EP1885904B1 - Low pressure carbonitriding method and device - Google Patents
Low pressure carbonitriding method and device Download PDFInfo
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- EP1885904B1 EP1885904B1 EP06743815A EP06743815A EP1885904B1 EP 1885904 B1 EP1885904 B1 EP 1885904B1 EP 06743815 A EP06743815 A EP 06743815A EP 06743815 A EP06743815 A EP 06743815A EP 1885904 B1 EP1885904 B1 EP 1885904B1
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- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000005256 carbonitriding Methods 0.000 title claims abstract description 41
- 238000005121 nitriding Methods 0.000 claims abstract description 38
- 238000005255 carburizing Methods 0.000 claims abstract description 23
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 11
- 239000010959 steel Substances 0.000 claims abstract description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 26
- 230000007935 neutral effect Effects 0.000 claims description 15
- 229910021529 ammonia Inorganic materials 0.000 claims description 13
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 8
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 5
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 5
- 239000001294 propane Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 description 73
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 57
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 28
- 229910052799 carbon Inorganic materials 0.000 description 28
- 238000009792 diffusion process Methods 0.000 description 26
- 229910052757 nitrogen Inorganic materials 0.000 description 26
- 238000002347 injection Methods 0.000 description 17
- 239000007924 injection Substances 0.000 description 17
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 238000010791 quenching Methods 0.000 description 8
- 230000000171 quenching effect Effects 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000008246 gaseous mixture Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
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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
- C23C8/28—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
- C23C8/28—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
- C23C8/34—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 present invention relates to processes for treating steel parts, and more particularly to carbonitriding processes, that is to say introducing carbon and nitrogen at the surface of steel parts to improve its performance. hardness and fatigue resistance.
- a first category of carbonitriding processes corresponds to so-called high-pressure carbonitriding processes insofar as the enclosure containing the workpieces is maintained at a pressure generally close to atmospheric pressure for the duration of the treatment.
- Such a process consists, for example, in maintaining the parts at a temperature level, for example at about 880 ° C., while supplying the enclosure with a gaseous mixture consisting of methanol and ammonia.
- the carbonitriding step is followed a quenching step, for example an oil quenching, and optionally a hardening step of the treated parts.
- a second category of carbonitriding processes corresponds to so-called low pressure or reduced pressure carbonitriding processes, insofar as the enclosure containing the workpieces is maintained at a pressure generally less than a few hundred pascals (a few millibars).
- the figure 1 corresponds to the Figure 5 (a) demand US 2004/0187966 and represents a temperature evolution curve in the enclosure of an oven in which a carbonitriding process is carried out according to a first embodiment comprising seven successive stages I to VII.
- the workpieces are heated (step I) to a temperature step 12 and held at temperature plateau 12 (step II) to achieve room temperature equalization.
- a carburising step (step III) is carried out at the temperature step 12 by injecting into the chamber a gaseous mixture of ethylene and hydrogen and is followed by a diffusion step (step IV) carried out at temperature step 12.
- the temperature in the chamber is then lowered (step V) to a temperature step 14 below the temperature step 12.
- a nitriding step (step VI) is performed at temperature step 14 by injecting ammonia in the enclosure.
- the pieces are finally quenched (stage VII), for example by quenching with oil.
- the figure 2 corresponds to the Figure 5 (b) demand US 2004/0187966 and represents a curve 16 for changing the temperature in the enclosure of an oven in which a carbonitriding process is carried out according to a second exemplary embodiment comprising four successive stages I 'to IV'.
- Steps I 'and II' respectively correspond to steps I and II of the first exemplary embodiment.
- Stage III ' corresponds to a carbonitriding step, carried out at a temperature step 18, during which a gaseous mixture of ethylene, hydrogen and ammonia is injected into the enclosure of the furnace.
- Step IV ' corresponds to an oil quenching step.
- a disadvantage of the first example of carbonitriding process described in the publication US 2004/0187966 is that the nitriding step is performed after the carburizing step at a temperature step below the carburizing temperature plateau.
- the total duration of the treatment can therefore be excessively long, which makes it difficult to use such a method in an industrial context.
- a disadvantage of the second example of carbonitriding process described in the publication US 2004/0187966 is due to the fact that carburizing and nitriding gases are injected simultaneously into the furnace chamber. It is then difficult to precisely control the gaseous environment that prevails in the chamber, and, therefore, to control, in a precise and reproducible manner, the nitrogen and carbon concentration profiles obtained in the treated parts.
- the document EP 1 160 349 describes a carbonitriding process in which ammonia is injected during the cementation and carbon diffusion phases.
- the document SU 1,159,960 discloses a process comprising pulsed injection of a carburizing gas.
- the document DE 103 22 255 discloses a carburizing process which comprises, during carburization and diffusion, the addition of a gas comprising nitrogen.
- the present invention provides a method of low-pressure carbonitriding of steel parts which allows to obtain, in a precise and reproducible manner, the desired carbon and nitrogen concentration profiles in the treated parts.
- Another object of the present invention is to provide a carbonitriding process whose implementation is compatible with the treatment of steel parts in an industrial context.
- the present invention provides a method of carbonitriding a steel part disposed in an enclosure maintained at a reduced internal pressure, the part being maintained at a temperature step.
- the method comprises an alternation of first and second stages, a carburizing gas being injected into the chamber only during the first stages and a nitriding gas being injected into the chamber only for at least a portion of at least two seconds steps.
- the carburising gas is propane or acetylene and the nitriding gas is ammonia.
- a neutral gas is injected into the chamber simultaneously with the nitriding gas.
- the nitriding gas is injected into the chamber during at least a second step for a duration less than the duration of said second step, the rest of said second step being carried out in the presence of a neutral gas.
- the first and second steps are performed at a constant pressure of less than 1500 pascals.
- the temperature plateau is between 800 ° C and 1050 ° C.
- the temperature plateau is greater than 900 ° C.
- the present invention consists in producing in an enclosure, containing steel parts to be treated maintained at a substantially constant temperature, an alternation of carbon enrichment stages during which a carburizing gas is injected into the chamber under a reduced pressure. and carbon diffusion steps during which the injection of the carburizing gas is interrupted.
- the present invention consists in providing for the injection into the chamber of a nitriding gas during all or part of the carbon diffusion steps.
- the carbon enrichment steps then correspond to nitrogen diffusion steps.
- the nitriding gas is injected during at least a portion of at least two carbon diffusion steps, i.e. during at least a portion of a carbon diffusion step sandwiched between two enrichment stages. carbon.
- the figure 3 schematically represents an embodiment of a low-pressure carbonitriding furnace 10.
- the furnace 10 comprises a sealed wall 12 delimiting an internal enclosure 14 in which is disposed a load to be treated 16, generally a large number of parts arranged on a suitable support.
- a vacuum of the order of a few hundred pascals (a few millibars) can be maintained in the chamber 14 by means of an extraction pipe 18 connected to an extractor 20.
- An injector 22 makes it possible to introduce gases distributed in the enclosure 14.
- gas inlets 22, 24, 26, 28 respectively controlled by valves 30, 32, 34, 36.
- the temperature in the enclosure 14 can be fixed by heating means 38.
- the figure 4 represents a curve 40 of evolution of the temperature in the chamber 14 of the carbonitriding furnace 10 of the figure 3 during a carbonitriding cycle according to an exemplary carbonitriding process of the invention.
- the method comprises an initial step H corresponding to an increase 42 of the temperature in the enclosure 14 containing the charge 16 to a temperature plateau 44 which, in the present example, is equal to 930 ° C. and which generally may be at temperatures between about 800 ° C and about 1050 ° C.
- Step H is followed by a step PH equalizing the temperature of the parts constituting the load 16 at the temperature step 44.
- the steps H and PH are performed in the presence of a neutral gas, to which a gas is optionally added. reducer.
- the neutral gas is, for example, nitrogen (N 2 ).
- the reducing gas for example hydrogen (H 2 )
- H 2 hydrogen
- the reducing gas may be added in a proportion ranging from 1% to 5% by volume of the neutral gas.
- Step PH is followed by an alternation of carbon enrichment steps C1 to C4, during which a cementation gas is injected into the chamber 14, and carbon diffusion stages D1 to D4 during which the The carburizing gas is no longer injected into the chamber 14.
- the enrichment and diffusion stages are carried out by maintaining the temperature in the chamber 14 at the temperature plateau 44.
- an injection of a nitriding gas is carried out in the enclosure 14.
- a quench step Q of the load 10 for example gas quenching, closes the carbonitriding cycle.
- a vacuum is maintained in the chamber 14 at pressures of a few hundred pascals (a few millibars).
- the injection of the carburizing gas is effected by pulses.
- the carburising gas is for example propane (C 3 H 8 ) or acetylene (C 2 H 2 ). It can also be any other hydrocarbon (C X H Y ) likely to dissociate at the enclosure temperatures to cementer the surface of the parts to be treated.
- the nitriding gas is, for example, ammonia (NH 3 ).
- Injection of the nitriding gas can be performed only during some of the diffusion steps.
- the injection of the nitriding gas can be carried out only during part of the diffusion step.
- a neutral gas for example nitrogen (N 2 ), may be injected during all the enrichment and diffusion steps, only during the diffusion steps, or only during part of the diffusion steps.
- the injection of the neutral gas is regulated so as to maintain constant the pressure in the chamber 14.
- the relative proportions of the nitriding gas and the neutral gas are determined as a function of desired nitrogen concentration profile in the treated parts.
- the relative proportions of the nitriding gas and the neutral gas may be different for each diffusion stage during which the Nitriding gas and neutral gas are simultaneously injected into the chamber 14.
- certain gases injected into the chamber 14 of the furnace 10 may be mixed before the injection into the chamber 14.
- Such a variant makes it possible, for example, during the temperature rise steps H and of equalization of temperature PH, to inject directly into the chamber 14 a mixture of nitrogen and hydrogen of the type containing a proportion of hydrogen of less than 5% by volume, such a proportion of hydrogen excluding any risk of 'explosion.
- the carbonitriding process is carried out without pressure variation and the injections, carburizing gas and nitriding gas (and / or optionally neutral gas), during the steps of enrichment and diffusion, are successive and the substitution between the carburizing gas and the nitriding gas (and / or possibly the neutral gas) is likely to occur very quickly.
- the figure 5 represents an example of a concentration profile by weight of the nitrogen element having diffused in a treated part as a function of the depth, measured from the surface of the part, when the carburizing gas is propane and the nitriding gas is ammonia.
- the Figures 6, 7 and 8 illustrate respectively an example of the carbonitriding process according to the invention and the carbon and nitrogen concentration profiles obtained for such a carbonitriding process wherein the carburizing gas is acetylene and the nitriding gas is ammonia.
- the carbonitriding is carried out at a temperature level of 880 ° C.
- the heating steps H and the temperature equalization PH last for 20 minutes and are followed by an alternation of three enrichment stages C1, C2, C3 (respectively 123 s, 51 s and 49 s) and three dissemination stages D1, D2, D3 (194 s, 286 s and 2957 s, respectively).
- the Figures 9, 10 and 11 illustrate respectively another example of a carbonitriding process according to the invention and the carbon and nitrogen concentration profiles obtained for such a carbonitriding process, in which the carburizing gas is acetylene and the nitriding gas is the ammonia.
- the carbonitriding is carried out at a temperature level of 930 ° C.
- the heating steps H and equalization of the temperature PH respectively last 29 minutes and 31 minutes and are followed by an alternation of five enrichment stages C1 to C5 (respectively of 329 s, 91 s, 80 s, 75 s and 71 s) and five dissemination stages D1 to D5 (108 s, 144 s, 176 s, 208 s and 2858 s, respectively).
- the Applicant has shown that the injection of ammonia during the diffusion steps allows an enrichment of the carburized layer of nitrogen to a depth of several hundred micrometers.
- the nitrogen content obtained is of the order of 0.2% by weight to a few microns in depth.
- the nitrogen content then decreases slowly from 0.2% for several hundred microns.
- the nitrogen concentration is of the order of 0.2% to 30 ⁇ m, 0.14% to 60 ⁇ m, 0.12% to 130 ⁇ m and 0.05% to 200 ⁇ m.
- the nitriding gas can be injected during step H of temperature rise, as soon as the temperature in the chamber 14 exceeds a given temperature, and / or during the equalizing step PH in temperature.
- the nitriding gas is ammonia
- the injection can be performed as soon as the temperature in the enclosure 14 exceeds about 800 ° C.
- Injecting the nitriding gas only during the carbon diffusion stages allows better nitrogen and carbon enrichment of the treated parts and allows to obtain, in a precise and reproducible way, the carbon and carbon concentration profiles. desired nitrogen. Indeed, if the nitriding gas is injected simultaneously with the carburizing gas, there is a dilution of the carburizing gas and the nitriding gas. This is not a factor favoring the reaction of carbon from the carburising gas or the reaction of the nitrogen from the nitriding gas with the parts to be treated, which slows the enrichment of the parts in nitrogen and carbon.
- the control of the gaseous environment in the chamber 14 can hardly be carried out accurately, which makes it more difficult to obtain accurately and reproducibly, desired nitrogen and carbon component concentration profiles.
- the diffusion of nitrogen in steel parts being, for the same processing conditions, faster than the diffusion of carbon, the injection of the nitriding gas and the cementation gas at different stages makes it possible to modify more easily the injection time of each gas while ensuring the maintenance of a constant pressure in the chamber 14.
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Abstract
Description
La présente invention concerne les procédés de traitement de pièces en acier, et plus particulièrement les procédés de carbonitruration, c'est-à-dire d'introduction de carbone et d'azote au niveau de la surface de pièces en acier pour en améliorer la dureté et la tenue en fatigue.The present invention relates to processes for treating steel parts, and more particularly to carbonitriding processes, that is to say introducing carbon and nitrogen at the surface of steel parts to improve its performance. hardness and fatigue resistance.
Il existe plusieurs types de procédés de carbonitruration de pièces en acier permettant l'introduction de carbone et d'azote au niveau de la surface des pièces jusqu'à des profondeurs pouvant atteindre plusieurs centaines de micromètres.There are several types of carbonitriding processes for steel parts that allow the introduction of carbon and nitrogen at the surface of parts to depths of up to several hundred micrometers.
Une première catégorie de procédés de carbonitruration correspond aux procédés de carbonitruration dits à haute pression dans la mesure où l'enceinte contenant les pièces à traiter est maintenue à une pression généralement proche de la pression atmosphérique pendant toute la durée du traitement. Un tel procédé consiste, par exemple, à maintenir les pièces à un palier de température, par exemple à environ 880°C, tout en alimentant l'enceinte avec un mélange gazeux constitué de méthanol et d'ammoniac. L'étape de carbonitruration est suivie d'une étape de trempe, par exemple une trempe à l'huile, et éventuellement d'une étape d'écrouissage des pièces traitées.A first category of carbonitriding processes corresponds to so-called high-pressure carbonitriding processes insofar as the enclosure containing the workpieces is maintained at a pressure generally close to atmospheric pressure for the duration of the treatment. Such a process consists, for example, in maintaining the parts at a temperature level, for example at about 880 ° C., while supplying the enclosure with a gaseous mixture consisting of methanol and ammonia. The carbonitriding step is followed a quenching step, for example an oil quenching, and optionally a hardening step of the treated parts.
Une seconde catégorie de procédés de carbonitruration correspond aux procédés de carbonitruration dits à basse pression ou à pression réduite, dans la mesure où l'enceinte contenant les pièces à traiter est maintenue à une pression généralement inférieure à quelques centaines de pascals (quelques millibars).A second category of carbonitriding processes corresponds to so-called low pressure or reduced pressure carbonitriding processes, insofar as the enclosure containing the workpieces is maintained at a pressure generally less than a few hundred pascals (a few millibars).
La publication
La
La
Un inconvénient du premier exemple de procédé de carbonitruration décrit dans la publication
Un inconvénient du second exemple de procédé de carbonitruration décrit dans la publication
Le document
La présente invention prévoit un procédé de carbonitruration à basse pression de pièces en acier qui permet d'obtenir, de façon précise et reproductible, les profils de concentrations de carbone et d'azote souhaités dans les pièces traitées.The present invention provides a method of low-pressure carbonitriding of steel parts which allows to obtain, in a precise and reproducible manner, the desired carbon and nitrogen concentration profiles in the treated parts.
Un autre objet de la présente invention est de prévoir un procédé de carbonitruration dont la mise en oeuvre est compatible avec le traitement de pièces en acier dans un contexte industriel.Another object of the present invention is to provide a carbonitriding process whose implementation is compatible with the treatment of steel parts in an industrial context.
Dans ce but, la présente invention prévoit un procédé de carbonitruration d'une pièce en acier disposée dans une enceinte maintenue à une pression interne réduite, la pièce étant maintenue à un palier de température. Le procédé comporte une alternance de premières et de secondes étapes, un gaz de cémentation étant injecté dans l'enceinte seulement pendant les premières étapes et un gaz de nitruration étant injecté dans l'enceinte seulement pendant au moins une partie d'au moins deux secondes étapes.For this purpose, the present invention provides a method of carbonitriding a steel part disposed in an enclosure maintained at a reduced internal pressure, the part being maintained at a temperature step. The method comprises an alternation of first and second stages, a carburizing gas being injected into the chamber only during the first stages and a nitriding gas being injected into the chamber only for at least a portion of at least two seconds steps.
Selon un mode de réalisation, le gaz de cémentation est le propane ou l'acétylène et le gaz de nitruration est l'ammoniac.According to one embodiment, the carburising gas is propane or acetylene and the nitriding gas is ammonia.
Selon un mode de réalisation, un gaz neutre est injecté dans l'enceinte simultanément au gaz de nitruration.According to one embodiment, a neutral gas is injected into the chamber simultaneously with the nitriding gas.
Selon un mode de réalisation, le gaz de nitruration est injecté dans l'enceinte au cours d'au moins une seconde étape pendant une durée inférieure à la durée de ladite seconde étape, le reste de ladite seconde étape étant réalisé en présence d'un gaz neutre.According to one embodiment, the nitriding gas is injected into the chamber during at least a second step for a duration less than the duration of said second step, the rest of said second step being carried out in the presence of a neutral gas.
Selon un mode de réalisation, les premières et secondes étapes sont réalisées à une pression constante inférieure à 1500 pascals.According to one embodiment, the first and second steps are performed at a constant pressure of less than 1500 pascals.
Selon un mode de réalisation, le palier de température est compris entre 800°C et 1050°C.According to one embodiment, the temperature plateau is between 800 ° C and 1050 ° C.
Selon un mode de réalisation, le palier de température est supérieur à 900°C.According to one embodiment, the temperature plateau is greater than 900 ° C.
Ces objets, caractéristiques et avantages, ainsi que d'autres de la présente invention seront exposés en détail dans la description suivante d'exemples de réalisation particuliers faite à titre non-limitatif en relation avec les figures jointes parmi lesquelles :
- les
figures 1 et 2 , précédemment décrites, illustrent des exemples classiques de procédé de carbonitruration à basse pression ; - la
figure 3 représente schématiquement un exemple de réalisation d'un four de carbonitruration à basse pression ; - la
figure 4 illustre un exemple de procédé de carbonitruration à basse pression selon la présente invention ; - la
figure 5 représente un exemple de profil de concentration d'azote obtenu dans des pièces en acier traitées selon un exemple de procédé de carbonitruration à basse pression de l'invention ; - les
figures 6, 7 et 8 illustrent respectivement un autre exemple de procédé de carbonitruration selon l'invention et les profils de concentration de carbone et d'azote obtenus pour un tel procédé de carbonitruration ; et - les
figures 9, 10 et 11 illustrent respectivement un autre exemple de procédé de carbonitruration selon l'invention et les profils de concentration de carbone et d'azote obtenus pour un tel procédé de carbonitruration.
- the
Figures 1 and 2 , previously described, illustrate conventional examples of low pressure carbonitriding process; - the
figure 3 schematically represents an embodiment of a low pressure carbonitriding furnace; - the
figure 4 illustrates an example of a low pressure carbonitriding process according to the present invention; - the
figure 5 represents an example of a nitrogen concentration profile obtained in treated steel parts according to an exemplary low pressure carbonitriding process of the invention; - the
Figures 6, 7 and 8 illustrate respectively another example of the carbonitriding process according to the invention and the carbon and nitrogen concentration profiles obtained for such a carbonitriding process; and - the
Figures 9, 10 and 11 illustrate respectively another example of the carbonitriding process according to the invention and the carbon and nitrogen concentration profiles obtained for such a carbonitriding process.
La présente invention consiste à réaliser dans une enceinte, contenant des pièces en acier à traiter maintenues à une température sensiblement constante, une alternance d'étapes d'enrichissement en carbone pendant lesquelles un gaz de cémentation est injecté dans l'enceinte sous une pression réduite et d'étapes de diffusion du carbone pendant lesquelles l'injection du gaz de cémentation est interrompue. La présente invention consiste à prévoir l'injection, dans l'enceinte, d'un gaz de nitruration pendant la totalité ou une partie des étapes de diffusion du carbone. Les étapes d'enrichissement en carbone correspondent alors à des étapes de diffusion de l'azote. Le gaz de nitruration est injecté pendant au moins une partie d'au moins deux étapes de diffusion de carbone, c'est-à-dire pendant au moins une partie d'une étape de diffusion du carbone intercalée entre deux étapes d'enrichissement en carbone. Ceci permet avantageusement de contrôler, de façon précise et reproductible, les profils de concentrations de carbone et d'azote obtenus dans les pièces traitées puisque l'injection du gaz de nitruration est réalisée séparément de l'injection du gaz de cémentation. En outre, comme l'injection du gaz de nitruration est réalisée pendant les étapes de diffusion du carbone, la durée totale du traitement de carbonitruration est sensiblement analogue à un traitement de cémentation classique.The present invention consists in producing in an enclosure, containing steel parts to be treated maintained at a substantially constant temperature, an alternation of carbon enrichment stages during which a carburizing gas is injected into the chamber under a reduced pressure. and carbon diffusion steps during which the injection of the carburizing gas is interrupted. The present invention consists in providing for the injection into the chamber of a nitriding gas during all or part of the carbon diffusion steps. The carbon enrichment steps then correspond to nitrogen diffusion steps. The nitriding gas is injected during at least a portion of at least two carbon diffusion steps, i.e. during at least a portion of a carbon diffusion step sandwiched between two enrichment stages. carbon. This advantageously makes it possible to control, in a precise and reproducible manner, the carbon and nitrogen concentration profiles obtained in the treated parts since the injection of the nitriding gas is carried out separately from the injection of the carburizing gas. In addition, since the injection of the nitriding gas is carried out during the carbon diffusion steps, the total duration of the carbonitriding treatment is substantially similar to a conventional cementation treatment.
La
La
L'étape PH est suivie d'une alternance d'étapes d'enrichissement en carbone C1 à C4, pendant lesquelles un gaz de cémentation est injecté dans l'enceinte 14, et d'étapes de diffusion du carbone D1 à D4 pendant lesquelles le gaz de cémentation n'est plus injecté dans l'enceinte 14. A titre d'exemple, quatre étapes d'enrichissement C1 à C4 et quatre étapes de diffusion D1 à D4 sont représentées en
Le gaz de cémentation est par exemple du propane (C3H8) ou de l'acétylène (C2H2). Il peut aussi s'agir de tout autre hydrocarbure (CXHY) susceptible de se dissocier aux températures de l'enceinte pour cémenter la surface des pièces à traiter. Le gaz de nitruration est par exemple de l'ammoniac (NH3). En reprenant le schéma de la
L'injection du gaz de nitruration peut être réalisée seulement pendant certaines des étapes de diffusion. En outre, pendant une étape de diffusion au cours de laquelle du gaz de nitruration est injecté, l'injection du gaz de nitruration peut être réalisée seulement pendant une partie de l'étape de diffusion. Un gaz neutre, par exemple de l'azote (N2), peut être injecté pendant la totalité des étapes d'enrichissement et de diffusion, seulement pendant les étapes de diffusion, ou seulement pendant une partie des étapes de diffusion. L'injection du gaz neutre est régulée de façon à maintenir constante la pression dans l'enceinte 14. Lorsque du gaz de nitruration et du gaz neutre sont injectés simultanément, les proportions relatives du gaz de nitruration et du gaz neutre sont déterminées en fonction du profil de concentration d'azote souhaité dans les pièces traitées. En outre, les proportions relatives du gaz de nitruration et du gaz neutre peuvent être différentes pour chaque étape de diffusion pendant laquelle du gaz de nitruration et du gaz neutre sont injectés simultanément dans l'enceinte 14.Injection of the nitriding gas can be performed only during some of the diffusion steps. In addition, during a diffusion step during which nitriding gas is injected, the injection of the nitriding gas can be carried out only during part of the diffusion step. A neutral gas, for example nitrogen (N 2 ), may be injected during all the enrichment and diffusion steps, only during the diffusion steps, or only during part of the diffusion steps. The injection of the neutral gas is regulated so as to maintain constant the pressure in the
Selon une variante de réalisation de l'invention, certains gaz injectés dans l'enceinte 14 du four 10 peuvent être mélangés avant l'injection dans l'enceinte 14. Une telle variante permet par exemple, lors des étapes de montée en température H et d'égalisation de température PH, d'injecter directement dans l'enceinte 14 un mélange d'azote et d'hydrogène du type contenant une proportion d'hydrogène inférieure à 5 % en volume, une telle proportion d'hydrogène excluant tout risque d'explosion.According to an alternative embodiment of the invention, certain gases injected into the
Selon le présent exemple de réalisation de l'invention, le procédé de carbonitruration est mis en oeuvre sans variation de pression et les injections, du gaz de cémentation et du gaz de nitruration (et/ou éventuellement du gaz neutre), lors des étapes d'enrichissement et de diffusion, sont successives et la substitution entre le gaz de cémentation et le gaz de nitruration (et/ou éventuellement le gaz neutre) est susceptible de se produire très rapidement.According to the present embodiment of the invention, the carbonitriding process is carried out without pressure variation and the injections, carburizing gas and nitriding gas (and / or optionally neutral gas), during the steps of enrichment and diffusion, are successive and the substitution between the carburizing gas and the nitriding gas (and / or possibly the neutral gas) is likely to occur very quickly.
La
Les
Les
La demanderesse a mis en évidence que l'injection d'ammoniac pendant les étapes de diffusion permet un enrichissement de la couche cémentée en azote sur une profondeur de plusieurs centaines de micromètres. Pour les trois exemples représentés, la teneur en azote obtenue est de l'ordre de 0,2 % en poids à quelques micromètres de profondeur. La teneur en azote décroît alors lentement à partir de 0,2 % pendant plusieurs centaines de micromètres. A titre d'exemple, pour l'exemple de réalisation précédemment décrit en relation aux
Selon une variante de l'invention, le gaz de nitruration peut être injecté pendant l'étape H de montée en température, dès que la température dans l'enceinte 14 dépasse une température donnée, et/ou pendant l'étape PH d'égalisation en température. A titre d'exemple, lorsque le gaz de nitruration est l'ammoniac, l'injection peut être réalisée dès que la température dans l'enceinte 14 dépasse environ 800°C.According to a variant of the invention, the nitriding gas can be injected during step H of temperature rise, as soon as the temperature in the
Le fait d'injecter le gaz de nitruration seulement pendant les étapes de diffusion du carbone permet un meilleur enrichissement en azote et en carbone des pièces traitées et permet d'obtenir, de façon précise et reproductible, les profils de concentrations de carbone et d'azote souhaités. En effet, si le gaz de nitruration est injecté simultanément au gaz de cémentation, il se produit une dilution du gaz de cémentation et du gaz de nitruration. Ceci n'est pas un facteur favorisant la réaction du carbone issu du gaz de cémentation ou la réaction de l'azote issu du gaz de nitruration avec les pièces à traiter, ce qui ralentit l'enrichissement des pièces en azote et en carbone. En outre, si le gaz de cémentation et le gaz de nitruration sont mélangés, le contrôle de l'ambiance gazeuse dans l'enceinte 14 peut difficilement être effectué avec précision, ce qui rend plus difficile l'obtention, de façon précise et reproductible, des profils de concentrations des pièces en azote et en carbone souhaités. En outre, la diffusion de l'azote dans des pièces en acier étant, pour des mêmes conditions de traitement, plus rapide que la diffusion du carbone, l'injection du gaz de nitruration et du gaz de cémentation à des étapes distinctes permet de modifier plus facilement la durée d'injection de chaque gaz tout en assurant le maintien d'une pression constante dans l'enceinte 14.Injecting the nitriding gas only during the carbon diffusion stages allows better nitrogen and carbon enrichment of the treated parts and allows to obtain, in a precise and reproducible way, the carbon and carbon concentration profiles. desired nitrogen. Indeed, if the nitriding gas is injected simultaneously with the carburizing gas, there is a dilution of the carburizing gas and the nitriding gas. This is not a factor favoring the reaction of carbon from the carburising gas or the reaction of the nitrogen from the nitriding gas with the parts to be treated, which slows the enrichment of the parts in nitrogen and carbon. In addition, if the carburizing gas and the nitriding gas are mixed, the control of the gaseous environment in the
Bien entendu, la présente invention est susceptible de diverses variantes et modifications qui apparaîtront à l'homme de l'art. A titre d'exemple, l'étape de trempe au gaz précédemment décrite peut être remplacée par une étape de trempe à l'huile.Of course, the present invention is susceptible of various variations and modifications which will be apparent to those skilled in the art. For example, the previously described gas quenching step can be replaced by an oil quenching step.
Claims (8)
- A method for carbonitriding a steel part arranged in an enclosure (14) maintained at a reduced internal pressure, the part being maintained at a temperature level, characterized in that it comprises an alternation of first and second steps, a carburizing gas being injected into the enclosure during the first steps only and a nitriding gas being injected into the enclosure only during at least part of at least two second steps.
- The method of claim 1, in which the carburizing gas is propane or acetylene.
- The method of claim 1, in which the nitriding gas is ammonia.
- The method of claim 1, in which a neutral gas is injected into the enclosure (14) simultaneously with the nitriding gas.
- The method of claim 1, in which the nitriding gas is injected into the enclosure (14) during at least a second step for a time shorter than the duration of said second step, the rest of the second step being carried out in the presence of a neutral gas.
- The method of claim 1, in which the first and second steps are performed at a constant pressure lower than 1,500 pascals.
- The method of claim 1, in which the temperature level ranges between 800°C and 1050°C.
- The method of claim 1, in which the temperature level is higher than 900°C.
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FR0550996A FR2884523B1 (en) | 2005-04-19 | 2005-04-19 | LOW PRESSURE CARBONITRUTING PROCESS AND FURNACE |
PCT/FR2006/050357 WO2006111683A1 (en) | 2005-04-19 | 2006-04-19 | Low pressure carbonitriding method and device |
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EP1885904A1 EP1885904A1 (en) | 2008-02-13 |
EP1885904B1 true EP1885904B1 (en) | 2009-12-09 |
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EP (1) | EP1885904B2 (en) |
JP (1) | JP5046245B2 (en) |
KR (1) | KR101328110B1 (en) |
CN (1) | CN100569992C (en) |
AT (1) | ATE451484T1 (en) |
BR (1) | BRPI0608493A2 (en) |
CA (1) | CA2604785C (en) |
DE (1) | DE602006010997D1 (en) |
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- 2006-04-19 KR KR1020077026914A patent/KR101328110B1/en active IP Right Grant
- 2006-04-19 CA CA2604785A patent/CA2604785C/en active Active
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Cited By (8)
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FR2981947A1 (en) * | 2011-10-31 | 2013-05-03 | Peugeot Citroen Automobiles Sa | LOW PRESSURE CARBONITRURATION PROCESS AT EXTENDED TEMPERATURE RANGE IN AN INITIAL NITRIDATION PHASE |
FR2981948A1 (en) * | 2011-10-31 | 2013-05-03 | Peugeot Citroen Automobiles Sa | LOW PRESSURE CARBONITRURATION PROCESS WITH REDUCED GRADIENT TEMPERATURE IN AN INITIAL NITRIDATION PHASE |
WO2013064335A1 (en) * | 2011-10-31 | 2013-05-10 | Peugeot Citroen Automobiles Sa | Method for low-pressure carbonitriding having an extended temperature range in an initial nitridation phase |
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CN103946412A (en) * | 2011-10-31 | 2014-07-23 | 标致·雪铁龙汽车公司 | Method for low-pressure carbonitriding using a reduced temperature gradient in an initial nitridation phase |
US9708704B2 (en) | 2011-10-31 | 2017-07-18 | Ecm Technologies | Method for low-pressure carbonitriding using a reduced temperature gradient in an initial nitridation phase |
US9765422B2 (en) | 2011-10-31 | 2017-09-19 | Ecm Technologies | Method for low-pressure carbonitriding having an extended temperature range in an initial nitridation phase |
CN108893705A (en) * | 2018-07-17 | 2018-11-27 | 嘉兴合邦机械科技有限公司 | A kind of vacuum nitriding processing technology |
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DE602006010997D1 (en) | 2010-01-21 |
JP5046245B2 (en) | 2012-10-10 |
JP2008538386A (en) | 2008-10-23 |
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US8784575B2 (en) | 2014-07-22 |
US8303731B2 (en) | 2012-11-06 |
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BRPI0608493A2 (en) | 2010-01-05 |
US20110036462A1 (en) | 2011-02-17 |
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MX2007012964A (en) | 2007-12-10 |
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