EP0370838B1 - Verfahren zum Schutz der Oberflächen von Metallteilen gegen Hochtemperaturkorrosion sowie dadurch behandeltes Teil - Google Patents

Verfahren zum Schutz der Oberflächen von Metallteilen gegen Hochtemperaturkorrosion sowie dadurch behandeltes Teil Download PDF

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Publication number
EP0370838B1
EP0370838B1 EP89402753A EP89402753A EP0370838B1 EP 0370838 B1 EP0370838 B1 EP 0370838B1 EP 89402753 A EP89402753 A EP 89402753A EP 89402753 A EP89402753 A EP 89402753A EP 0370838 B1 EP0370838 B1 EP 0370838B1
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Prior art keywords
accordance
plating
phase
treatment
nickel
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Expired - Lifetime
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EP89402753A
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English (en)
French (fr)
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EP0370838A1 (de
Inventor
Serge Alperine
Pierre Josso
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Office National dEtudes et de Recherches Aerospatiales ONERA
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Office National dEtudes et de Recherches Aerospatiales ONERA
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
    • 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
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/02—Pretreatment of the material to be coated
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12875—Platinum group metal-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12931—Co-, Fe-, or Ni-base components, alternative to each other

Definitions

  • the invention relates to protection against corrosion at high temperature of metallic materials, and more particularly of materials based on nickel, cobalt and / or iron, including steels.
  • the invention relates more particularly to superalloys, in particular nickel-based, used for the manufacture of hot parts of a turbomachine, for example fixed or mobile turbine blades and distributors, which must have excellent resistance to oxidation and to corrosion at high temperature, in particular in the presence of molten sodium sulphate from the spray and sulfur impurities contained in the fuel.
  • a known protection method for this purpose consists in forming, by deposition and / or diffusion on the surface of the substrate to be protected, a layer containing a nickel, cobalt and / or iron aluminide, by a treatment comprising bringing into contact. of the part to be treated with a filler material containing aluminum.
  • the filler material comprises an alloy with chromium base comprising aluminum in a proportion by weight of 5 to 25% and, optionally, silicon in a proportion by weight of 3 to 10%, and the parts to be treated are brought into contact with the finely divided filler material, under a hydrogenated atmosphere, at a temperature between 750 and 1200 ° C.
  • the aluminization treatment can be either the low activity aluminization already mentioned, or a variant thereof called high activity aluminization, or another type of treatment, for example a vapor phase aluminization such as that designated under the reference RT22 by the Chromalloy Company.
  • High activity aluminization differs from low activity aluminization described above in that the metallic part of the filler material is composed by weight of 55 to 70% aluminum and 45 to 30% chromium, in that that the treatment temperature is between 650 and 750 ° C, and preferably equal to approximately 700 ° C, its duration being between 7 and 8 hours and preferably equal to approximately 7 hours 30.
  • This high activity deposit is followed by a post-diffusion treatment in a non-oxidizing atmosphere (argon or hydrogen), the duration and temperature of which vary depending on the substrate.
  • argon or hydrogen non-oxidizing atmosphere
  • a nickel or chromium pre-deposit precedes the platinum mine metal pre-deposit or accompanies the aluminization treatment.
  • platinum mine metal in the pre-deposit treatment is platinum itself, which significantly improves the protection provided by the aluminization treatment.
  • platinum has the disadvantage of being very expensive.
  • the object of the invention is to obtain an aluminide coating modified by a pre-deposit containing palladium, by avoiding the occlusion of hydrogen or any other gas capable of causing the phenomenon of blistering.
  • the invention relates to a method of protecting the surface of a metallic substrate based on nickel, cobalt and / or iron, comprising a pre-deposition treatment followed by a deposition treatment, the deposition treatment comprising the deposition and / or the diffusion of aluminum on the surface of the pretreated substrate and the pre-deposit treatment comprising one or more successive phases during which are provided with material which is deposited and / or which is diffused on the surface of the substrate, the composition of the filler material being able to be different from one phase to another and said filler material containing , during at least one phase, palladium, characterized in that palladium is the only metal of the platinum mine present in the filler material and that this contains, during any phase for which it contains palladium and / or at least one subsequent phase of the pre-deposition treatment, at least one barrier metal chosen from nickel, cobalt and chromium.
  • the pretreated substrate can in particular be brought into contact with a filler material containing aluminum and chromium.
  • a deposition treatment is, for example, a high activity or low activity aluminization as defined above.
  • At least one phase of the pre-deposition treatment can comprise a deposition operation of filler material at low temperature followed by a diffusion operation at high temperature under vacuum, this diffusion operation being carried out, preferably, at a temperature of about 850 ° C under an air pressure at most equal to 1.3 mPa (10 ⁇ 5 torr).
  • At least one phase of the pre-deposition treatment comprises the deposition and / or diffusion of a palladium alloy and at least one barrier metal.
  • the pre-deposit treatment can then comprise a single material supply phase.
  • the filler material in a first phase of the pre-deposition treatment, is formed essentially of palladium, and in a second phase subsequent to the first, the filler material is formed essentially of at least one barrier metal.
  • first phase and second phase do not refer here to the absolute position of the phases in the course of the pre-deposit processing but are simply used to identify one compared to the other the two phases considered.
  • the first and second phases can then follow each other directly and constitute, for example, the only two phases of supply of material from the pre-deposit treatment.
  • the invention applies more particularly to a nickel-based substrate, the aluminide being essentially a nickel aluminide and the barrier metal preferably also being essentially nickel.
  • this advantageously comprises approximately 80% of palladium and 20% of nickel by weight and can be deposited for example by electrolytic means.
  • the first can be deposited chemically autocatalytically and the second by triode sputtering.
  • a pre-deposit of pure palladium 8 ”m thick was sprayed on an IN100 superalloy substrate. cathode triode. The sample was then subjected to a 2-hour heat treatment to diffuse the pre-deposit at 850 ° C, under a total air pressure at most equal to 1.3 mPa (10 ⁇ 5 torr). A high activity type nickel aluminide coating as defined above was then produced on this sample by activated case hardening in a pack. At the end of the final post-diffusion operation, the surface of the sample was covered with a very large number of blisters ( Figure 1).
  • Such a coating surface condition makes the material unusable for turbomachine components.
  • the sample was then subjected to a high temperature corrosion test consisting of thermal cycling in an air oven between temperatures of about 850 ° C and 200 ° C, with one hour increments at 850 ° C and with periodic contamination of the sample with sodium sulfate at a rate of 0.5 mg / cm2 every 50 cycles.
  • This test is representative of the stresses on the components of the hot parts of the turbomachinery under so-called hot corrosion conditions.
  • the resistance of the coating to hot corrosion has been found to be very low.
  • the degraded state of the sample is critical (Figure 2) and there is significant pitting corrosion.
  • the mass gain is very high ( Figure 3, curve A).
  • the behavior of this sample is comparable to that of a sample having undergone a conventional high activity aluminization in the absence of any pre-deposit, as can be seen in Figure 3 where curve B relates to this last sample.
  • Example 2 The procedure was as in Example 1, replacing the high activity aluminization by an aluminization of the standard low activity type. The same result was obtained (see FIG. 3, curve E), FIGS. 6 and 7 showing the sample respectively before and after the corrosion test.
  • Example 1 differs from Example 1 only in the pre-filing processing.
  • the latter here comprises two phases of material input.
  • the first phase approximately 8 ⁇ m of pure palladium was deposited by autocatalytic chemistry.
  • the sample was then subjected to a 2 hour diffusion heat treatment at 850 ° C under a total air pressure at most equal to 1.3 mPa (10 ⁇ 5 torr).
  • a deposit of approximately 3 m of pure nickel was applied by triode sputtering.
  • the sample then underwent a second diffusion heat treatment identical to the first.
  • FIG. 8 shows that the sample obtained is free from all blisters and has an integrity condition.
  • Example 4 The procedure was as in Example 4, but omitting the diffusion heat treatment between the palladium deposit and the nickel deposit.
  • the surface of the sample was free of any blistering and its surface condition was integrity.
  • Example 5 The procedure was as in Example 5, replacing the deposit of nickel with a deposit of approximately 3 m of cobalt by electrolytic route under the conditions below: Composition of the bath: - hydrated cobalt sulfate: 175 g / l - cobalt chloride: 80 g / l - boric acid : 20 g / l Current density between 2 and 4 A / dm2 Temperature: 45 ° C.
  • Example 7 The procedure was as in Example 7, replacing the low activity aluminide coating with a standard high activity aluminide coating.
  • Example 9 The procedure was as in Example 9, replacing the low activity aluminide coating with a standard high activity type aluminide coating.
  • the pre-deposit can be carried out in particular by chemical, electrolytic, thermochemical, physical or by spraying.
  • the aluminization can be carried out in particular by diffusion or by chemical, electrolytic, thermochemical or physical way.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Physical Vapour Deposition (AREA)

Claims (18)

  1. Verfahren zum Oberflächenschutz eines Metallsubstrats auf der Basis von Nickel, Kobalt und/oder Eisen, das eine Vorabscheidungsbehandlung gefolgt von einer Abscheidungsbehandlung umfaßt, wobei die Abscheidungsbehandlung die Abscheidung und/oder die Diffusion von Aluminium an der Oberfläche des vorbehandelten Substrats umfaßt und die Vorabscheidungsbehandlung eine oder mehrere aufeinanderfolgende Phasen umfaßt, in deren Verlauf Material zugeführt wird, das an der Oberfläche des Substrats aufgebracht und/oder diffundiert wird, wobei die Zusammensetzung des Zufuhrmaterials von einer Phase zur anderen unterschiedlich sein kann und das Zufuhrmaterial wenigstens während einer Phase Palladium enthält,
    dadurch gekennzeichnet,
    daß Palladium das einzige Metall des Platinerzes ist, das in dem Zufuhrmaterial vorliegt, und daß dieses während der gesamten Phase, in der es Palladium enthält, und/ oder wenigstens einer späteren Phase der Vorabscheidungsbehandlung wenigstens ein Sperrmetall enthält, das aus Nickel, Kobalt und Chrom ausgewählt ist.
  2. Verfahren nach Anspruch 1,
    dadurch gekennzeichnet,
    daß das vorbehandelte Substrat bei der Abscheidungsbehandlung mit einem Zufuhrmaterial in Kontakt gebracht wird, das Aluminium und Chrom enthält.
  3. Verfahren nach Anspruch 2,
    dadurch gekennzeichnet,
    daß die Abscheidungsbehandlung eine hochaktive Veraluminierung ist.
  4. Verfahren nach Anspruch 2,
    dadurch gekennzeichnet,
    daß die Abscheidungsbehandlung eine schwachaktive Veraluminierung ist.
  5. Verfahren nach einem der vorhergehenden Ansprüche,
    dadurch gekennzeichnet,
    daß wenigstens eine Phase der Vorabscheidungsbehandlung einen Abscheidungsvorgang eines Zufuhrmaterials bei niedriger Temperatur gefolgt von einem Diffusionsvorgang bei hoher Temperatur unter Vakuum umfaßt.
  6. Verfahren nach Anspruch 5,
    dadurch gekennzeichnet,
    daß der Diffusionsvorgang bei einer Temperatur von etwa 850°C unter einem Luftdruck von wenigstens gleich 1,3 mPA (10⁻⁵ Torr) durchgeführt wird.
  7. Verfahren nach einem der vorhergehenden Ansprüche,
    dadurch gekennzeichnet,
    daß wenigstens eine Phase der Vorabscheidungsbehandlung die Abscheidung und/oder die Diffusion einer Palladiumlegierung und wenigstens eines Sperrmetalls beinhaltet.
  8. Verfahren nach Anspruch 7,
    dadurch gekennzeichnet,
    daß die Vorabscheidungsbehandlung eine einzige Materialzufuhrphase aufweist.
  9. Verfahren nach einem der Ansprüche 1 bis 6,
    dadurch gekennzeichnet,
    daß das Zufuhrmaterial in einer ersten Phase der Vorabscheidungsbehandlung im wesentlichen aus Palladium und in einer zweiten, auf die erste Phase folgenden Phase im wesentlichen aus wenigstens einem Sperrmetall gebildet ist.
  10. Verfahren nach Anspruch 9,
    dadurch gekennzeichnet,
    daß die zweite Phase direkt auf die erste Phase folgt.
  11. Verfahren nach Anspruch 10,
    dadurch gekennzeichnet,
    daß die Vorabscheidungsbehandlung zwei Materialzufuhrphasen beinhaltet.
  12. Verfahren nach einem der vorhergehenden Ansprüche,
    dadurch gekennzeichnet,
    daß das Substrat Nickel als Basis hat, daß das Aluminid im wesentlichen ein Nickelaluminid ist, und daß das Sperrmetall im wesentlichen Nickel ist.
  13. Verfahren nach einem der Ansprüche 7 und 8,
    dadurch gekennzeichnet,
    daß die Legierung etwa 80 Gew.% Palladium und 20 Gew.% Nickel aufweist.
  14. Verfahren nach Anspruch 13,
    dadurch gekennzeichnet,
    daß die Legierung auf elektrolytischem Wege aufgebracht wird.
  15. Verfahren nach einem der Ansprüche 9 bis 11,
    dadurch gekennzeichnet,
    daß das Zufuhrmaterial der ersten Phase im wesentlichen Palladium und das der zweiten Phase im wesentlichen Nickel ist.
  16. Verfahren nach Anspruch 15,
    dadurch gekennzeichnet,
    daß das Palladium auf autokatalytischem, chemischem Wege und das Nickel durch Trioden-Kathodensputtern aufgebracht werden.
  17. Metallteil auf der Basis von Nickel, Kobalt und/oder Eisen, das durch das Verfahren nach einem der vorhergehenden Ansprüche geschützt ist.
  18. Teil nach Anspruch 17,
    dadurch gekennzeichnet,
    daß es zur Bildung eines heißen Teils einer Turbomaschine bestimmt ist.
EP89402753A 1988-10-26 1989-10-05 Verfahren zum Schutz der Oberflächen von Metallteilen gegen Hochtemperaturkorrosion sowie dadurch behandeltes Teil Expired - Lifetime EP0370838B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8813991 1988-10-26
FR8813991A FR2638174B1 (fr) 1988-10-26 1988-10-26 Procede de protection de surface de pieces metalliques contre la corrosion a temperature elevee, et piece traitee par ce procede

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Publication Number Publication Date
EP0370838A1 EP0370838A1 (de) 1990-05-30
EP0370838B1 true EP0370838B1 (de) 1994-07-20

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US (1) US4962005A (de)
EP (1) EP0370838B1 (de)
JP (1) JP2700931B2 (de)
DE (1) DE68916914T2 (de)
FR (1) FR2638174B1 (de)

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Also Published As

Publication number Publication date
JPH02277784A (ja) 1990-11-14
JP2700931B2 (ja) 1998-01-21
DE68916914D1 (de) 1994-08-25
US4962005A (en) 1990-10-09
FR2638174A1 (fr) 1990-04-27
EP0370838A1 (de) 1990-05-30
DE68916914T2 (de) 1994-12-15
FR2638174B1 (fr) 1991-01-18

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