EP1537252B1 - Procede et dispositif de carburation en depression - Google Patents

Procede et dispositif de carburation en depression Download PDF

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Publication number
EP1537252B1
EP1537252B1 EP03747994A EP03747994A EP1537252B1 EP 1537252 B1 EP1537252 B1 EP 1537252B1 EP 03747994 A EP03747994 A EP 03747994A EP 03747994 A EP03747994 A EP 03747994A EP 1537252 B1 EP1537252 B1 EP 1537252B1
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EP
European Patent Office
Prior art keywords
treatment
treatment chamber
hydrocarbonous
gas
chamber
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
EP03747994A
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German (de)
English (en)
Other versions
EP1537252A2 (fr
Inventor
Alexander Di Jurmann
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.)
Linde GmbH
Original Assignee
Linde GmbH
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Publication date
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Publication of EP1537252A2 publication Critical patent/EP1537252A2/fr
Application granted granted Critical
Publication of EP1537252B1 publication Critical patent/EP1537252B1/fr
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C8/00Solid 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
    • C23C8/06Solid 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
    • C23C8/08Solid 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
    • C23C8/20Carburising

Definitions

  • the invention relates to a method for carburizing at subatmospheric pressures, wherein a treatment chamber is at least temporarily supplied with a hydrocarbon-containing treatment gas and an exhaust gas stream is withdrawn from the treatment chamber by means of at least one vacuum pump.
  • the invention relates to a device for carburizing at subatmospheric pressures, comprising at least one treatment chamber, at least one supply line, over which the treatment space is at least temporarily supplied a hydrocarbon-containing treatment gas, and at least one pumping line, via which the exhaust gas flow by means of a pumping out of the treatment room is deducted.
  • the reason for this is based on the fact that it can lead to the uncontrolled decomposition of excess hydrocarbons in the supply of a predetermined amount and composition of or a hydrocarbon-containing treatment gas in the treatment room. Furthermore, the calculated hydrocarbon requirement may be too low, resulting in erroneous calculations in the carbon transition and carbon evolution calculations.
  • a disadvantage of the prior art method is furthermore that in the calculation of the transferred carbon is always based on the theoretical composition of the hydrocarbon-containing treatment gas used. This means, for example, that when using propane as the hydrocarbon-containing treatment gas of the composition C 3 H 8 is assumed. When using technical propane, however, only the calorific value, but not the exact composition is guaranteed. The sum of the carbon in the technical propane is therefore not identical to the theoretical C content of pure propane, which is taken into account in the calculation of the transferred carbon quantity. This also results in errors in the calculation result.
  • Object of the present invention is to provide a generic method and a generic device for carburizing at subatmospheric pressures, which avoids the aforementioned disadvantages.
  • a reference sample or a reference body which has a defined carbon surface or carbonatable surface is introduced into the treatment space.
  • Gravimetric methods for determining mass transfer values are known in principle to the person skilled in the art by means of a weighing process of the reference body or the reference sample
  • the mass flow of the hydrocarbon-containing treatment gas supplied to the treatment space can be determined.
  • C P stands for the maximum possible C content, whereby the soot limit is defined.
  • C P is always a function of temperature in non-equilibrium atmospheres, while C r is the actual carbon content of the reference sample.
  • the sum (C P -C r ) thus represents the distance to the carbide or soot boundary.
  • a process-typical correction factor may need to be determined and integrated into the measuring system.
  • the reference sample or the reference body used may consist of pure iron and art or melt-like material. Those parts of the reference body which are not to be carburized can be protected, for example, by copper plating. When realizing the method according to the invention, the reference body must either be abraded after each treatment or exchanged for a non-carburized reference body.
  • an evacuable weighing chamber in which a weighing cell is arranged, is assigned to the treatment space.
  • a lock for the purpose of entering and removing the reference body in or out of the treatment room.
  • the figure shows a treatment chamber 3, shown only schematically, to which the hydrocarbon-containing treatment gas is supplied via a feed line 1.
  • the hydrocarbon-containing treatment gases used are preferably alkanes, alkenes, alkynes, derivatives of the abovementioned, if appropriate in combination with hydrogen and / or nitrogen.
  • the desired subatmospheric pressure in the treatment space 3 is set via the pumping line 7, in which a vacuum pump 8 is arranged.
  • work is carried out predominantly at pressures of up to 20 mbar, preferably at pressures of between 3 and 20 mbar
  • an evacuable weighing chamber 4 is now assigned to the treatment chamber 3.
  • a weighing cell 5 is arranged.
  • Means are provided by means of which the reference sample or the reference body 6 can be introduced into the treatment space 3. After completion of the carburization process of the reference sample or the reference body 6, this or this is weighed in the load cell 5 and determined in this way the carbon mass flow.
  • the reference sample 6 is preferably designed as a solid sample which can be carburized at least on one side and has a defined area and with a defined initial carbon content.
  • the weighing cell 5 is connected via a data line 10 to an evaluation unit 9, which preferably comprises a diffusion computer.
  • the evaluation unit 9 in turn is connected via a data line 11 with a arranged in the supply line 1 valve 2, which is preferably a control valve, in conjunction.
  • valve 2 is now actuated via the evaluation unit 9, so that regulation of the hydrocarbon-containing treatment gas supplied to the treatment chamber 3 via the supply line 1 can be effected as a function of the determined mass flow.
  • the invention thus allows a continuous or discontinuous control of the treatment chamber 1 supplied to the hydrocarbon-containing treatment gas 1.
  • the supply of hydrocarbon-containing treatment gas into the treatment room is thus controlled, thereby uncontrolled decomposition of excess hydrocarbons in the treatment chamber and the Abpumptechnisch and thus a Soot and tar formation can be effectively avoided.
  • a large part of the unwanted deposits within the treatment chamber, on the material to be treated in the treatment chamber or in the pumping line is reliably avoided by the method according to the invention or by the device according to the invention.

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)
  • Vehicle Body Suspensions (AREA)
  • Chemical Vapour Deposition (AREA)
  • Devices That Are Associated With Refrigeration Equipment (AREA)

Claims (7)

  1. Procédé en vue de la carburation à des pressions sous-atmosphériques, un gaz de traitement contenant des hydrocarbures étant alimenté au moins pendant une partie du temps à une chambre de traitement, et un courant de gaz de rejet étant évacué à l'aide d'au moins une pompe à ride hors de la chambre de traitement, caractérisé
    - en ce que l'on introduit, dans la chambre de traitement (3), un échantillon de référence (6), qui présente une surface de carburation définie,
    - en ce que l'on détermine, à l'aide d'un processus de pesée de l'échantillon de référence (6), le courant massique du gaz de traitement contenant des hydrocarbures (1) et
    - en ce que l'on règle, en fonction du courant massique déterminé, l'apport du gaz' de traitement contenant des hydrocarbures (1) dans la chambre de traitement (3).
  2. Procédé selon la revendication 1, caractérisé en ce que l'on règle, dans la chambre de traitement (3), une pression comprise entre 3 et 20 mbars.
  3. Procédé selon la revendication 1, caractérisé en ce que l'on utilise, en tant que gaz de traitement contenant des hydrocarbures (1), des alcanes, des alcènes, des alcynes ou des dérivés des produits susnommés, auxquels est mélangé de l'hydrogène et/ou de l'azote.
  4. Dispositif en vue de la carburation à des pressions sous-atmosphériques, présentant au moins une chambre de traitement, au moins un conduit d'apport, grâce auquel l'on alimente, au moins pendant une partie du temps à la chambre de traitement (3), un gaz de traitement contenant des hydrocarbures (1), et au moins un conduit de pompage, grâce auquel l'on évacue, hors de la chambre de traitement, un courant de gaz de rejet, à l'aide d'un dispositif de pompage, caractérisé
    - en ce que l'on attribue à la chambre de traitement (3) une chambre de pesée pouvant être évacuée (4), dans laquelle est disposée une cellule de pesée (5),
    - en ce que l'on prévoit des moyens en vue de l'introduction d'un échantillon de référence (6), qui présente une surface de carburation définie dans la chambre de traitement (3),,
    - en ce que l'on dispose, dans le conduit d'apport (1), au moins une vanne (2),
    - en ce que l'on prévoit une unité d'évaluation (9), qui règle par une commande de la vanne (2) en fonction du courant massique déterminé à l'aide de l'échantillon de référence (6),
    - l'apport du gaz de traitement contenant des hydrocarbures (1) dans la chambre de traitement (3).
  5. Dispositif selon la revendication 4, caractérisé en ce que la vanne (2) est une vanne de réglage.
  6. Dispositif selon la revendication 4 ou 5, caractérisé en ce que l'échantillon de référence (6) est formé en tant qu'échantillon massif, capable de carburation au moins sur une face, ayant une surface définie et une teneur définie en carbone initial.
  7. Dispositif selon l'une quelconque des revendications 4 à 6, caractérisé en ce que l'unité d'évaluation (9) comprend un ordinateur de diffusion.
EP03747994A 2002-09-13 2003-09-09 Procede et dispositif de carburation en depression Expired - Lifetime EP1537252B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10242616A DE10242616A1 (de) 2002-09-13 2002-09-13 Verfahren und Vorrichtung zum Unterdruckaufkohlen
DE10242616 2002-09-13
PCT/EP2003/010014 WO2004031432A2 (fr) 2002-09-13 2003-09-09 Procede et dispositif de carburation en depression

Publications (2)

Publication Number Publication Date
EP1537252A2 EP1537252A2 (fr) 2005-06-08
EP1537252B1 true EP1537252B1 (fr) 2006-01-18

Family

ID=31895964

Family Applications (1)

Application Number Title Priority Date Filing Date
EP03747994A Expired - Lifetime EP1537252B1 (fr) 2002-09-13 2003-09-09 Procede et dispositif de carburation en depression

Country Status (5)

Country Link
EP (1) EP1537252B1 (fr)
AT (1) ATE316161T1 (fr)
AU (1) AU2003267331A1 (fr)
DE (2) DE10242616A1 (fr)
WO (1) WO2004031432A2 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
PL210958B1 (pl) * 2007-04-02 2012-03-30 Seco Warwick Społka Akcyjna Sposób i układ kontrolno-pomiarowy do kontroli aktywnej powierzchni wsadu w procesie nawęglania w podciśnieniu
US9212416B2 (en) 2009-08-07 2015-12-15 Swagelok Company Low temperature carburization under soft vacuum
AU2013210034A1 (en) 2012-01-20 2014-09-11 Swagelok Company Concurrent flow of activating gas in low temperature carburization

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5064620A (en) * 1989-06-01 1991-11-12 Pierre Beuret Probe for measuring carbon flux

Also Published As

Publication number Publication date
DE10242616A1 (de) 2004-03-25
WO2004031432A3 (fr) 2004-12-29
AU2003267331A1 (en) 2004-04-23
DE50302246D1 (de) 2006-04-06
AU2003267331A8 (en) 2004-04-23
EP1537252A2 (fr) 2005-06-08
WO2004031432A2 (fr) 2004-04-15
ATE316161T1 (de) 2006-02-15

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