EP2773788B1 - Verfahren für niederdruck-carbonitrierung mit erweitertem temperaturbereich in der ersten nitrierungsphase - Google Patents

Verfahren für niederdruck-carbonitrierung mit erweitertem temperaturbereich in der ersten nitrierungsphase Download PDF

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Publication number
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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English (en)
French (fr)
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EP2773788A1 (de
Inventor
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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    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C8/00—Solid 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
    • C23C8/06—Solid 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
    • C23C8/28—Solid 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
    • C23C8/30—Carbo-nitriding
    • C23C8/32—Carbo-nitriding of ferrous surfaces
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C8/00—Solid 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
    • C23C8/02—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C8/00—Solid 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
    • C23C8/06—Solid 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
    • C23C8/34—Solid 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C8/00—Solid 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
    • C23C8/80—After-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)

Claims (5)

  1. Verfahren für Niederdruck-Carbonitrierung von Stahlteilen, insbesondere von Teilen, die für die Herstellung von Kraftfahrzeugen verwendet werden, umfassend abwechselnde Schritte einer Aufkohlung (C1-Cn) und einer Nitrierung (N2-Nn) bei konstanter Temperatur, denen ein Schritt eines Temperaturanstiegs vorausgeht, umfassend eine Phase eines einfachen Temperaturanstiegs (M) und gefolgt von einem Schritt eines Härtens (T), dadurch gekennzeichnet, dass die Phase des einfachen Temperaturanstiegs (M) mit einem Temperaturgradienten von zwischen 8 °C/min und 75 °C/min ausgeführt wird und von einer Phase einer ersten Nitrierung (Ni) gefolgt wird, die mit einem Temperaturgradienten unter Fortsetzung des Temperaturanstiegs ausgeführt wird, dadurch, dass die Phase der ersten Nitrierung ab einer Temperatur von zwischen 700 °C und 750 °C und bis zu einer Temperatur von zwischen 860 °C und 1000 °C ausgeführt wird, und dadurch, dass während der Phase der ersten Nitrierung (Ni) der Temperaturanstieg mit einem Temperaturgradienten von zwischen 3,5 °C/min und 16 °C/min ausgeführt wird.
  2. Verfahren für Niederdruck-Carbonitrierung nach Anspruch 1, dadurch gekennzeichnet, dass die Phase der ersten Nitrierung unmittelbar von einem ersten Schritt einer Aufkohlung gefolgt wird.
  3. Verfahren für Niederdruck-Carbonitrierung nach Anspruch 1, dadurch gekennzeichnet, dass es einen Schritt der abschließenden Nitrierung (Nn) enthält, der von einer Temperaturabnahme unmittelbar vor dem Härten (T) begleitet wird.
  4. Verfahren für Niederdruck-Carbonitrierung nach Anspruch 3, dadurch gekennzeichnet, dass die Temperaturabnahme bis zu einer Temperatur von zwischen 900 °C und 800 °C ausgeführt wird.
  5. Verfahren für Niederdruck-Carbonitrierung nach Anspruch 3, dadurch gekennzeichnet, dass die Temperaturabnahme mit einem Temperaturgradienten von zwischen 10 °C/min und 1 °C/min ausgeführt wird.
EP12772301.3A 2011-10-31 2012-10-08 Verfahren für niederdruck-carbonitrierung mit erweitertem temperaturbereich in der ersten nitrierungsphase Active EP2773788B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1159875A FR2981947B1 (fr) 2011-10-31 2011-10-31 Procede de carbonitruration basse pression, a plage de temperature etendue dans une phase de nitruration initiale
PCT/EP2012/069888 WO2013064335A1 (fr) 2011-10-31 2012-10-08 Procede de carbonitruration basse pression, a plage de temperature etendue dans une phase de nitruration initiale

Publications (2)

Publication Number Publication Date
EP2773788A1 EP2773788A1 (de) 2014-09-10
EP2773788B1 true EP2773788B1 (de) 2019-02-20

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EP12772301.3A Active EP2773788B1 (de) 2011-10-31 2012-10-08 Verfahren für niederdruck-carbonitrierung mit erweitertem temperaturbereich in der ersten nitrierungsphase

Country Status (9)

Country Link
US (1) US9765422B2 (de)
EP (1) EP2773788B1 (de)
JP (1) JP6189849B2 (de)
KR (1) KR101945006B1 (de)
CN (1) CN103946411B (de)
BR (1) BR112014010314A2 (de)
FR (1) FR2981947B1 (de)
MX (1) MX359961B (de)
WO (1) WO2013064335A1 (de)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013006589A1 (de) * 2013-04-17 2014-10-23 Ald Vacuum Technologies Gmbh Verfahren und Vorrichtung für das thermochemische Härten von Werkstücken
FR3004731B1 (fr) * 2013-04-18 2016-05-13 Peugeot Citroen Automobiles Sa Procede de traitement thermochimique comportant une unique phase de nitruration avant une cementation
FR3028530B1 (fr) 2014-11-14 2020-10-23 Peugeot Citroen Automobiles Sa Procede et installation de carbonitruration de piece(s) en acier sous basse pression et haute temperature
CN105420663B (zh) * 2015-11-20 2018-07-10 贵州师范大学 一种钛合金碳氮复合渗的表面处理方法

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Publication number Priority date Publication date Assignee Title
FR1159875A (fr) 1956-10-17 1958-07-03 Machal Projecteurs Appareil clignoteur
JPH02294461A (ja) * 1989-05-09 1990-12-05 Mazda Motor Corp 鋼部材の浸炭処理方法
US5273585A (en) 1990-03-27 1993-12-28 Mazda Motor Corporation Heat-treating apparatus
FR2777911B1 (fr) * 1998-04-28 2000-07-28 Aubert & Duval Sa Procede de carbonitruration a basse pression de pieces en alliage metallique
JP3960697B2 (ja) * 1998-12-10 2007-08-15 株式会社日本テクノ 浸炭および浸炭窒化処理方法
AU2002221138A1 (en) * 2001-12-13 2003-06-23 Koyo Thermo Systems Co., Ltd. Vacuum carbo-nitriding method
PL204747B1 (pl) * 2002-10-31 2010-02-26 Politechnika & Lstrok Odzka Sposób nawęglania wyrobów stalowych w podciśnieniu
JP2006002194A (ja) * 2004-06-16 2006-01-05 Nsk Ltd 軸の製造方法
JP4655528B2 (ja) * 2004-07-12 2011-03-23 日産自動車株式会社 高強度機械構造用部品の製造方法、および高強度機械構造用部品
FR2884523B1 (fr) * 2005-04-19 2008-01-11 Const Mecaniques Sa Et Procede et four de carbonitruration a basse pression
JP5295813B2 (ja) * 2009-02-17 2013-09-18 Ｄｏｗａサーモテック株式会社 鉄族系合金の窒化処理方法
DE102009002985A1 (de) * 2009-05-11 2010-11-18 Robert Bosch Gmbh Verfahren zur Carbonitrierung
DE102010028165A1 (de) * 2010-04-23 2011-10-27 Robert Bosch Gmbh Verfahren zur Carbonitrierung von metallischen Bauteilen

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Also Published As

Publication number Publication date
US20140238549A1 (en) 2014-08-28
CN103946411B (zh) 2016-01-20
JP2014532808A (ja) 2014-12-08
KR101945006B1 (ko) 2019-02-01
MX2014005219A (es) 2015-03-09
CN103946411A (zh) 2014-07-23
EP2773788A1 (de) 2014-09-10
US20170241008A9 (en) 2017-08-24
WO2013064335A1 (fr) 2013-05-10
US9765422B2 (en) 2017-09-19
BR112014010314A2 (pt) 2017-05-02
FR2981947B1 (fr) 2014-01-03
FR2981947A1 (fr) 2013-05-03
MX359961B (es) 2018-10-17
KR20140101751A (ko) 2014-08-20
JP6189849B2 (ja) 2017-08-30

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