EP0545069A1 - Procédé de traitement d'aciers et de métaux réfractaires - Google Patents

Procédé de traitement d'aciers et de métaux réfractaires Download PDF

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Publication number
EP0545069A1
EP0545069A1 EP19920118403 EP92118403A EP0545069A1 EP 0545069 A1 EP0545069 A1 EP 0545069A1 EP 19920118403 EP19920118403 EP 19920118403 EP 92118403 A EP92118403 A EP 92118403A EP 0545069 A1 EP0545069 A1 EP 0545069A1
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EP
European Patent Office
Prior art keywords
chamber
pressure
temperature
bar
treatment
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.)
Granted
Application number
EP19920118403
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German (de)
English (en)
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EP0545069B1 (fr
Inventor
Albrecht Dr. Melber
Peter Dr. Minarski
Friedrich Dr. Preisser
Klaus Dr. Zimmermann
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.)
Leybold Durferrit GmbH
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Leybold Durferrit GmbH
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Publication date
Priority claimed from DE4139975A external-priority patent/DE4139975C2/de
Application filed by Leybold Durferrit GmbH filed Critical Leybold Durferrit GmbH
Publication of EP0545069A1 publication Critical patent/EP0545069A1/fr
Application granted granted Critical
Publication of EP0545069B1 publication Critical patent/EP0545069B1/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
    • C23C8/02—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
    • C23C8/80—After-treatment

Definitions

  • the invention relates to a process for the treatment of steels and metals, in particular for the passivation and for the subsequent thermochemical surface treatment or for the thermochemical surface treatment and a subsequent thermochemical aftertreatment in a process chamber under the action of pressure and temperature.
  • thermochemical surface treatment e.g. nitriding, nitro-carburizing or boriding
  • refractory metals e.g. Ti, Zr, Mo, W. Nb, Ta, V
  • the passive layers exist namely mostly made of oxides and form a thin protective skin, which prevent the undisturbed diffusion of non-metals such as N, C, and B during the surface treatment. This completely prevents diffusion, for example, in the case of refractory metals, and in some cases in the case of high-alloy steels, which leads to uneven treatment results.
  • pre-oxidation is carried out to achieve a uniform treatment result. This means that impurities on the surfaces are oxidized and the already existing oxide layer is influenced. In some cases, this can influence the uniformity of the layer formation.
  • the layers produced are very thin and contain ever larger amounts of oxygen.
  • thermochemical surface treatment of metals e.g. carburizing, tempering, annealing, carbonitriding, nitrocarburizing
  • edge oxidation This edge oxidation reduces the fatigue strength, so that the life of edge-oxidized components is reduced.
  • Components that have oxidation after heat treatment are therefore usually post-treated with mechanical processing with the aim of removing the oxidation (e.g. grinding gear wheels).
  • the drop in fatigue strength due to edge oxidation can also be compensated for by means of solidification processes (e.g. shot peening of gear wheels) of the components.
  • thermochemical surface treatment a heat treatment process is carried out in which the intercrystalline oxidation of metals is removed.
  • a first gas or gas mixture from the group N2, H2 or NH3 is let into a process chamber for de-passivation, a pressure greater than 1 bar a and a temperature between 100 ° C and 1,000 ° C independently of one another in the chamber and in a second process step, a second gas or gas mixture from the group of N-, C- or B-containing gases for thermochemical surface treatment is let into a process chamber and a temperature between 100 ° C and 1,000 ° C at a pressure greater than or equal to 1 bar a.
  • the de-passivation of alloyed steels and refractory metals is advantageously carried out by heat treatment in gas mixtures containing, for example, NH3 and / or H2, at temperatures between 100 and 1,000 ° C and pressures greater than 1 bar, whereby the disruptive oxide skin is reduced and the pure metal or the alloy is coated with a thin nitride layer as protection against renewed oxidation.
  • gas mixtures containing, for example, NH3 and / or H2
  • the disruptive oxide skin is reduced and the pure metal or the alloy is coated with a thin nitride layer as protection against renewed oxidation.
  • thermochemical removal of the oxides takes place in gas mixtures containing NH3, H2 and N2, at temperatures between 100 ° C and 1,000 ° C and pressures greater than 1 bar a.
  • the oxides are reduced by reacting with the gas phase and releasing their oxygen atoms or forming nitrides.
  • parts heat-treated in this way can be almost completely deoxidized.
  • Such a heat treatment can be carried out for higher alloyed steels as a replacement for the tempering treatment which is to be carried out anyway, tempering and deoxidizing are then carried out in one step.
  • This method makes it possible to continue to carry out thermochemical treatments with oxidizing gas components and to achieve higher fatigue properties on the components through the subsequent deoxidation. As a result, the use of expensive and complicated mechanical post-treatments can be dispensed with.
  • a refractory metal for example Ti
  • a treatment chamber 1 FIG. 1
  • NH3 is let into the chamber and the passivated titanium is reduced at a pressure of 10 bar a.
  • a gas change takes place in the chamber.
  • NH3 is exchanged for N2 and at a constant temperature the second process step begins, namely the thermochemical treatment.
  • This nitriding process is carried out at 30 bar a process pressure.
  • the treatment time is usually two to four hours and depends on the desired nitride layer thickness.
  • the desired TiN coating is obtained as the end product after the second process step.
  • a second system configuration is also conceivable, which consists of a combination of two different treatment chambers 1 and 2 (FIG. 2). This is used e.g. in the treatment of bulk steels, such as a high-alloy steel X 20 CrMoV 12 1.
  • the steel After the steel has been introduced into the treatment chamber 1, it is heated to 580 ° C and at a pressure of e.g. 10 bar a H2 and / or NH3 is let in.
  • a pressure of e.g. 10 bar a H2 and / or NH3 is let in.
  • the steel used is de-passivated and at the same time provided with a thin nitride layer as protection against further oxidation.
  • the steel which is protected against oxidation, is then brought into a second treatment chamber 2.
  • a material-specific nitriding temperature of 550 ° C is set and at a pressure of 1 bar a a gas mixture of NH3, H2 is let in.
  • a nitrided X 20 CrMo V 12 1 steel is obtained as the end product.
  • carbon-containing gases such as CO2 or CO can be used for coal at temperatures between 800 ° C and 1,000 ° C.
  • thermochemical treatment process for example nitriding
  • a pressure chamber which, as shown in FIG. 1, must be designed, for example, for 30 bar a.
  • 16 MnCr5 steel free of edge oxidation is obtained.

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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)
  • Treatment Of Steel In Its Molten State (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Furnace Details (AREA)
EP92118403A 1991-12-04 1992-10-27 Procédé de traitement d'aciers et de métaux réfractaires Expired - Lifetime EP0545069B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE4139975A DE4139975C2 (de) 1991-12-04 1991-12-04 Verfahren zur Behandlung von legierten Stählen und Refraktärmetallen und Anwendung des Verfahrens
DE4139975 1991-12-04
DE4208848 1992-03-19
DE4208848A DE4208848C2 (de) 1991-12-04 1992-03-19 Verfahren zur thermochemischen Nachbehandlung von Stählen und Metallen

Publications (2)

Publication Number Publication Date
EP0545069A1 true EP0545069A1 (fr) 1993-06-09
EP0545069B1 EP0545069B1 (fr) 1995-12-06

Family

ID=25909771

Family Applications (1)

Application Number Title Priority Date Filing Date
EP92118403A Expired - Lifetime EP0545069B1 (fr) 1991-12-04 1992-10-27 Procédé de traitement d'aciers et de métaux réfractaires

Country Status (5)

Country Link
EP (1) EP0545069B1 (fr)
JP (1) JPH0665631A (fr)
AT (1) ATE131216T1 (fr)
DE (2) DE4208848C2 (fr)
ES (1) ES2080416T3 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2719057A1 (fr) * 1994-04-22 1995-10-27 Innovatique Sa Procédé pour la nitruration à bsase pression d'une pièce métallique et four pour la mise en Óoeuvre dudit procédé.
WO1995029269A1 (fr) * 1994-04-22 1995-11-02 Innovatique S.A. Procede pour la nitruration a basse pression d'une piece metallique et four pour la mise en ×uvre dudit procede
WO2003027349A2 (fr) * 2001-09-25 2003-04-03 Robert Bosch Gmbh Procede de traitement thermique de pieces en aciers resistants a la temperature
WO2004040033A1 (fr) * 2002-10-31 2004-05-13 Seco/Warwick Sp. Z O.O. Procede de cementation par sous-pression de pieces d'acier
EP2430210B1 (fr) * 2009-05-11 2018-01-24 Robert Bosch GmbH Procédé de carbonitruration

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2851387A (en) * 1957-05-08 1958-09-09 Chapman Valve Mfg Co Method of depassifying high chromium steels prior to nitriding
DE1933439A1 (de) * 1968-07-01 1970-01-15 Gen Electric Nitrierverfahren
GB1495703A (en) * 1973-12-12 1977-12-21 Gkn Group Services Ltd Nitriding of ferrous metals
EP0105835A1 (fr) * 1982-09-07 1984-04-18 Vereinigte Drahtwerke AG Procédé de production d'une couche dure sur des pièces en Ti ou alliages de Ti
EP0242089A1 (fr) * 1986-04-10 1987-10-21 LUCAS INDUSTRIES public limited company Procédé pour augmenter la résistance à l'usure de la surface d'un composant métallique
EP0408168A1 (fr) * 1989-07-10 1991-01-16 Daidousanso Co., Ltd. Procédé pour le prétraitement préalable de matériaux métalliques et procédé pour la nitruration d'acier

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE738244C (de) * 1939-02-02 1943-08-07 Messerschmitt Boelkow Blohm Verfahren und Einrichtung zum Nitrieren von Staehlen
DE2510460A1 (de) * 1975-03-11 1976-09-23 Ipsen Ind Int Gmbh Verfahren zur waermebehandlung von werkstuecken aus stahl ohne die bildung von randoxyden der legierungselemente
PL192437A1 (pl) * 1976-09-16 1978-03-28 Inst Mech Precyz Sposob obrobki cieplno-chemicznej metali
JP2732403B2 (ja) * 1988-10-27 1998-03-30 財団法人応用科学研究所 難窒化金属材料のアンモニアガス窒化処理方法
DE4139975C2 (de) * 1991-12-04 2001-02-22 Ald Vacuum Techn Ag Verfahren zur Behandlung von legierten Stählen und Refraktärmetallen und Anwendung des Verfahrens

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2851387A (en) * 1957-05-08 1958-09-09 Chapman Valve Mfg Co Method of depassifying high chromium steels prior to nitriding
DE1933439A1 (de) * 1968-07-01 1970-01-15 Gen Electric Nitrierverfahren
GB1495703A (en) * 1973-12-12 1977-12-21 Gkn Group Services Ltd Nitriding of ferrous metals
EP0105835A1 (fr) * 1982-09-07 1984-04-18 Vereinigte Drahtwerke AG Procédé de production d'une couche dure sur des pièces en Ti ou alliages de Ti
EP0242089A1 (fr) * 1986-04-10 1987-10-21 LUCAS INDUSTRIES public limited company Procédé pour augmenter la résistance à l'usure de la surface d'un composant métallique
EP0408168A1 (fr) * 1989-07-10 1991-01-16 Daidousanso Co., Ltd. Procédé pour le prétraitement préalable de matériaux métalliques et procédé pour la nitruration d'acier

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 6, no. 78 (C-102)(956) 15. Mai 1982 & JP-A-57 13 171 ( KAWASAKI JUKOGYO K.K. ) 23. Januar 1982 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2719057A1 (fr) * 1994-04-22 1995-10-27 Innovatique Sa Procédé pour la nitruration à bsase pression d'une pièce métallique et four pour la mise en Óoeuvre dudit procédé.
WO1995029269A1 (fr) * 1994-04-22 1995-11-02 Innovatique S.A. Procede pour la nitruration a basse pression d'une piece metallique et four pour la mise en ×uvre dudit procede
WO2003027349A2 (fr) * 2001-09-25 2003-04-03 Robert Bosch Gmbh Procede de traitement thermique de pieces en aciers resistants a la temperature
WO2003027349A3 (fr) * 2001-09-25 2003-12-04 Bosch Gmbh Robert Procede de traitement thermique de pieces en aciers resistants a la temperature
US7108756B2 (en) 2001-09-25 2006-09-19 Robert Bosch Gmbh Method for heat-treating work pieces made of temperature-resistant steels
WO2004040033A1 (fr) * 2002-10-31 2004-05-13 Seco/Warwick Sp. Z O.O. Procede de cementation par sous-pression de pieces d'acier
EP2430210B1 (fr) * 2009-05-11 2018-01-24 Robert Bosch GmbH Procédé de carbonitruration

Also Published As

Publication number Publication date
JPH0665631A (ja) 1994-03-08
ATE131216T1 (de) 1995-12-15
EP0545069B1 (fr) 1995-12-06
DE59204598D1 (de) 1996-01-18
ES2080416T3 (es) 1996-02-01
DE4208848C2 (de) 2001-08-30
DE4208848A1 (de) 1993-09-23

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