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EP3445878B1 - Procédé de fabrication d'une pièce en acier inoxydable martensitique à partir d'une tôle - Google Patents

Procédé de fabrication d'une pièce en acier inoxydable martensitique à partir d'une tôle Download PDF

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EP3445878B1
EP3445878B1 EP17713465.7A EP17713465A EP3445878B1 EP 3445878 B1 EP3445878 B1 EP 3445878B1 EP 17713465 A EP17713465 A EP 17713465A EP 3445878 B1 EP3445878 B1 EP 3445878B1
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Prior art keywords
sheet
traces
shaping
temperature
volume
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English (en)
French (fr)
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EP3445878A1 (fr
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Pierre-Olivier Santacreu
Christophe Cazes
Guillaume BADINIER
Jean-Benoit MOREAU
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Aperam SA
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Aperam SA
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    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/008—Martensite

Definitions

  • the invention relates to the hot forming of stainless steels from a sheet to give them a complex shape and remarkable mechanical properties, these steels being intended, for example, for the automotive industry.
  • Martensitic steels (or, more generally, with martensitic structure for more than 50%) have such mechanical characteristics, but their cold forming capacity is limited. We therefore have to either form them cold in the ferritic state, then heat treat the part to obtain the martensitic structure, or put them into hot form in the austenitic state by terminating the treatment by quenching. in order to obtain the martensitic structure.
  • the object of the invention is to propose a method for producing a hot-transformed martensitic steel part, making it possible to manufacture parts of complex shape from a sheet, this final part also having high mechanical properties. making it suitable, in particular, for use in the automotive industry.
  • Said sheet may have a martensitic transformation start temperature (Ms) ⁇ 400 ° C.
  • the martensitic transformation start temperature (Ms) of the sheet can be between 390 and 220 ° C.
  • the thickness of the sheet can be between 0.1 and 10 mm.
  • the austenitization temperature can be at least 850 ° C.
  • the austenitization temperature can be between 925 and 1200 ° C.
  • the sheet can be reheated, during at least one of the steps of transferring and / or changing the configuration of the tool or the steps of shaping or cutting the sheet.
  • a surface treatment can be carried out on the final part, intended to increase its roughness or its fatigue properties.
  • the final part can be left between 90 and 500 ° C for 10 s to 1 h, then let it cool naturally in air.
  • This process begins with an austenitization of the sheet, that is to say by an elevation of its temperature above the temperature Ac1 of the steel so as to form austenite in place of ferrite and carbides constituting the starting microstructure, and under conditions which limit as much as possible the surface decarburization and oxidation of the sheet.
  • shaping step includes operations as diverse as deformation or removal of material as, in particular, deep drawing, hot stamping, stamping, cutting , drilling, these steps can take place in any order chosen by the manufacturer.
  • the part obtained is cooled without any particular constraints on cooling.
  • This cooling can be preceded by a cutting or final shaping step carried out between Ms and Mf (end temperature of martensitic transformation), under conditions where the microstructure consists of at least 10% austenite, at most 20% ferrite, the rest being martensite.
  • composition of the martensitic stainless steel used in the process according to the invention is as follows. All percentages are weight percentages.
  • Its C content is between 0.005% and 0.3%.
  • the minimum content of 0.005% is justified by the need to obtain an austenitization of the microstructure during the first stage of the hot forming process, so that the final mechanical properties targeted are obtained. Above 0.3%, the weldability and, above all, the resilience of the sheet become insufficient, in particular for an application in the automotive industry.
  • Mn content is between 0.2 and 2.0%.
  • Si content is between traces (that is to say simple impurities resulting from the production, without Si having been added) and 1.0%.
  • Si can be used as a deoxidizer during production, just like Al, to which it can be added or substituted. Above 1.0%, it is considered that it excessively promotes the formation of ferrite and therefore makes austenitization more difficult, and that it weakens the sheet too much for the shaping of a complex part to be assured. perform satisfactorily.
  • Its Cr content is between 10.5 and 17.0%, preferably between 10.5% and 14.0% to have faster dissolution of the carbides during austenitization.
  • the minimum content of 10.5% is justified to ensure the oxidability of the sheet.
  • a content higher than 17% would make austenitization difficult and unnecessarily increase the cost of steel.
  • Ni content is between traces and 4.0%.
  • Ni is not essential to the invention.
  • the presence of Ni within the prescribed limit of 4.0% maximum may, however, be advantageous for promoting austenitization. Exceeding the 4.0% limit would however lead to an excessive presence of residual austenite and an insufficient presence of martensite in the microstructure after cooling.
  • Mo is not essential. However, it is favorable to good resistance to corrosion. Above 2.0%, austenitization would be hindered and the cost of steel unnecessarily increased.
  • Cu content is between traces and 3.0%, preferably between traces and 0.5%.
  • Cu requirements are classic for this type of steel. In practice, this means that adding Cu is not useful and that the presence of this element is only due to the raw materials used. A content greater than 0.5%, which would correspond to a voluntary addition, is not desired for automotive applications, because it would degrade the weldability. Cu can however aid in austenitization, and if the steel of the invention is applied to a field which does not require welding, the Cu content can range up to 3.0%.
  • Ti is a deoxidizer, like Al and Si, but its cost and its lower efficiency than that of Al makes its use in general not very interesting from this point of view. It may be advantageous in that the formation of nitrides and carbonitrides of Ti can limit the growth of the grains and favorably influence certain mechanical properties and the weldability. However, this formation can be a drawback in the case of the process according to the invention, since Ti tends to hinder austenitization due to the formation of carbides, and TiNs degrade the resilience. A maximum content of 0.5% should therefore not be exceeded.
  • V and Zr are also elements capable of forming nitrides degrading the resilience, and in general, the sum Ti + V + Zr must not exceed 0.5%.
  • Al is used as a deoxidizer during production. After deoxidation, there should not remain in the steel an amount exceeding 0.2%, because there would be a risk of forming an excessive amount of AlN degrading the mechanical properties, and also of having difficulties in obtain the martensitic microstructure.
  • the requirements on the O content are those which are conventional on martensitic stainless steels, depending on the ability to shape them without cracks starting from the inclusions and the quality of the mechanical properties sought after. the final part, and which the excessive presence of oxidized inclusions is likely to alter. Conversely, if a minimum machinability of the sheet is sought, it may be advantageous to have oxidized inclusions in significant number, if their composition makes them sufficiently malleable so that they serve as a lubricant for the cutting tool. This technique for controlling the number and composition of oxidized inclusions is classic in the steel industry. Control of the composition of the oxides can be advantageously obtained by controlled addition of Ca and / or adjustment of the composition of the slag with which the liquid steel is in contact and in chemical equilibrium during the production.
  • Nb content is between 0.05% and 1.0%
  • Nb + Ta content is between 0.05% and 1.0%.
  • Nb and Ta are important elements for obtaining good resilience, and Ta improves the resistance to pitting corrosion. But as they can interfere with austenitization, they must not be present in quantities exceeding what has just been prescribed. Also, Nb and Ta capture C and N by forming carbonitrides which prevent too strong growth of the austenite grains during austenitization. This is favorable for obtaining a very good resilience when cold, between -100 ° C. and 0 ° C. On the other hand, if the content of Nb and / or Ta is too high, C and N will be entirely trapped in the carbonitrides and there will no longer be enough in dissolved form for the targeted mechanical properties to be achieved, in particular the resilience and the mechanical resistance.
  • V content is between traces and 0.3%.
  • V an embrittling element which is capable of forming nitrides, and must not be present in too large an amount.
  • Ti + V + Zr must not exceed 0.5%.
  • the total contents of Cu, Ni and Co must be between traces and 5.0%, so as not to leave too much residual austenite after the martensitic transformation and not to degrade the weldability in the applications which require it.
  • Sn content is between traces and 0.05% (500 ppm). This element is not desired because it is detrimental to the weldability and the ability of the steel to be hot processed.
  • the 0.05% limit is a tolerance.
  • Zr content is between traces and 0.5%, because it reduces the resilience and hinders austenitization. It is also recalled that the total content of Ti + V + Zr must not exceed 0.5%.
  • H content is between traces and 5 ppm, preferably not more than 1 ppm. Excessive H content tends to weaken martensite. It will therefore be necessary to choose a method of production of steel in the liquid state which can ensure this low presence of H. Typically, treatments ensuring a thorough degassing of the liquid steel (by massive injection of argon in the liquid steel, well-known process known as “AOD”, or by a vacuum passage during which the steel is decarbonized by release of CO, process known as “VOD”) are indicated.
  • N content is between traces and 0.2% (2000 ppm). N is an impurity of which the same treatments which make it possible to reduce the H content help to limit the presence, or even to reduce it substantially. It is not always necessary to have a particularly low N content, but for the reasons that have been said it is necessary that its content, considered jointly with those of elements with which it can combine to form nitrides or carbonitrides obeys the relation 8 ⁇ (Nb + Ta) / (C + N) ⁇ 0.25.
  • the rest of the steel is made up of iron and impurities resulting from the production.
  • composition of the steel relate to the temperatures at the start of martensitic transformation Ms and at the end of martensitic transformation Mf.
  • Ms should preferably be at most 400 ° C. If Ms is higher, there is a risk that the different transfer and shaping operations for the part will not follow each other quickly enough and that there will not be time to carry out all of the shaping at a temperature higher than Ms. However, this risk can be limited or avoided by providing that the part undergoes reheating or temperature maintenance between the shapings, and / or during these if using heating tools of known types integrating , for example, electrical resistors. This condition Ms ⁇ 400 ° C is therefore not always imperative, but only recommended for economical and easy application of the process according to the invention under industrial conditions.
  • Ms must be greater than or equal to 200 ° C. to avoid subsistence in the final part of too high a content of residual austenite, which, in particular, would degrade Rp0.2 by bringing it below 800 MPa.
  • Ms is between 390 and 320 ° C.
  • Mf must be greater than or equal to -50 ° C to guarantee that there will not be too much residual austenite in the final part.
  • Ms and Mf are preferably determined experimentally, for example by dilatometric measurements as is well known, see for example the article "Uncertainties in dilatometric determination of martensite start temperature", Yang and Badeshia, Materials Science and Technology, 2007/5, pp 556-560 .
  • thermomechanical treatments which will be described can be carried out either on a bare sheet which may possibly be coated subsequently, or on a sheet already coated, for example with an Al-based alloy and / or Zn.
  • This coating typically 1 to 200 ⁇ m thick and present on one or two faces of the sheet, may have been deposited by any technique conventionally used for this purpose, it is simply necessary that, if it has been deposited before austenitization, it does not evaporate during the stay of the sheet at austenitization and deformation temperatures, and is not deteriorated during deformations.
  • the process according to the invention is as follows, applied to the manufacture and shaping of a sheet.
  • an initial stainless steel sheet bare or coated, having the composition just described and a thickness which is typically from 0.1 to 10 mm, is conventionally prepared.
  • This preparation can include operations of hot and / or cold transformation and cutting of the semi-finished product resulting from the casting and the solidification of the liquid steel.
  • This initial sheet must have a microstructure consisting of ferrite and / or returned martensite and from 0.5% to 5% by volume of carbides.
  • the size of the ferritic grains measured according to standard NF EN ISO 643, is between 1 and 80 ⁇ m, preferably between 5 and 40 ⁇ m. A ferritic grain size of 40 ⁇ m at most is recommended to promote the austenitization which will follow and thus obtain at least the 80% of austenite desired. A ferritic grain size of at least 5 ⁇ m is recommended to obtain good cold forming capacity.
  • the sheet is first austenitized by passing through an oven which brings it to a range of temperatures greater than Ac1 (temperature at the start of the appearance of austenite), therefore typically greater than approximately 850 ° C. for the compositions concerned). It should be understood that this austenitization temperature must relate to the entire volume of the sheet, and that the treatment must be long enough so that, taking into account the thickness of the sheet and the kinetics of the transformation, the austenitization is complete throughout this volume.
  • the maximum temperature of this austenitization is not a characteristic specific to the invention. It must simply be such that the sheet remains in an entirely solid state (the temperature must therefore be lower, in any case, than the solidus temperature of the steel) and is not too soft to support without transfer the transfer between the oven and the shaping tool which will follow the austenitization. Also, the temperature should not be raised to the point of causing significant surface oxidation and / or decarburization of the sheet in the heating atmosphere. A surface oxidation would lead to the need to descaling the sheet mechanically or chemically before it is shaped to avoid encrustation of scale in the surface of the sheet, and would cause a loss of material.
  • the austenitization takes place at a temperature between 925 and 1200 ° C. for a duration tm of 10 s to 1 h (this duration being that which the sheet passes over Ac1), preferably between 2 min and 10 min for heating in a conventional oven and between 30 s and 1 min for an induction oven.
  • An induction furnace has the advantage, known in itself, of providing rapid reheating to the nominal austenitization temperature. It therefore allows a shorter treatment than a conventional oven to achieve the desired result. These temperatures and durations make it possible to ensure that the continuation of the treatments will lead to a sufficient formation of martensite, and this for a reasonable duration allowing good productivity of the process.
  • This austenitization is to pass the metal from the initial ferrite + carbides structure to an austenitic structure containing at most 0.5% carbides by volume fraction, and at most 20% residual ferrite by volume fraction.
  • An object of this austenitization is, in particular, to lead to a dissolution of at least the majority of the carbides initially present, so as to release C atoms to form the austenitic structure then the martensitic structure during the following stages of the process.
  • the maximum residual ferrite content of 20%, which must remain until the final product, is justified by the resilience and the conventional elastic limit which it is desired to obtain.
  • the austenitized sheet is then transferred to a suitable forming tool (such as a stamping or stamping tool) or a cutting tool.
  • a suitable forming tool such as a stamping or stamping tool
  • This transfer has a duration t0 as short as possible, and during this transfer the sheet must remain at a temperature higher than Ms and keep an austenitic microstructure at 0.5% maximum of carbides and 20% maximum of residual ferrite.
  • the sheet is at a temperature TP0, which is as close as possible to the nominal austenitization temperature for obvious reasons of energy saving.
  • a first shaping or cutting step is then carried out, of duration t1 typically between 0.1 and 10 s.
  • duration t1 typically between 0.1 and 10 s.
  • the precise duration of this stage is not in itself a fundamental characteristic of the invention. It must be sufficiently brief so that the temperature of the sheet does not drop below Ms, that there is no decarburization and / or significant oxidation of the sheet surface, and that an austenitic microstructure with 0.5% maximum of carbides and 20% maximum of residual ferrite is always present at the end of the operation. If necessary, one can use a shaping tool provided with sheet heating means so that these temperature and microstructure conditions are met, since the contact of a non-heating shaping tool with the sheet causes sheet cooling which is often greater than 100 ° C / s.
  • the sheet thus formed is then transferred to another tool for a second shaping step in the broad sense of the term.
  • the same tool is used in the two stages but by modifying its configuration in the meantime (for example by replacing the punch in the case where a drawing is made in each of the two stages).
  • the duration t2 of this transfer is typically from 1 to 10 s, the aim being that it is fast enough for the temperature of the sheet to remain above Ms during the transfer and for the microstructure to remain austenitic, at 0.5% maximum. of carbides and 20% maximum of residual ferrite.
  • the second shaping step is then carried out, of duration t3 typically between 0.1 and 10 s.
  • duration t3 typically between 0.1 and 10 s.
  • the temperature of the sheet remains above Ms and the microstructure remains austenitic, at 0.5% maximum of carbides and 20% maximum of residual ferrite.
  • the average cooling rate between TP0 and TPn defined by the quantity (TP0-TPn) / ⁇ ti, ⁇ ti constituting the sum of the durations of transfers and shaping, must be at least 0.5 ° C / s.
  • composition of the steel is precisely chosen so that, compared to the carbon steels which it is the most common to use in the automotive industry for the production of sheets capable of being welded, this nose is shifted towards the durations higher, thus making possible on usual shaping tools the avoidance of the bainitic domain, a fortiori of the ferritic and perlitic domains, and therefore a execution as complete as possible of the transformation of austenite into martensite.
  • each step taken individually must make it possible to maintain an austenitic microstructure with a maximum of 0.5% of carbides and a maximum of 20% of residual ferrite.
  • the duration / cooling rate of each stage must therefore be chosen accordingly, and, if necessary, reheating of the sheet between and / or during shaping or cutting is carried out so that this microstructure can be maintained during all the steps.
  • At least one additional shaping step in the broad sense at a temperature between Ms and Mf, in a field where the microstructure comprises at least 5% by volume of austenite. If this additional step is a cut, the final shape of the part can be reached with less wear of the tools, and if this additional step is a deformation, at least 5% of austenite will provide sufficient ductility for this deformation to be still possible despite the sometimes already significant presence of martensite.
  • the sheet is allowed to cool, for example in the open air, to room temperature, thereby obtaining the final part according to the method of the invention. It is not necessary to impose a minimum speed during this cooling, because the composition of the steel ensures that the sheet will remain anyway in the area where the martensitic transformation can also take place during this cooling down to the ambient, at least if no means are used which significantly slow down cooling compared to natural cooling in the open air, such as a covering of the sheet. Of course, it is not excluded to accelerate this cooling, by means of forced air or a spray of water or another fluid.
  • a surface treatment can be applied to the final part such as shot blasting or sandblasting, with the aim of increasing the roughness of its surface to improve the adhesion of a coating which would be subsequently applied, such as a paint, or to create residual stresses improving the fatigue resistance of the sheet.
  • This type of operation is known in itself.
  • a final heat treatment can be carried out on the final part, therefore after cooling to the ambient, to improve its elongation at break and bring it to a value of more than 8% according to ISO standards, which corresponds substantially more than 10% according to JIS standards.
  • This treatment consists in making the final part stay between 90 and 500 ° C for 10 s to 1 h, then in performing a natural air cooling.
  • the part thus obtained by the process according to the invention has high mechanical properties at room temperature, in particular because of its high martensite content of at least 80%.
  • Rm is at least 1000 MPa
  • Re is at least 800 MPa
  • the elongation at break A measured according to ISO 6892 standard is at least 8%
  • the bending angle capacity for a 1.5 mm thickness is at least 60 °, measured according to VDA 238-100.
  • Table 2 shows the intermediate metallurgical structures (during the processing stages where the steel temperature is above Ms) and final structures of these same examples, with the mechanical properties of the final part: tensile strength Rm, elastic limit Rp0,2, elongation A, resilience KCU, bending angle capacity.
  • MC designates the proportion of carbides.
  • the invention also includes the cases where a sheet having the composition required by the invention is joined to a sheet having another composition, and where the assembly thus obtained is deformed by the process which has just been described.
  • the structures and properties according to the invention will normally only be obtained on the part of the assembly having the composition of the invention.

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EP17713465.7A 2016-04-22 2017-03-21 Procédé de fabrication d'une pièce en acier inoxydable martensitique à partir d'une tôle Active EP3445878B1 (fr)

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EP3645764B1 (fr) * 2017-06-30 2022-01-19 Aperam Procédé de soudage par points de tôles d'acier inoxydable martensitique
WO2019086934A1 (fr) * 2017-11-03 2019-05-09 Aperam Acier inoxydable martensitique, et son procédé de fabrication
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JP6532990B1 (ja) * 2018-07-18 2019-06-19 株式会社ソディック 積層造形物の製造方法
CN110076246B (zh) * 2019-04-25 2020-11-20 北京航星机器制造有限公司 一种可热处理强化铝合金高效热成形装备及方法
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CN113637924A (zh) * 2020-04-27 2021-11-12 靖江市中信特种机械泵阀厂 一种醪液泵新型材料
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CN112251681B (zh) * 2020-09-29 2022-03-18 中国科学院金属研究所 一种超高强度纳米晶40Cr16Co4W2Mo不锈钢及其制备方法
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CN117286419A (zh) * 2022-06-16 2023-12-26 通用电气公司 具有改善的韧度和强度的微合金化403Cb级马氏体不锈钢
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CA3022115A1 (fr) 2017-10-26
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EP3445878A1 (fr) 2019-02-27
CN109415776B (zh) 2020-09-08
CN109415776A (zh) 2019-03-01
KR102395730B1 (ko) 2022-05-09
RU2018136969A (ru) 2020-04-22
BR112018071587B1 (pt) 2022-03-29
AU2017252037A1 (en) 2018-11-22
RU2018136969A3 (zh) 2020-05-15
ES2805067T3 (es) 2021-02-10
BR112018071587A2 (pt) 2019-02-12
KR20180136455A (ko) 2018-12-24
US20190127829A1 (en) 2019-05-02
JP6840771B2 (ja) 2021-03-10
SI3445878T1 (sl) 2020-08-31
JP2019518609A (ja) 2019-07-04
US11001916B2 (en) 2021-05-11
RU2724767C2 (ru) 2020-06-25

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