EP1122331B1 - Procédé pour la nitruration et/ou carbonitruration d' acier fortement allié - Google Patents

Procédé pour la nitruration et/ou carbonitruration d' acier fortement allié Download PDF

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Publication number
EP1122331B1
EP1122331B1 EP00102359A EP00102359A EP1122331B1 EP 1122331 B1 EP1122331 B1 EP 1122331B1 EP 00102359 A EP00102359 A EP 00102359A EP 00102359 A EP00102359 A EP 00102359A EP 1122331 B1 EP1122331 B1 EP 1122331B1
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EP
European Patent Office
Prior art keywords
workpieces
gas atmosphere
ammonia
temperature
nitriding
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP00102359A
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German (de)
English (en)
Other versions
EP1122331A1 (fr
Inventor
Wolfgang Lerche
Bernd Edenhofer
Michael Lohrmann
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ipsen International GmbH
Original Assignee
Ipsen International GmbH
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Filing date
Publication date
Application filed by Ipsen International GmbH filed Critical Ipsen International GmbH
Priority to DE50001540T priority Critical patent/DE50001540D1/de
Priority to EP00102359A priority patent/EP1122331B1/fr
Priority to AT00102359T priority patent/ATE235581T1/de
Priority to US09/562,695 priority patent/US6328819B1/en
Publication of EP1122331A1 publication Critical patent/EP1122331A1/fr
Application granted granted Critical
Publication of EP1122331B1 publication Critical patent/EP1122331B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C23C8/08—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 only one element being applied
    • C23C8/24—Nitriding
    • C23C8/26—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
    • C23C8/06—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

Definitions

  • the invention relates to a method for heat treatment of metallic Workpieces, in particular for nitriding or nitrocarburizing alloyed Ferrous materials, such as higher alloy steels.
  • the invention also relates on the use of a device for performing such a method.
  • thermochemical heat treatment To create defined workpiece properties, such as a high one Wear resistance or sufficient corrosion resistance metallic workpieces are subjected to a thermochemical heat treatment.
  • the result of the heat treatment is, for example, nitriding or nitrocarburizing Enriching the edge layer of the workpieces with nitrogen and / or Carbon in order to achieve the required mechanical and to impart chemical properties on the surface and in the edge area.
  • the surface layer is enriched with nitrogen by the ammonia (NH 3 ) contained in a reaction gas at temperatures of generally above 500 ° C under the catalytic effect of the surface of the workpieces to be nitrided decays into nitrogen (N) and hydrogen (H).
  • the ammonia molecule is adsorbed and gradually degraded on the workpiece surface, whereby the required nitrogen is released in atomic form and is available for solution in iron and for the formation of iron nitride (Fe x N).
  • the surface layer is simultaneously enriched with carbon.
  • Atomic carbon (C) diffuses in an analogous manner through the workpiece surface into the boundary layer.
  • the surface layer which, in addition to hexagonal ⁇ -nitride (Fe 2-3 N), also face-centered cubic ⁇ '-nitride (Fe 4 N) and also nitrides of nitride-forming alloy elements, such as chromium, molybdenum, manganese, titanium, niobium, tungsten, vanadium or aluminum nitride.
  • the invention has for its object a method for To create heat treatment of metallic workpieces, which also includes Workpieces made of higher alloyed iron materials are largely uniform nitriding layer can be achieved.
  • Such a procedure embraces the surprising finding that a largely uniform nitriding layer can be achieved if the Workpieces before the actual heat treatment in process step d, for example, nitriding or nitrocarburizing, initially only in one ammonia-containing gas atmosphere warmed and then in an additional one Gas atmosphere containing oxidizing agent to the treatment temperature, for example, the nitriding temperature, heated and then for a certain Duration may be kept at this temperature with the result that possibly in the case of high-alloy materials, existing passive layers are eliminated or something that be converted into a uniform diffusion of nitrogen into the Material is favored.
  • the temperature at which in each Process steps is heated, and the length of time for which the workpieces in the respective gas atmospheres are based on the Composition of the reaction gas and the material to be treated Workpieces and the desired treatment success.
  • the ratio of the amounts of ammonia and the oxidizing agent in the gas atmosphere is expediently between 1: 1 and 5: 1 when air is used as the oxidizing agent, and between 1: 0.1 and 1: 1 when carbon dioxide, water vapor or nitrous oxide is used Oxidizing agents are used.
  • a particularly advantageous procedure is also given when the Time period when the workpieces are kept in an ammonia or Ammonia and the carbon-donating gas atmosphere in Dependence on the desired thickness of the surface layer to be enriched is chosen.
  • Procedural management may also be useful as carbon donor substance carbon dioxide, carbon monoxide or Hydrocarbons can be used individually or as a mixture.
  • the workpieces in one reducing or neutral gas atmosphere for example from an endogas or nitrogen, or in a liquid quenching medium Room temperature can be cooled to an economically beneficial Ensure procedure.
  • the first workpiece sample shown in FIG. 1 was preheated to a temperature of approximately 450 ° C. in an endogas-containing gas atmosphere and then in a reaction gas consisting of 50 vol.% Ammonia (NH 3 ) and 50 vol.% Endogas the nitriding temperature of approx. 580 ° C warmed. After approximately 240 minutes, during which the workpiece sample was exposed to the gas atmosphere at this temperature, the workpiece sample was cooled to room temperature in an endogenous gas atmosphere.
  • a reaction gas consisting of 50 vol.% Ammonia (NH 3 ) and 50 vol.% Endogas the nitriding temperature of approx. 580 ° C warmed.
  • the second workpiece sample shown in FIG. 2 was first preheated in an ammonia-containing gas atmosphere to a temperature of approximately 450 ° C. and then in an ammonia-containing reaction gas, the air as the oxidizing agent in a ratio of 3.5 (ammonia): 1 (air ) was added, heated to the nitriding temperature of approx. 580 ° C. The workpiece sample was then held at this temperature and in this gas atmosphere for a period of about 1.5 hours. The gas atmosphere was then exchanged and the workpiece sample was exposed at 580 ° C. to a reaction gas with the composition 50% by volume ammonia (NH 3 ) and 50% by volume endogas for approx. 4 h, in order to achieve the desired nitriding depth of approx. 80 ⁇ m to reach. Finally, the second workpiece sample was then cooled to room temperature in an endogas-containing gas atmosphere.
  • ammonia ammonia
  • the comparison of the micrographs shown in the drawing shows that the 1, structure of the first produced by conventional nitriding Workpiece sample in the range from 0 ⁇ m to 40 ⁇ m from the edge uneven nitriding layer, while that after the last Methodically generated nitriding layer of the second workpiece sample is evenly formed.
  • Iron materials such as stainless steels
  • their high corrosion resistance is inextricably linked to surface passivation, on proportionate achieve better treatment results in a simple way.

Landscapes

  • 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)

Claims (7)

  1. Procédé pour le traitement thermique de pièces à usiner métalliques, notamment pour la nitruration ou la carbonitruration de produits ferreux alliés, constitué des étapes de procédé suivantes :
    f) chauffage des pièces à usiner dans un four de nitruration à une température comprise entre 400°C et 500°C dans une atmosphère gazeuse ammoniacale,
    g) chauffage continu des pièces à usiner à une température comprise entre 500°C et 700°C dans une atmosphère gazeuse ammoniacale et contenant un oxydant ajouté,
    h) maintien des pièces à usiner à cette température et dans cette atmosphère pendant une durée comprise entre 0,1h et 5h,
    i) maintien continu des pièces à usiner à cette température pendant une durée comprise entre 1h et 100h dans une atmosphère gazeuse ammoniacale ou dans une atmosphère gazeuse ammoniacale et contenant une substance cédant du carbone, et
    j) refroidissement des pièces à usiner à température ambiante.
  2. Procédé selon la revendication 1, caractérisé en ce que de l'air, du dioxyde de carbone (CO2), de la vapeur d'eau (H2O) ou du protoxyde d'azote (N2O) ont été ajoutés comme oxydant.
  3. Procédé selon la revendication 2, caractérisé par un rapport des volumes d'ammoniaque et d'oxydant dans l'atmosphère gazeuse entre 1/1 et 5/1 lorsque l'air est utilisé comme oxydant, et entre 1/0,1 et 1/1 lorsqu'on utilise du dioxyde de carbone, de la vapeur d'eau ou du protoxyde d'azote comme oxydant.
  4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que la durée, lors du maintien continu des pièces à usiner dans une atmosphère gazeuse ammoniacale ou dans une atmosphère gazeuse ammoniacale et contenant une substance cédant du carbone, est sélectionnée en fonction de l'épaisseur recherchée de la couche superficielle à enrichir.
  5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce que du dioxyde de carbone, du monoxyde de carbone ou des hydrocarbures sont utilisés individuellement ou mélangés comme substance cédant du carbone.
  6. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que les pièces à usiner sont refroidies à température ambiante dans une atmosphère gazeuse réductrice ou neutre, par exemple composée d'un gaz endothermique ou d'azote ou dans un liquide de trempe.
  7. Utilisation d'un dispositif pour la réalisation du procédé selon l'une quelconque des revendications 1 à 6, consistant en un four de traitement thermique avec un espace intérieur pouvant être chauffé et étanche aux gaz pour la nitruration ou la carbonitruration de pièces à usiner métalliques et en un dispositif pour l'adjonction dosée d'ammoniaque, d'une substance cédant du carbone et d'un oxydant.
EP00102359A 2000-02-04 2000-02-04 Procédé pour la nitruration et/ou carbonitruration d' acier fortement allié Expired - Lifetime EP1122331B1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
DE50001540T DE50001540D1 (de) 2000-02-04 2000-02-04 Verfahren zum Nitrieren und/oder Nitrocarburieren von höher legierten Stählen
EP00102359A EP1122331B1 (fr) 2000-02-04 2000-02-04 Procédé pour la nitruration et/ou carbonitruration d' acier fortement allié
AT00102359T ATE235581T1 (de) 2000-02-04 2000-02-04 Verfahren zum nitrieren und/oder nitrocarburieren von höher legierten stählen
US09/562,695 US6328819B1 (en) 2000-02-04 2000-04-28 Method and use of an apparatus for the thermal treatment, in particular nitriding treatment, of metal workpieces

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP00102359A EP1122331B1 (fr) 2000-02-04 2000-02-04 Procédé pour la nitruration et/ou carbonitruration d' acier fortement allié

Publications (2)

Publication Number Publication Date
EP1122331A1 EP1122331A1 (fr) 2001-08-08
EP1122331B1 true EP1122331B1 (fr) 2003-03-26

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EP00102359A Expired - Lifetime EP1122331B1 (fr) 2000-02-04 2000-02-04 Procédé pour la nitruration et/ou carbonitruration d' acier fortement allié

Country Status (4)

Country Link
US (1) US6328819B1 (fr)
EP (1) EP1122331B1 (fr)
AT (1) ATE235581T1 (fr)
DE (1) DE50001540D1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013226091A1 (de) 2013-12-16 2015-06-18 Robert Bosch Gmbh Zylindertrommel einer hydrostatischen Axialkolbenmaschine mit einer Verschleißschutzschicht
DE102013226090A1 (de) 2013-12-16 2015-06-18 Robert Bosch Gmbh Verfahren zum Gasnitrocarburieren
DE102016221891A1 (de) 2016-11-08 2018-05-09 Robert Bosch Gmbh Verfahren zur Wärmebehandlung eines aus einem hochlegierten Stahl bestehenden Werkstücks

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6929757B2 (en) * 2003-08-25 2005-08-16 General Motors Corporation Oxidation-resistant magnetorheological fluid
US7622197B2 (en) * 2006-11-20 2009-11-24 Ferroxy-Aled, Llc Seasoned ferrous cookware
ITMI20110366A1 (it) * 2011-03-10 2012-09-11 Sol Spa Procedimento per il trattamento di acciai.
RU2519356C2 (ru) * 2012-05-24 2014-06-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Московский автомобильно-дорожный государственный технический университет (МАДИ)" Способ циклического газового азотирования штампов из сталей для горячего деформирования
BR112014032480A2 (pt) * 2012-06-26 2017-06-27 Cavina Fulvio Fabrizio processo e instalação para o tratamento antioxidante de superfície de peças de aço
JP6930738B2 (ja) * 2018-08-03 2021-09-01 錦見鋳造株式会社 調理器具の製造方法
CN114174550A (zh) 2019-08-23 2022-03-11 医乐世医疗技术皮诺公司 用于牙植入物的表面硬化

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GB1351234A (en) * 1970-07-21 1974-04-24 Nissan Motor Process for forming a soft nitride layer in a metal surface
DD119822A1 (fr) * 1975-06-20 1976-05-12
JPS52138027A (en) * 1976-04-08 1977-11-17 Nissan Motor Ferrous member superior in initial fitting and wear resisting property and production process therefor
US4496401A (en) * 1981-10-15 1985-01-29 Lucas Industries Corrosion resistant steel components and method of manufacture thereof
FR2524006B1 (fr) * 1982-03-23 1985-10-11 Air Liquide Procede de durcissement superficiel de pieces metalliques
JPS60215756A (ja) * 1984-01-27 1985-10-29 プロセダイン　コ−ポレイシヨン ステンレス鋼の硬化方法
US5037491A (en) * 1986-02-28 1991-08-06 Fox Patrick L Shallow case hardening and corrosion inhibition process
DE3718240C1 (de) * 1987-05-30 1988-01-14 Ewald Schwing Verfahren zur Waermebehandlung von metallischen Werkstuecken in einer gasdurchstroemten Wirbelschicht
DE4339404A1 (de) * 1993-11-18 1995-05-24 Ipsen Ind Int Gmbh Verfahren zur Herstellung einheitlicher Oxidationsschichten auf metallischen Werkstücken und Vorrichtung zur Durchführung des Verfahrens

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013226091A1 (de) 2013-12-16 2015-06-18 Robert Bosch Gmbh Zylindertrommel einer hydrostatischen Axialkolbenmaschine mit einer Verschleißschutzschicht
DE102013226090A1 (de) 2013-12-16 2015-06-18 Robert Bosch Gmbh Verfahren zum Gasnitrocarburieren
US9970093B2 (en) 2013-12-16 2018-05-15 Robert Bosch Gmbh Method for gas carbonitriding
US10281042B2 (en) 2013-12-16 2019-05-07 Robert Bosch Gmbh Cylinder drum of a hydrostatic axial piston machine having a wear-resistant layer
DE102016221891A1 (de) 2016-11-08 2018-05-09 Robert Bosch Gmbh Verfahren zur Wärmebehandlung eines aus einem hochlegierten Stahl bestehenden Werkstücks
WO2018086930A1 (fr) 2016-11-08 2018-05-17 Robert Bosch Gmbh Procédé de traitement thermique d'une pièce à usiner constituée d'un acier fortement allié

Also Published As

Publication number Publication date
US6328819B1 (en) 2001-12-11
EP1122331A1 (fr) 2001-08-08
ATE235581T1 (de) 2003-04-15
DE50001540D1 (de) 2003-04-30

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