EP2881492B1 - Procédé de carburation d'un article thermoformé ou d'un article plié-découpé à partir d'acier inoxydable austénitique - Google Patents

Procédé de carburation d'un article thermoformé ou d'un article plié-découpé à partir d'acier inoxydable austénitique Download PDF

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Publication number
EP2881492B1
EP2881492B1 EP13196076.7A EP13196076A EP2881492B1 EP 2881492 B1 EP2881492 B1 EP 2881492B1 EP 13196076 A EP13196076 A EP 13196076A EP 2881492 B1 EP2881492 B1 EP 2881492B1
Authority
EP
European Patent Office
Prior art keywords
gas
gas mixture
article
process step
temperature
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
EP13196076.7A
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German (de)
English (en)
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EP2881492A1 (fr
Inventor
Cord-Hinrich Bremer
Rolf Lange
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.)
Hubert Stueken & Co KG GmbH
Original Assignee
Hubert Stueken & Co KG GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Hubert Stueken & Co KG GmbH filed Critical Hubert Stueken & Co KG GmbH
Priority to EP13196076.7A priority Critical patent/EP2881492B1/fr
Priority to PL13196076T priority patent/PL2881492T3/pl
Priority to US14/557,574 priority patent/US9738962B2/en
Priority to CN201410737053.1A priority patent/CN104451534B/zh
Publication of EP2881492A1 publication Critical patent/EP2881492A1/fr
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Publication of EP2881492B1 publication Critical patent/EP2881492B1/fr
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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
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/20—Carburising
    • C23C8/22—Carburising of ferrous surfaces
    • 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
    • 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

Definitions

  • the invention relates to a method for carburizing a thermoformed article or a stamped and bent article made of austenitic stainless steel with a wall thickness which is at least partially suitable for such articles.
  • customary low wall thicknesses are below 2000 ⁇ m.
  • Such stainless steel articles are made of very thin sheets by tensile or compression bending and sometimes take on very filigree structures.
  • articles with varying or constant wall thickness can be produced, whereby they then have a wall thickness of less than 2000 ⁇ m, at least in regions or as a whole.
  • filigree articles are used in a variety of fields of technology such. used as bearing covers in gearboxes, valve seats in ABS systems or as sample carriers for hazardous substances in high-precision measurements where they are exposed to extreme mechanical, thermal and chemical stresses.
  • the demand for high hardness corrosion resistant materials is therefore correspondingly high.
  • the US 6,461,448 shows a method for carburizing a steel article, wherein said steel article is treated in a Schmelzalkalibad.
  • Such an aggressive type of treatment leads to filigree articles in the context of the invention due to the small wall thickness sometimes severe corrosion phenomena, which has a highly inhomogeneous edge layer result.
  • liquid treatments in filigree articles due to incomplete surface wetting lead to unsatisfactory results.
  • the EP 0 678 589 B1 discloses in this context a method of carburizing an austenitic metal.
  • the metal is exposed to a fluorine-containing gas.
  • Fluorine-containing gases are highly corrosive due to their reactivity and, as a result, aggressively affect the surface of the metal. While the resulting removal of surface is even desirable for articles with high wall thickness due to a corresponding material wealth, it can not be compensated for thin-walled thermoforming and stamping bending articles and leads to the irreversible destruction of the article.
  • the gases used there due to their high toxicity, their high corrosiveness and their highly environmentally hazardous properties enormous demands on the reactor to be used, storage and work safety.
  • the EP 1 553 204 A1 discloses a method of edge hardening an austenitic steel part.
  • the method is characterized in that the steel part is heated in a first process step to a temperature between 200 ° C and 500 ° C for a time between 10 minutes and 3 hours.
  • the heating takes place in an atmosphere consisting of between 0.5 to 20% by volume of a halogen gas or a halide gas and the balance of nitrogen, hydrogen or an inert gas to activate the steel surface.
  • the surface of the steel part is nitrocarburized in a second process step. This is done within a temperature range of 430 ° C to 600 ° C for 20 minutes or more within a mixed atmosphere comprising ammonia for nitrification and carbon monoxide and / or methane for carburizing.
  • D3 discloses a method for carburizing a steel part.
  • the steel part is heated in a first process step to a temperature between 500 ° F and 600 ° F in a halogenated hydrogen atmosphere, preferably HCL or HF.
  • a halogenated hydrogen atmosphere preferably HCL or HF.
  • the activation with strong bases the coating with iron or a treatment in the cyanide melt bath can be used for the activation.
  • the thus activated steel part is then initially heated to a temperature of 1125 ° C.
  • Said initial carburizing temperature is cooled to 925 ° F in the course of the carburizing process.
  • hydrocarbon gases such as methane, ethane and propane, oxygen-containing gases such as carbon monoxide and carbon dioxide or mixtures of these gases such as synthesis gases can be used as the carburizing gas.
  • the EP 1 193 413 A1 discloses a method for carburizing an austenitic steel roller bearing.
  • said roller bearing is activated at a temperature between 200 ° C and 400 ° C a fluorine-containing gas, preferably NF3 in the nitrogen.
  • the activated rolling bearing is treated at a temperature between 460 ° C and 520 ° C with a carburizing gas.
  • Said carburizing gas may consist of either RX gas or a gas containing an unsaturated hydrocarbon, preferably acetylene or ethylene.
  • the EP 0 497 409 A2 discloses a method of edge hardening an austenitic steel part.
  • the steel part is either at a temperature between 250 ° C and 400 ° C in a fluoride-containing gas atmosphere or at a temperature between 100 ° C. and heated at 250 ° C in a fluorine-containing atmosphere.
  • the steel part activated in the first step would be heated in a second process step to a temperature of 530 ° C and treated in an atmosphere consisting of nitrogen and hydrogen over a period of 30 minutes.
  • the activated steel part is then nitrocarborated in an ammonia-containing gas mixture at a temperature of 480 ° C to 700 ° C over a period of three to five hours.
  • the ammonia-containing atmosphere may be formed in particular of ammonia and RX gas or ammonia, carbon dioxide and RX gas.
  • thermoforming and stamping bending articles With the invention, a method with mild conditions is proposed in an advantageous manner, which are tailored to the specifics of thin-walled thermoforming and stamping bending articles.
  • the article is introduced into an oven for carrying out the method. It has been shown that in particular oxygen and water residues interfere with the surface hardening. To exclude these disturbing factors, the article is heated to a temperature which is above the boiling point of water. Preference is given here to a temperature of 110 ° C to 140 ° C, more preferably 120 ° C.
  • the oxygen-containing atmosphere in the furnace is replaced in accordance with the invention by a first gas mixture.
  • the furnace therefore advantageously has gas inlets and gas outlets.
  • the furnace may be provided to flood the furnace with an inert gas before the introduction of the first gas mixture.
  • the oxygen displacement is accelerated in an advantageous manner and a potentially existing hazard potential, resulting from the contact of the oxygen-containing normal atmosphere with the first gas mixture is lowered.
  • the inert gas it is preferable to use known chemically unreactive gases such as, in particular, nitrogen or argon.
  • Stainless steels include, among others, chromium as an alloying constituent. Upon contact with atmospheric oxygen, a passivating and corrosion-resistant chromium (III) oxide layer is formed on the surface of the material.
  • the first gas mixture has reducing properties in order to avoid further oxidation of the chromium.
  • this gas mixture already initiated the depassivation of the surface.
  • the first gas mixture consists of H2 and N2. It has been found that this gas mixture, in particular in conjunction with the mild temperature of the first process step, exerts a particularly mild and advantageous effect on the chromium oxide layer without adversely affecting the morphology of the surface of the filigree articles.
  • the oxygen concentration is measured continuously or at intervals by means of a sensor.
  • a control unit connected to the sensor checks the actual value here continuously or at intervals with a freely selectable desired value and releases the furnace in the case of an identity between the actual and desired value for a second method step.
  • the inventive method is thereby greatly simplified in an advantageous manner and minimizes in this way possible user-side sources of error.
  • a second method step in which the article is heated to the target temperature, the second temperature, for the carburization.
  • the second temperature is chosen so that it is well below the recrystallization temperature of strongly cold-worked iron alloys (680 ° C). A possible change in the morphology of the surface is thereby effectively prevented, whereby the formation of a homogeneous surface layer is promoted.
  • the second temperature is 450 ° C to 550 ° C and preferably 500 ° C.
  • the heating phase serves in particular the careful and complete depassivation of the chromium oxide layer.
  • the heating rate in a certain temperature range between 0.5 and 1 ° C / min, more preferably between 0.5 and 0.7 ° C / min and more preferably 0.5 ° C / min.
  • the temperature range in which this low heating rate is selected is preferably 420 ° C to 550 ° C, more preferably 450 ° C to 500 ° C, and most preferably 480 ° C to 500 ° C.
  • the first gas mixture is replaced by a second gas mixture in the second method step. It has been found that mild depassivation of the thin-walled deep-drawn parts takes place during the heating phase to the second temperature by a gas mixture consisting of H 2 , N 2 and a carbon-containing gas from an unsaturated hydrocarbon.
  • a gas mixture consisting of H 2 , N 2 and a carbon-containing gas from an unsaturated hydrocarbon.
  • the low heating rate may preferably be a particularly slow and therefore mild and easy to control Depassivation of the chromium oxide layer can be achieved.
  • the article is treated with additives which selectively or completely dissolve the passive layer.
  • additives which selectively or completely dissolve the passive layer.
  • it means salt compounds and / or organic substances and acid generators, which are applied in solid or liquid form to the product or in the oven.
  • the application is preferably carried out before the article is placed in the oven or during the second process step.
  • solids and / or liquids are used which form acid reaction products in conjunction with the reaction gases, which would give a pH ⁇ 7 when introduced into water, as the application of the substances has proven particularly advantageous directly on or in the article surface , As a result, local depassivation processes, which initiate and promote uniform depassivation earlier, already occur at low temperatures.
  • an unsaturated hydrocarbon in particular ethyne used.
  • elemental nitrogen is used in the second gas mixture.
  • the temperature is measured continuously or at intervals by means of a sensor.
  • the control unit connected to the sensor checks the actual value here continuously or at intervals with a freely selectable setpoint value for the second temperature and releases the oven in the case of an identity between the actual and setpoint values for a third method step.
  • the inventive method is thereby greatly simplified in an advantageous manner and minimizes in this way possible user-side sources of error.
  • a third method step is provided in which the deep-drawn part is kept constant at the second temperature.
  • the third step in this context serves to carburize the thin-walled deep-drawn part. It has been found that the second temperature advantageously allows a careful construction of the surface layer to be hardened. The diffusion of the carbon into the edge region of the deep-drawn part takes place slowly at these temperatures, is therefore easy to control and causes the formation of a homogeneous carbon-rich surface layer. Too high a temperature is to avoid in any case, as it comes to the formation of irregular layers and the formation of carbide particles due to the high diffusion rate and the high kinetic energy of the molecules involved.
  • the second gas mixture is replaced by a third gas mixture, which is particularly suitable for gentle carburizing under mild conditions.
  • a gas mixture which is composed of a hydrogen-containing gas, a nitrogen-containing gas and a carbon-containing gas. It is further provided according to the invention to add a further carbon-containing component to this gas mixture, whereby the formation of a homogeneous carbon-rich surface layer is promoted by the two different carbon components in a synergetic manner.
  • the carbon-containing component of the second gas mixture according to the invention an unsaturated hydrocarbon, in particular ethyne, is used .
  • the second gas mixture contains elemental nitrogen.
  • the individual concentrations of the gas components are measured continuously or at intervals by means of respective sensors.
  • the control unit connected to the sensors checks the respective actual values here continuously or at intervals with freely selectable desired values for the respective concentration of the gas component and compensates for changes within a fault tolerance continuously or at intervals.
  • the process control is advantageously simplified and allows the provision of constant process conditions, which is for the construction of a homogeneous carbon-rich surface layer of crucial importance.
  • the layer thickness of the carbon-rich surface layer can be adjusted over the gassing time.
  • a period of 2 to 10 hours is required to generate a 10-40 microns thick edge layer.
  • control unit which has a corresponding device for time recording, releases the furnace for the fourth method step after the expiration of a freely selectable carburizing time.
  • the inventive method is thereby greatly simplified in an advantageous manner and minimizes in this way possible user-side sources of error.
  • a fourth method step is provided in which the deep-drawn part is cooled to a third temperature. It is provided here, the deep-drawn part to a temperature of 50 ° C to 80 ° C and more preferably cool to 60 ° C.
  • the choice of atmosphere in the cooled is crucial for the formation of a homogeneous surface layer. It is therefore provided according to the invention to replace the third gas mixture by a fourth gas mixture.
  • the fourth gas mixture consists of a hydrogen-containing gas and a nitrogen-containing gas. It is envisaged here that the fourth gas mixture is formed from H2 and N2.
  • the composition of the fourth gas mixture advantageously from 5% to 25% H2 and 75% to 95% N2, more preferably 5% to 10% H2 and 90% to 95% N2 and more preferably 5% H2 and 95% N2. It has been found that the cooling according to the invention of the thin-walled deep-drawn part effectively prevents the escape of the carbon from the hardened edge layer.
  • the invention relates to an edge-hardened thermoforming article with very small wall thicknesses.
  • the deep-drawing article produced by the method according to the invention has a soft, elastic core with a hardness of 350 to 400 HV1 and a hard carbon-rich surface layer.
  • the edge layer is free of defects and / or particles, circumferentially completely closed and has a substantially planar surface.
  • the thin-walled thermoforming article produced by the method according to the invention has mechanical properties of unprecedented quality.
  • thermoforming article produced by means of the method according to the invention has in its edge region a carbon-rich layer with a hardness of 700 to 1000 HV0.01 and with a layer thickness of 10 to 40 ⁇ m.
  • the corrosion and abrasion resistance of the thermoforming article is better than that of the starting material.
  • the former in particular, is surprising in that carburizing generally worsens the corrosion properties of a steel product.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Heat Treatment Of Articles (AREA)

Claims (5)

  1. Procédé de carburation de paroi mince d'un article thermoformé ou d'un article plié-découpé en acier inoxydable austénitique.
    dans lequel on introduit l'article, qui comprend une épaisseur de paroi de moins de 2000 µm au moins dans quelques parties, dans un fourneau au cours d'une première étape de procédé et on le chauffe à une première température comprise entre 100°C et 140 °C,
    dans lequel on remplace une atmosphère contenant de l'oxygène, qui est présente dans le fourneau, par un premier mélange de gaz, le premier mélange de gaz étant composé de N2 et H2,
    et dans lequel on chauffe l'article à une deuxième température comprise entre 450°C et 550°C au cours d'une deuxième étape de procédé,
    le premier mélange de gaz étant remplacé par un deuxième mélange de gaz, le deuxième mélange de gaz étant composé de H2, N2 et d'un gaz carboné à partir d'un hydrocarbure insaturé,
    et dans lequel on maintient l'article à la deuxième température au cours d'une troisième étape de procédé,
    le deuxième mélange de gaz étant remplacé par un troisième mélange de gaz, le troisième mélange de gaz consistant en un gaz contenant de l'hydrogène, un gaz contenant de l'azote, un premier gaz carboné et un deuxième gaz carboné, le deuxième gaz carboné étant un gaz différent du premier gaz carboné,
    et dans lequel on refroidit l'article à une troisième température comprise entre 50°C et 80°C au cours d'une quatrième étape de procédé.
    le troisième mélange de gaz étant remplacé par un quatrième mélange de gaz, le quatrième mélange de gaz consistant en N2 et H2.
  2. Procédé selon la revendication 1, caractérisé en ce qu'on mesure une teneur résiduelle en oxygène par moyen d'un capteur au cours de la première étape de procédé, et qu'au moment où une valeur d'oxygène résiduelle, qui peut être choisie librement, est atteinte, on initie la deuxième étape de procédé.
  3. Procédé selon l'une des revendications précédentes 1 ou 2, caractérisé en ce qu'au moment où la deuxième température est atteinte, la troisième étape de procédé sera initiée automatiquement.
  4. Procédé selon l'une des revendications précédentes, caractérisé en ce qu'on traite l'article avec au moins un composé de sel dépassivant.
  5. Procédé selon l'une des revendications précédentes, caractérisé en ce qu'on initie la quatrième étape de procédé dès qu'une durée du traitement, qu'on peut choisir librement, soit échue.
EP13196076.7A 2013-12-06 2013-12-06 Procédé de carburation d'un article thermoformé ou d'un article plié-découpé à partir d'acier inoxydable austénitique Active EP2881492B1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP13196076.7A EP2881492B1 (fr) 2013-12-06 2013-12-06 Procédé de carburation d'un article thermoformé ou d'un article plié-découpé à partir d'acier inoxydable austénitique
PL13196076T PL2881492T3 (pl) 2013-12-06 2013-12-06 Sposób nawęglania wyrobu głęboko tłoczonego lub giętnego wyrobu wykrawanego z austenitycznej, nierdzewnej stali szlachetnej
US14/557,574 US9738962B2 (en) 2013-12-06 2014-12-02 Method for the carburization of a deep-drawn part or a stamped-bent part made of austenitic rustproof stainless steel
CN201410737053.1A CN104451534B (zh) 2013-12-06 2014-12-04 用于对由奥氏体防锈不锈钢制成的深拉件或冲压弯折件渗碳的方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP13196076.7A EP2881492B1 (fr) 2013-12-06 2013-12-06 Procédé de carburation d'un article thermoformé ou d'un article plié-découpé à partir d'acier inoxydable austénitique

Publications (2)

Publication Number Publication Date
EP2881492A1 EP2881492A1 (fr) 2015-06-10
EP2881492B1 true EP2881492B1 (fr) 2017-05-03

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EP13196076.7A Active EP2881492B1 (fr) 2013-12-06 2013-12-06 Procédé de carburation d'un article thermoformé ou d'un article plié-découpé à partir d'acier inoxydable austénitique

Country Status (4)

Country Link
US (1) US9738962B2 (fr)
EP (1) EP2881492B1 (fr)
CN (1) CN104451534B (fr)
PL (1) PL2881492T3 (fr)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4086366A1 (fr) 2014-07-31 2022-11-09 Case Western Reserve University Activation améliorée de métaux à auto passivation
US11193197B2 (en) 2018-06-11 2021-12-07 Swagelok Company Chemical activation of self-passivating metals
US11396692B2 (en) 2019-02-21 2022-07-26 Fluid Controls Private Limited Method of heat treating an article
US11885027B2 (en) 2020-04-29 2024-01-30 Swagelok Company Activation of self-passivating metals using reagent coatings for low temperature nitrocarburization

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DE3933053C1 (fr) 1989-10-04 1990-05-03 Degussa Ag, 6000 Frankfurt, De
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Also Published As

Publication number Publication date
EP2881492A1 (fr) 2015-06-10
CN104451534A (zh) 2015-03-25
US20150159260A1 (en) 2015-06-11
US9738962B2 (en) 2017-08-22
PL2881492T3 (pl) 2017-10-31
CN104451534B (zh) 2018-04-27

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