EP2773788A1 - Method for low-pressure carbonitriding having an extended temperature range in an initial nitridation phase - Google Patents
Method for low-pressure carbonitriding having an extended temperature range in an initial nitridation phaseInfo
- Publication number
- EP2773788A1 EP2773788A1 EP12772301.3A EP12772301A EP2773788A1 EP 2773788 A1 EP2773788 A1 EP 2773788A1 EP 12772301 A EP12772301 A EP 12772301A EP 2773788 A1 EP2773788 A1 EP 2773788A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- temperature
- phase
- nitriding
- pressure carbonitriding
- low pressure
- 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.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000005256 carbonitriding Methods 0.000 title claims abstract description 16
- 238000010791 quenching Methods 0.000 claims abstract description 13
- 230000000171 quenching effect Effects 0.000 claims abstract description 11
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 9
- 239000010959 steel Substances 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 238000005121 nitriding Methods 0.000 claims description 52
- 230000000630 rising effect Effects 0.000 claims 1
- 230000007423 decrease Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 3
- 238000005255 carburizing Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
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
- C23C8/28—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
- C23C8/02—Pretreatment of the material to be coated
-
- 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
-
- 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
Definitions
- the present invention relates to a low-pressure carbonitriding process for steel parts, including, but not limited to, parts used in the manufacture of motor vehicles.
- the invention also applies to parts used in the manufacture of agricultural machinery, machine tool, or parts in the aeronautical field.
- a low pressure carbonitriding process of steel parts comprising alternating steps of carburizing and nitriding at a constant temperature, preceded by a temperature rise step comprising a single temperature rise phase followed by an initial nitriding phase with continued rise in temperature, and followed by a quenching step, wherein the initial nitriding phase is carried out from a temperature between 700 ° C and 750 ° C, and up to a temperature between 860 ° C and 1000 ° C.
- the initial nitriding phase is immediately followed by a first step of cementation.
- the total elimination of the temperature equalization phase makes it possible to lengthen the initial nitriding phase in an optimum temperature range for nitriding.
- the temperature rise is performed with a reduced temperature gradient compared to the simple temperature rise phase.
- the treatment time is further increased in an optimum temperature range for nitriding.
- the method comprises a final nitriding step accompanied by a lowering temperature immediately before quenching.
- the final nitriding step is also carried out in an optimum temperature range, so that the quality of the treatment is improved.
- the method according to the invention comprises a first step of temperature rise comprising a first phase M of simple temperature rise, illustrated by a line in continuous line, from room temperature to at a point at a temperature of 700 ° C, denoted Ni 1 in the figure.
- the simple temperature rise phase can be carried out up to a temperature of between 700 ° C. and 750 ° C., and has a duration of between 10 minutes and 90 minutes. that is to say that the simple temperature rise is carried out with a temperature gradient of between 8 ° C./min and 75 ° C./min.
- the method then comprises an initial nitriding phase Ni with continuation of the temperature rise step to a temperature of 940 ° C in the example shown.
- the temperature of 940 ° C corresponds to a compromise between a temperature of 860 ° C which allows a treatment of better quality and a temperature of 1000 ° C which allows for faster processing.
- the rise in temperature continues on a regular basis but with a temperature gradient of between 3.5 ° C / min and 16 ° C / min less than the temperature gradient during the simple temperature rise.
- the duration of the initial nitriding phase is between 15 minutes and 45 minutes, depending on the amount of nitrogen that it is desired to set in this initial step and the composition of the steel to be treated.
- the initial nitriding phase comprises injection phases of a nitriding gas such as alternating ammonia with diffusion phases.
- the rise in temperature continues with the same temperature gradient as during the single temperature rise to a point at a temperature comprised between between 750 ° C and 850 ° C, here 800 ° C, denoted Ni2 in the figure.
- the temperature is then maintained in a step until a moment noted Ni3 in Figure 2 from which a high temperature rise is performed to reach the carburizing temperature.
- the temperature of the bearing is chosen in a manner known per se to perform the initial nitriding phase under optimal conditions given the composition of the parts to be treated. Note in this connection that because of the bearing, the final temperature rise can be carried out very rapidly, for example 80 ° C / min at 100 ° C / min without subjecting the parts to unacceptable constraints.
- the rise in temperature continues from the point Ni 1 with a lower temperature gradient than in the first mode. embodiment, preferably in a range of 2 ° C / min to 8 ° C / min, up to a moment noted Ni4, here corresponding to a temperature of 850 ° C, from which a high temperature rise is achieved to reach the carburising temperature, according to a gradient similar to that of the second embodiment.
- the method then comprises n alternating carburizing phases with nitriding phases.
- the carburizing and nitriding steps comprise alternating treatment gas injection phases with diffusion phases not shown in the figures.
- the diagram has been interrupted between the nitriding step N1 and the last cementation step Cn.
- the method comprises a final nitriding step Nn accompanied by a temperature drop immediately before the T quenching.
- the temperature is lowered continuously to a temperature within the optimum temperature range for nitriding while remaining high enough to allow effective quenching.
- the final temperature before quenching is 840 ° C.
- satisfactory results are obtained for a final temperature before quenching between 900 ° C. and 800 ° C. It has been found that this limited descent of temperature decreases the stress on the parts during quenching.
- the final nitriding step has a duration of preferably between 15 minutes and 60 minutes, which corresponds to a temperature gradient of between 10 ° C / min and 1 ° C / min.
- the final nitriding step preferably comprises alternating nitriding gas injection phases with diffusion phases.
- the temperature drop is first of all carried out in a strong manner, with a gradient as strong as possible without creating undue stresses in the steel, up to the optimum nitriding temperature for the steel being treated, noted Nn1 in the figure, here 840 ° C, then the temperature is maintained at a level until the beginning of the quench.
- the method according to the invention can be implemented by combining any of the embodiments of the initial nitriding phase with any of the embodiments of the final nitriding phase, or even finish the treatment cycle so conventional, that is to say with a quench performed directly from the carburizing temperature.
- the initial rise in temperature can be carried out according to a constant gradient as illustrated by a dashed line in the figure.
- the nitriding phase has a shortened duration as illustrated by a mixed line in the figure. Due to the reduced temperature gradient during the initial nitriding phase, it has been experimented that the temperature of the workpieces has time to equalize so that it is possible to eliminate the equalization step provided in the aforementioned document. If this is necessary, for example because of a particular configuration of the parts to be treated, it may however provide a temperature equalization step of reduced duration between the initial nitriding phase and the first cementation step.
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)
- Heat Treatment Of Articles (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR1159875A FR2981947B1 (en) | 2011-10-31 | 2011-10-31 | LOW PRESSURE CARBONITRURATION METHOD AT EXTENDED TEMPERATURE RANGE IN AN INITIAL NITRIDATION PHASE |
PCT/EP2012/069888 WO2013064335A1 (en) | 2011-10-31 | 2012-10-08 | Method for low-pressure carbonitriding having an extended temperature range in an initial nitridation phase |
Publications (2)
Publication Number | Publication Date |
---|---|
EP2773788A1 true EP2773788A1 (en) | 2014-09-10 |
EP2773788B1 EP2773788B1 (en) | 2019-02-20 |
Family
ID=47018193
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP12772301.3A Active EP2773788B1 (en) | 2011-10-31 | 2012-10-08 | Method for low-pressure carbonitriding having an extended temperature range in an initial nitridation phase |
Country Status (9)
Country | Link |
---|---|
US (1) | US9765422B2 (en) |
EP (1) | EP2773788B1 (en) |
JP (1) | JP6189849B2 (en) |
KR (1) | KR101945006B1 (en) |
CN (1) | CN103946411B (en) |
BR (1) | BR112014010314A2 (en) |
FR (1) | FR2981947B1 (en) |
MX (1) | MX359961B (en) |
WO (1) | WO2013064335A1 (en) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102013006589A1 (en) * | 2013-04-17 | 2014-10-23 | Ald Vacuum Technologies Gmbh | Method and device for the thermochemical hardening of workpieces |
FR3004731B1 (en) * | 2013-04-18 | 2016-05-13 | Peugeot Citroen Automobiles Sa | THERMO-CHEMICAL PROCESSING METHOD COMPRISING A SINGLE NITRIDING PHASE BEFORE CEMENTATION |
FR3028530B1 (en) | 2014-11-14 | 2020-10-23 | Peugeot Citroen Automobiles Sa | PROCESS AND PLANT FOR CARBONITRURING STEEL PART (S) UNDER LOW PRESSURE AND HIGH TEMPERATURE |
CN105420663B (en) * | 2015-11-20 | 2018-07-10 | 贵州师范大学 | A kind of surface treatment method of titanium alloy compound carbonitriding |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR1159875A (en) | 1956-10-17 | 1958-07-03 | Machal Projecteurs | Flashing device |
JPH02294461A (en) * | 1989-05-09 | 1990-12-05 | Mazda Motor Corp | Carburizing treating method for steel member |
KR930007148B1 (en) | 1990-03-27 | 1993-07-30 | 마쓰다 가부시끼가이샤 | Heat treating apparatus |
FR2777911B1 (en) * | 1998-04-28 | 2000-07-28 | Aubert & Duval Sa | LOW PRESSURE CARBONITRURATION OF METAL ALLOY PARTS |
JP3960697B2 (en) * | 1998-12-10 | 2007-08-15 | 株式会社日本テクノ | Carburizing and carbonitriding methods |
EP1454998B1 (en) | 2001-12-13 | 2010-02-10 | Koyo Thermo Systems Co., Ltd. | Vacuum carbo-nitriding method |
PL204747B1 (en) * | 2002-10-31 | 2010-02-26 | Politechnika & Lstrok Odzka | Method of metal product carburization under negative pressure |
JP2006002194A (en) * | 2004-06-16 | 2006-01-05 | Nsk Ltd | Method for manufacturing shaft |
JP4655528B2 (en) * | 2004-07-12 | 2011-03-23 | 日産自動車株式会社 | Manufacturing method of high-strength machine structure parts and high-strength machine structure parts |
FR2884523B1 (en) * | 2005-04-19 | 2008-01-11 | Const Mecaniques Sa Et | LOW PRESSURE CARBONITRUTING PROCESS AND FURNACE |
JP5295813B2 (en) * | 2009-02-17 | 2013-09-18 | Dowaサーモテック株式会社 | Method for nitriding iron group alloys |
DE102009002985A1 (en) * | 2009-05-11 | 2010-11-18 | Robert Bosch Gmbh | Process for carbonitriding |
DE102010028165A1 (en) * | 2010-04-23 | 2011-10-27 | Robert Bosch Gmbh | Process for the carbonitriding of metallic components |
-
2011
- 2011-10-31 FR FR1159875A patent/FR2981947B1/en not_active Expired - Fee Related
-
2012
- 2012-10-08 BR BR112014010314A patent/BR112014010314A2/en active Search and Examination
- 2012-10-08 EP EP12772301.3A patent/EP2773788B1/en active Active
- 2012-10-08 JP JP2014539273A patent/JP6189849B2/en active Active
- 2012-10-08 CN CN201280053989.1A patent/CN103946411B/en active Active
- 2012-10-08 MX MX2014005219A patent/MX359961B/en active IP Right Grant
- 2012-10-08 US US14/354,418 patent/US9765422B2/en active Active
- 2012-10-08 KR KR1020147015029A patent/KR101945006B1/en active IP Right Grant
- 2012-10-08 WO PCT/EP2012/069888 patent/WO2013064335A1/en active Application Filing
Non-Patent Citations (1)
Title |
---|
See references of WO2013064335A1 * |
Also Published As
Publication number | Publication date |
---|---|
EP2773788B1 (en) | 2019-02-20 |
WO2013064335A1 (en) | 2013-05-10 |
FR2981947B1 (en) | 2014-01-03 |
BR112014010314A2 (en) | 2017-05-02 |
CN103946411B (en) | 2016-01-20 |
US20140238549A1 (en) | 2014-08-28 |
MX359961B (en) | 2018-10-17 |
US9765422B2 (en) | 2017-09-19 |
CN103946411A (en) | 2014-07-23 |
FR2981947A1 (en) | 2013-05-03 |
JP2014532808A (en) | 2014-12-08 |
US20170241008A9 (en) | 2017-08-24 |
KR101945006B1 (en) | 2019-02-01 |
MX2014005219A (en) | 2015-03-09 |
KR20140101751A (en) | 2014-08-20 |
JP6189849B2 (en) | 2017-08-30 |
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