EP0801142B1 - Oberflächenbehandlung eines Metallsubstrates, so hergestelltes Metallsubstrat und seine Anwendungen - Google Patents

Oberflächenbehandlung eines Metallsubstrates, so hergestelltes Metallsubstrat und seine Anwendungen Download PDF

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Publication number
EP0801142B1
EP0801142B1 EP19970400816 EP97400816A EP0801142B1 EP 0801142 B1 EP0801142 B1 EP 0801142B1 EP 19970400816 EP19970400816 EP 19970400816 EP 97400816 A EP97400816 A EP 97400816A EP 0801142 B1 EP0801142 B1 EP 0801142B1
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EP
European Patent Office
Prior art keywords
process according
metal part
surface layer
metal
gaseous
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Expired - Lifetime
Application number
EP19970400816
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English (en)
French (fr)
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EP0801142A2 (de
EP0801142A3 (de
Inventor
Jean-Paul Lebrun
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Nitruvid SA
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Nitruvid SA
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Publication of EP0801142A3 publication Critical patent/EP0801142A3/de
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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
    • C23C8/36—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 using ionised gases, e.g. ionitriding
    • C23C8/38—Treatment 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
    • C23C8/36—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 using ionised gases, e.g. ionitriding

Definitions

  • the present invention relates to a method for processing surface of a metal part, and more particularly, a method of surface hardening by enriching carbon or boron with surface layer located near a surface of the part.
  • a surface treatment of a metal part has been described in which a gas atmosphere containing an element is brought into contact with a surface of the part brought to a temperature between 270 and 550 ° C. interstitial such as carbon or nitrogen, in the ionized state, at a pressure below 1.33.10 -2 mbar (10 mtorr). Due to the low pressure of the gaseous atmosphere, the interstitial content of the surface layer remains low even for treatment times of several hours.
  • these compounds In the case of surface treatment of a steel part stainless, these compounds contain chromium which is taken up in the surface layer of the stainless steel part. This results in a degradation of the part's resistance to corrosion.
  • An object of the present invention is to remedy this drawback by proposing a method for hardening the surface of a part metallic which does not deteriorate its resistance to corrosion.
  • Another object of the present invention is to provide a treatment of the surface of a metal part which can be used industrially, under favorable conditions with regard to costs and duration of treatment.
  • the gaseous compound can consist of a hydrocarbon aliphatic or aromatic or by a cyclan.
  • the gaseous compound can also consist of methane and in this case, the gaseous atmosphere can contain from 5 to 30% in methane volume.
  • the gaseous compound can also consist of a derivative boron gas, for example, a diborane.
  • the gaseous atmosphere may also contain nitrogen or a gaseous derivative of nitrogen such as ammonia.
  • the process applies, in particular, to alloy parts metallic whose structure is face centered cubic, centered cubic or tetragonal, more particularly, to stainless steel parts austenitic or martensitic, with nickel-based alloy parts and to cobalt-based alloy parts.
  • the process can also be applied to alloy parts metallic based on aluminum or based on titanium.
  • the metal part obtained has a surface layer hardened by an interstitial element consisting of at least one of the carbon and boron elements, and optionally, additionally, with nitrogen; the surface layer consists of a homogeneous solid solution free of precipitates containing 5 and 50 atom% and preferably between 10% and 30% interstitial.
  • the part is placed in the enclosure of a treatment furnace surface by plasma.
  • the enclosure is placed under vacuum and then introduced into the enclosure a mixture of gases, the pressure of which is lower than the pressure atmospheric can be between 0.5 and 200 mbar.
  • the mixture of gas consists of a reactive gas on the one hand, and dilution gas on the other parts which are, for example, hydrogen and argon.
  • the reactive gas is a gaseous compound either of carbon or of boron; for example, a aliphatic hydrocarbon, an aromatic hydrocarbon or a cyclane, and, in particular methane, or, for example, a diborane.
  • the mixture gas may also contain a small proportion of a compound nitrogen gas.
  • the gas mixture creating a cold plasma.
  • ionization of the gas mixture creates ions which, by bombarding the surface of the part, can passivate it to make it reactive and heat, and, on the other hand, creates very reactive species of carbon or of boron, which are atoms of which certain electron layers are excited. Highly reactive carbon or boron species react with the surface and penetrate inside by diffusion to form a interstitial solid solution free of precipitates.
  • the surface temperature must be sufficient, and preferably above 300 ° C. But to avoid the formation of precipitated the surface temperature must remain below 460 ° C. So that the penetration of the active elements in the metal takes place satisfactorily it is also necessary that the production of element active on the surface of the part is not too important. Indeed, with the carbon, for example, if the production of active carbon is too fast, it a harmful carbon black deposit forms on the surface of the part for the treatment. To avoid this, the active gas content of the product is limited. gas mixture in order to balance the kinetics of production of active element on the surface of the part, and the kinetics of penetration of the active element in the room.
  • the active gas when the active gas is methane, its content in the gas mixture, is between 5 and 30% and, from preferably around 10%.
  • the gaseous atmosphere in contact with the surface of the part is maintained at a pressure which must be higher at 0.5 and which can go up to 200 mbar.
  • the plasma can be a so-called “discharge plasma", that is to say a plasma generated by an electric discharge between an anode and a cathode, the part to be treated being brought to a cathodic potential and which can itself be the cathode.
  • discharge plasma that is to say a plasma generated by an electric discharge between an anode and a cathode, the part to be treated being brought to a cathodic potential and which can itself be the cathode.
  • the ions are accelerated, they bombard the surface of the part which heats it up enough so that there is no need to provide a means of additional heating.
  • the plasma can also be a plasma generated by a electromagnetic wave generator, or microwave generator, or a "post-discharge" plasma, that is to say a plasma transferred from a plasma generator to the enclosure in which it is located the room.
  • a plasma generated by a electromagnetic wave generator, or microwave generator or a "post-discharge" plasma, that is to say a plasma transferred from a plasma generator to the enclosure in which it is located the room.
  • bombardment of the workpiece surface may be insufficient to cause the necessary heating.
  • we heats the surface of the room for example, by radiation.
  • the duration of the treatment depends on the thickness of the layer treated we want to obtain, this duration can vary between 1 hour and a few tens of hours.
  • the solid solution contains a high proportion of element interstitial, between 5 and 50 atom% and, generally between between 10 and 30 atom%. According to the conditions of implementation of the treatment and in particular, depending on the duration of treatment, it is possible to obtain a hardened surface layer with a thickness of 1 to 60 ⁇ m.
  • the surface layer of the part may present after the treatment of a Vickers Hv hardness greater than 800.
  • This treatment which is applicable to a very wide variety of metal alloys and, in particular, to alloys with a structure face centered cubic, centered cubic or tetragonal (for example, austenitic, ferritic or martensitic stainless steels), allows to obtain a layer 1 to 60 ⁇ m thick, of a solid solution saturated, or even supersaturated, with carbon or boron, homogeneous, that is to say free of carbide or boride precipitates, the hardness of which can be greater than 800 Vickers or even 1000 Vickers and that is very resistant to corrosion. Carbon can be combined with nitrogen to form the layer of solid solution.
  • the alloy is an austenitic steel, the carburetted layer cannot be attacked by chemical reagents commonly used in metallography and has a resistance to attack by salt spray greater than 1000 hours.
  • a second phase we submit the parts to an atmosphere containing carbon in activated form at a temperature generally lower than the treatment temperature during the first phase and for example, between 300 and 350 ° C.
  • the surface layer of the parts is loaded with carbon, so so that a solid solution of carbon in the steel of the nitrogen-laden part, during the first phase.
  • the martensitic steel parts then have both a high wear resistance and very good corrosion resistance.
  • This treatment in two successive phases applies in particular highly stressed martensitic steel mechanical parts such as than parts used in the field of oil drilling or tools or cutting blades.
  • the treatment according to the invention which allows obtain very hard, wear-resistant surface layers and very resistant to corrosion, can be performed on all kinds of parts, and in particular, on any mechanical part subject to wear in corrosive environment (for example: food industry, chemical industry, nuclear industry, marine environment, biomedical applications); mostly austenitic steel container to resist scratching, for example austenitic stainless steel dishes that can be coated before forming; on the blades of sharp stainless steel objects martensitics such as knives and scalpels; on implants orthopedic; on valves; on turbine parts or condensers subject to pitting corrosion.
  • the treatment can, also, be made on a strip or on a metal blank, set work after treatment.
  • the treatment applies in particular, in the case of panels in decorative austenitic stainless steel, for example, with polished panels and / or colored by a process such as anodization.
  • the hardening of the surface of the panels by formation of a solution homogeneous solid of carbon in a surface layer of panels avoids the risk of scratches and degradation of the aesthetic appearance of the panels.

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)

Claims (28)

  1. Verfahren für die Behandlung der Oberfläche eines Metallteils, bei dem mindestens ein interstitielles Element, das aus mindestens einem der Elemente Kohlenstoff und Bor besteht, in die Oberfläche des benachbarten Teils einer Oberfläche des Teils eingeleitet wird, und dieses interstitielle Element im aktivierten Zustand mit der Oberfläche des Teils in Kontakt gebracht wird und dieses interstitielle Element in der Oberfläche des Teils diffundiert wird,
    dadurch gekennzeichnet, dass
    das Teil mindestens in seinem Oberflächenbereich auf eine Temperatur erwärmt wird, die zwischen 300 und 460° C liegt; und
    eine gasförmige Atmosphäre eingehalten wird, welche das aktivierte interstitielle Element enthält und mit der Oberfläche des Teils in Kontakt steht, die auf einem Druck gehalten wird, der zwischen 0,5 und 200 mbar liegt,
    um dadurch in der Oberflächenschicht eine feste Lösung frei von Ablagerungen zu erreichen, die 5 bis 50 Atom-% des interstitiellen Elementes enthalten.
  2. Verfahren nach Anspruch 1,
    dadurch gekennzeichnet, dass
    der Druck der gasförmigen Atmosphäre zwischen 0,5 und 20 mbar liegt.
  3. Verfahren nach einem der Ansprüche 1 und 2,
    dadurch gekennzeichnet, dass
    die gasförmige Atmosphäre in einem kalten Plasma mindestens eine gasförmige Verbindung enthält, die das aktivierte interstitielle Element aufweist.
  4. Verfahren nach Anspruch 3,
    dadurch gekennzeichnet, dass
    die gasförmige Atmosphäre eine Verdünnung der gasförmigen Verbindung enthält, die mindestens aus einem der folgenden Gase besteht: Wasserstoff, Argon, oder einem Gemisch aus Wasserstoff und Argon.
  5. Verfahren nach einem der Ansprüche 3 und 4,
    dadurch gekennzeichnet, dass
    die gasförmige Verbindung aus einem aliphatischen oder aromatischen Kohlenwasserstoff oder einem Cyclan besteht.
  6. Verfahren nach einem der Ansprüche 3 und 4,
    dadurch gekennzeichnet, dass
    die gasförmige Verbindung aus Methan besteht, und dass die Atmosphäre 5 bis 30 Volumen-% Methan enthält.
  7. Verfahren nach einem der Ansprüche 3 und 4,
    dadurch gekennzeichnet, dass
    die gasförmige Verbindung ein gasförmiges Derivat von Bor, wie zum Beispiel ein Diboran ist.
  8. Verfahren nach einem der Ansprüche 3 bis 7,
    dadurch gekennzeichnet, dass
    die gasförmige Atmosphäre außerdem Stickstoff oder ein gasförmiges Derivat von Stickstoff, wie zum Beispiel Ammoniak enthält.
  9. Verfahren nach einem der Ansprüche 3 bis 8,
    dadurch gekennzeichnet, dass
    das Plasma durch eine elektrische Entladung zwischen einer Anode und einer Kathode erzeugt wird, die aus einem Metallteil bestehen kann.
  10. Verfahren nach einem der Ansprüche 3 bis 8,
    dadurch gekennzeichnet, dass
    das Plasma durch einen Generator von Mikrowellen, oder einen Generator von elektromagnetischen Wellen erzeugt und eventuell transferiert wird, um mit der Oberfläche des Teils in Kontakt gebracht zu werden.
  11. Verfahren nach einem der Ansprüche 1 bis 10,
    dadurch gekennzeichnet, dass
    die Oberfläche des Teils durch Bestrahlung erwärmt wird.
  12. Verfahren nach einem der Ansprüche 1 bis 9,
    dadurch gekennzeichnet, dass
    das Teil aus einer metallischen Legierung besteht, dessen Struktur kubisch mit einer zentrierten Fläche, oder kubisch zentriert oder aber tetragonal ist.
  13. Verfahren nach Anspruch 12,
    dadurch gekennzeichnet, dass
    die Legierung des Metalls aus einer der folgenden Legierungen besteht: austenitischer rostfreier Stahl, martensitischer rostfreier Stahl, einer Legierung auf der Grundlage von Nickel, einer Legierung auf der Grundlage von Kobalt.
  14. Verfahren nach Anspruch 12,
    dadurch gekennzeichnet, dass
    die metallische Legierung eine Legierung auf der Basis von Aluminium, oder eine Legierung auf der Basis von Titan ist.
  15. Verfahren nach Anspruch 1 bei einem Teil aus einem rostfreien Martensitstahl,
    dadurch gekennzeichnet, dass
    in einer ersten Phase das Teil einer Stickstoff enthaltenden Atmosphäre bei einer Temperatur zwischen 340 und 450° C, und vorzugsweise einer Temperatur zwischen 350 und 380° unterzogen wird, um eine Oberfläche des Teils mit Stickstoff zu beladen, und
    in einer zweiten Phase das mit Stickstoff beladene Teil bei einer Temperatur, die allgemein niedriger ist, als die Temperatur der Behandlung während der ersten Phase, und die vorzugsweise zwischen 300 und 380° C liegt, einer Atmosphäre unterzogen wird, welche Kohlenstoff im aktivierten Zustand enthält.
  16. Metallteil, das eine Oberfläche aufweist, welche durch ein interstitielles Element gehärtet wurde, das mindestens eines der Elemente Kohlenstoff und Bor und eventuell zusätzlich Stickstoff aufweist,
    dadurch gekennzeichnet, dass
    die Oberflächenschicht aus einer homogenen festen Lösung besteht, die frei von Ablagerungen ist, und die 5 bis 50 Atom-% des interstitiellen Elementes enthält.
  17. Metallteil nach Anspruch 16,
    dadurch gekennzeichnet, dass
    die Oberfläche 10 bis 30 Atom-% des interstitiellen Elementes enthält.
  18. Metallteil nach einem der Ansprüche 16 und 17,
    dadurch gekennzeichnet, dass
    die Oberflächenschicht eine Dicke zwischen 1 und 160 µm hat.
  19. Metallteil nach einem der Ansprüche 16 bis 18,
    dadurch gekennzeichnet, dass
    die Oberfläche eine Vickershärte H über 800 aufweist.
  20. Verwendung eines Metallteils nach einem der Ansprüche 16 bis 19 als Reibteil in korrosiver Umgebung, und insbesondere als Sperrventil, Hahnkegel, Sitz oder Innenhütchen eines Hahns oder Ventils, die in einer korrosiven Umgebung eingesetzt werden.
  21. Verwendung eines Metallteils aus einem rostfreiem Austenitstahl nach einem der Ansprüche 16 bis 19 als Teil einer Schraubverbindung, wie einer Mutter, einer Schraube oder eines Bolzens, die in einer korrosiver Umgebung eingesetzt werden.
  22. Verwendung eines Metallteils aus rostfreiem Austenitstahl nach einem der Ansprüche 16 bis 19 als Verbindungsstück für den Transport von speziellen Fluiden.
  23. Verwendung eines Metallteils nach einem der Ansprüche 16 bis 19 als Transportrolle für Bleche in einer Beizanlage.
  24. Verwendung eines Metallteils nach einem der Ansprüche 16 bis 19 als mobiles Teil einer Pumpe, die in der chemischen Industrie oder der Lebensmittelindustrie eingesetzt wird, wie zum Beispiel ein Kolben, eine Zylinderbuchse, ein Rotor, ein Käfig, eine Führung oder ein Mischgerät.
  25. Verwendung eines Metallteils nach einem der Ansprüche 16 bis 19 als orthopädisches Implantat.
  26. Verwendung eines Metallteils nach einem der Ansprüche 16 bis 19 als poliertes und/oder farbiges Dekorpaneel.
  27. Metallteil nach einem der Ansprüche 16 bis 19,
    dadurch gekennzeichnet, dass
    es aus einem flachen Produkt aus rostfreiem Austenitstahl besteht, das geschmiedet werden soll.
  28. Metallteil nach einem der Ansprüche 16 bis 19,
    dadurch gekennzeichnet, dass
    es aus einem Schneidgerät aus rostfreiem Martensitstahl besteht, wie zum Beispiel einem Messer oder einem Skalpell.
EP19970400816 1996-04-12 1997-04-09 Oberflächenbehandlung eines Metallsubstrates, so hergestelltes Metallsubstrat und seine Anwendungen Expired - Lifetime EP0801142B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9604561 1996-04-12
FR9604561A FR2747398B1 (fr) 1996-04-12 1996-04-12 Procede de traitement de surface d'une piece metallique

Publications (3)

Publication Number Publication Date
EP0801142A2 EP0801142A2 (de) 1997-10-15
EP0801142A3 EP0801142A3 (de) 1998-09-16
EP0801142B1 true EP0801142B1 (de) 2002-07-03

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EP (1) EP0801142B1 (de)
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FR (1) FR2747398B1 (de)

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GB9715180D0 (en) * 1997-07-19 1997-09-24 Univ Birmingham Process for the treatment of austenitic stainless steel articles
FR2807956B1 (fr) * 2000-04-19 2003-10-24 Nitruvid Procede de traitement de surface d'une piece et piece obtenue
GB0209797D0 (en) * 2002-04-29 2002-06-05 Univ Birmingham Method of surface hardening cobalt-chromium based alloy articles
LU90986B1 (en) * 2002-11-07 2004-05-10 Plasma Metal S A Process for nitriding articles in bulk.
FR2888586B1 (fr) * 2005-07-13 2008-01-11 Nitruvid Snc Procede de traitement d'une piece en titane ou alliage de titane et piece obtenue
FR2980804B1 (fr) 2011-09-30 2014-06-27 Areva Np Procede de realisation a partir d'une ebauche en acier inoxydable austenitique a faible teneur en carbone d'une gaine resistant a l'usure et a la corrosion pour reacteur nucleaire, gaine et grappe de commande correspondantes
FR2980803B1 (fr) 2011-09-30 2013-10-25 Areva Np Procede de realisation d'une piece en acier inoxydable resistant a l'usure et a la corrosion pour reacteur nucleaire, piece et grappe de commande correspondantes.
DE102012216117A1 (de) * 2012-09-12 2014-03-13 Hilti Aktiengesellschaft Verfahren zum Herstellen einer selbstschneidenden Schraube
KR101726236B1 (ko) 2012-11-07 2017-04-13 아레바 엔피 부분 및 대응 마스크를 마스킹하면서 부품을 열화학적으로 처리하기 위한 방법
EP2757423B1 (de) 2013-01-17 2018-07-11 Omega SA Bauteil für Uhrwerk
CN108486525A (zh) * 2017-02-22 2018-09-04 学校法人丰田学园 金属制品的制造方法

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FR2653137B1 (fr) * 1989-10-17 1993-06-11 Siderurgie Fse Inst Rech Procede de traitement de surface de produits siderurgiques par action d'un plasma.
GB2261227B (en) * 1991-11-08 1995-01-11 Univ Hull Surface treatment of metals
JP2917810B2 (ja) * 1994-04-28 1999-07-12 住友金属工業株式会社 表面の耐剥離特性に優れた炭窒化処理鋼

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Publication number Publication date
DE69713662D1 (de) 2002-08-08
EP0801142A2 (de) 1997-10-15
DE69713662T2 (de) 2002-12-05
EP0801142A3 (de) 1998-09-16
FR2747398A1 (fr) 1997-10-17
FR2747398B1 (fr) 1998-05-15

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