EP1280943B1 - Procede de cementation basse pression - Google Patents

Procede de cementation basse pression Download PDF

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Publication number
EP1280943B1
EP1280943B1 EP02704886A EP02704886A EP1280943B1 EP 1280943 B1 EP1280943 B1 EP 1280943B1 EP 02704886 A EP02704886 A EP 02704886A EP 02704886 A EP02704886 A EP 02704886A EP 1280943 B1 EP1280943 B1 EP 1280943B1
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EP
European Patent Office
Prior art keywords
pressure
low
gas
enrichment
kpa
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
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EP02704886A
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German (de)
English (en)
French (fr)
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EP1280943A1 (fr
Inventor
Aymeric Goldsteinas
Laurent Pelissier
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Etudes et Constructions Mecaniques SA
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Etudes et Constructions Mecaniques SA
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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
    • C23C8/20—Carburising
    • C23C8/22—Carburising of ferrous surfaces

Definitions

  • the present invention relates to the treatment of metal parts and more particularly cementation, that is to say the introduction of carbon to a certain depth of the parts to improve their mechanical characteristics.
  • the patent Russian version 6678978 filed on 2 June 1977 proposes to inject acetylene into the cement chamber at a temperature of 850 to 1000 ° C, by varying the pressure from 0.01 to 0.95 atmosphere (1 to 95 kPa) at a rate of change of pressure of 0.001 to 1 atmosphere per hour. It is explained that the amount of soot is reduced especially when the rate of increase of pressure is very low. However, this process is complex. To the knowledge of the applicant, the process described in this Russian patent has not been the subject of industrial exploitation and the results of the proposed solution could not be verified.
  • the present invention provides a novel process for the efficient use of acetylene and more generally any carburizing gas that may produce soot and tar.
  • the present invention provides a low-pressure cementation method of using alternating low pressure enrichment steps and diffusion stages in the presence of a neutral gas in which, during the steps of enrichment, using a mixture of enrichment gas and carrier gas, the carrier gas being in a proportion of 5 to 50% by volume of the enrichment gas.
  • the enriching gas is acetylene (C 2 H 2 ).
  • the carrier gas is nitrogen.
  • the carrier gas is hydrogen
  • the carrier gas comprises nitrogen and hydrogen in a proportion of 5 to 60%.
  • the pressure in the carburizing chamber is greater than 1 kPa.
  • the pressure in the cement chamber is between 1 and 2 kPa.
  • the diffusion and enrichment steps are carried out substantially at the same pressure.
  • the treatment temperature is of the order of 850 to 1200 ° C.
  • each of the enrichment steps is divided into substeps of less than one minute durations separated by diffusion substeps of less than half a minute duration, preferably the order of ten seconds.
  • the Applicant has carried out various cementation experiments on a specimen of the type shown in FIG. 1, consisting of a steel cylinder provided with a non-through bore, and measurements have been made as to the degree of carburizing of ext at the outside of the specimen and at the carburization depth of int within the bore formed in the specimen.
  • FIG. 2 represents a carburizing-diffusion cycle of the type described in the patent French 2678287 and used according to the present invention.
  • the carburizing-diffusion operations are carried out at constant temperature and at constant pressure after an initial phase of setting temperature and pressure.
  • E enrichment phases E are successively carried out during the course of time, during which a carburizing gas is injected into a carburizing enclosure containing charges, of which at least one specimen of the type shown in FIG. 1, and diffusion phases. in which a neutral gas is inserted into the enclosure.
  • the durations and the number of the respective stages of enrichment and diffusion are modified.
  • the temperature is between 850 and 1200 ° C., the duration of each of the enrichment and / or diffusion phases being of the order of a few minutes.
  • FIGS. 3, 4 and 5 correspond to three particular pressures maintained during the carburizing-diffusion phases, ie respectively 0.3 kPa for FIG. 3, 0.7 kPa for FIG. 4 and 1, 2 kPa for Figure 5.
  • Each of the curves represents the hardness as a function of the carburizing depth for a point taken outside (Ext) of the specimen and for a point taken inside (Int) of the specimen. The different points of each curve result from the testing of various test pieces having undergone distinct treatment periods.
  • FIG. 5 represents results obtained for a pressure of 1.2 kPa: when the depth of carburization outside the test piece reaches 1 mm, the case-hardening depth inside reaches 0.8 mm, which corresponds to the generally accepted standards.
  • soot and tars have been tested and it has been noted that the creation of soot and tar is negligible in the case where the pressure is 0.3 kPa, but becomes significant from 0, 7 kPa.
  • the present invention provides to use a cycle of the type shown in Figure 2 and to inject either a pure carburizing gas but a mixture of a carburizing gas and a carrier gas.
  • the proportion of carrier gas will be chosen from about 25 to 50% of the amount of enrichment gas.
  • FIG. 6 indicates that, for example, a mixture of acetylene (C 2 H 2 ) and nitrogen N 2 with a total pressure of 1.5 kPa and a proportion of approximately 30% of nitrogen, satisfactory cementation substantially identical to that illustrated in Figure 5.
  • acetylene C 2 H 2
  • nitrogen N 2 with a total pressure of 1.5 kPa and a proportion of approximately 30% of nitrogen
  • Figure 7 shows the concentration of benzene (C 6 H 6 ) observed at the end of successive enrichment cycles. Indeed, it is known that the formation of tars implies a generation phase of aromatic compounds such as benzene and phenylethylene. Benzene generation is therefore a good indicator of the formation of soot and tar.
  • the curves marked C 2 H 2 and C 2 H 2 + N 2 respectively correspond to the cases described in relation to FIGS. 5 and 6. It can be seen that, using pure acethylene according to the prior art, the concentration of benzene increases noticeably at the end of each enrichment cycle, which corresponds to a significant formation of tars.
  • the concentration of benzene remains substantially constant, at a low value, which corresponds well to negligible tar formation.
  • the present invention provides, in all cases where it is carried out a cementation in the presence of an aliphatic hydrocarbon under conditions where there are problems of generation of soot and tars, to add a neutral gas.
  • a neutral gas Preferably the proportion of neutral gas will be chosen from about 5 to 50% of the amount of enrichment gas.
  • the neutral gas is not necessarily nitrogen but may be any other type of gas not involved in the carburizing reaction, for example argon or a mixture of gases. Nitrogen will preferably be chosen because of its low cost. But, for specific requirements, or if the costs of gas come down, we can choose another neutral gas or carrier gas to solve the problem of soot generation and tars.
  • the Applicant has shown that the formation of tars can be further reduced by reviewing the relative duration of enrichment (E) and diffusion (D) cycles described in connection with FIG. Conventionally, provision is made, for example, for six enrichment and diffusion cycles having durations of the order of those indicated in the table below (in seconds).
  • E1 D1 E2 D2 E3 D3 E4 D4 E5 D5 E6 D6 520 100 190 150 150 300 100 350 80 450 60 600
  • each of the enrichment cycles into brief steps followed by short diffusion times. For example, enrichment steps of up to 50 s followed by a step broadcasting time of the order of 10 s.
  • the first enrichment cycle E1 will then comprise 10 or 11 enrichment steps, each of which is followed by a diffusion step of about ten seconds, the final diffusion phase D1 being maintained substantially at its initial duration indicated in the table. above.
  • the second enrichment cycle E2 will comprise 4 enrichment stages, each of which is followed by a diffusion step of about ten seconds, the final diffusion phase D2 being maintained substantially at its initial duration indicated in the table above. . And so on.
  • the concentration of benzene at the end of each enrichment cycle for this pulsed mode of operation is indicated in FIG. 7 by the curve C 2 H 2 + N 2 (pulse). It can be seen that the concentration of benzene is substantially divided by two compared to the case where uninterrupted cycles are conventionally used.

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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)
  • Luminescent Compositions (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)
  • Gas Separation By Absorption (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Door And Window Frames Mounted To Openings (AREA)
  • Valves And Accessory Devices For Braking Systems (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • Separation By Low-Temperature Treatments (AREA)
EP02704886A 2001-02-23 2002-02-22 Procede de cementation basse pression Expired - Lifetime EP1280943B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR0102513A FR2821362B1 (fr) 2001-02-23 2001-02-23 Procede de cementation basse pression
FR0102513 2001-02-23
PCT/FR2002/000674 WO2002068707A1 (fr) 2001-02-23 2002-02-22 Procede de cementation basse pression

Publications (2)

Publication Number Publication Date
EP1280943A1 EP1280943A1 (fr) 2003-02-05
EP1280943B1 true EP1280943B1 (fr) 2007-10-31

Family

ID=8860388

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EP02704886A Expired - Lifetime EP1280943B1 (fr) 2001-02-23 2002-02-22 Procede de cementation basse pression

Country Status (14)

Country Link
US (1) US7118634B2 (pl)
EP (1) EP1280943B1 (pl)
JP (1) JP3833615B2 (pl)
KR (1) KR100875547B1 (pl)
CN (1) CN1220788C (pl)
AT (1) ATE377097T1 (pl)
BR (1) BR0204223A (pl)
CA (1) CA2407372C (pl)
DE (1) DE60223202T2 (pl)
ES (1) ES2295315T3 (pl)
FR (1) FR2821362B1 (pl)
MX (1) MXPA02010434A (pl)
PL (1) PL356901A1 (pl)
WO (1) WO2002068707A1 (pl)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2874079B1 (fr) * 2004-08-06 2008-07-18 Francis Pelissier Machine de traitement thermochimique de cementation
US7514035B2 (en) * 2005-09-26 2009-04-07 Jones William R Versatile high velocity integral vacuum furnace
EP1989335A4 (en) * 2005-11-23 2010-04-07 Surface Comb Inc SURFACE TREATMENT OF METAL OBJECTS IN AN ATMOSPHERIC OVEN
CN100510156C (zh) * 2007-04-10 2009-07-08 中国矿业大学 医用钛合金髋关节球头表面渗碳工艺
DE102007047074A1 (de) 2007-10-01 2009-04-02 Robert Bosch Gmbh Verfahren zur Aufkohlung von Werkstücken sowie Verwendung
CA2771090C (en) 2009-08-07 2017-07-11 Swagelok Company Low temperature carburization under soft vacuum
US9617632B2 (en) 2012-01-20 2017-04-11 Swagelok Company Concurrent flow of activating gas in low temperature carburization
JP6135177B2 (ja) * 2013-02-22 2017-05-31 大同特殊鋼株式会社 真空浸炭処理方法
PL422596A1 (pl) * 2017-08-21 2019-02-25 Seco/Warwick Spółka Akcyjna Sposób nawęglania podciśnieniowego (LPC) elementów wykonanych ze stopów żelaza i innych metali
PL424224A1 (pl) * 2018-01-08 2019-07-15 Seco/Warwick Spółka Akcyjna Sposób nawęglania niskociśnieniowego (LPC)
FR3081884B1 (fr) 2018-06-05 2021-05-21 Safran Helicopter Engines Procede de cementation basse pression d'une piece comprenant de l'acier
US10973908B1 (en) 2020-05-14 2021-04-13 David Gordon Bermudes Expression of SARS-CoV-2 spike protein receptor binding domain in attenuated salmonella as a vaccine

Family Cites Families (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1799614A (en) * 1925-01-05 1931-04-07 Kobe Inc Method of producing slots
US4035203A (en) * 1973-12-21 1977-07-12 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method for the heat-treatment of steel and for the control of said treatment
GB1510481A (en) * 1976-04-02 1978-05-10 British Steel Corp Carburising coiled strip
GB1559690A (en) * 1976-11-10 1980-01-23 British Steel Corp Treatment of steel products
FR2446322A2 (fr) * 1979-01-15 1980-08-08 Air Liquide Procede de traitement thermique de l'acier et de controle dudit traitement
DE3038078A1 (de) * 1980-10-08 1982-05-06 Linde Ag, 6200 Wiesbaden Verfahren und vorrichtung zum aufkohlen metallischer werkstuecke
DE3146042A1 (de) * 1981-11-20 1983-05-26 Linde Ag, 6200 Wiesbaden Verfahren zum einsatzhaerten metallischer werkstuecke
US5139584A (en) * 1989-07-13 1992-08-18 Solo Fours Industriels Sa Carburization process
FR2678287B1 (fr) * 1991-06-26 1993-10-29 Etudes Constructions Mecaniques Procede et four de cementation a basse pression.
FR2681332B1 (fr) * 1991-09-13 1994-06-10 Innovatique Sa Procede et dispositif de cementation d'un acier dans une atmosphere a basse pression.
WO1996030556A1 (fr) * 1995-03-29 1996-10-03 Jh Corporation Procede et equipement de cementation, et produits de cette operation
EP0882811B2 (de) * 1997-06-03 2010-12-15 Ipsen International GmbH Verfahren zur Aufkohlung metallischer Werkstücke in einem Vakuum-Ofen
JP3894635B2 (ja) * 1997-08-11 2007-03-22 株式会社小松製作所 浸炭部材とその製造方法並びに浸炭処理システム
JP2000336469A (ja) * 1999-05-28 2000-12-05 Nachi Fujikoshi Corp 真空浸炭方法及び装置

Also Published As

Publication number Publication date
MXPA02010434A (es) 2003-04-25
JP2004519556A (ja) 2004-07-02
DE60223202D1 (de) 2007-12-13
EP1280943A1 (fr) 2003-02-05
CN1457373A (zh) 2003-11-19
ES2295315T3 (es) 2008-04-16
WO2002068707A1 (fr) 2002-09-06
CN1220788C (zh) 2005-09-28
KR100875547B1 (ko) 2008-12-24
CA2407372A1 (en) 2002-09-06
BR0204223A (pt) 2003-02-18
PL356901A1 (pl) 2004-07-12
ATE377097T1 (de) 2007-11-15
US20030168125A1 (en) 2003-09-11
DE60223202T2 (de) 2008-08-14
JP3833615B2 (ja) 2006-10-18
FR2821362B1 (fr) 2003-06-13
KR20030014204A (ko) 2003-02-15
US7118634B2 (en) 2006-10-10
FR2821362A1 (fr) 2002-08-30
CA2407372C (en) 2011-04-19

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