperature T1.
• the strip is maintained at this temperature T1 in the second zone, during a holding time M, and then cooled at a speed V2 in a cooling zone located just after the exit of the oven.
• the installation comprises a pickling device which comprises at least one acid-resistant pickling tank, and containing a pickling solution.
• the previously hot rolled austenitic steel strip is cold rolled at room temperature, with a reduction ratio of between 55 and 85%.
• a cold-rolled strip having a thickness of between 0.6 and 2 mm is thus obtained.
• deformation martensite ⁇ ' is observed by micrography and its volume fraction can be measured by X-ray diffraction or magnetic induction measurement (ferromagnetic phase).
• a recrystallization annealing should be carried out making it possible to obtain austenite grains whose average size does not exceed 4 ⁇ m.
• the elastic limit Rp 0.2 is inversely proportional to the square root of the grain size.
• a fine-grained structure ie a structure in which the average size of the austenite grains does not exceed 4 ⁇ m, is significantly resistant, as will be seen later, to the phenomenon of matting (loss brightness) during cold forming operations, for example by stamping.
• the reduction ratio is between 70 and 85%, so as to obtain a band having a smooth surface topography, ie an arithmetic average roughness Ra of between 0.07 and 0.12 ⁇ m, free micro-defects of shot blasting craters and / or etched grain boundaries.
• This also makes it possible to store sufficient plastic deformation energy to promote faster recrystallization at low temperatures.
• the inventors have demonstrated that when the strip is cold rolled with a sufficiently high reduction ratio, and with work rollers having an arithmetic mean roughness Ra less than or equal to 0.15 ⁇ m, then is subject to partial recrystallization annealing at a temperature of the order of 800 ° C, in a hydrocarbon combustor, to form an oxide layer sufficiently thin to be readily removed by acid stripping, without the grain boundaries are attacked, then the strip has both excellent mechanical characteristics and a glossy, gloss-like surface finish.
• the average arithmetic roughness Ra transferred to the strip by the working rolls during the operation of Cold rolling is very little degraded. So, to get a band with a shine greater than 50, it is essential that the working rolls have an arithmetic average roughness of less than or equal to 0.15 ⁇ m, and preferably less than 0.10 ⁇ m.
• the brightness measured in the context of the present invention corresponds to the measurement of the reflectivity of the surface and is measured at an angle of 60 °.
• the cold-rolled strip is then passed through the open chamber of the hydrocarbon combustion furnace, inside which there is an oxidizing atmosphere with respect to the iron, in order for it to undergo a heat treatment. consisting of a partial recrystallization annealing of the steel, followed by forced cooling.
• the atmosphere in the furnace is composed of a gaseous mixture of air and at least one hydrocarbon in an air / hydrocarbon volume ratio of between 1.1 and 1.5, the gas mixture comprising in addition 3 to 8 % by volume of oxygen.
• the furnace atmosphere is preferably a gaseous mixture of air and hydrocarbon in an air / hydrocarbon volume ratio of between 1.1 and 1.5, the gaseous mixture further comprising 3 to 8% by volume of oxygen.
• the at least one hydrocarbon is chosen from natural gas, butane and methane. Natural gas is preferentially chosen because of its low cost and ease of transportation.
• the atmosphere in the annealing furnace is too oxidizing and the formed oxide layer is so thick that to eliminate it, aggressive pickling solutions will have to be used. that will attack the grain boundaries. The surface appearance of the strip will then be dull.
• the air / hydrocarbon volume ratio is less than 1.1, the atmosphere in the annealing furnace is too reducing. Therefore, the re-carburization of the steel by the hydrocarbons can not be avoided, and the corrosion resistance of the steel will be degraded.
• the heat treatment is adjusted so as to obtain a steel strip whose recrystallized volume fraction is between 60 and 75%. Indeed, if the non-recrystallized volume fraction (measured by micrographic observation and image analysis) is greater than 40%, the microstructure of the steel induces mechanical properties that are too high, and the elongation A 80 of the strip is less than at 40%. On the other hand, if the non-recrystallized volume fraction is less than 25%, the mechanical characteristics such as the elastic limit Rp 0.2 , will be insufficient.
• the partial recrystallization annealing is carried out at a speed V1 of between 10 and 80 ° C./s, a temperature T of between 800 and 950 ° C. and a holding time M of between 10 and 100 seconds, advantageously between 60 and 80 seconds.
• the annealing of the strip at a temperature T between 800 and 950 ° C makes it possible to limit the diffusion of chromium at the grain boundaries, and consequently limits the attack of the grain boundaries during the subsequent chemical stripping of the strip, which promotes obtaining a glossy surface appearance.
• the steel When the temperature T is less than 800 ° C., the steel does not recrystallize sufficiently to obtain the desired mechanical properties. Indeed, the steel has an elastic limit Rp 0.2 greater than 600 MPa but an elongation A 80 less than 40% mediocre, which greatly limits its cold deformation capabilities.
• the stainless steel can only recrystallize during a very long maintenance time M which is not compatible with the industrial requirements.
• the austenite grains increase in favor of martensite, and the elastic limit Rp 0.2 is insufficient to give the stainless steel good mechanical properties.
• the recrystallized volume fraction of the strip will be less than 60%, and the elongation A 80 of the strip is insufficient.
• the austenitic grains grow in favor of martensite, and the mechanical characteristics, such as the elastic limit Rp 0.2 , become insufficient.
• the partially recrystallized steel strip then undergoes forced cooling at a speed V 2 of between 10 and 80 ° C / s, for example by blowing air or by blowing air under pressure and spraying water.
• V 2 a speed of between 10 and 80 ° C / s
• the yield point Rp 0.2 and the breaking load Rm increase.
• the strip When the strip is cooled, it is stripped with an acid pickling solution capable of completely removing said oxide layer depending on its thickness and nature, without attacking the grain boundaries of the steel.
• the strip undergoes a first electrolytic pickling in a bath containing sodium sulphate whose concentration is between 150 and 200 g / l, with a pH of less than 3, and with an amperage of between 5 and 12 kA.
• austenitic stainless steel strips according to the invention have comparable weldability to standard annealed austenitic stainless steel or standard annealed-pickled stainless steel strips.
• an austenitic stainless steel strip according to the invention will be compared with, on the one hand, a austenitic stainless steel strip of the standard annealed-pickled type (2D standard), and on the other hand a standard annealing-austenitic stainless steel strip (standard 2RB).
• Table 1 chemical composition of the stainless steel according to the invention, expressed in% by weight, the balance being iron and unavoidable impurities.
• AS33 steel is cast to form a slab that is hot rolled to a thickness of 4.5 mm. This slab is then cold-rolled with working rolls having an arithmetic average roughness Ra of 0.1 ⁇ m, with a reduction ratio of 82% so as to obtain in a passage a strip of 0.8 mm thickness.
• This cold-rolled strip is subjected to a partial recrystallization annealing of the steel in a combustion furnace, heating it with a heating rate of 50 ° C / sec, up to a holding temperature of 820 ° C and during a hold time of 50 seconds.
• the atmosphere in the furnace is a mixture of air and natural gas comprising an oxygen level of 4% by volume.
• the volume ratio of air to natural gas is 1.3.
• the web is then cooled at a cooling rate of 70 ° C / sec to room temperature.
• the strip undergoes a first electrolytic pickling in a bath containing sodium sulphate whose concentration is 175 g / l, pH 2, with an amperage of 9 kA, and for a duration of 15 s, then a second etching electrochemical in a bath containing nitric acid whose concentration is 100 g / l, pH 2, with an amperage of 9 kA, and for a period of 15 s.
• the band obtained undergoes no further treatment, nor polishing of the surface, nor skin pass.
• AS33 steel is cast to form a slab that is hot rolled to a thickness of 4.5 mm. This slab is then laminated to cold with a reduction rate of 82% so as to obtain in one pass a 0.8 mm thick strip.
• This cold-rolled strip is subjected to a complete recrystallization annealing of the steel, in a combustion furnace, at a temperature of 1120 ° C. for a period of 50 seconds.
• the atmosphere in the furnace is a mixture of air and natural gas comprising an oxygen level of 4% by volume.
• the volume ratio of air to natural gas is 1.3.
• the web is then cooled at a cooling rate of 80 ° C / sec to room temperature.
• the strip is stripped to completely remove the 0.2 ⁇ m thick formed oxide layer in sodium sulfate and sulfuric acid baths.
• the band obtained undergoes no further treatment, nor polishing of the surface, nor skin pass.
• AS33 steel is cast to form a slab that is hot rolled to a thickness of 4.5 mm. This slab is then cold rolled with working rolls which give a glossy surface appearance to the strip, with a reduction rate of 82% so as to obtain in one pass a 0.8 mm thick strip.
• This cold-rolled strip is subjected to a complete recrystallization annealing of the steel, in a bright-annealing furnace inside which an atmosphere consisting of a gaseous mixture comprising 10% by volume of nitrogen and 90% prevails. in volume of hydrogen and having a dew point of -50 ° C, heating it with a heating rate of 50 ° C / sec, up to a holding temperature of 1100 ° C.
• the strip is cooled at a cooling rate of 60 ° C / s to room temperature.
• the band obtained undergoes no further treatment, nor polishing of the surface, nor skin pass.
• Table 2 shows the mechanical and appearance characteristics of these three types of tape.
• Elastic limit Rp 0.2 (MPa) 312 308 596 Breaking Load
• Rm MPa 656 677 796 Lengthening
• A80 % 59 59 42
• Grain size ⁇ m 12 to 25 15 to 20 1 to 4
• Appearance characteristics 2D standard tape 2RB standard tape Strip according to the invention Brightness (60 °, long direction) 21 55 50 Avg. Roughness arithm., Ra ( ⁇ m) 0.12 0.12 0.07 Surface hardness (HV 5 ) 169 172 286
• the strip according to the invention has, compared to standard 2D and standard 2RB strips, both a glossy surface appearance and good mechanical characteristics. It also has a superficial hardness greater than the two bands of the prior art.
• Blanks are cut in the steel strip according to the invention, in the standard 2RB band and in the standard 2D band. These blanks are then stamped in a stamping press conventionally comprising a punch, a die and a blank holder, to form buckets.
• the brightness of the surface is measured both in the bottom of the bucket and on the skirt of the bucket, which estimates an average value of gloss of the stamped part.
• the loss of gloss is low, and much lower than that observed for the standard 2B and standard 2RB strips.
• the scratch resistance tests are carried out on the steel strip according to the invention, and the standard strip 2RB according to the ISO 1518 standard using a Clemen machine whose hemispherical steel hardened tip has a hardness of 1500 Hv, and a diameter of 1 mm.
• the tests consist of applying, with variable loads of 50 g, 200 g and 400 g, the hemispherical tip to the surface of the strip so as to create a scratch.
• the test results are summarized in Table 4. TABLE 4 Charge (g) Depth of scratch ( ⁇ m) for standard 2RB tape Depth of scratch ( ⁇ m) for the strip according to the invention Relative difference (%) 50 1.08 0.73 32 200 3 1.35 55 400 3.35 2.33 30
• test results show that the steel strip according to the invention is more resistant to scratching than the standard 2RB strips, an order of magnitude of 40% on average, corresponding to the difference in relative surface hardness of the strip.
• the intergranular corrosion resistance test is carried out on samples taken from the steel strip according to the invention and from the standard 2D strip.
• This test is performed according to the NFA 05-159 standard. It involves immersing the sample in a boiling solution of sulfuric acid and copper sulphate for a period of 20 hours. The sample is then bent at 90 ° and the observation of the convex face of the latter, in comparison with a reference sample which has not been immersed in said solution, makes it possible to determine the degree of cracking in the extreme skin.
• a low resistance to intergranular corrosion is characterized by the presence of numerous cracks on the convex face of the folded sample.
• the intergranular corrosion resistance tests show that the austenitic stainless steel strip according to the invention is more resistant to intergranular corrosion than the standard 2D strip.

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• Chemical & Material Sciences (AREA)
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• Chemical Treatment Of Metals (AREA)
• Heat Treatment Of Steel (AREA)
• Metal Rolling (AREA)

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