EP2773787B1 - Verfahren für niederdruck-carbonitrierung mit reduziertem temperaturgradienten in der ersten nitrierungsphase - Google Patents

Verfahren für niederdruck-carbonitrierung mit reduziertem temperaturgradienten in der ersten nitrierungsphase Download PDF

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Publication number
EP2773787B1
EP2773787B1 EP12769125.1A EP12769125A EP2773787B1 EP 2773787 B1 EP2773787 B1 EP 2773787B1 EP 12769125 A EP12769125 A EP 12769125A EP 2773787 B1 EP2773787 B1 EP 2773787B1
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Prior art keywords
temperature
nitriding
phase
initial
low
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EP12769125.1A
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English (en)
French (fr)
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EP2773787A1 (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
    • 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
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • 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 document DE 10 2010 028 165 A1 discloses a carbonitriding process wherein an initial nitriding phase is performed after the rise and stabilization of the process temperature.
  • the object of the invention is 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 invention proposes a method for the low-pressure carbonitriding of steel parts according to claim 1.
  • the parts are maintained longer in a temperature range favorable to good nitriding.
  • the initial nitriding phase comprises a temperature step.
  • the initial nitriding phase is carried out under optimal temperature conditions, so that it is possible to shorten or to eliminate one of the nitriding steps subsequent to the carburizing temperature, and thus to reduce the total time of treatment.
  • 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 process comprises a final nitriding step accompanied by a temperature drop immediately before quenching.
  • the final nitriding step comprises a temperature step.
  • 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 is carried out up to a temperature of between 700 ° C. and 750 ° C., and has a duration of between 10 minutes and 90 minutes. That is, 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 smoothly 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 rise in temperature continues with the same temperature gradient as during the simple rise in temperature to a point at a temperature of between 750 ° C. and 850 ° C., here 800 ° C. noted Ni2 on the figure 2 .
  • 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 carried out very rapidly, for example 80 ° C / min at 100 ° C / min without subjecting the parts to unacceptable constraints.
  • the rise in temperature continues from the point Ni1 with a lower temperature gradient than in the first embodiment, preferably within a range of 2 ° C / min at 8 ° C / min, up to a Ni4 moment, corresponding here to a temperature of 850 ° C, from which a high temperature rise is performed to reach the carburizing temperature, according to a gradient similar 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 within the optimum temperature range for all nitriding. in remaining high enough to allow effective quenching.
  • the final temperature before quenching is 840 ° C.
  • 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.
  • the final nitriding step has a duration of preferably between 15 minutes and 60 minutes, 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 descent of temperature is first of all carried out in a strong way, with a gradient as strong as possible without generating undue stresses in the steel, up to the optimum nitriding temperature for the steel being treated, noted Nn1 in the figure, here 840 ° C, then the temperature is maintained at a plateau until the beginning of quenching.
  • the method according to the invention can be implemented by combining any of the embodiments of the initial nitriding phase with any of the embodiments of the final nitriding phase, or even terminate the cycle. treatment in conventional manner, that is to say with a quench performed directly from the carburizing temperature.
  • 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)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Heat Treatment Of Articles (AREA)

Claims (4)

  1. Verfahren für Niederdruck-Carbonitrierung von Teilen aus Stahl, insbesondere Teilen, die in die Herstellung von Kraftfahrzeugen einfließen, das abwechselnde Schritte des Zementierens (C1 bis Cn) und Nitrierens (N1 bis Nn) bei konstanter Temperatur umfasst, welchen ein Temperaturanstiegsschritt vorangeht, der eine Phase einfachen Temperaturanstiegs (M) gefolgt von einer ersten Nitrierungsphase (N1) mit Fortsetzen des Temperaturanstiegs und gefolgt von einem Härtschritt (T) umfasst, dadurch gekennzeichnet, dass während der ersten Nitrierungsphase (N1) der Temperaturanstieg mit einem Temperaturgradienten ausgeführt wird, der zwischen 3,5 °C/Min. und 16 °C/Min. liegt, der in Bezug auf die einfache Temperaturanstiegsphase (M), die mit einem Temperaturgradienten zwischen 8 °C/Min. und 70 °C/Min. ausgeführt wird, verringert ist, dass die erste Nitrierungsphase (N1) ausgehend von einer Temperatur ausgeführt wird, die zwischen 700 °C und 750 °C liegt, und bis zu einer Temperatur, die zwischen 860 °C und 1000 °C liegt, und dass es einen abschließenden Nitrierungsschritt (Nn) umfasst, der von einem Temperatursenken unmittelbar vor dem Härten (T) begleitet ist, wobei das Temperatursenken bis zu einer Temperatur, die zwischen 900 °C und 800 °C liegt, und mit einem Temperaturgradienten zwischen 10 °C/Min. und 1 °C/Min. ausgeführt wird.
  2. Verfahren für Niederdruck-Carbonitrierung nach Anspruch 1, dadurch gekennzeichnet, dass die erste Nitrierungsphase (Ni) eine Temperaturstufe (Ni2-Ni3) umfasst.
  3. Verfahren für Niederdruck-Carbonitrierung nach Anspruch 1, dadurch gekennzeichnet, dass auf die erste Nitrierungsphase (N1) unmittelbar ein erster Zementierungsschritt (C1) folgt.
  4. Verfahren für Niederdruck-Carbonitrierung nach Anspruch 1, dadurch gekennzeichnet, dass der abschließende Nitrierungsschritt eine Temperaturstufe (Nn1) umfasst.
EP12769125.1A 2011-10-31 2012-10-08 Verfahren für niederdruck-carbonitrierung mit reduziertem temperaturgradienten in der ersten nitrierungsphase Active EP2773787B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1159877A FR2981948B1 (fr) 2011-10-31 2011-10-31 Procede de carbonitruration basse pression, a gradient reduit de temperature dans une phase de nitruration initiale
PCT/EP2012/069889 WO2013064336A1 (fr) 2011-10-31 2012-10-08 Procede de carbonitruration basse pression, a gradient reduit de temperature dans une phase de nitruration initiale

Publications (2)

Publication Number Publication Date
EP2773787A1 EP2773787A1 (de) 2014-09-10
EP2773787B1 true EP2773787B1 (de) 2018-07-04

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EP12769125.1A Active EP2773787B1 (de) 2011-10-31 2012-10-08 Verfahren für niederdruck-carbonitrierung mit reduziertem temperaturgradienten in der ersten nitrierungsphase

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US (1) US9708704B2 (de)
EP (1) EP2773787B1 (de)
JP (1) JP6189850B2 (de)
KR (1) KR101945004B1 (de)
CN (1) CN103946412B (de)
BR (1) BR112014010315A2 (de)
FR (1) FR2981948B1 (de)
IN (1) IN2014CN03952A (de)
MX (1) MX360731B (de)
WO (1) WO2013064336A1 (de)

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Publication number Priority date Publication date Assignee Title
FR1159877A (fr) 1956-10-17 1958-07-03 Boucle de sangle réglable à ouverture rapide
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
JP3931276B2 (ja) * 2001-12-13 2007-06-13 光洋サーモシステム株式会社 真空浸炭窒化方法
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
CN101851735B (zh) * 2010-04-19 2011-09-07 东风汽车有限公司 一种球墨铸铁的强化工艺及其制成品
DE102010028165A1 (de) * 2010-04-23 2011-10-27 Robert Bosch Gmbh Verfahren zur Carbonitrierung von metallischen Bauteilen

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Publication number Publication date
US9708704B2 (en) 2017-07-18
JP6189850B2 (ja) 2017-08-30
WO2013064336A1 (fr) 2013-05-10
CN103946412A (zh) 2014-07-23
EP2773787A1 (de) 2014-09-10
IN2014CN03952A (de) 2015-10-23
MX360731B (es) 2018-11-14
CN103946412B (zh) 2016-10-05
KR20140101749A (ko) 2014-08-20
KR101945004B1 (ko) 2019-02-01
JP2014532809A (ja) 2014-12-08
US20150101710A1 (en) 2015-04-16
FR2981948B1 (fr) 2014-01-03
FR2981948A1 (fr) 2013-05-03
MX2014005220A (es) 2015-03-05
BR112014010315A2 (pt) 2017-05-02

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