EP2352856B1 - Couche de protection contre la corrosion à haute température et procédé de fabrication - Google Patents

Couche de protection contre la corrosion à haute température et procédé de fabrication Download PDF

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Publication number
EP2352856B1
EP2352856B1 EP09760703.0A EP09760703A EP2352856B1 EP 2352856 B1 EP2352856 B1 EP 2352856B1 EP 09760703 A EP09760703 A EP 09760703A EP 2352856 B1 EP2352856 B1 EP 2352856B1
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EP
European Patent Office
Prior art keywords
temperature
diffusion
metal
layer
temperature material
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EP09760703.0A
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German (de)
English (en)
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EP2352856A1 (fr
Inventor
Horst Pillhöfer
Markus Niedermeier
Siegfried Seuss
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MTU Aero Engines AG
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MTU Aero Engines GmbH
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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
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/06—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases
    • 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
    • C23C10/06—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases
    • C23C10/08—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases only one element being diffused
    • C23C10/10—Chromising
    • 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
    • C23C10/06—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases
    • C23C10/08—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases only one element being diffused
    • C23C10/10—Chromising
    • C23C10/12—Chromising of ferrous surfaces

Definitions

  • the present invention relates to a method for producing a metal-containing high-temperature protective layer on a metallic high-temperature material, wherein the metal to be deposited is chromium or a chromium-containing alloy and the high-temperature material is a Ni-based alloy and / or a turbine blade material.
  • Oxidation or hot gas corrosion protection layers for protecting metallic materials which are used at high temperatures are known from the prior art. For example, these are in Michael Schütze: Protective Oxide Scales and their Breakdown, John Wiley & Sons Ltd., Chichester, New York, Weinheim, Brisbane, Singapore, Toronto (ISBN: 0-471-95904-9 ).
  • chromium-containing and aluminum-containing layers are used as protective layers, since these form slow-growing chromium oxide or aluminum oxide layers.
  • chromium layers it is known to form these as diffusion layers, wherein initially chromium is deposited electrolytically or via the gas phase in a powder pack in order subsequently to diffuse into the material to be protected.
  • the component to be coated is packed in a powder pack of the so-called.
  • Donor metal wherein in the powder pack in addition an activator is included and provided a neutral filler to avoid agglomeration of the powder can be.
  • the activator is usually a halogen compound, in particular a chlorine compound which is volatile and which takes over the transport of the donor material to the surface to be coated, so that it is deposited there.
  • the high-temperature protective layer is the disadvantages of Avoid prior art and in particular have good mechanical properties in terms of fatigue strength and ductility.
  • the corresponding method should be easy to control and regulate and easy to apply.
  • the invention is based on the recognition that an improvement of the known from the prior art deposition from the gas phase in a powder pack can be achieved in that the component to be coated is not embedded in the powder pack, but arranged at a distance from the donor metal is, so that a pure deposition takes place via the gas phase, wherein the surface to be coated of the high-temperature material is not in contact with solids or liquids, but has only one interface solid / gas. Accordingly, any deposition via the gas phase is conceivable, regardless of how the gas phase is generated.
  • the deposition via the gas phase is possible if, according to the known methods with donor metal particles and an activator, the donor metal particles or the activator are kept at a distance from the surface of the high-temperature material to be coated.
  • the distance here is 0.1 to 200 mm, preferably 0.5 to 50 mm.
  • the donor metal powder may be present in a bed near the surface to be treated.
  • the bulk of the donor metal powder may have a density that includes 80% space fill or less, more preferably 70% space fill or less, to allow for a sufficiently large surface area for the reaction of the donor metal with the activator.
  • the donor metal powder may accordingly be present with an average or maximum particle size of 2 mm or greater, in particular 3 mm or greater, which in turn favors the provision of a sufficient reaction surface of the donor metal.
  • the process is carried out at a process temperature at which on the one hand diffusion of the deposited metal into the high-temperature material takes place and, on the other hand, when using a corresponding chemical vapor deposition process (CVD Chemical Vapor Deposition) with donor metal powder and activator, sufficient metal transport of the metal to be deposited takes place.
  • the activator is preferably chosen so that at the process temperature or diffusion temperature of the activator has a vapor pressure of 0.1 to 600 mbar, preferably 0.5 to 500 mbar.
  • the method which is carried out in the absence of reactive gases, such as oxygen and the like, in a vacuum chamber or comparable reaction chamber, also provides that the corresponding reaction chamber is rinsed before and / or after the coating and / or during a pure diffusion phase, namely in particular with an inert or noble gas, preferably argon.
  • reactive gases such as oxygen and the like
  • a two-stage treatment process can be used.
  • a first process step may be provided in which both deposition of metal for the high-temperature protective layer takes place and at the same time the diffusion of the deposited metal into the high-temperature material takes place.
  • a second method step only a corresponding diffusion of the previously deposited metal can take place, so that the amount of deposited material and / or the diffusion depth can be adjusted in a targeted manner.
  • the process temperature at which deposition as well as diffusion takes place which is therefore also referred to as the diffusion temperature, can be in the range of 900 ° C to 1200 ° C, especially 1100 ° C to 1150 ° C and most preferably in the range of 1130 ° C to 1135 ° C.
  • the holding time, also referred to as the diffusion time, ie the time during which the high-temperature material is kept at the diffusion temperature can be between 2 hours and 15 hours, in particular 4 hours and 8 hours.
  • the pure diffusion phase in which there is no deposition of additional material, 1/10 to 1/15 of the total hold time, in particular 1/12 of the total hold time, ie in particular a quarter of an hour to three quarters of an hour, preferably approximately half an hour.
  • the method can be carried out in a two-shell apparatus, wherein an outer chamber provided around the reaction chamber may have a lower pressure, so that only excess gas can escape from the reaction chamber due to the overpressure, but no impurities can enter the reaction chambers.
  • the method according to the invention can be used in particular for the deposition of a chromium protective layer, specifically on corresponding nickel-base alloys for turbine blades.
  • the donor material may be chromium powder
  • the activator may be a halogen-containing, in particular chlorine-containing compound, in particular a chloride or a halide of a constituent of the high-temperature material or of the metal to be deposited.
  • nickel chlorides, cobalt chlorides, aluminum chlorides or chromium chlorides can be used.
  • the method according to the invention can be used to form a chrome-based ductile gradient protective layer which has a support layer, an inwardly directed diffusion layer and a buildup zone arranged between the diffusion and support layers, the chromium content of the buildup zone being between that of the diffusion layer and the support layer.
  • the support layer has the modification of ⁇ -chromium and a chromium content of 25 to 90% by weight, in particular 30 to 80% by weight.
  • the thickness of the support layer can be selected in the range of 0.1 to 20 .mu.m, in particular 0.2 to 15 microns.
  • the buildup zone may have a chromium content of 15 to 40% by weight and in particular 20 to 30% by weight and a thickness of 2 to 75 ⁇ m, in particular 5 to 50 ⁇ m.
  • the diffusion layer which has a chromium content of 5 to 30% by weight, in particular 10 to 20% by weight may also have a thickness of 2 to 75 .mu.m, in particular 5 to 50 microns.
  • FIG. 1 shows a purely schematic representation of an apparatus for carrying out the coating method according to the invention.
  • the apparatus comprises five process chambers 1, which are of identical construction and stacked one above the other in a reaction space 2, a so-called retort.
  • the reaction space 2 is in turn surrounded by a hood furnace 3, by means of which the corresponding process temperature or diffusion temperature can be adjusted.
  • the hood furnace 3 comprises, for example, an electrical resistance heater 9, which has the electrical connections 10 and 11.
  • the process chambers 1 each have a gas supply 6, which are supplied via a non-illustrated central gas supply with appropriate gas.
  • the gas supply 6 is arranged on the reaction chambers 1 such that a gas stream directed into the reaction chamber 1 is directed onto a powder bed 4 arranged at the bottom of the reaction chamber 1.
  • the powder bed 4 comprises the donor metal or the donor metal alloy, such as For example, chromium or a chromium alloy, which are to be coated in the reaction chambers 1 on the components 5. Since the gas supply lines 6 are directed to the powder bed 4, this can be flushed with a gas flow in an effective manner.
  • the reaction chambers 1 also have gas outlets 7, which in the illustration of FIG. 2 are shown only schematically.
  • the gas outlet 7 can be formed in many different ways as a check valve or as a semi-permeable seal, ie seal with a passage, so that it is ensured that only gas escape from the reaction chambers 1, but no additional gas can get into this. This ensures that when rinsing the reaction chambers 1 corresponding reaction products can be removed from the chamber and in this a clean atmosphere can be adjusted.
  • reaction chamber 2 also has a gas inlet 12 and a gas outlet 8, which is connected, for example, to a gas scrubber 13.
  • a corresponding powder of a donor metal or a donor metal alloy is introduced, for example, a chromium powder.
  • an activator is evenly distributed to the loose bed of the donor metal powder, which has a density of maximum 70 or 80% space utilization.
  • the activator may be, for example, a halogen compound, in particular a chloride of the donor metal or a chloride of the high-temperature material to be coated.
  • nickel-base alloy comprising, for example, nickel, cobalt, aluminum and the like
  • nickel chlorides, cobalt chlorides, aluminum chlorides, chromium chlorides and the like can be used.
  • the component 5 to be coated is arranged in the vicinity of the bed or the powder bed 4, wherein a distance of the surface to be coated is set by the powder bed 4 in the order of 0.5 to 50 mm.
  • the correspondingly prepared reaction chambers 1, which are closed, for example, by a lid, are then stacked on one another in order to be received in the reaction space (retort) 2.
  • the entire structure of stacked reaction chambers 1, which are arranged in the reaction chamber 2 is surrounded by the hood furnace 3, so that by heating the hood furnace 3 located in the powder bed 4 materials and the component to be coated. 5 to be heated.
  • the metal halides or chlorides become volatile and cause them to transport the corresponding metal component, that is to say the donor metal, onto the surface of the component 5, where the donor metal is deposited accordingly.
  • the liberated halogen or chlorine in turn reacts with the donor metal, for example chromium, and thus promotes the donor metal to the surface of the component 5.
  • the process temperature is selected so that the donor metal can diffuse into the component 5, that is, for example, when chromating a nickel-base alloy used for turbine blades, a temperature in the range of 1100 to 1150 ° C., in particular 1130 to 1135 ° C.
  • the component 5 to be coated and the materials located in the process chambers 1 are held for a certain treatment time, which is in the range of 3 to 7 hours, in particular 3.75 to 6.25 Hours, and most preferably in the range of 5 to 6 hours.
  • the coating process can be selected in two stages, by allowing only diffusion of the deposited metal into the component in the second part of the coating process, while preventing further deposition.
  • an inert gas such as argon
  • argon is blown into the reaction chambers 1 via the gas feeds 6 of the reaction chambers 1, so that the halogen compounds which are required for transporting the donor metal to the component surface are flushed out via the gas outlets 7, which are permeable only in one direction.
  • the reaction gases are also removed from the reaction space 2, wherein a purification of the exhaust gas via the gas scrubber 13 takes place.
  • the second part of the treatment process only the diffusion is maintained, since the process or diffusion temperature is maintained.
  • the second part of the treatment can be about 1/10 to 1/15 of the total holding time, preferably 1/12 of the holding time, the holding period being the time at which the desired diffusion temperature is reached in the reaction chamber 1. Due to the two-stage process with on the one hand simultaneous deposition and diffusion of the layer material in the first process part and on the other hand, the process section in which only a diffusion takes place, the amount of deposited material and thus the thickness of the deposited layer can be varied and adjusted.
  • the reaction space 2 can be purged with an inert gas, such as argon, in order to remove process gases leaving the reaction chambers 1.
  • an inert gas such as argon
  • the pressure in the reaction chamber 2 is kept lower than in the reaction chambers 1, to allow only a gas flow from the reaction chambers 1 in the reaction chamber 2.
  • the method can be carried out such that the flushing rate is adjusted such that a 10 to 1000 times replacement of the process chamber volume or of the powder bed volume takes place at the end of the process.
  • the chromation according to the invention is a layer in the modification of the ⁇ -chromium, wherein the chromium content may vary between 25 and 80% by weight.
  • the layer thickness can be between 0.2 ⁇ m and 15 ⁇ m.
  • the buildup zone 21 has a lower chromium content in the range of 15 to 30% by weight of chromium and a layer thickness of 5 ⁇ m and 50 ⁇ m.
  • the inner chromium diffusion layer 22 has the lowest chromium content in the range of 5 to 20% by weight with a layer thickness of 5 ⁇ m and 50 ⁇ m.
  • the support layer 20 apart from the deposited chromium, there may also be elements made of the material of the component to be coated, for example nickel, cobalt, aluminum and the like.

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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)
  • Turbine Rotor Nozzle Sealing (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Claims (13)

  1. Procédé de fabrication d'une couche de protection réfractaire contenant du métal sur un matériau réfractaire métallique (5), le métal à déposer étant du chrome ou un alliage contenant du chrome et le matériau réfractaire étant un alliage à base de Ni et/ou un matériau d'aube de turbine,
    comprenant les étapes suivantes
    - dépôt de chrome pour la formation de la couche de protection réfractaire sur le matériau réfractaire en passant par la phase gazeuse, le matériau réfractaire étant conservé pendant un certain temps à une température de diffusion, de telle sorte qu'au moins une partie du métal déposé diffuse dans le matériau réfractaire pour former une zone de diffusion,
    - pas de mise en contact du matériau réfractaire avec des solides ou liquides dans la zone de la surface à revêtir, mais celui-ci présente uniquement une interface solide-gaz,
    - chauffage de particules de métal donneur et d'un activateur à une température telle que le métal donneur se dépose au moyen de l'activateur sur le matériau réfractaire sous la forme de composés volatiles du métal donneur, le métal donneur étant disposé à une distance de 0,1 à 200 mm du matériau réfractaire à revêtir,
    - réalisation du procédé dans une chambre de réaction (1), laquelle permet de purger la chambre de réaction avant et/ou après le revêtement et/ou pendant une phase de diffusion pure, la purge de la chambre de réaction étant effectuée à l'aide d'un gaz inerte ou d'un gaz rare, en particulier l'argon,
    - formation d'une couche de protection à gradient ductile à base de chrome, comprenant
    o une couche déposée (20),
    o une couche de diffusion (22) tournée vers l'intérieur et
    o une zone de transition (21) située entre la couche déposée et la couche de diffusion, la teneur en chrome de la zone de transition (21) se situant entre celle de la couche de diffusion (22) et de la couche déposée, la couche déposée (20) présentant la modification de α-chrome et une teneur en chrome de 25 à 90 % en poids.
  2. Procédé selon la revendication 1,
    caractérisé en ce que
    les particules de métal donneur se trouvent dans un granulat (4) ayant une densité inférieure ou égale à 70 % de remplissage de l'espace, et/ou les particules de métal donneur présentes ont une granulométrie moyenne ou minimale supérieure ou égale à 2 mm ou plus.
  3. Procédé selon la revendication 1 ou 2,
    caractérisé en ce que
    l'activateur présente une pression de vapeur de 0,1 à 600 mbar à la température de diffusion.
  4. Procédé selon l'une des revendications précédentes,
    caractérisé en ce qu'un
    procédé en deux étapes est réalisé, dans lequel, lors d'une première étape, un dépôt de métal de la couche de protection réfractaire et la diffusion du métal dans le matériau réfractaire sont effectués, tandis que, lors d'une seconde étape, il ne se produit sensiblement qu'une diffusion dans le matériau réfractaire du métal auparavant déposé.
  5. Procédé selon l'une des revendications précédentes,
    caractérisé en ce que
    la température de diffusion est de 900 °C à 1200 °C et/ou le temps de maintien à la température de diffusion est compris entre 2 h et 16 h, la deuxième étape représentant en particulier 1/10 à 1/15, en particulier 1/12 du temps de maintien total.
  6. Procédé selon l'une des revendications précédentes,
    caractérisé en ce qu'une
    chambre extérieure supplémentaire (2) est utilisée en plus de la chambre de réaction (1), de sorte à créer un boîtier en deux parties, la chambre extérieure étant soumise à une pression inférieure à celle de la chambre de réaction, la chambre extérieure en particulier étant purgée pendant tout le procédé à l'aide d'un gaz inerte ou d'un gaz rare.
  7. Procédé selon l'une des revendications précédentes,
    caractérisé en ce que
    l'activateur est un composé contenant du chlore, en particulier un chlorure, d'un composant du matériau réfractaire ou du métal à déposer.
  8. Procédé selon la revendication 1,
    caractérisé en ce que
    le métal à déposer est introduit sous forme de gaz dans un réacteur pour le dépôt sur le matériau réfractaire.
  9. Composant constitué d'un matériau réfractaire comportant une couche de protection contre la corrosion par les gaz chauds, fabriquée selon un procédé selon l'une des revendications 1 à 8.
  10. Composant selon la revendication 9,
    caractérisé en ce que
    la couche déposée (20) présente une épaisseur de 0,1 à 20 µm.
  11. Composant selon l'une des revendications 9 et 10,
    caractérisé en ce que
    la zone de transition (21) présente une teneur en chrome de 15 à 40 % en poids et/ou une épaisseur de 2 à 75 µm.
  12. Composant selon l'une des revendications 9 à 11,
    caractérisé en ce que
    la couche de diffusion (22) présente une teneur en chrome de 5 à 30 % en poids et/ou une épaisseur de 2 à 75 µm.
  13. Composant selon l'une des revendications 9 à 12,
    caractérisé en ce que
    le composant est une aube de turbine.
EP09760703.0A 2008-10-28 2009-10-24 Couche de protection contre la corrosion à haute température et procédé de fabrication Active EP2352856B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102008053540A DE102008053540A1 (de) 2008-10-28 2008-10-28 Hochtemperaturkorrosionsschutzschicht und Verfahren zur Herstellung
PCT/DE2009/001497 WO2010048932A1 (fr) 2008-10-28 2009-10-24 Couche de protection contre la corrosion à haute température et procédé de fabrication

Publications (2)

Publication Number Publication Date
EP2352856A1 EP2352856A1 (fr) 2011-08-10
EP2352856B1 true EP2352856B1 (fr) 2018-06-27

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EP09760703.0A Active EP2352856B1 (fr) 2008-10-28 2009-10-24 Couche de protection contre la corrosion à haute température et procédé de fabrication

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Country Link
EP (1) EP2352856B1 (fr)
CA (1) CA2741957A1 (fr)
DE (1) DE102008053540A1 (fr)
WO (1) WO2010048932A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102011089131A1 (de) * 2011-12-20 2013-06-20 Mtu Aero Engines Gmbh Diffusionsbeschichtungsverfahren und damit hergestellte Chromschicht
CN117187738A (zh) * 2023-11-07 2023-12-08 中国航发沈阳黎明航空发动机有限责任公司 空心叶片内外表面气相沉积铬铝渗层的工艺方法

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Publication number Priority date Publication date Assignee Title
GB1549845A (en) * 1975-04-04 1979-08-08 Secr Defence Diffusion coating of metal or other articles
JP3029546B2 (ja) * 1994-03-09 2000-04-04 株式会社荏原製作所 クロム拡散浸透耐熱合金部材とその製法
DE19730007C1 (de) * 1997-07-12 1999-03-25 Mtu Muenchen Gmbh Verfahren und Vorrichtung zur Gasphasendiffusionsbeschichtung von Werkstücken aus warmfestem Material mit einem Beschichtungsmaterial
DE19803740C2 (de) * 1998-01-30 2001-05-31 Mtu Aero Engines Gmbh Gasphasenbeschichtungsverfahren und Vorrichtung zur Gasphasenbeschichtung von Werkstücken
DE10036620C2 (de) * 2000-07-27 2002-09-26 Mtu Aero Engines Gmbh Verfahren und Vorrichtung zum Chromieren einer inneren Oberfläche eines Bauteils
SG97203A1 (en) * 2000-10-13 2003-07-18 Gen Electric Vapor-coating system including coating container with control of coating-vapor activity
DE10101070C1 (de) * 2001-01-11 2002-10-02 Mtu Aero Engines Gmbh Verfahren zum Gasphasendiffusionsbeschichten von metallischen Bauteilen
US7645485B2 (en) 2004-04-30 2010-01-12 Honeywell International Inc. Chromiumm diffusion coatings
FR2900416B1 (fr) * 2006-04-28 2008-10-24 Snecma Sa Dispositif et procede de traitement thermochimique de diffusion de chrome dans un substrat

Non-Patent Citations (1)

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Title
None *

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Publication number Publication date
EP2352856A1 (fr) 2011-08-10
CA2741957A1 (fr) 2010-05-06
DE102008053540A1 (de) 2010-04-29
WO2010048932A1 (fr) 2010-05-06

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