EP2773788B1 - Method for low-pressure carbonitriding having an extended temperature range in an initial nitridation phase - Google Patents

Method for low-pressure carbonitriding having an extended temperature range in an initial nitridation phase Download PDF

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EP2773788B1
EP2773788B1 EP12772301.3A EP12772301A EP2773788B1 EP 2773788 B1 EP2773788 B1 EP 2773788B1 EP 12772301 A EP12772301 A EP 12772301A EP 2773788 B1 EP2773788 B1 EP 2773788B1
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Prior art keywords
temperature
nitriding
phase
initial
done
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German (de)
French (fr)
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EP2773788A1 (en
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Philippe Lapierre
Jérôme LARDINOIS
Yves Giraud
Alfred RALLO
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ECM Technologies SAS
PSA Automobiles SA
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ECM Technologies SAS
PSA Automobiles SA
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/28Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases more than one element being applied in one step
    • C23C8/30Carbo-nitriding
    • C23C8/32Carbo-nitriding of ferrous surfaces
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02Pretreatment of the material to be coated
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/34Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases more than one element being applied in more than one step
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/80After-treatment

Definitions

  • the present invention relates to a low pressure carbonitriding process for steel parts, including, but not limited to, parts used in the manufacture of motor vehicles.
  • the invention also applies to parts used in the manufacture of agricultural machinery, machine tool, or parts in the aeronautical field.
  • the object of the invention and to improve the process of the aforementioned document, that is to say to improve the quality of the parts obtained, preferably with a reduction of the treatment time.
  • the nitrogen enrichment which is carried out under conditions favorable to good nitriding is increased so that it is possible to shorten or to eliminate one of the stages of subsequent nitriding and thus reduce the total treatment time.
  • the initial nitriding phase is immediately followed by a first cementation step.
  • the total elimination of the temperature equalization phase makes it possible to lengthen the initial nitriding phase in an optimum temperature range for nitriding.
  • the temperature rise is carried out with a reduced temperature gradient compared to the simple temperature rise phase.
  • the treatment time is further increased in an optimum temperature range for nitriding.
  • the process comprises a final nitriding step accompanied by a lowering of temperature immediately before the quenching.
  • the final nitriding step is also carried out in an optimum temperature range, so that the quality of the treatment is improved.
  • the method according to the invention comprises a first step of temperature rise comprising a first phase M of simple temperature rise, illustrated by a line in continuous line, from the ambient temperature to a point at a temperature of 700 ° C. , denoted Ni1 in the figure.
  • the simple temperature rise phase can be carried out up to a temperature of between 700 ° C. and 750 ° C., and has a duration of between 10 min and 90 min. that is to say that the simple temperature rise is carried out with a temperature gradient of between 8 ° C./min and 75 ° C./min.
  • the process then comprises an initial nitriding phase Ni with continuation of the temperature rise step up to a temperature of 940 ° C. in the example illustrated.
  • the temperature of 940 ° C corresponds to a compromise between a temperature of 860 ° C which allows a treatment of better quality and a temperature of 1000 ° C which allows for faster processing.
  • the rise in temperature continues on a regular basis but with a temperature gradient of between 3.5 ° C./min and 16 ° C./min less than the temperature gradient during the simple temperature rise.
  • the duration of the initial nitriding phase is between 15 minutes and 45 minutes, depending on the amount of nitrogen that it is desired to set in this initial step and the composition of the steel to be treated.
  • the initial nitriding phase comprises injection phases of a nitriding gas such as alternating ammonia with diffusion phases.
  • the temperature rise of the nitriding phase is continued with the same temperature gradient as during the single temperature rise to a point at a temperature of between 750 ° C. and 850 ° C, here 800 ° C, denoted Ni2 in the figure.
  • the temperature is then maintained according to a plateau until a moment noted Ni3 on the figure 2 from which a high temperature rise is performed to reach the carburizing temperature.
  • the temperature of the bearing is chosen in a manner known per se to perform the initial nitriding phase under optimal conditions given the composition of the parts to be treated. Note in this connection that because of the bearing, the final temperature rise can be performed very rapidly, for example 80 ° C / min at 100 ° C / min without subjecting the parts to unacceptable constraints.
  • the rise in temperature of the nitriding phase is continued from point Ni1 with a lower temperature gradient than in the first embodiment, preferably in a range of 2 ° C / min at 8 ° C / min. , up to a moment noted Ni4, here corresponding to a temperature of 850 ° C, from which a high temperature rise is made to reach the carburizing temperature, according to a similar gradient to that of the second embodiment.
  • the process then comprises n alternating cementation phases with nitriding phases.
  • the carburizing and nitriding steps comprise alternating treatment gas injection phases with diffusion phases not shown in the figures.
  • the diagram has been interrupted between the nitriding step N1 and the last cementation step Cn.
  • the process comprises a final nitriding step Nn accompanied by a descent of temperature immediately before T quenching.
  • the temperature is lowered continuously to a temperature in the optimum temperature range for nitriding while remaining high enough to allow effective quenching.
  • the final temperature before quenching is 840 ° C.
  • this limited descent of temperature decreases the stress on the parts during quenching.
  • the final nitriding step has a duration of preferably between 15 min and 60 min, which corresponds to a temperature gradient of between 10 ° C / min and 1 ° C / min.
  • the final nitriding step preferably comprises alternating nitriding gas injection phases with diffusion phases.
  • the last nitriding step Nn illustrated by a long dashed line in the figure, the descent of temperature is first of all carried out in a strong way, with a gradient as strong as possible without causing undue stresses in the steel, up to the optimum nitriding temperature for the steel being treated, denoted Nn1 in the figure, here 840 ° C, then the temperature is maintained at a plateau until the beginning of quenching.
  • the process according to the invention can even terminate the treatment cycle in a conventional manner, that is to say with a quench carried out directly from the carburising temperature.
  • the initial rise in temperature can be carried out according to a constant gradient as illustrated by a dashed line in the figure.
  • the nitriding phase has a shortened duration as illustrated by a mixed line in the figure.
  • the temperature of the workpieces has time to equalize so that it is possible to eliminate the equalization step provided in the aforementioned document. If this is necessary, for example because of a particular configuration of the parts to be treated, it may however provide a temperature equalization step of reduced duration between the initial nitriding phase and the first cementation step.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Heat Treatment Of Articles (AREA)

Description

La présente invention revendique la priorité de la demande française 1159875 déposée le 31 octobre 2011 dont le contenu (texte, dessins et revendications) est ici incorporé par référence.The present invention claims the priority of the French application 1159875 filed on October 31, 2011 whose content (text, drawings and claims) is hereby incorporated by reference.

La présente invention concerne un procédé de carbonitruration basse pression de pièces en acier, notamment bien que non exclusivement, des pièces entrant dans la fabrication de véhicules automobiles. En particulier l'invention s'applique également à des pièces entrant dans la fabrication de machines agricoles, de machine-outil, ou à des pièces dans le domaine aéronautique.The present invention relates to a low pressure carbonitriding process for steel parts, including, but not limited to, parts used in the manufacture of motor vehicles. In particular the invention also applies to parts used in the manufacture of agricultural machinery, machine tool, or parts in the aeronautical field.

ARRIÈRE-PLAN DE L'INVENTIONBACKGROUND OF THE INVENTION

On connaît du document EP 1885904 , un procédé de carbonitruration basse pression de pièces en acier comportant des étapes alternées de cémentation et de nitruration à température constante, précédées d'une étape de montée en température et d'une étape d'égalisation en température, et suivies d'une étape de trempe. En variante il est proposé d'injecter un gaz de nitruration pendant l'étape de montée en température et/ou pendant l'étape d'égalisation en température, à partir d'une température de 800°C.Document is known EP 1885904 , a low pressure carbonitriding process of steel parts comprising alternating steps of carburizing and nitriding at a constant temperature, preceded by a temperature rise step and a temperature equalization step, and followed by a step quenching. Alternatively it is proposed to inject a nitriding gas during the temperature rise step and / or during the temperature equalization step, from a temperature of 800 ° C.

OBJET DE L'INVENTIONOBJECT OF THE INVENTION

Le but de l'invention et d'améliorer le procédé du document précité, c'est-à-dire d'améliorer la qualité des pièces obtenues, de préférence avec une réduction du temps de traitement.The object of the invention and to improve the process of the aforementioned document, that is to say to improve the quality of the parts obtained, preferably with a reduction of the treatment time.

BRÈVE DESCRIPTION DE L'INVENTIONBRIEF DESCRIPTION OF THE INVENTION

En vue de la réalisation de ce but, on propose selon l'invention un procédé de carbonitruration basse pression de pièces en acier, notamment des pièces entrant dans la fabrication de véhicules automobiles, conforme à la revendication 1.In view of the achievement of this object, it is proposed according to the invention a low pressure carbonitriding process of steel parts, in particular parts used in the manufacture of motor vehicles, according to claim 1.

Ainsi, sans augmenter la durée de l'étape de montée en température on augmente l'enrichissement en azote qui est effectué dans des conditions favorables à une bonne nitruration de sorte qu'il est possible de raccourcir ou de supprimer l'une des étapes de nitruration ultérieure et de réduire ainsi le temps de traitement total.Thus, without increasing the duration of the temperature rise stage, the nitrogen enrichment which is carried out under conditions favorable to good nitriding is increased so that it is possible to shorten or to eliminate one of the stages of subsequent nitriding and thus reduce the total treatment time.

Selon une version avantageuse de l'invention, la phase de nitruration initiale est immédiatement suivie d'une première étape de cémentation. Ainsi, la suppression totale de la phase d'égalisation en température permet d'allonger la phase de nitruration initiale dans une plage de température optimale pour la nitruration.According to an advantageous version of the invention, the initial nitriding phase is immediately followed by a first cementation step. Thus, the total elimination of the temperature equalization phase makes it possible to lengthen the initial nitriding phase in an optimum temperature range for nitriding.

Selon un autre aspect avantageux de l'invention, pendant la phase de nitruration initiale la montée en température est effectuée avec un gradient de température réduit par rapport à la phase de montée en température simple. Ainsi on augmente encore la durée du traitement dans une plage de température optimale pour la nitruration.According to another advantageous aspect of the invention, during the initial nitriding phase the temperature rise is carried out with a reduced temperature gradient compared to the simple temperature rise phase. Thus the treatment time is further increased in an optimum temperature range for nitriding.

Selon encore un autre aspect avantageux de l'invention, le procédé comporte une étape de nitruration finale accompagnée d'une descente de température immédiatement avant la trempe. Ainsi l'étape de nitruration finale est également effectuée dans une plage de température optimale, de sorte que la qualité du traitement est améliorée.According to yet another advantageous aspect of the invention, the process comprises a final nitriding step accompanied by a lowering of temperature immediately before the quenching. Thus the final nitriding step is also carried out in an optimum temperature range, so that the quality of the treatment is improved.

BRÈVE DESCRIPTION DES DESSINSBRIEF DESCRIPTION OF THE DRAWINGS

D'autres caractéristiques et avantages de l'invention apparaîtront à la lecture de la description qui suit d'un mode de mise en oeuvre particuliers du procédé de carbonitruration basse pression selon l'invention, en référence à la figure 1 annexée illustrant les différentes étapes du procédé selon l'invention. Les figures 2 et 3 illustrent un procédé de carbonitruration basse pression.Other features and advantages of the invention will appear on reading the following description of a particular embodiment of the low pressure carbonitriding process according to the invention, with reference to the figure 1 annexed illustrating the different steps of the method according to the invention. The figures 2 and 3 illustrate a low pressure carbonitriding process.

DESCRIPTION DETAILLÉE DE L'INVENTIONDETAILED DESCRIPTION OF THE INVENTION

En référence à la figure 1, le procédé selon l'invention comporte une première étape de montée en température comprenant une première phase M de montée en température simple, illustrée par une droite en trait continu, depuis la température ambiante jusqu'à un point à une température de 700°C, noté Ni1 sur la figure. En fonction de la composition de l'acier à traiter, la phase de montée en température simple peut être effectuée jusqu'à une température comprise entre 700°C et 750°C, et a une durée comprise entre 10 min et 90 min c'est-à-dire que la montée en température simple est effectuée avec un gradient de température compris entre 8°C/min et 75°C/min.With reference to the figure 1 the method according to the invention comprises a first step of temperature rise comprising a first phase M of simple temperature rise, illustrated by a line in continuous line, from the ambient temperature to a point at a temperature of 700 ° C. , denoted Ni1 in the figure. Depending on the composition of the steel to be treated, the simple temperature rise phase can be carried out up to a temperature of between 700 ° C. and 750 ° C., and has a duration of between 10 min and 90 min. that is to say that the simple temperature rise is carried out with a temperature gradient of between 8 ° C./min and 75 ° C./min.

Le procédé comporte ensuite une phase de nitruration initiale Ni avec poursuite de l'étape de montée en température jusqu'à une température de 940°C dans l'exemple illustré. En pratique la température de 940°C correspond à un compromis entre une température de 860°C qui permet de réaliser un traitement de meilleure qualité et une température de 1000°C qui permet de réaliser un traitement plus rapide.The process then comprises an initial nitriding phase Ni with continuation of the temperature rise step up to a temperature of 940 ° C. in the example illustrated. In practice the temperature of 940 ° C corresponds to a compromise between a temperature of 860 ° C which allows a treatment of better quality and a temperature of 1000 ° C which allows for faster processing.

Dans l'exemple de réalisation de la figure 1, correspondant à un premier mode de réalisation de la phase de nitruration initiale, la montée en température se poursuit de façon régulière mais avec un gradient de température compris entre 3,5°C/min et 16°C/min inférieur au gradient de température pendant la montée en température simple. La durée de la phase de nitruration initiale est comprise entre 15 min et 45 min, en fonction de la quantité d'azote que l'on souhaite fixer dans cette étape initiale et de la composition de l'acier à traiter.In the exemplary embodiment of the figure 1 , corresponding to a first embodiment of the initial nitriding phase, the rise in temperature continues on a regular basis but with a temperature gradient of between 3.5 ° C./min and 16 ° C./min less than the temperature gradient during the simple temperature rise. The duration of the initial nitriding phase is between 15 minutes and 45 minutes, depending on the amount of nitrogen that it is desired to set in this initial step and the composition of the steel to be treated.

De façon connue en soi la phase de nitruration initiale comporte des phases d'injection d'un gaz nitrurant tel que de l'ammoniac alternées avec des phases de diffusion.In a manner known per se, the initial nitriding phase comprises injection phases of a nitriding gas such as alternating ammonia with diffusion phases.

Selon la figure 2, la montée en température de la phase de nitruration se poursuit avec le même gradient de température que pendant la montée en température simple jusqu'à un point à une température comprise entre 750°C et 850°C, ici 800°C, noté Ni2 sur la figure. La température est alors maintenue selon un palier jusqu'à un instant noté Ni3 sur la figure 2 à partir duquel une montée en température forte est réalisée pour atteindre la température de cémentation. La température du palier est choisie de façon connue en soi pour réaliser la phase de nitruration initiale dans des conditions optimales compte tenu de la composition des pièces à traiter. On notera à ce propos qu'en raison du palier, la montée en température finale peut s'effectuer de façon très rapide, par exemple 80°C/min à 100°C/min sans soumettre les pièces à des contraintes inacceptables.According to figure 2 the temperature rise of the nitriding phase is continued with the same temperature gradient as during the single temperature rise to a point at a temperature of between 750 ° C. and 850 ° C, here 800 ° C, denoted Ni2 in the figure. The temperature is then maintained according to a plateau until a moment noted Ni3 on the figure 2 from which a high temperature rise is performed to reach the carburizing temperature. The temperature of the bearing is chosen in a manner known per se to perform the initial nitriding phase under optimal conditions given the composition of the parts to be treated. Note in this connection that because of the bearing, the final temperature rise can be performed very rapidly, for example 80 ° C / min at 100 ° C / min without subjecting the parts to unacceptable constraints.

Selon la figure 3, la montée en température de la phase de nitruration se poursuit à partir du point Ni1 avec un gradient de température plus faible que dans le premier mode de réalisation, de préférence compris dans une plage de 2°C/min à 8°C/min, jusqu'à un instant noté Ni4, correspondant ici à une température de 850°C, à partir duquel une montée en température forte est réalisée pour atteindre la température de cémentation, selon un gradient analogue à celui du deuxième mode de réalisation.According to figure 3 the rise in temperature of the nitriding phase is continued from point Ni1 with a lower temperature gradient than in the first embodiment, preferably in a range of 2 ° C / min at 8 ° C / min. , up to a moment noted Ni4, here corresponding to a temperature of 850 ° C, from which a high temperature rise is made to reach the carburizing temperature, according to a similar gradient to that of the second embodiment.

Le procédé comporte ensuite n phases de cémentation alternées avec des phases de nitruration. De façon connue en soi les étapes de cémentation et de nitruration comprennent des phases d'injection d'un gaz de traitement alternées avec des phases de diffusion non représentées sur les figures. Sur la figure, le diagramme a été interrompu entre l'étape de nitruration N1 et la dernière étape de cémentation Cn. À l'issue de cette dernière étape de cémentation Cn, le procédé comporte une étape de nitruration finale Nn accompagnée d'une descente de température immédiatement avant la trempe T.The process then comprises n alternating cementation phases with nitriding phases. In a manner known per se, the carburizing and nitriding steps comprise alternating treatment gas injection phases with diffusion phases not shown in the figures. In the figure, the diagram has been interrupted between the nitriding step N1 and the last cementation step Cn. At the end of this last cementation step Cn, the process comprises a final nitriding step Nn accompanied by a descent of temperature immediately before T quenching.

Selon l'invention, la dernière étape de nitruration Nn, illustré par un trait en tirets courts sur la figure, la descente de température est effectuée de façon continue jusqu'à une température comprise dans la plage de température optimale pour la nitruration tout en restant suffisamment élevée pour permettre une trempe efficace. Dans l'exemple illustré la température finale avant la trempe est de 840°C. En pratique des résultats satisfaisants sont obtenus pour une température finale avant la trempe comprise entre 900°C et 800°C. Il a été constaté que cette descente limitée de température diminue la contrainte sur les pièces lors de la trempe.According to the invention, the last nitriding step Nn, illustrated by a dashed line in the figure, the temperature is lowered continuously to a temperature in the optimum temperature range for nitriding while remaining high enough to allow effective quenching. In the example illustrated, the final temperature before quenching is 840 ° C. In practice satisfactory results are obtained for a final temperature before quenching between 900 ° C and 800 ° C. It has been found that this limited descent of temperature decreases the stress on the parts during quenching.

L'étape de nitruration finale à une durée de préférence comprise entre 15 min et 60 min, ce qui correspond à un gradient de température compris entre 10°C/min et 1°C/min. Comme pour la phase de nitruration initiale, l'étape de nitruration finale comporte de préférence des phases d'injection d'un gaz nitrurant alternées avec des phases de diffusion.The final nitriding step has a duration of preferably between 15 min and 60 min, which corresponds to a temperature gradient of between 10 ° C / min and 1 ° C / min. As for the initial nitriding phase, the final nitriding step preferably comprises alternating nitriding gas injection phases with diffusion phases.

Selon la figure 2, la dernière étape de nitruration Nn, illustré par un trait en tirets longs sur la figure, la descente de température est tout d'abord effectuée de façon forte, avec un gradient aussi fort que possible sans engendrer des contraintes indues dans l'acier, jusqu'à la température de nitruration optimale pour l'acier en cours de traitement, notée Nn1 sur la figure, ici 840°C, puis la température est maintenue à un palier jusqu'au début de la trempe.According to figure 2 , the last nitriding step Nn, illustrated by a long dashed line in the figure, the descent of temperature is first of all carried out in a strong way, with a gradient as strong as possible without causing undue stresses in the steel, up to the optimum nitriding temperature for the steel being treated, denoted Nn1 in the figure, here 840 ° C, then the temperature is maintained at a plateau until the beginning of quenching.

En pratique le procédé selon l'invention peut même terminer le cycle de traitement de façon conventionnelle, c'est-à-dire avec une trempe effectuée directement à partir de la température de cémentation.In practice, the process according to the invention can even terminate the treatment cycle in a conventional manner, that is to say with a quench carried out directly from the carburising temperature.

On remarquera qu'en raison de l'efficacité accrue des phases de nitruration selon l'invention il est possible de remplacer au moins une étape de nitruration comprise entre deux étapes de cémentation par une étape de diffusion simple. Une telle étape est plus courte qu'une étape de nitruration de sorte que la durée totale du traitement est raccourcie.It will be noted that because of the increased efficiency of the nitriding phases according to the invention it is possible to replace at least one nitriding step between two carburizing steps by a simple diffusion step. Such a step is shorter than a nitriding step so that the total duration of the treatment is shortened.

Bien entendu l'invention n'est pas limitée au mode de mise en oeuvre décrit et on peut y apporter des variantes de réalisation sans sortir du cadre de l'invention telle que définie par les revendications. En particulier la montée en température initiale peut-être effectuée selon un gradient constant comme illustré par un trait en pointillés sur la figure. Dans ce cas on notera toutefois que la phase de nitruration à une durée raccourcie comme illustré par un trait mixte sur la figure.Naturally, the invention is not limited to the embodiment described and alternative embodiments can be made without departing from the scope of the invention as defined by the claims. In particular, the initial rise in temperature can be carried out according to a constant gradient as illustrated by a dashed line in the figure. In this case, however, it will be noted that the nitriding phase has a shortened duration as illustrated by a mixed line in the figure.

En raison du gradient de température réduit pendant la phase de nitruration initiale, il a été expérimenté que la température des pièces à traiter a le temps de s'égaliser de sorte qu'il est possible de supprimer l'étape d'égalisation prévue dans le document précité. Si cela est nécessaire, par exemple en raison d'une configuration particulière des pièces à traiter, on peut toutefois prévoir une étape d'égalisation de température de durée réduite entre la phase de nitruration initiale et la première étape de cémentation.Due to the reduced temperature gradient during the initial nitriding phase, it has been experimented that the temperature of the workpieces has time to equalize so that it is possible to eliminate the equalization step provided in the aforementioned document. If this is necessary, for example because of a particular configuration of the parts to be treated, it may however provide a temperature equalization step of reduced duration between the initial nitriding phase and the first cementation step.

Claims (5)

  1. Method for low pressure nitrocarburizing steel parts, in particular entering into the production of motor vehicles, comprising alternate steps of cementation (C1-Cn) and of nitriding (N2-Nn), at a constant temperature preceded by a step of increasing temperature comprising a simple temperature increasing phase (M), and followed by a soaking (T) step, characterised in that the simple temperature increasing phase (M) is done with a temperature gradient of between 8 °C/min and 75 °C/min and is followed by an initial nitriding phase (Ni) done with a temperature gradient continuing the temperature increase, in that the initial nitriding phase is done from a temperature of between 700 °C and 750 °C, and until a temperature of between 860 °C and 1000 °C and in that during the initial nitriding phase (Ni), the temperature increase is done with a temperature gradient of between 3.5 °C/min and 16 °C/min.
  2. Low pressure nitrocarburization method according to claim 1, characterised in that the initial nitriding phase is immediately followed by a first cementation step.
  3. Low pressure nitrocarburization method according to claim 1, characterised in that it comprises a final nitriding step (Nn) accompanied by a fall in temperature immediately before the soaking (T).
  4. Low pressure nitrocarburization method according to claim 3, characterised in that the fall in temperature is done until a temperature of between 900 °C and 800 °C.
  5. Low pressure nitrocarburization method according to claim 3, characterised in that the fall in temperature is done with a temperature gradient of between 10 °C/min and 1 °C/min.
EP12772301.3A 2011-10-31 2012-10-08 Method for low-pressure carbonitriding having an extended temperature range in an initial nitridation phase Active EP2773788B1 (en)

Applications Claiming Priority (2)

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FR1159875A FR2981947B1 (en) 2011-10-31 2011-10-31 LOW PRESSURE CARBONITRURATION METHOD AT EXTENDED TEMPERATURE RANGE IN AN INITIAL NITRIDATION PHASE
PCT/EP2012/069888 WO2013064335A1 (en) 2011-10-31 2012-10-08 Method for low-pressure carbonitriding having an extended temperature range in an initial nitridation phase

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FR3004731B1 (en) * 2013-04-18 2016-05-13 Peugeot Citroen Automobiles Sa THERMO-CHEMICAL PROCESSING METHOD COMPRISING A SINGLE NITRIDING PHASE BEFORE CEMENTATION
FR3028530B1 (en) * 2014-11-14 2020-10-23 Peugeot Citroen Automobiles Sa PROCESS AND PLANT FOR CARBONITRURING STEEL PART (S) UNDER LOW PRESSURE AND HIGH TEMPERATURE
CN105420663B (en) * 2015-11-20 2018-07-10 贵州师范大学 A kind of surface treatment method of titanium alloy compound carbonitriding

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FR2777911B1 (en) * 1998-04-28 2000-07-28 Aubert & Duval Sa LOW PRESSURE CARBONITRURATION OF METAL ALLOY PARTS
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US20170241008A9 (en) 2017-08-24
US20140238549A1 (en) 2014-08-28
US9765422B2 (en) 2017-09-19
FR2981947A1 (en) 2013-05-03
CN103946411A (en) 2014-07-23
EP2773788A1 (en) 2014-09-10
KR20140101751A (en) 2014-08-20
WO2013064335A1 (en) 2013-05-10
FR2981947B1 (en) 2014-01-03
BR112014010314A2 (en) 2017-05-02
CN103946411B (en) 2016-01-20
MX2014005219A (en) 2015-03-09
JP2014532808A (en) 2014-12-08
MX359961B (en) 2018-10-17
JP6189849B2 (en) 2017-08-30

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