WO2018086930A1 - Method for the heat treatment of a workpiece consisting of a high-alloy steel - Google Patents
Method for the heat treatment of a workpiece consisting of a high-alloy steel Download PDFInfo
- Publication number
- WO2018086930A1 WO2018086930A1 PCT/EP2017/077741 EP2017077741W WO2018086930A1 WO 2018086930 A1 WO2018086930 A1 WO 2018086930A1 EP 2017077741 W EP2017077741 W EP 2017077741W WO 2018086930 A1 WO2018086930 A1 WO 2018086930A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- workpiece
- temperature
- process gas
- holding phase
- treatment step
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
- C21D1/76—Adjusting the composition of the atmosphere
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/06—Surface hardening
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
- C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
-
- 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
- C23C8/08—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
- C23C8/24—Nitriding
- C23C8/26—Nitriding of ferrous surfaces
Definitions
- the present invention relates to a method of heat treating a high alloy steel workpiece.
- nitriding near-surface areas. By nitriding, different nitrides separate within the metallic material in the
- the nitriding is i.a. also used for high-alloy steels in particular for components such as nozzle body, valve body or throttle plates.
- Alloy elements a natural oxide layer of a few nanometers. This oxide layer is formed on contact with air and consists for example of chromium oxide, vanadium oxide, iron oxide and other oxides. Since the oxide layer is very compact and partially diffusion-tight, subsequent diffusion of nitrogen at elevated temperatures, in particular between 480 ° C and 590 ° C can be adversely affected and even completely prevented. inhomogeneous
- the naturally occurring oxide layer can be removed, for example, chemically via a pickling process with an acid prior to the actual nitration process. Furthermore, the oxide layer can also be removed mechanically by brushing and / or grinding, or else electrically by the application of a corresponding voltage.
- EP 1 122 331 Bl is a method for heat treatment of metallic workpieces, in particular for nitriding or nitrocarburizing of alloyed
- the workpieces are heated in a nitriding oven to a temperature between 400 ° C and 500 ° C in an ammonia-containing
- Temperature is heated between 500 ° C and 700 ° C in a gas atmosphere containing ammonia and an added oxidant.
- the workpieces are exposed to this temperature and this gaseous atmosphere for a period of up to 5 hours.
- the made of a high-alloy steel workpiece is in a
- Vacuum environment heated to a first temperature the first
- Temperature is kept constant during a first holding phase, wherein the workpiece is then heated to a second temperature higher than the first temperature, wherein the second temperature is kept constant during a second holding phase, and wherein the workpiece preferably after the second holding phase in gaseous , or evaporating media is quenched.
- a surface of the workpiece, in particular also the inner contours, are dispensed with a hydrogen during the first holding phase in a first treatment step
- Process gas and / or process gas mixture for cleaning and activation of the surface flows around, wherein the surface is flowed around during the first holding phase in a second treatment step with a nitrogen-emitting process gas and / or process gas mixture to form a thin nitride-containing layer, and wherein the nitride-containing layer is provided to optimize a downstream gas nitriding process.
- the heat treatment according to the invention is divided in the
- tempering of the workpieces is a second heat treatment.
- Heat treatment step instead, in which by means of gas nitriding at preferably 480 - 590 ° C required for the workpiece, in particular the workpiece surface properties are adjusted by diffusing nitrogen into the workpiece.
- Atmosphere prevents or slows down the formation of a new one
- holding phase is to be understood as meaning the constant holding of a temperature at which the workpiece determines the internal temperature of the vacuum furnace
- the high-alloy steel is in a first
- Treatment step flows around a hydrogen-releasing process gas and / or process gas mixture.
- the injection of the gas takes place constantly.
- the flowing around of the workpiece in the first treatment step constitutes a cleaning and activating step to prevent the nitrogen from diffusing into the surface of the steel in the second processing step due to the surface cleaned and activated thereby and the high temperature
- Treatment step is preferably between 800 and 1090 ° C, preferably at 900 ° C, to an optimal interaction of the hydrogen-emitting process gas and / or process gas mixture with the surface of the To ensure workpiece.
- the oxide layer is broken and repassivation of the surface by means of the vacuum is prevented.
- the surface of the workpiece is thus highly reactive to the diffusion of nitrogen in the second treatment step.
- Treatment step at the constant first temperature of the furnace is flowed around with a nitrogen-emitting process gas and / or process gas mixture to form a nitride-containing layer.
- N2 pure nitrogen
- N H3 ammonia
- High-alloyed steels are preferably suitable for nitriding, since the
- Alloy elements of these steels preferably connect with the atomic nitrogen to nitrides.
- unalloyed steels can form brittle nitriding layers that tend to flake off during nitriding.
- Particularly suitable for nitriding are steels with carbon contents between 0.3 and 0.6% by mass and alloying elements such as chromium or vanadium
- Vacuum environment and the cleaning and activation by the hydrogen-releasing process gas and / or process gas mixture forms a homogeneous and dense nitride layer on the surface during nitriding in the second treatment step of the curing process.
- This nitride layer can be regarded as a seed layer or passivation layer, since the actual nitriding step takes place only after tempering and before the hard machining of the workpiece.
- the pre-nitriding in the hardening process also optimizes the gas nitriding in the downstream production step. Due to the homogeneous seed layer from the hardening process, gas nitriding forms in the chamber furnace
- the nitriding effect which is described with the help of the so-called nitriding index, is correspondingly higher due to the pre-nitriding in the hardening process.
- the nitriding index results from the partial pressures of the nitrogen donating Process gas and / or process gas mixture and the partial pressure of hydrogen. The higher the nitriding index, the stronger the potential for nitride formation. If the nitrogen content in the material exceeds the maximum
- Solubility of nitrogen in the base material is formed by nitrides. Directly on the surface, these nitride precipitates form the bonding layer.
- this area is called a diffusion layer.
- this area are small nitride precipitates as well as dissolved in the metal lattice nitrogen available.
- iron is formed into iron nitrides, and in high-alloy steels, for example, chromium and vanadium combine to form corresponding nitrides. Because of the nitriding in the hardening process a nitrided
- Seed layer is present, a lower nitriding ratio is required in the nitriding process, whereby the process management is facilitated and simplified.
- the gas nitriding process can thereby be shortened and / or carried out at lower temperatures, which additionally makes the process more cost-effective.
- the nitrided layer makes after the hardening process
- composition of the steel more special carbides eliminated as well as a lower hardness can be adjusted without an interaction of the
- the high-alloy steel is heated to the second temperature.
- the second temperature is also to be understood as austenitizing temperature.
- the high-alloy steel is essentially ferrite and carbide, which converts to austenite at high temperatures and the carbides partially dissolve. The aim is therefore the high solubility of
- the duration of the second treatment step, the second temperature of the high-alloy steel during the second treatment step and / or the nitrogen partial pressure on the surface of the high-alloy steel during the second treatment step are preferably selected so that the nitride-containing layer having a thickness of less than 2 ⁇ m, preferably with a thickness of 0.001 ⁇ to 1 ⁇ , is formed.
- the nitride-containing layer preferably has sheet-like or crystalline
- Chromium can form sheet-shaped nitrides, with iron preferably forming crystalline nitrides.
- the hydrogen-emitting process gas and / or process gas mixture flows around the surface at a first treatment pressure and the nitrogen-emitting process gas and / or process gas mixture flows around the surface at a second treatment pressure, the respective
- the selected pressure range is highly dependent on the properties of the workpiece.
- the first treatment pressure is less than the second
- Treatment pressure The higher the second treatment pressure, the greater the potential for nitride formation in the region near the edge of the workpiece, and the lower the nitrogen diffuses into the workpiece.
- Figure 1 shows the course of the temperature T and the pressure p over time in an embodiment of the inventive method
- Figure 1 shows an example of the process control for an embodiment of the method according to the invention.
- the left ordinate 4 describes the temperature axis
- the right ordinate 5 describes the partial pressure axis
- the abscissa 6 describes the time axis.
- the upper continuous curve indicates the course of the temperature T over time.
- the lower continuous curve indicates the course of the partial pressure p over time.
- sections AI, Hl, A2, H2, F and Bl and B2 are defined, in which different activities take place.
- a first heating phase AI the workpiece S is first of
- the vacuum furnace in which the process is carried out is under a technical vacuum, with a negative pressure of less than 50 mbar ( Figure 2). Furthermore, it is also conceivable that the vacuum to produce only after reaching a certain temperature.
- the first temperature Tl is kept constant at about 900 ° C.
- the heating phase AI no hydrogen or nitrogen-containing process gas or process gas mixture Gl, G2 is supplied.
- the first treatment step Bl begins, in which the workpiece S is flowed around with a hydrogen-containing process gas or process gas mixture Gl with a first treatment pressure PI.
- the first treatment pressure PI corresponds the acting on the surface 1 of the workpiece S hydrogen partial pressure.
- the partial pressure corresponds to the pressure that would be exerted by the single gas component, in this case hydrogen, when present in a given volume.
- the flow of the hydrogen-containing process gas or process gas mixture G1 is constant (FIG. 3).
- Treatment step B2 in which the workpiece S is flowed around with a nitrogen-containing process gas or process gas mixture G2 with a second treatment pressure P2.
- the second treatment pressure P2 corresponds to the nitrogen partial pressure acting on the surface 1 of the workpiece S.
- the flow of the nitrogenous process gas or process gas mixture G2 is constant ( Figure 4).
- the second treatment pressure P2 is higher than the first treatment pressure PI, wherein the respective treatment pressure PI, P2 is between 10 mbar and 3000 mbar.
- the first holding phase H1 is followed by a second heating phase A2 with a subsequent second holding phase H2.
- the heating rate is constant.
- the workpiece S is first heated from the first temperature Tl to the second temperature T2, which is then kept constant.
- the second temperature T2 corresponds to the
- Austenitizing temperature of the workpiece S In the edge region, a phase transition to an austenitic structure takes place while holding at austenitizing temperature.
- the nitrogen-containing process gas or process gas mixture G2 continues to flow around the workpiece S in the second holding phase H2 with a second treatment pressure P2 and constant flow.
- the second holding phase H2 corresponds to a nitriding phase. Due to the second temperature T2 atomic nitrogen diffuses from the nitrogenous
- nitride-forming alloying elements such as for example, chromium, vanadium or iron.
- Treatment step B2 the second temperature T2 of the workpiece S during the second treatment step B2 and the second treatment pressure B2 on the surface 1 of the workpiece S during the second treatment step B2 affect the thickness of the nitride-containing layer 2, which is between ⁇ . ⁇ and
- the second holding phase H2 and the second treatment step B2 are finally followed by a quenching phase F for setting a substantially martensitic structure.
- the vacuum furnace 3 and the workpiece S are quenched to room temperature.
- FIGS. 2 to 5 describe the method steps according to the invention for the heat treatment of a high-alloy steel
Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP17800725.8A EP3538676B1 (en) | 2016-11-08 | 2017-10-30 | Method for the heat treatment of a workpiece consisting of a high-alloy steel |
CN201780069175.XA CN109923219B (en) | 2016-11-08 | 2017-10-30 | Method for heat treating workpieces made of high-alloy steel |
BR112019008898-9A BR112019008898B1 (en) | 2016-11-08 | 2017-10-30 | PROCESS FOR HOT TREATMENT OF A WORK PIECE CONSISTING OF A HIGH ALLOY STEEL |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102016221891.3 | 2016-11-08 | ||
DE102016221891.3A DE102016221891A1 (en) | 2016-11-08 | 2016-11-08 | Process for the heat treatment of a high-alloy steel workpiece |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2018086930A1 true WO2018086930A1 (en) | 2018-05-17 |
Family
ID=60387985
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2017/077741 WO2018086930A1 (en) | 2016-11-08 | 2017-10-30 | Method for the heat treatment of a workpiece consisting of a high-alloy steel |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP3538676B1 (en) |
CN (1) | CN109923219B (en) |
BR (1) | BR112019008898B1 (en) |
DE (1) | DE102016221891A1 (en) |
FR (1) | FR3058423A1 (en) |
WO (1) | WO2018086930A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111172371A (en) * | 2020-01-16 | 2020-05-19 | 成都航宇超合金技术有限公司 | Method for reducing depth of metal depleted layer on surface of part |
CN113840673A (en) * | 2019-02-26 | 2021-12-24 | 索尼奥环球控股有限责任公司 | High-nitrogen steel powder and manufacturing method thereof |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0516899A1 (en) * | 1991-06-04 | 1992-12-09 | Daido Hoxan Inc. | Method of nitriding steel |
EP1122331B1 (en) | 2000-02-04 | 2003-03-26 | Ipsen International GmbH | Process of nitriding and/or carbonitriding of high-alloyed steel |
EP1612290A1 (en) * | 2004-07-02 | 2006-01-04 | METAPLAS IONON Oberflächenveredelungstechnik GmbH | Process and apparatus for gaseous nitriding of a workpiece and workpiece. |
US20080003376A1 (en) * | 2004-01-30 | 2008-01-03 | Hubert Patrovsky | Nitriding Method for Improving Surface Characteristics of Cobalt-Chromium Based Alloys |
US20100021796A1 (en) * | 2007-03-07 | 2010-01-28 | Nissan Motor Co., Ltd. | Transition metal nitride, separator for fuel cells, fuel cell stack, fuel cell vehicle, method of manufacturing transition metal nitride, and method of manufacturing separator for fuel cells |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101338358B (en) * | 2007-07-05 | 2010-06-02 | 刘正贤 | Method for increasing surface hardness of martensitic stainless steel |
-
2016
- 2016-11-08 DE DE102016221891.3A patent/DE102016221891A1/en not_active Withdrawn
-
2017
- 2017-10-30 CN CN201780069175.XA patent/CN109923219B/en active Active
- 2017-10-30 BR BR112019008898-9A patent/BR112019008898B1/en active IP Right Grant
- 2017-10-30 EP EP17800725.8A patent/EP3538676B1/en active Active
- 2017-10-30 WO PCT/EP2017/077741 patent/WO2018086930A1/en unknown
- 2017-11-07 FR FR1760412A patent/FR3058423A1/en not_active Withdrawn
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0516899A1 (en) * | 1991-06-04 | 1992-12-09 | Daido Hoxan Inc. | Method of nitriding steel |
EP1122331B1 (en) | 2000-02-04 | 2003-03-26 | Ipsen International GmbH | Process of nitriding and/or carbonitriding of high-alloyed steel |
US20080003376A1 (en) * | 2004-01-30 | 2008-01-03 | Hubert Patrovsky | Nitriding Method for Improving Surface Characteristics of Cobalt-Chromium Based Alloys |
EP1612290A1 (en) * | 2004-07-02 | 2006-01-04 | METAPLAS IONON Oberflächenveredelungstechnik GmbH | Process and apparatus for gaseous nitriding of a workpiece and workpiece. |
US20100021796A1 (en) * | 2007-03-07 | 2010-01-28 | Nissan Motor Co., Ltd. | Transition metal nitride, separator for fuel cells, fuel cell stack, fuel cell vehicle, method of manufacturing transition metal nitride, and method of manufacturing separator for fuel cells |
Non-Patent Citations (3)
Title |
---|
JORDAN D ET AL: "Low torr-range vacuum nitriding of 4140 steel", HEAT TREATING PROGRESS, ASM INTERNATIONAL, MATERIALS PARK, OH, US, vol. 8, no. 2, 29 February 2008 (2008-02-29), pages 33 - 38, XP009503102, ISSN: 1536-2558 * |
MENTHE E ET AL: "Further investigation of the structure and properties of austenitic stainless steel after plasma nitriding", SURFACE AND COATINGS TECHNOLOGY, ELSEVIER BV, AMSTERDAM, NL, vol. 116-119, 1 September 1999 (1999-09-01), pages 199 - 204, XP027345973, ISSN: 0257-8972, [retrieved on 19990901] * |
N RENEVIER ET AL: "Low temperature nitriding of AISI 316L stainless steel and titanium in a low pressure arc discharge", SURFACE AND COATINGS TECHNOLOGY, vol. 111, no. 2-3, 1 January 1999 (1999-01-01), AMSTERDAM, NL, pages 128 - 133, XP055445601, ISSN: 0257-8972, DOI: 10.1016/S0257-8972(98)00722-1 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113840673A (en) * | 2019-02-26 | 2021-12-24 | 索尼奥环球控股有限责任公司 | High-nitrogen steel powder and manufacturing method thereof |
CN111172371A (en) * | 2020-01-16 | 2020-05-19 | 成都航宇超合金技术有限公司 | Method for reducing depth of metal depleted layer on surface of part |
Also Published As
Publication number | Publication date |
---|---|
BR112019008898B1 (en) | 2022-08-09 |
BR112019008898A2 (en) | 2019-08-13 |
CN109923219B (en) | 2021-10-12 |
FR3058423A1 (en) | 2018-05-11 |
EP3538676B1 (en) | 2022-01-05 |
EP3538676A1 (en) | 2019-09-18 |
CN109923219A (en) | 2019-06-21 |
DE102016221891A1 (en) | 2018-05-09 |
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