EP2732066B1 - Procédé de refroidissement de pièces métalliques ayant subi un traitement de nitruration / nitrocarburation en bain de sel fondu, l'installation pour la mise en oeuvre du procédé et les pièces métalliques traitées - Google Patents

Procédé de refroidissement de pièces métalliques ayant subi un traitement de nitruration / nitrocarburation en bain de sel fondu, l'installation pour la mise en oeuvre du procédé et les pièces métalliques traitées Download PDF

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Publication number
EP2732066B1
EP2732066B1 EP12743503.0A EP12743503A EP2732066B1 EP 2732066 B1 EP2732066 B1 EP 2732066B1 EP 12743503 A EP12743503 A EP 12743503A EP 2732066 B1 EP2732066 B1 EP 2732066B1
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EP
European Patent Office
Prior art keywords
parts
chamber
nitriding
cooling
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.)
Active
Application number
EP12743503.0A
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German (de)
English (en)
French (fr)
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EP2732066A1 (fr
Inventor
Bernard Michalot
Bernard Zabinski
Houcine HADJ RABAH
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.)
Hydromecanique et Frottement SAS
Original Assignee
HEF SAS
Hydromecanique et Frottement SAS
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Priority to PL12743503T priority Critical patent/PL2732066T3/pl
Publication of EP2732066A1 publication Critical patent/EP2732066A1/fr
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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
    • C23C8/80—After-treatment
    • 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
    • C23C8/40—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 liquids, e.g. salt baths, liquid suspensions
    • C23C8/42—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 liquids, e.g. salt baths, liquid suspensions only one element being applied
    • C23C8/48—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
    • C23C8/40—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 liquids, e.g. salt baths, liquid suspensions
    • C23C8/52—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 liquids, e.g. salt baths, liquid suspensions more than one element being applied in one step
    • C23C8/54—Carbo-nitriding

Definitions

  • the invention relates to a method and a cooling system for metal parts which have undergone nitriding / nitrocarburizing treatment in a bath of molten salts.
  • the invention also relates to the parts thus treated.
  • thermochemical nitrogen diffusion nitriding or nitrocarburizing in baths of molten salts.
  • these salt baths generally consist of cyanate and alkali carbonate.
  • the alkaline cyanate releases nitrogen and carbon that diffuse on the surface of the room.
  • the treatment times are generally between 20 and 180 min at temperatures between 400 and 700 ° C.
  • this treatment generally induces the formation of two characteristic zones: a first zone at the surface, with a thickness of between 5 and 30 ⁇ m composed mainly of nitrides ⁇ (Fe2 .... 3n) and nitrides ⁇ (Fe4N)), called the combination zone, followed by a second zone, generally between 0.2 and 1.5 mm thick, characterized by the presence of nitrogen in solid solution in the iron grains and in the form of nitride alloy elements, called diffusion layer.
  • the latter are arranged in a metal rack to facilitate their transport, for example, by means of robots between the different processing stations.
  • the rack's fill rate is at a maximum, so that the parts are likely to be in contact with each other.
  • the transfer of the pieces from the nitriding bath to the cooling zone is carried out for a period such that, on contact with the ambient air, oxidation or superficial discoloration spots appear on the surface of a part more or less important parts treated. Tests carried out in the laboratory have shown that from a transfer time greater than about 30 seconds, the appearance of oxidation spots on only a few parts is observed, whereas from a transfer time of 120 seconds order, all parts are oxidized. However, the industrial transfer time between two successive processing zones is generally between these two values.
  • the technical field of the invention relates to an industrial processing of parts that is not comparable with a nitriding / nitrocarburizing treatment, carried out at the scale of a laboratory where the parts are not treated only in small quantities. In the laboratory, it is therefore possible, after the nitriding bath, to transfer the parts rapidly enough to avoid oxidation during cooling with water, for example.
  • the patent US 3560271 relates to a nitriding process in molten salt baths with the aim of slowing the cooling after nitriding in order to limit the level of stresses so as to limit the risks of cracking of the layer. Cooling is carried out under vacuum only by radiation, which leads to cooling times which are difficult to reconcile with an industrial process (from several hours to several tens of hours).
  • the object of the invention is to remedy these disadvantages in a simple, safe, effective and rational manner.
  • the problem which the invention proposes to solve is thus to guarantee, in the case of an industrial treatment of metal parts having undergone nitriding / nitrocarburizing treatment in molten salt baths, the absence of corrosion-oxidation traces, with the aim of improving their ductility.
  • the refrigerant is liquid nitrogen which will vaporize very quickly thanks to the heat of the bath and parts.
  • Such a vaporization will produce a volume of gas approximately 630 times higher, which will evacuate oxygen very quickly inside the enclosure.
  • the chamber is filled with liquid nitrogen 2 to 3 minutes before the end of the nitriding / nitrocarburizing treatment.
  • the parts are transferred vertically to the chamber filled with liquid nitrogen at a minimum speed of 6 m / min.
  • the cooling chamber according to claim 5 is arranged in direct relationship with the nitriding / nitrocarburizing station being secured to a transfer carriage for fast transfer at a minimum speed of 6 m / min. min of all the parts in said enclosure.
  • the enclosure is constituted by a double-walled bell in which is injected liquid nitrogen, said double wall having arrangements for the diffusion of nitrogen inside the bell.
  • the base of the check cooperates with means able to give free access to the inside of said bell for the transfer of parts, and to close this access during the cooling phase.
  • the means consist of by doors integral with a part of the treatment station.
  • the invention also relates to the parts having undergone nitriding / nitrocarburizing treatment in molten salt baths, according to the characteristics of the claimed process. More generally, the invention relates to metal parts on which there is an absence of oxidation task and the presence of nitride precipitate in the diffusion zone.
  • the installation is adapted to process parts industrially, that is to say, not in a unitary manner, but in batches, for example by arranging said parts in a metal rack in order to facilitate their transfer by robots between the various stations. treatment.
  • a cooling chamber (1) is arranged in direct relation with the nitriding / nitrocarburizing station while being secured to a transfer carriage for fast transfer at a minimum speed of 6 m / min of the assembly. of considered pieces (P) in said enclosure (1). As indicated, the pieces (P) are for example arranged in a rack (R).
  • the enclosure (1) is constituted by a double-walled bell (1a) into which liquid nitrogen is injected.
  • This double wall (la) has arrangements for the diffusion of liquid nitrogen inside the bell (1).
  • the double wall (1a) has baffles (1b) for the diffusion of liquid nitrogen through calibrated orifices (1c).
  • the supply of liquid nitrogen is carried out by any known and appropriate means (2).
  • the bell (1) is secured to the transfer carriage. The opening of the bell, located at its lower end, cooperates with doors (3) and (4) integral with the nitrocarburizing station.
  • FIGs 2, 3 and 4 show the main phases of the process on which the characteristics of the invention are based.
  • the nitrocarburizing treatment as such can for example be of the type known under the trademark SURSULF, TENIFER .
  • the duration of the treatment generally between 20 and 180 min is typically of the order of 50 to 60 minutes.
  • the bell (1) is disposed above the bath (T) in which is dipped the set of pieces (P) disposed in the rack (R). Doors (3) and (4) are open ( figure 2 ).
  • liquid nitrogen (A) is injected through the double wall (1a) as indicated previously, in order to evacuate very rapidly the oxygen inside the bell (1) to allow the pieces (P) to cool metallurgically slowly under the inert atmosphere ( figure 3 ).
  • the speed of 6 m / min depends on the distance between the level of the nitriding bath and the entry into the bell; this speed can therefore be higher depending on the case: the higher the speed, the more the results will be correct.
  • the whole of the parts is rinsed, which rinsing can be carried out in a water brought to a temperature of 40 to 50 ° C, then to a water brought to a temperature of the order of 20 ° vs.
  • the cooling is carried out according to the prior art by soaking the parts in the water or immediately after the nitriding / nitrocarburizing treatment (impossible under industrial conditions), figure 5 after a longer or shorter period after treatment, ie 30 seconds after treatment ( figure 6 ), 60 seconds after treatment ( figure 7 ) and 120 seconds after treatment ( figure 8 ).
  • the cooling with liquid nitrogen clearly shows the absence of traces of superficial oxidation and the presence of nitride precipitates, with consequently improved mechanical properties.

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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 Treatments In General, Especially Conveying And Cooling (AREA)
  • Heat Treatment Of Articles (AREA)
  • Manufacture And Refinement Of Metals (AREA)
EP12743503.0A 2011-07-15 2012-07-12 Procédé de refroidissement de pièces métalliques ayant subi un traitement de nitruration / nitrocarburation en bain de sel fondu, l'installation pour la mise en oeuvre du procédé et les pièces métalliques traitées Active EP2732066B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL12743503T PL2732066T3 (pl) 2011-07-15 2012-07-12 Sposób schładzania elementów metalowych poddanych obróbce azotowania /azotonawęglania w kąpieli ze stopioną solą, instalacja do zastosowania sposobu i obrabiane elementy metalowe

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1156459A FR2977897B1 (fr) 2011-07-15 2011-07-15 Procede de refroidissement de pieces metalliques ayant subi un traitement de nitruration / nitrocarburation en bain de sel fondu, l'installation pour la mise en oeuvre du procede et les pieces metalliques traitees
PCT/FR2012/051651 WO2013011228A1 (fr) 2011-07-15 2012-07-12 Procédé de refroidissement de pièces métalliques ayant subi un traitement de nitruration / nitrocarburation en bain de sel fondu, l'installation pour la mise en oeuvre du procédé et les pièces métalliques traitées

Publications (2)

Publication Number Publication Date
EP2732066A1 EP2732066A1 (fr) 2014-05-21
EP2732066B1 true EP2732066B1 (fr) 2018-11-07

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EP12743503.0A Active EP2732066B1 (fr) 2011-07-15 2012-07-12 Procédé de refroidissement de pièces métalliques ayant subi un traitement de nitruration / nitrocarburation en bain de sel fondu, l'installation pour la mise en oeuvre du procédé et les pièces métalliques traitées

Country Status (22)

Country Link
US (1) US9464346B2 (es)
EP (1) EP2732066B1 (es)
JP (1) JP6053777B2 (es)
KR (1) KR101873367B1 (es)
CN (1) CN103732784B (es)
AU (1) AU2012285581B2 (es)
BR (1) BR112014000933B8 (es)
CA (1) CA2855927C (es)
DK (1) DK2732066T3 (es)
ES (1) ES2695975T3 (es)
FR (1) FR2977897B1 (es)
HU (1) HUE039994T2 (es)
MA (1) MA35605B1 (es)
MX (1) MX350500B (es)
MY (1) MY185963A (es)
PL (1) PL2732066T3 (es)
RU (1) RU2596539C2 (es)
TN (1) TN2014000012A1 (es)
TW (1) TWI580793B (es)
UA (1) UA111215C2 (es)
WO (1) WO2013011228A1 (es)
ZA (1) ZA201400092B (es)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101661432B1 (ko) * 2015-11-09 2016-10-10 변상덕 부품 냉각장치
MX2019015782A (es) * 2017-07-07 2020-08-03 Ind Mailhot Inc Metodo y sistema para enfriar piezas metalicas despues de la nitruracion.
CN111139425A (zh) * 2020-01-21 2020-05-12 江苏丰东热技术有限公司 一种氮碳共渗方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201351173Y (zh) * 2009-01-05 2009-11-25 周磊 一种脉冲等离子体氮碳共渗淬火装置

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Publication number Priority date Publication date Assignee Title
FR1577966A (es) * 1967-05-17 1969-08-14
SU739129A1 (ru) * 1977-07-21 1980-06-05 Предприятие П/Я А-1450 Автоматизированна лини карбонитрации инструмента
US4191599A (en) * 1978-09-13 1980-03-04 Ford Motor Company Method of heat treating high carbon alloy steel parts to develop surface compressive residual stresses
US4461656A (en) * 1983-03-15 1984-07-24 Ross John A Low temperature hardening of the surface of a ferrous metal workpiece in a fluidized bed furnace
JPH03140456A (ja) * 1989-10-27 1991-06-14 Iwate Seitetsu Kk アルカリ金属塩を含む熔融塩で処理した金属の冷却方法
RU2003732C1 (ru) * 1992-09-30 1993-11-30 Михаил Александрович Шелагуров Способ обработки стальных деталей
JP3442447B2 (ja) * 1993-01-20 2003-09-02 トヨタ自動車株式会社 浸炭又は浸炭窒化焼入れ方法
US5741372A (en) * 1996-11-07 1998-04-21 Gugel; Saveliy M. Method of producing oxide surface layers on metals and alloys
JP2007162136A (ja) * 2005-12-12 2007-06-28 Metaplas Ionon Oberflaechenveredelungstechnik Gmbh 加工品表面の結合層なしのガス窒化方法及び加工品

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201351173Y (zh) * 2009-01-05 2009-11-25 周磊 一种脉冲等离子体氮碳共渗淬火装置

Also Published As

Publication number Publication date
HUE039994T2 (hu) 2019-02-28
JP2014520960A (ja) 2014-08-25
TWI580793B (zh) 2017-05-01
MX2014000607A (es) 2014-02-27
TN2014000012A1 (fr) 2015-07-01
CA2855927A1 (fr) 2013-01-24
MY185963A (en) 2021-06-14
JP6053777B2 (ja) 2016-12-27
ES2695975T3 (es) 2019-01-11
UA111215C2 (uk) 2016-04-11
WO2013011228A1 (fr) 2013-01-24
BR112014000933A2 (pt) 2017-02-14
AU2012285581A1 (en) 2014-02-06
AU2012285581B2 (en) 2017-06-29
BR112014000933B8 (pt) 2023-01-03
DK2732066T3 (en) 2018-12-03
MA35605B1 (fr) 2014-11-01
RU2014105318A (ru) 2015-08-27
CA2855927C (fr) 2019-05-21
US20140216608A1 (en) 2014-08-07
KR101873367B1 (ko) 2018-07-02
RU2596539C2 (ru) 2016-09-10
ZA201400092B (en) 2016-03-30
CN103732784A (zh) 2014-04-16
FR2977897A1 (fr) 2013-01-18
US9464346B2 (en) 2016-10-11
FR2977897B1 (fr) 2017-06-16
TW201323617A (zh) 2013-06-16
CN103732784B (zh) 2015-11-25
BR112014000933B1 (pt) 2020-11-10
MX350500B (es) 2017-09-07
PL2732066T3 (pl) 2019-02-28
KR20140076544A (ko) 2014-06-20
EP2732066A1 (fr) 2014-05-21

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