EP3620548A1 - Procédé de fabrication d'un composant résistant à l'oxydation à partir d'un alliage à base de molybdène - Google Patents

Procédé de fabrication d'un composant résistant à l'oxydation à partir d'un alliage à base de molybdène Download PDF

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Publication number
EP3620548A1
EP3620548A1 EP19196205.9A EP19196205A EP3620548A1 EP 3620548 A1 EP3620548 A1 EP 3620548A1 EP 19196205 A EP19196205 A EP 19196205A EP 3620548 A1 EP3620548 A1 EP 3620548A1
Authority
EP
European Patent Office
Prior art keywords
semi
finished product
slip
powder
component
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.)
Withdrawn
Application number
EP19196205.9A
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German (de)
English (en)
Inventor
Heinrich Walter
Philipp Utz
Martin Frommherz
Ludwig Hilser
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.)
MTU Aero Engines AG
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MTU Aero Engines AG
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Filing date
Publication date
Application filed by MTU Aero Engines AG filed Critical MTU Aero Engines AG
Publication of EP3620548A1 publication Critical patent/EP3620548A1/fr
Withdrawn legal-status Critical Current

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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
    • C23C10/18—Solid state diffusion of only metal elements or silicon into metallic material surfaces using liquids, e.g. salt baths, liquid suspensions
    • C23C10/20—Solid state diffusion of only metal elements or silicon into metallic material surfaces using liquids, e.g. salt baths, liquid suspensions only one element being diffused
    • 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
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04—Alloys based on tungsten or molybdenum
    • 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
    • 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
    • C23C10/60—After-treatment
    • 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
    • C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces

Definitions

  • the present invention relates to a method for improving the high temperature oxidation resistance of molybdenum-based alloys or molybdenum-based alloys.
  • the present invention relates to a correspondingly manufactured component made of a molybdenum base alloy, which component can in particular be a component of a turbomachine and in particular an aircraft engine.
  • molybdenum and its alloys are interesting materials for high-temperature applications.
  • the component should also be reliably protected against high-temperature oxidation.
  • the invention proposes to apply the silicon either via a liquid or a gaseous phase to a corresponding area of a molybdenum-based semifinished product to be protected from high temperature oxidation, in order to produce a correspondingly protected component.
  • the method according to the invention comprises either providing a silicon-containing slip or a silicon-containing powder.
  • the silicon-containing slip is applied to the areas of the semi-finished product to be protected from high-temperature oxidation, with diffusion annealing then taking place, so that silicon can diffuse from the slip into at least the near-surface areas of the molybdenum-based semi-finished product, in order to provide silicon there for the formation of a silicon oxide layer.
  • the silicon-containing powder is provided in order to introduce silicon into the region of the semi-finished product near the surface via the gas phase.
  • the silicon-containing powder is arranged at a distance from the semifinished product to be protected, so that the diffusion heat treatment of the semifinished product with the silicon-containing powder allows the silicon to diffuse into the surface of the semifinished product.
  • the semi-finished product prepared in this way can also be conditioned by an oxidation treatment, so that a thin, slowly growing silicon oxide layer is already formed on the component, which protects the component from further oxidation.
  • the conditioning can be carried out by an oxidation treatment at a temperature of more than 900 ° C., in particular in the temperature range from 1000 ° C. to 1400 ° C., in particular at 1380 ° C., for a period of up to 2 to 100 hours, preferably 10 to 15 hours. in particular 12 hours. Heating to the treatment temperature and cooling from the treatment temperature can take place slowly, in particular with a heating and / or cooling rate of less than or equal to 10 K / min.
  • Conditioning can be carried out in ambient air or with specially prepared oxygen-containing gases.
  • the semi-finished product can be used from Mo alloys with Si and / or titanium and / or boron and / or Fe.
  • the proportion of Si can be in the range from 5 to 25 at.%, While Ti can be alloyed in the range from 0 to 30 at.% And B in the range from 5 to 15 at.%.
  • a corresponding Mo-based alloy can have up to 5 at.% Iron, any combination of the alloying elements being possible, while the rest is formed by Mo.
  • silicon is enriched in at least partial areas of the surfaces of the semi-finished product by applying a slip or via the gas phase, in particular directly on the materials of the semi-finished product described above, so that no additional intermediate layers are required on the surface of the semi-finished product.
  • halogens can be used in contain the silicon-containing powder to improve the diffusion of silicon into the semi-finished product.
  • NH 4 F, NH 4 CL or NaF can be used as halogen-containing compounds.
  • the silicon-containing powder for the conversion of the silicon via the gas phase into the semi-finished product can contain additional components in addition to the silicon powder.
  • additional constituents of the powder can serve as filling material, which prevent the powder from caking.
  • additional components can affect the total amount of silicon and control the gas phase activity of the silicon.
  • the silicon-containing powder for transferring the silicon via the gas phase into the semi-finished product can preferably be arranged in a ceramic container below the semi-finished product during the diffusion heat treatment.
  • the diffusion heat treatment of the semifinished product with the silicon-containing powder arranged at a distance can be carried out at a temperature of over 900 ° C., in particular in the temperature range from 1100 ° C. to 1300 ° C.
  • the holding time at the corresponding heat treatment temperature can be in the range from 0.5 to 5 hours and preferably in the range from 1 to 2 hours.
  • the semi-finished product with the powder can be arranged in a protective gas atmosphere, for example an argon atmosphere or a hydrogen atmosphere.
  • the slip can comprise silicon-containing powder or silicon powder as well as a solvent and a binder.
  • Water, alcohols or alcoholic solvents or liquid-organic solvents are suitable as solvents.
  • Polyvinyl alcohols or resins can be used as binders.
  • the slip can contain further constituents, such as Mo, W, B, Ta, Cr, Fe, Ti and alloys thereof, whereby these components can either be contained as alloy constituents in the silicon-containing powder or can be added as separate powder particles.
  • components for controlling the silicon activity or the adaptation of the thermal expansion coefficients of the layer produced and the substrate or semi-finished product can be added.
  • the slip can contain further constituents in the form of oxide, carbide or nitride particles, which can be built into a silicon oxide layer on the component in order to reduce the viscosity of the oxide layer and to prevent the oxide layer from flowing off at high operating temperatures of the component.
  • the slip can contain aluminum oxide, zirconium oxide, yttrium oxide, hafnium oxide, neodymium oxide, silicon carbide and / or silicon nitride.
  • the powder particles can be contained in the slurry with an average grain size or a maximum grain size of 0.5 ⁇ m to 100 ⁇ m and in particular 1-60 ⁇ m.
  • the slip can be applied to the semi-finished product by dipping, spraying, printing and in particular by screen printing or stencil printing.
  • the diffusion annealing of the semi-finished product with the applied slip can be carried out at temperatures above 900 ° C and in particular at temperatures from 1000 ° C to 1400 ° C.
  • the holding time at the annealing temperature can range from 1 to 3 hours and in particular up to 2 hours.
  • position information is used in the present description, such as, for example, below, above or the like, these information relate to the usual position when used in the gravitational system of the earth, so that above indicates the position away from the earth's surface, while below towards the earth's surface is localized.
  • molybdenum-based alloy or molybdenum-based alloy is understood to mean an alloy whose largest constituent is molybdenum. Alloys in which an alloy component has an equally high or similarly high proportion in the alloy as molybdenum should also fall under the term of the molybdenum-based alloy or molybdenum-based alloy. Accordingly, molybdenum-based alloys or molybdenum-based alloys are understood to mean alloys which have more than 50 percent by weight or atomic percent of molybdenum.
  • high-temperature oxidation is understood to mean oxidation at temperatures which are higher than usual ambient temperatures and in particular higher than 500 ° C., preferably higher than 1000 ° C.
  • the Figure 1 shows an example of an arrangement for producing an Si-containing edge layer in a semifinished product 4 via the gas phase.
  • a container 1 for example made of aluminum oxide, is provided with a lid 2, in which there is a silicon powder with NH 4 F.
  • the semi-finished product 4 to be processed is located above the silicon powder, so that when the container 1 is heated in an argon atmosphere to a temperature of approximately 1190 ° C., silicon can diffuse into the peripheral layer of the semi-finished product 4 for a period of 2 hours.
  • the diffusion heat treatment forms an edge region of the semifinished product 4, as shown in FIG Figure 3 is shown in cross section.
  • a silicide layer 6 has been formed above the base material 5 by the diffusion of silicon.
  • the semifinished product 4 After the formation of the silicide layer 6 by the heat treatment under an argon atmosphere, as shown schematically in Figure 1 the semifinished product 4 has been exposed to air at a temperature of approx. 1400 ° C. for 8 hours, so that a silicate layer 8 is formed above the silicide layer 6 by oxidation of the silicon, while between the silicide layer 6 and an interdiffusion layer 7 is formed on the base material, which serves as a silicon reservoir.
  • This structure of the border area is in Fig. 4 shown.
  • the Figure 2 shows in the partial images a) and b) an alternative embodiment in which the silicide layer 6 is formed by applying a slip 12, which is located in a container 10, to the semifinished product 4 by a brush 11 and then one Drying is carried out at approx. 50 ° C. Subsequently, heat treatment takes place in a vacuum at 1400 ° C. for 1 hour, so that silicon can in turn penetrate into the base material 5 of the semifinished product 4 and a silicide layer 6, as shown in FIG Figure 3 is shown, is formed.
  • the semi-finished product 4 enriched with silicon is conditioned accordingly, so that the edge region is formed in accordance with the illustration of FIG Figure 4 results as already described above.
  • Silicon enrichment using the slip process can of course be applied to all molybdenum-containing materials in the same way as silicon gas phase coating.
  • the slip is formed by a silicon powder with a grain size of 45 ⁇ m in a water solution, wherein additional components, for example boron powder with a grain size of 35 ⁇ m or the like, can be added to the slip solution.

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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)
  • Powder Metallurgy (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
EP19196205.9A 2018-09-10 2019-09-09 Procédé de fabrication d'un composant résistant à l'oxydation à partir d'un alliage à base de molybdène Withdrawn EP3620548A1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102018215313.2A DE102018215313A1 (de) 2018-09-10 2018-09-10 Verfahren zur Herstellung eines oxidationsbeständigen Bauteils aus einer Molybdän-Basislegierung

Publications (1)

Publication Number Publication Date
EP3620548A1 true EP3620548A1 (fr) 2020-03-11

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EP19196205.9A Withdrawn EP3620548A1 (fr) 2018-09-10 2019-09-09 Procédé de fabrication d'un composant résistant à l'oxydation à partir d'un alliage à base de molybdène

Country Status (3)

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US (1) US20200080184A1 (fr)
EP (1) EP3620548A1 (fr)
DE (1) DE102018215313A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3084891B1 (fr) * 2018-08-07 2022-06-24 Commissariat Energie Atomique Revetement pour piece en alliage refractaire
DE102019218784A1 (de) * 2019-12-03 2021-06-10 MTU Aero Engines AG Verfahren zur herstellung eines oxidationsbeständigen bauteils aus einer legierung auf basis eines refraktärmetalls

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992000256A2 (fr) * 1990-06-25 1992-01-09 Lanxide Technology Company, Lp Corps composites et leurs procedes de fabrication
US6340398B1 (en) * 2000-04-04 2002-01-22 The United States Of America As Represented By The Secretary Of The Air Force Oxidation protective coating for Mo-Si-B alloys
WO2005022065A2 (fr) * 2003-05-01 2005-03-10 Wisconsin Alumni Research Foundation Revetements resistant a l'oxydation pour des metaux de transition a temperature ultraelevee et alliages de metal de transition
WO2005035819A1 (fr) * 2003-10-11 2005-04-21 Mtu Aero Engines Gmbh Procede de traitement a l'alite, a la silice ou au chrome de composants metalliques
EP2980263A1 (fr) * 2014-07-30 2016-02-03 MTU Aero Engines GmbH Composant en alliage de molybdène et son procédé de fabrication
CN107523785A (zh) * 2016-06-21 2017-12-29 张家港市思杰五金工具有限公司 钼基合金表面抗氧化涂层及其制备方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB709806A (en) * 1950-12-08 1954-06-02 Gen Electric Co Ltd Improvements in or relating to electrical resistance heating elements
US2865088A (en) * 1952-10-16 1958-12-23 Fansteel Metallurgical Corp Refractory metal bodies
EP1900842A1 (fr) * 2006-09-11 2008-03-19 Difcon GmbH Melange de diffusion au-dessus d'une couche intermediàre
DE102016202872A1 (de) * 2016-02-24 2017-08-24 MTU Aero Engines AG Bauteil aus einer Molybdän-Legierung und Verfahren zur Ausbildung einer Oxidationsschutzschicht hierfür
DE102016224546A1 (de) * 2016-12-09 2018-06-14 MTU Aero Engines AG HEIßGASKORROSIONS - UND OXIDATIONSSCHUTZSCHICHT FÜR TIAL-LEGIERUNGEN

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992000256A2 (fr) * 1990-06-25 1992-01-09 Lanxide Technology Company, Lp Corps composites et leurs procedes de fabrication
US6340398B1 (en) * 2000-04-04 2002-01-22 The United States Of America As Represented By The Secretary Of The Air Force Oxidation protective coating for Mo-Si-B alloys
WO2005022065A2 (fr) * 2003-05-01 2005-03-10 Wisconsin Alumni Research Foundation Revetements resistant a l'oxydation pour des metaux de transition a temperature ultraelevee et alliages de metal de transition
WO2005035819A1 (fr) * 2003-10-11 2005-04-21 Mtu Aero Engines Gmbh Procede de traitement a l'alite, a la silice ou au chrome de composants metalliques
EP2980263A1 (fr) * 2014-07-30 2016-02-03 MTU Aero Engines GmbH Composant en alliage de molybdène et son procédé de fabrication
CN107523785A (zh) * 2016-06-21 2017-12-29 张家港市思杰五金工具有限公司 钼基合金表面抗氧化涂层及其制备方法

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US20200080184A1 (en) 2020-03-12

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