EP2536864A1 - Procédé de carbonitruration d'au moins un élément dans une chambre de traitement - Google Patents

Procédé de carbonitruration d'au moins un élément dans une chambre de traitement

Info

Publication number
EP2536864A1
EP2536864A1 EP11700010A EP11700010A EP2536864A1 EP 2536864 A1 EP2536864 A1 EP 2536864A1 EP 11700010 A EP11700010 A EP 11700010A EP 11700010 A EP11700010 A EP 11700010A EP 2536864 A1 EP2536864 A1 EP 2536864A1
Authority
EP
European Patent Office
Prior art keywords
gas
treatment chamber
carbonitriding
process gas
nitrogen
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
EP11700010A
Other languages
German (de)
English (en)
Other versions
EP2536864B1 (fr
Inventor
Jochen Schwarzer
Laszlo Hagymasi
Thomas Waldenmaier
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.)
Robert Bosch GmbH
Original Assignee
Robert Bosch GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Robert Bosch GmbH filed Critical Robert Bosch GmbH
Publication of EP2536864A1 publication Critical patent/EP2536864A1/fr
Application granted granted Critical
Publication of EP2536864B1 publication Critical patent/EP2536864B1/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • C23C8/06—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 according to the preamble of claim 1, and a treatment chamber and a control and / or regulating device according to the independent claims.
  • the process control in carbonitriding takes place in at least one
  • Treatment chamber by presetting pressure, temperature, time,
  • Carbonitriding can be a by-product of the carbon and Nitrogen donor gases form molecular hydrogen.
  • Hydrogen content can be determined by suitable sensors.
  • the sensors used must be suitable for use in low-pressure or
  • PNH3 pressure of ammonia
  • Nitrogen uptake constantly changes, which can be set at constant hold the nitriding index no consistent, reproducible carburizing and nitriding.
  • the progress of the gas decomposition or the onset of reactions takes place as a function of pressure, temperature and reactive or catalytically acting surface of the component batch or
  • Treatment chamber is thus the residence time of the gases in the chamber resulting from the flow rate. For this reason, in practice through complex test series
  • DE 101 18 494 C2 describes in one embodiment, a low-pressure carbonitriding with amounts of solid gas.
  • the inventive method has the advantage of being able to perform a uniform, reproducible carbonitriding by means of low-pressure carbonitriding regardless of a batch size or a furnace installation on at least one component located in the treatment chamber by means of a detection of a hydrogen content in a treatment chamber.
  • Nitrogen donor gas supply adjusted or regulated. This is based on the consideration that regardless of the structure of the component charge and / or the treatment chamber by means of the measured variable of the hydrogen content can be concluded on a carbon or nitrogen donor gas supply in the process gas atmosphere, so that building on the
  • Treatment chamber inflowing amount of the process gas in terms
  • the carbon or nitrogen uptake changes during the process time due to the already taken up carbon or nitrogen and because of the limited solubility of both elements in the metallic matrix of the surfaces of the components.
  • Nitrogen supply can be avoided, making it as efficient as possible
  • Argon rinsed to a simultaneous presence for example of To avoid carbon and nitrogen donor gas. This can prevent unwanted chemical reactions, such as the formation of cyanides.
  • the hydrogen content in the atmosphere of the treatment chamber detected during the process gas change can also be indirectly used as a measure of the proportions of the carbon or nitrogen donor gases. Will be at a
  • the process gas exchange is purged with an inert gas, it can be assumed that hydrogen concentrations of less than 5% by volume, desirably less than 1% by volume, mean that the concentrations of the carbon donor or nitrogen donor gases are sufficiently low to sufficiently reduce or avoid environmental damage. If the treatment chamber is evacuated in a process gas exchange, it is necessary a pressure in the processing chamber of at least less than 1 x10 "1 mbar, desirably less than 1 x10" to fall below 2 mbar, which can be assumed that the
  • Concentration of the carbon or nitrogen donor gases are sufficiently low in order to reduce or avoid environmental damage sufficiently.
  • the method is particularly easy to use when controlling a flow rate of the introduced into the treatment chamber process gas. For example, by an adjustable valve at an inlet of the
  • Treatment chamber the amount of the introduced process gas controlled and / or regulated.
  • the method provides that the process gas comprises a carbon donor gas.
  • This provides a first gas or a first gas composition for a process phase for the carbonitriding of components, with which the carbon fraction important for the carbonitriding is directly influenced, which allows a fast and precise control.
  • the carbon donor gas is a compound selected from a group consisting of acetylene, ethylene, propane, propene,
  • the process gas comprises a nitrogen donor gas.
  • the nitrogen donor gas is a compound selected from a group consisting of ammonia, nitrogen or
  • the method works particularly advantageous if at least two chemically different process gases act on the one component chemically in succession, and that between the gaseous process phases
  • Treatment chamber is at least partially evacuated.
  • Process phases successively act on the at least one component - for example, a carbon donor gas and a nitrogen donor gas - each specific chemical effects can be achieved with respect to the process. It makes sense not to mix these gas compositions when changing the process phases. By means of the at least partial evacuation of the treatment chamber, this can be achieved in a simple manner.
  • Process gases sequentially act on the component chemically, and that between the gaseous process phases, the treatment chamber is purged with an inert gas.
  • the change between two gaseous process phases can take place, whereby the pressure existing in the treatment chamber can essentially remain unchanged.
  • the method according to the invention makes it possible for the purging or the evacuation to be ended when the detected hydrogen content or the total pressure of the atmosphere falls below a predetermined threshold value.
  • the detection of the hydrogen content can also be used between the process phases to the effect of the evacuation or the
  • Treatment chamber itself, a radiator located therein, the atmosphere and / or the supplied process gas to be heated or heated.
  • Figure 1 is a schematic representation of a treatment chamber for
  • FIG. 2 shows a time diagram of a low-pressure carbonitriding process with a representation of process phases and process temperatures
  • FIG. 1 shows a schematic representation of a system 10 for low-pressure carbonitriding of metallic components 12, which are arranged on a support 14 in a treatment chamber 16.
  • the components 12 can be heated by means of a heater 18 located in the lower area of the drawing.
  • a first inlet 20 and a second inlet 22 with associated flow control valves 24 and 26 allow introduction of carbon donor gas 28 and nitrogen donor gas 30.
  • a temperature sensor 32, a pressure sensor 34, and a low pressure carbonitride suitable hydrogen sensor 36 are shown in the drawing at the top of FIG.
  • Treatment chamber 16 is arranged.
  • a control and / or regulating device 38 shown above assumes, among other things, that of the
  • Hydrogen sensor 36 detected hydrogen content 44 regulated.
  • FIG. 2 shows a time diagram of a process control of a low-pressure carbonitriding, which is used, for example, in the plant 10 shown in FIG.
  • the time t is plotted on the abscissa of the diagram and the temperature T of the atmosphere 46 is plotted on the ordinate.
  • a curve 48 shows the time profile of the temperature T.
  • Carbonitriding involves a heating phase A, a
  • Temperature equalization phase B three nitriding phases C1, C2 and C3, three carburizing phases D1, D2 and D3, four process gas change phases E1, E2, E3 and E4, and a diffusion phase F and a cooling phase G.
  • Two interruptions 50 indicate that the process phases shown do not each drawn durations must have, but can also deviate arbitrarily from the representation of Figure 2.
  • Reference numerals E1 to E4 process gas exchange phases shown is that the detected hydrogen content 44 during the process gas exchange phases E1 to E4 for monitoring and thus reducing or avoiding unwanted reaction products, such as cyanides, is used, with no process gas is supplied and no process gas exchange takes place.
  • the process or method can be interrupted to a Reduce or eliminate environmental hazards.
  • the hydrogen content 44 is detected by the hydrogen sensor 36 and used for process control throughout the illustrated period of Figure 2.
  • FIG. 2 shows that, during the heating phase A, the temperature T is increased continuously up to a treatment temperature of about 950 ° C. with an approximately constant heating rate.
  • the temperature T is in an optimum range of 750 ° C to 1050 ° C for the present application.
  • Temperature equalization phase B the treatment temperature is kept constant at about 950 ° C. During the heating phase A and the temperature equalizing phase B, neither a nitrogen donor gas 30 nor a carbon donor gas 28 is supplied.
  • a nitrogen donor gas 30 for example
  • Ammonia fed with a nitrogen donor gas partial pressure of about 50 mbar. This can be seen on the right vertical axis of the diagram of Figure 2.
  • a first process gas change E1 in which the treatment chamber 16 is evacuated or filled with an inert gas, e.g.
  • the total pressure of the treatment chamber 16 or the detected hydrogen fraction 44 is used to monitor the remaining portion of the nitrogen donor gas 30 from the nitriding C1 phase to environmentally hazardous
  • Process gas exchange phase E1 evacuated and the total pressure of
  • Treatment chamber 16 is less than 1 x 10 "1 mbar, ideally less than 1 x 10 " 2 mbar, the carburization phase D1 can begin. Otherwise, a
  • the first process gas change E1 is followed by a carburizing phase D1 with a partial pressure of the carbon donor gas 28 of about 10 mbar.
  • Treatment chamber 16 evacuated or alternatively with an inert gas, e.g.
  • treatment temperature 950 ° C is no longer maintained and carried out a rapid cooling in the cooling phase G to room temperature to adjust the desired structural composition of the metallic components 12.
  • Threshold 45 for the hydrogen content 44 After the carburizing phase D and before the nitriding phase C, a process gas exchange phase E takes place.
  • carbon donor gas 28 is introduced into the treatment chamber 16. Due to the decay of the
  • Flow control valve 24 is set or regulated. This is shown in FIG. 3 by an arrow 51.
  • a region 55 for the hydrogen portion 44 provided in FIG. 3 extends between 60% by volume and 70% by volume.
  • nitrogen donor gas 30 is introduced into the
  • the treatment chamber 16 is either evacuated or rinsed with a suitable inert gas.

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)

Abstract

L'invention concerne un procédé de carbonitruration d'au moins un élément (12) dans une chambre de traitement (16), procédé selon lequel au moins un gaz de traitement (28 ; 30) est introduit dans la chambre de traitement (16), une teneur en hydrogène (44) étant détectée dans une atmosphère (46) obtenue dans la chambre de traitement (16) et maintenue au moins temporairement dans une plage souhaitée (55 ; 57) par l'influence de la quantité de gaz de traitement (28 ; 30) introduite.
EP11700010.9A 2010-02-15 2011-01-03 Procédé de carbonitruration d'au moins un élément dans une chambre de traitement Active EP2536864B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102010001936A DE102010001936A1 (de) 2010-02-15 2010-02-15 Verfahren zur Carbonitrierung mindestens eines Bauteils in einer Behandlungskammer
PCT/EP2011/050025 WO2011098306A1 (fr) 2010-02-15 2011-01-03 Procédé de carbonitruration d'au moins un élément dans une chambre de traitement

Publications (2)

Publication Number Publication Date
EP2536864A1 true EP2536864A1 (fr) 2012-12-26
EP2536864B1 EP2536864B1 (fr) 2017-03-15

Family

ID=43533446

Family Applications (1)

Application Number Title Priority Date Filing Date
EP11700010.9A Active EP2536864B1 (fr) 2010-02-15 2011-01-03 Procédé de carbonitruration d'au moins un élément dans une chambre de traitement

Country Status (6)

Country Link
US (1) US9399811B2 (fr)
EP (1) EP2536864B1 (fr)
CN (1) CN102762760B (fr)
BR (1) BR112012020154A2 (fr)
DE (1) DE102010001936A1 (fr)
WO (1) WO2011098306A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102012212918A1 (de) * 2012-07-24 2014-01-30 Karlsruher Institut für Technologie Verfahren zur Herstellung mindestens eines Bauteils und Steuer- und/oder Regeleinrichtung
FR3029938B1 (fr) * 2014-12-11 2019-04-26 Ecm Technologies Procede et four de carbonitruration a basse pression
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
AT524143B1 (de) 2020-09-10 2022-12-15 Miba Sinter Austria Gmbh Verfahren zur Härtung eines Sinterbauteils

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DE3937699A1 (de) * 1989-11-13 1991-05-16 Thaelmann Schwermaschbau Veb Verfahren zum herstellen von (epsilon)-karbonitridschichten definierter zusammensetzung
US5273585A (en) * 1990-03-27 1993-12-28 Mazda Motor Corporation Heat-treating apparatus
DE4211395B4 (de) * 1992-04-04 2004-04-08 Process-Electronic Analyse- und Regelgeräte GmbH Verfahren zum Nitrocarburieren oder Carbonitrieren von Werkstücken und Ofen hierzu
DE19644051C2 (de) * 1996-10-31 2000-09-28 Moebius Hans Heinrich Verfahren und Einrichtung zur Überwachung und Kennwert-Bestimmung von Gasmischungen bei Nitrocarburier- und Nitrier-Prozessen in der Härtereitechnik
EP0909951B1 (fr) * 1997-10-07 2001-02-28 Ipsen International GmbH Méthode et dispositif pour la détermination quantitiv de hydrogène lié et/ou libre
DE19909694A1 (de) 1999-03-05 2000-09-14 Stiftung Inst Fuer Werkstoffte Verfahren zum Varbonitrieren bei Unterdruckverfahren ohne Plasmaunterstützung
DE10003526A1 (de) * 2000-01-27 2001-08-09 Messer Griesheim Gmbh Frankfur Verfahren zum Karbonitrieren von kohlenstoffreichen und hochlegierten Stählen
JP3531736B2 (ja) * 2001-01-19 2004-05-31 オリエンタルエンヂニアリング株式会社 浸炭方法及び浸炭装置
DE10118494C2 (de) 2001-04-04 2003-12-11 Aichelin Gesmbh Moedling Verfahren zur Niederdruck-Carbonitrierung von Stahlteilen
AU2002218508A1 (en) * 2001-11-30 2003-06-17 Koyo Thermo Systems Co., Ltd. Method and apparatus for vacuum heat treatment
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
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Also Published As

Publication number Publication date
US20130037173A1 (en) 2013-02-14
DE102010001936A1 (de) 2011-08-18
US9399811B2 (en) 2016-07-26
BR112012020154A2 (pt) 2020-11-03
CN102762760A (zh) 2012-10-31
EP2536864B1 (fr) 2017-03-15
CN102762760B (zh) 2015-12-02
WO2011098306A1 (fr) 2011-08-18

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