EP3249059A1 - Procédé de traitement thermique d'aciers austénitiques et aciers austénitiques ainsi obtenus - Google Patents

Procédé de traitement thermique d'aciers austénitiques et aciers austénitiques ainsi obtenus Download PDF

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Publication number
EP3249059A1
EP3249059A1 EP16171672.5A EP16171672A EP3249059A1 EP 3249059 A1 EP3249059 A1 EP 3249059A1 EP 16171672 A EP16171672 A EP 16171672A EP 3249059 A1 EP3249059 A1 EP 3249059A1
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Prior art keywords
hns
steel
austenitic
temperature
precipitates
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EP16171672.5A
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German (de)
English (en)
French (fr)
Inventor
Joël Porret
Christian Charbon
Vincent Fays
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Swatch Group Research and Development SA
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Swatch Group Research and Development SA
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Priority to EP16171672.5A priority Critical patent/EP3249059A1/fr
Priority to EP17167986.3A priority patent/EP3249060B1/fr
Priority to US15/589,067 priority patent/US11136638B2/en
Priority to JP2017101408A priority patent/JP6509944B2/ja
Priority to CN201710383822.6A priority patent/CN107435087B/zh
Publication of EP3249059A1 publication Critical patent/EP3249059A1/fr
Withdrawn legal-status Critical Current

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    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26—Methods of annealing
    • 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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/002—Heat treatment of ferrous alloys containing Cr
    • 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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/02—Hardening by precipitation
    • 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
    • C22C38/04—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
    • 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
    • C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium 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
    • C22C38/38—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of manganese
    • 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
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/001—Austenite
    • 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
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/004—Dispersions; Precipitations
    • 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
    • C21D2261/00—Machining or cutting being involved

Definitions

  • the present invention relates to a heat treatment process of austenitic steels as well as the austenitic steels obtained by the implementation of this heat treatment process. More specifically, the present invention is concerned with nitrogen-austenitic steels well known by their Anglo-Saxon name Austenitic High Nitrogen Steel or austenitic HNS steels. The invention is also interested in austenitic steels with high concentrations of interstitial atoms, better known by their Anglo-Saxon name Austenitic High Interstitial Steel or austenitic steels HIS.
  • Austenitic steels alloyed with nitrogen that, for convenience, we will call later austenitic steels HNS, and austenitic steels with high concentrations of interstitial atoms which will be called hereinafter austenitic steels HIS have properties of hardness, resistant to corrosion and hypoallergenic which make them very interesting especially for applications in the field of watchmaking and jewelery, both for the manufacture of dressing elements intended to come into contact with the skin due to their very low concentration of nickel, and for the manufacture of components of watch movements because they are very hard, especially after hardening.
  • the austenitic HNS steels contain interstitial nitrogen atoms in high concentrations which can range up to 1.5% by weight depending on the composition and implementation of the alloy.
  • HIS austenitic steels directly derived from HNS austenitic steels, contain significant quantities of interstitial carbon atoms in addition to interstitial nitrogen atoms.
  • certain austenitic steels HNS and HIS exhibit particularly interesting hypoallergenic properties because of their very low nickel content and their resistance to corrosion.
  • the austenitic steels HNS and HIS are very difficult to machine, in particular because they have a very high yield strength, work hardening rate and ductility. Tests show, for example, that the machining operations are two to three times longer than for 1.4435 steel and the wear of the machining tools is very important.
  • the machining of these austenitic steels HNS and HIS which in many ways approaches the machining of titanium, is therefore long, difficult and expensive and is the main obstacle to the use of these steels especially in the field of watchmaking and jewelery.
  • the present invention relates to a heat treatment process of austenitic steels of HNS and HIS type whose purpose is to make such austenitic steels more easily machinable.
  • the present invention relates to a heat treatment process of an austenitic steel HNS or HIS which consists in performing a slow cooling of this steel austenitic HNS or HIS immediately after its austenitization or sintering, so as to reveal precipitates.
  • Slow cooling is understood to mean cooling which, after austenitization or sintering, favors the appearance of precipitates in the microstructure of the austenitic steels HNS and HIS thus treated, as opposed to the conventional quenching heat treatment which consists of rapidly cooling the HNS steels and HIS after austenitization or sintering to avoid the formation of precipitates.
  • HNS and HIS austenitic steels undergo a slow cooling heat treatment to promote the appearance of precipitates
  • the present invention is totally contrary to the usual practice of cooling the precipitates. alloys as quickly as possible in order to avoid as much as possible the formation of precipitates in the resulting HNS and HIS austenitic steels.
  • the Applicant has indeed found that by subjecting the austenitic steels HNS and HIS to the heat treatment process according to the invention, the nitrogen and carbon atoms, for example, tend to migrate towards the grain boundaries and to combine relatively easily. with chromium or molybdenum atoms to form precipitates of the nitride, carbide or even chromium / molybdenum carbonitride type. However, these precipitates have a very low adhesion with the matrix, so that they make the chips brittle and facilitate the machining operations.
  • the heat treatment process according to the present invention applies equally well to parts obtained by casting and subsequent thermomechanical treatment, as well as to parts obtained by powder metallurgy such as molding. by metal injection still known under the name Anglo-Saxon Metal Injection Molding or MIM. Indeed, immediately after sintering the alloy at its austenitization temperature in order to obtain an austenitic steel of the HNS or HIS type, it is possible to cool slowly the alloy to promote the formation of precipitates in accordance with the teachings of the present invention.
  • the present invention relates to a heat treatment process of an austenitic steel HNS or HIS which consists of subjecting the austenitic steel HNS or HIS to cooling from the austenitization or sintering temperature, and then to interrupt the cooling austenitic steel HNS or HIS when the temperature reaches a value at which precipitates may appear, and to maintain the steel at this temperature and for a period such as appear precipitates, then finally to bring the steel temperature room.
  • the austenitic steel HNS or HIS after the austenitic steel HNS or HIS has undergone a heat treatment of austenitization or sintering then quenching, the austenitic steel HNS or HIS is heated to a temperature and for a time such that precipitates appear.
  • This third variant is the most practical because it allows to perfectly control the parameters of different heat treatments.
  • the precipitates are re-dissolved after machining by again bringing the austenitic steel HNS or HIS to its annealing temperature, and then cooling rapidly enough to avoid forming precipitates again.
  • This feature is very advantageous because it allows, when desired, to remove after machining parts precipitates that have been created through the heat treatment process according to the invention.
  • this possibility can be used to eliminate precipitates in covering elements (middle, back of watch cases, glasses, crowns, pushers, clasps, bracelets, etc.) in order to make the material as homogeneous as possible and to eliminate the residual stresses.
  • the resulting steels will thus have better corrosion resistance and greater ductility.
  • clockwork components it is preferable not to subject these clockwork components to a second austenitization heat treatment, in order to preserve the hardness obtained by deformation. Cold.
  • the first, second and third variants of implementation of the heat treatment process of an austenitic steel HNS or HIS according to the invention are therefore more particularly intended to obtain cladding elements for timepieces, because they promote the corrosion resistance of these steels.
  • These first three variants have in common that after application of the heat treatment according to the invention to austenitic steel HNS or HIS and subsequent machining, it is indeed possible to bring the resulting part to the annealing temperature, and then soak it in order to put back precipitates in solution.
  • an austenitic steel HNS or HIS is brought to its annealing temperature, in other words to its austenitization temperature, and then cooled rapidly (quenching) so that no precipitate is formed, it is deformed cold then this austenitic steel HNS or HIS is brought to a temperature and for a period such that appear precipitates.
  • the hardness of the austenitic steel HNS or HIS obtained after austenitization and cold deformation is very little affected by the precipitation treatment according to the invention carried out subsequently.
  • the machinability of such steels is substantially improved.
  • the steel austenitic HNS or HIS is deformed cold after this steel has been brought back to room temperature.
  • the present invention proceeds from the general inventive idea of subjecting the austenitic HNS and HIS steels to a heat treatment of precipitation.
  • the term "heat treatment of precipitation” is intended to mean a treatment which aims at placing these austenitic steels HNS and HIS for a certain period of time under temperature conditions which allow the appearance of precipitates such as nitrides, carbides or carbonitrides, especially molybdenum and / or chromium. It has indeed been observed that these precipitates are generally not very bound to the matrix of the material, so that they favor the formation and removal of chips when machining parts.
  • each austenitic steel composition HNS or HIS has a time-temperature-transformation diagram which is specific to it and which is also a function of the nature of the precipitate in question.
  • the figure 1 is a time (t) - temperature (T) - transformation diagram which illustrates the heat treatment of an austenitic steel HNS or HIS according to the first alternative embodiment of the method of the invention.
  • Tr1 is the austenitizing temperature or annealing of a type of austenitic steel HNS or HIS and either a curve which, on the time-temperature-transformation diagram figure 1 , defines an area that corresponds to conditions of time and temperature that allow the formation of precipitates.
  • 1 is the fast cooling curve which allows to bring back the austenitic steel HNS or HIS since its annealing temperature to ambient temperature avoiding any formation of precipitates
  • 2 the cooling curve according to the invention which combines the time and temperature parameters in such a way that by lowering the temperature of the austenitic steel HNS or HIS following this curve 2, allows the appearance of precipitates in this steel.
  • the figure 2 is a time (t) - temperature (T) - transformation diagram which illustrates the heat treatment of an austenitic steel HNS or HIS according to the second alternative embodiment of the method of the invention.
  • Tr2 be the austenitization or annealing temperature of an austenitic steel of the HNS or HIS type and let b be the curve which, on the time-temperature-transformation chart of the figure 2 , defines an area that corresponds to conditions of time and temperature that allow the formation of precipitates.
  • the austenitic steel HNS or HIS is rapidly cooled rapidly from its annealing temperature Tr2 according to curve 4, and cooling of the austenitic steel HNS or HIS is interrupted when the temperature reaches a value Tp2 at which precipitates can appear. and this steel is maintained at this temperature Tp2 for a time such that precipitates appear (curve 6). Finally, the steel is brought back to room temperature (curve 8).
  • the figure 3 is a time (t) - temperature (T) - transformation diagram which illustrates the heat treatment of an austenitic steel HNS or HIS according to the third alternative embodiment of the method of the invention.
  • Tr3 is the austenitizing temperature or annealing of a HNS type austenitic steel or HIS and c is the curve, the time-temperature-transformation diagram figure 3 , defines an area that corresponds to conditions of time and temperature that allow the formation of precipitates.
  • the steel in question here is an austenitic steel HNS or HIS which has been cooled sufficiently rapidly from its annealing temperature Tr3 to room temperature in order to avoid any formation of precipitates.
  • such austenitic steel HNS or HIS is heated according to curve 10 and maintained at a temperature and for a time such that precipitates appear (curve 12), and then is cooled (curve 14).
  • the fourth alternative embodiment of the process of the invention differs from the third variant of the same process only in that, after annealing treatment followed by quenching and before the precipitation treatment, the austenitic steel HNS or HIS is hardened, that is to say deformed cold.
  • the heat treatment according to the invention which consists in wearing an austenitic steel at a temperature and for a period of time such that precipitates are formed is therefore applied, in this fourth variant, to a material that has been hardened beforehand by hardening.
  • the fifth and last alternative embodiment of the process of the invention consists in subjecting the austenitic steel to a cold deformation treatment after heat treatment according to one of the first three processing variants.
  • the figure 4 is a view of a metallographic section of a HIS X20CrMnMoN17-11-3 steel sample that has been annealed at its austenitization temperature and quenched. It is noted on examining this figure that the grain boundaries are not very marked, which indicates the absence of precipitates.
  • the figure 5 is a view of a metallographic section of a sample of austenitic steel HIS X20CrMnMoN17-11-3 having undergone a heat treatment according to the third variant of implementation of the method according to the invention.
  • the grain boundaries are marked, indicating the presence of large amounts of precipitates along these grain boundaries.
  • the idea see (areas surrounded by a circle on the figure 5 ) that some larger precipitates have grown inside the grains since the grain boundaries.
  • Such a Concentration of precipitates could be obtained by carrying, after cooling rapidly from the annealing temperature, the austenitic steel HIS X20CrMnMoN17-11-3 at a temperature of 800 ° C for two hours.
  • Samples of austenitic steel HIS X20CrMnMoN17-11-3 were therefore subjected to a heat treatment process according to the fourth variant embodiment of the invention and consisting, after annealing treatment followed by quenching and hardening, to wear the austenitic steel HIS X20CrMnMoN17-11-3 at a temperature and for a time such that precipitates form. It has been observed that after cold deformation, the formation of the precipitates is much faster. Indeed, the dislocations and the gaps induced by the cold deformation create diffusion paths favorable to the germination and the growth of the precipitates.
  • the figure 6 is a view of a metallographic section of a sample of austenitic steel HIS X20CrMnMoN17-11-3 which is in the form of a bar whose outer diameter is reduced from 3 mm to 2.5 mm by cold deformation by wire drawing, a diameter reduction of 16.6%.
  • this sample was then heated to a temperature of 800 ° C. for two hours according to the temperature curve represented in FIG. figure 3 . It can be seen that steel has many precipitates, both at the grain boundaries and inside the grains.
  • the figure 7 is a graph that shows the evolution of the hardness of austenitic steel HIS X20CrMnMoN17-11-3 of the figure 6 depending on the temperature at which this steel is worn to form the precipitates. It is observed that the hardness of the austenitic steel without treatment of precipitation according to the invention and after cold work-hardening is 450 HV10 (symbol in the form of a square on the graph). The same austenitic steel is, after cold working, heat-treated according to the fourth alternative embodiment of the method according to the invention.
  • Samples of this steel are respectively heated to temperatures of 750 ° C, 800 ° C, 850 ° C, 900 ° C and 950 ° C for a period of two hours, then cooled (diamond symbols on the graph) . It is observed that for samples heated between 700 ° C and 900 ° C, the hardness is between about 425 HV10 and 375 HV10. In other words, the hardness of these samples of austenitic steel heat-treated according to the fourth variant of the invention varies little with respect to the hardness of the austenitic steel hardened but not subjected to a treatment of precipitation.
  • the machinability of the austenitic steel samples having undergone a heat treatment of precipitation according to this fourth variant of the invention is clearly improved. Only the austenitic steel sample heated at 950 ° C for two hours has a hardness substantially lower than that of austenitic steel without precipitation treatment (less than 350 HV10). Finally, a sample of austenitic steel HIS X20CrMnMoN17-11-3 having undergone only annealing treatment followed by quenching (triangular symbol on the graph) has a hardness less than 250 HV10.
  • the figure 8 is a view of a metallographic section of a sample of austenitic steel HIS X20CrMnMoN17-11-3 in the form of a bar whose outer diameter is reduced from 3 mm to 2 mm by cold deformation by wire drawing a larger diameter reduction of 33.3%.
  • This steel sample undergoes the same heat treatment as at figure 6 by being heated to a temperature of 800 ° C. for two hours in accordance with the fourth variant embodiment of the invention.
  • the phenomenon of precipitation is even more pronounced since, besides the precipitates which are formed along the grain boundaries and from the joints of grains inward grains, there is a high concentration of precipitates inside-even grains.
  • the figure 9 is a graph that shows the evolution of the hardness of the steel of the figure 8 depending on the time and temperature at which this steel is worn after work hardening to form the precipitates. It is observed that the hardness of the austenitic steel without precipitation treatment according to the invention and after cold working is between 550 HV10 and 560 HV10 (symbol in the form of a square on the graph). This hardness is greater than that at figure 7 because the rate of work hardening is higher.
  • the diamond shaped symbols on the figure 9 correspond to samples of austenitic steel heated to temperatures of 700 ° C, 750 ° C, 800 ° C and 850 ° C respectively for 45 minutes.
  • the round symbols correspond to samples of austenitic steel heated to temperatures of 700 ° C, 750 ° C, 800 ° C and 850 ° C respectively for two hours. If we compare the graphs of figures 7 and 9 it is observed that the higher the rate of work hardening, the more the formation of precipitates is facilitated. Indeed, the mechanical stresses at the heart of the steel make it possible to germinate and grow the precipitates.
  • HNS and HIS steels to which the process Precipitation according to the invention can be applied are: X5CrMnN18-18, X8CrMnN19-19, X8CrMnMoN18-18-2, X13CrMnMoN18-14-3, X20CrMnMoN17-11-3 or alternatively X5MnCrMoN23-21.
  • precipitates that may form during the precipitation process are: M23C, MC, M6C or even M2N, where M denotes one or more of the metal elements of the alloy that can combine with carbon or nitrogen to form carbides or nitrides or carbonitrides.
  • M denotes one or more of the metal elements of the alloy that can combine with carbon or nitrogen to form carbides or nitrides or carbonitrides.
  • the invention applies in particular to jewelery and trim elements of timepieces, as well as to watch components.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
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EP16171672.5A 2016-05-27 2016-05-27 Procédé de traitement thermique d'aciers austénitiques et aciers austénitiques ainsi obtenus Withdrawn EP3249059A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP16171672.5A EP3249059A1 (fr) 2016-05-27 2016-05-27 Procédé de traitement thermique d'aciers austénitiques et aciers austénitiques ainsi obtenus
EP17167986.3A EP3249060B1 (fr) 2016-05-27 2017-04-25 Procédé de traitememnt thermique d'aciers austénitiques
US15/589,067 US11136638B2 (en) 2016-05-27 2017-05-08 Method for heat treatment of austenitic steels and austenitic steels obtained thereby
JP2017101408A JP6509944B2 (ja) 2016-05-27 2017-05-23 オーステナイト鋼の熱処理方法およびそれにより得られるオーステナイト鋼
CN201710383822.6A CN107435087B (zh) 2016-05-27 2017-05-26 奥氏体钢的热处理方法及由此得到的奥氏体钢

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EP16171672.5A EP3249059A1 (fr) 2016-05-27 2016-05-27 Procédé de traitement thermique d'aciers austénitiques et aciers austénitiques ainsi obtenus

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CN115976303A (zh) * 2023-02-06 2023-04-18 昆明理工大学 一种提高含v合金化高锰钢铸件耐磨性能的方法

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CH715726B1 (fr) * 2019-01-11 2022-10-14 Richemont Int Sa Procédé d'obtention d'un composant fonctionnel pour mouvement horloger.
JP2021139827A (ja) * 2020-03-09 2021-09-16 セイコーエプソン株式会社 時計用部品の製造方法

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