WO2004031432A2 - Procede et dispositif de carburation en depression - Google Patents

Procede et dispositif de carburation en depression Download PDF

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Publication number
WO2004031432A2
WO2004031432A2 PCT/EP2003/010014 EP0310014W WO2004031432A2 WO 2004031432 A2 WO2004031432 A2 WO 2004031432A2 EP 0310014 W EP0310014 W EP 0310014W WO 2004031432 A2 WO2004031432 A2 WO 2004031432A2
Authority
WO
WIPO (PCT)
Prior art keywords
treatment room
hydrocarbon
treatment
reference sample
room
Prior art date
Application number
PCT/EP2003/010014
Other languages
German (de)
English (en)
Other versions
WO2004031432A3 (fr
Inventor
Alexander Jurmann
Original Assignee
Linde Aktiengesellschaft
Jurmann, Susanne
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 Linde Aktiengesellschaft, Jurmann, Susanne filed Critical Linde Aktiengesellschaft
Priority to DE50302246T priority Critical patent/DE50302246D1/de
Priority to EP03747994A priority patent/EP1537252B1/fr
Priority to AU2003267331A priority patent/AU2003267331A1/en
Publication of WO2004031432A2 publication Critical patent/WO2004031432A2/fr
Publication of WO2004031432A3 publication Critical patent/WO2004031432A3/fr

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
    • C23C8/08—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
    • C23C8/20—Carburising

Definitions

  • the invention relates to a method for carburizing at subatmospheric pressures, wherein a treatment gas containing hydrocarbon is at least temporarily supplied to a treatment room and an exhaust gas stream is withdrawn from the treatment room by means of at least one vacuum pump.
  • the invention relates to a device for carburizing at subatmospheric pressures, comprising at least one treatment room, at least one feed line, via which the treatment room at least temporarily
  • Hydrocarbon-containing treatment gas is supplied, and at least one pumping line, via which the exhaust gas stream is withdrawn from the treatment room by means of a pumping device.
  • a disadvantage of the methods belonging to the prior art is furthermore that the calculation of the transferred carbon always starts from the theoretical composition of the hydrocarbon-containing treatment gas used. This means, for example, that the composition C 3 H 8 is used when propane is used as the hydrocarbon-containing treatment gas. When using technical propane, however, only "the calorific value is guaranteed, but not the exact composition. The sum of carbon in technical propane is therefore not identical to the theoretical C content of pure propane, which is taken into account when calculating the amount of carbon transferred This also results in errors in the calculation result.
  • the 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.
  • this object is achieved in that a reference sample, which has a defined carburizing surface, is introduced into the treatment room, by means of a weighing process of the reference sample
  • Hydrocarbon-containing treatment gas is determined and the supply of the hydrocarbon-containing treatment gas into the treatment room is regulated as a function of the mass flow determined.
  • the object is achieved in that the treatment room is assigned an evacuable weighing room in which a weighing cell is arranged,
  • Means for introducing a reference sample, which has a defined carburizing surface ' , are provided in the treatment room, at least one valve is arranged in the feed line, an evaluation unit is provided which, depending on the mass flow of the hydrocarbon-containing treatment gas determined by means of the reference sample, the feed of hydrocarbon-containing Treating treatment gas in the treatment room by controlling the valve.
  • a reference sample or a reference body which has a defined carburizing surface or carburable surface, is now introduced into the treatment room.
  • Gravimetric methods for determining mass transfer values are known in principle to the person skilled in the art.
  • the mass flow of the hydrocarbon-containing treatment gas, which is supplied to the treatment room, can be determined by means of a weighing process of the reference body or the reference sample.
  • the factor ß can be determined with known mass flow and assumed potential difference - for example 10% below the carbide and soot limit.
  • variable C P stands for the maximum possible C content, which means that the
  • Soot limit is defined.
  • C P is always a function of temperature in imbalance atmospheres, while C r stands for the current carbon content of the reference sample.
  • the sum (C P -C r ) thus represents the distance to the carbide or soot limit.
  • a process-typical correction factor may have to be determined and integrated into the measurement system.
  • the reference sample used or the reference body used can consist of pure iron and of the same type or of the same material. Those parts of the reference body that are not to be carburized can be protected from them, for example, by copper plating. When implementing the method according to the invention, the reference body must either be ground down after each treatment or exchanged for a non-carburized reference body.
  • the treatment room is assigned an evacuable weighing room in which a weighing cell is arranged.
  • a weighing cell is arranged.
  • the figure shows a treatment room 3, shown only schematically, to which the hydrocarbon-containing treatment gas is fed via a feed line 1.
  • the following are preferably used as hydrocarbon-containing treatment gases: alkanes, alkenes, alkynes, derivatives of the aforementioned, optionally in combination with hydrogen and / or nitrogen.
  • the desired subatmospheric pressure in the treatment room 3 is set via the pumping line 7, in which a vacuum pump 8 is arranged.
  • work is predominantly carried out at pressures up to 20 mbar, preferably at pressures between 3 and 20 mbar.
  • the treatment room 3 is now assigned an evacuable weighing room 4.
  • a weighing cell 5 is in turn arranged in the weighing chamber 4.
  • Means are provided by means of which the reference sample or the reference body 6 can be introduced into the treatment room 3. After the carburizing process of the reference sample or reference body 6 has been completed, the reference sample 6 is weighed in the weighing cell 5 and the carbon mass flow is determined in this way.
  • the reference sample 6 is preferably designed as a solid sample, which can be carburized at least on one side, with a defined area and with a defined initial carbon content.
  • the load 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 to a valve 2 arranged in the feed line 1, which is preferably a control valve.
  • the valve 2 is now controlled via the evaluation unit 9, so that the hydrocarbon-containing treatment gas supplied to the treatment chamber 3 via the feed line 1 can be regulated as a function of the determined mass flow.
  • the invention thus enables continuous or discontinuous control of the hydrocarbon-containing treatment gas 1 supplied to the treatment room 3.
  • the supply of the hydrocarbon-containing treatment gas into the treatment room is thus controlled, thereby causing an uncontrolled decomposition of excess hydrocarbons in the treatment room and the pumping line and thus one Soot and tar formation can be effectively avoided.
  • a large part of the undesired deposits within the treatment room, on the material to be treated in the treatment room or in the pump-off 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)

Abstract

L'invention concerne un procédé et un dispositif de carburation à des pressions subatmosphériques. Selon ledit procédé, une chambre de traitement est alimentée, au moins par intermittence, en gaz de traitement à base d'hydrocarbures et un flux de gaz brûlés est évacué de la chambre de traitement, à l'aide d'au moins une pompe à vide. Selon l'invention, un échantillon de référence (6) présentant une surface de carburation définie est introduit dans la chambre de traitement (3) ; le débit massique du gaz de traitement (1) à base d'hydrocarbures est déterminé au moyen d'une méthode de pesée de l'échantillon de référence (6) et, en fonction du débit massique déterminé, l'alimentation du gaz de traitement à base d'hydrocarbures (1) dans la chambre de traitement (3) est régulée.
PCT/EP2003/010014 2002-09-13 2003-09-09 Procede et dispositif de carburation en depression WO2004031432A2 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE50302246T DE50302246D1 (de) 2002-09-13 2003-09-09 Verfahren und vorrichtung zum unterdruckaufkohlen
EP03747994A EP1537252B1 (fr) 2002-09-13 2003-09-09 Procede et dispositif de carburation en depression
AU2003267331A AU2003267331A1 (en) 2002-09-13 2003-09-09 Method and device for low-pressure carburising

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10242616.3 2002-09-13
DE10242616A DE10242616A1 (de) 2002-09-13 2002-09-13 Verfahren und Vorrichtung zum Unterdruckaufkohlen

Publications (2)

Publication Number Publication Date
WO2004031432A2 true WO2004031432A2 (fr) 2004-04-15
WO2004031432A3 WO2004031432A3 (fr) 2004-12-29

Family

ID=31895964

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2003/010014 WO2004031432A2 (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)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10156006B2 (en) 2009-08-07 2018-12-18 Swagelok Company Low temperature carburization under soft vacuum
US10246766B2 (en) 2012-01-20 2019-04-02 Swagelok Company Concurrent flow of activating gas in low temperature carburization

Families Citing this family (1)

* 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

Citations (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

Patent Citations (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

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
BAMMIDIPATI SREEKANTH ET AL: "Chemical vapor deposition of carbon on graphite by methane pyrolysis" AICHE J; AICHE JOURNAL NOV 1996 AICHE, NEW YORK, NY, US, Bd. 42, Nr. 11, November 1996 (1996-11), Seiten 3123-3132, XP000937830 *
HOFFMANN R ET AL: "PROBLEME DER KINETIK UND DER KEIMBILDUNG BEIM GASNITRIEREN" H[RTEREI - TECHNISCHE MITTEILUNGEN, Bd. 38, Nr. 3, Mai 1983 (1983-05), Seiten 103-109, XP009037775 CARL HANSER VERLAG, M]NCHEN, DE *
KL]MPER-WESTKAMP H ET AL: "BESTIMMUNG DES KOHLENSTOFFGEHALTES IN AUFKOHLUNGSFOLIEN" H[RTEREI - TECHNISCHE MITTEILUNGEN, Bd. 57, Nr. 5, 1. September 2002 (2002-09-01), Seiten 364-372, XP001140765 CARL HANSER VERLAG, M]NCHEN, DE ISSN: 0341-101X *
MATAMALA G ET AL: "Carburization and decarburization kinetics of iron in CH4 - H2 mixtures between 1000 - 1100 °C" MATERIALS CHEMISTRY AND PHYSICS SWITZERLAND, Bd. 12, Nr. 4, April 1985 (1985-04), Seiten 313-319, XP002299774 ISSN: 0254-0584 *
ROEMPLER D ET AL: "KOHLENSTOFF- UND H[RTEVERLAUF IN DER EINSATZH[RTUNGSSCHICHT - ZUSATZMODUL F]R DIFFUSIONSRECHNER" H[RTEREI - TECHNISCHE MITTEILUNGEN, Bd. 44, Nr. 6, 1. November 1989 (1989-11-01), Seiten 360-365, XP000163077 CARL HANSER VERLAG, M]NCHEN, DE ISSN: 0341-101X *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10156006B2 (en) 2009-08-07 2018-12-18 Swagelok Company Low temperature carburization under soft vacuum
US10934611B2 (en) 2009-08-07 2021-03-02 Swagelok Company Low temperature carburization under soft vacuum
US10246766B2 (en) 2012-01-20 2019-04-02 Swagelok Company Concurrent flow of activating gas in low temperature carburization
US11035032B2 (en) 2012-01-20 2021-06-15 Swagelok Company Concurrent flow of activating gas in low temperature carburization

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
EP1537252B1 (fr) 2006-01-18
AU2003267331A8 (en) 2004-04-23
EP1537252A2 (fr) 2005-06-08
ATE316161T1 (de) 2006-02-15

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