EP1548153B1 - Procédé de fabrication d'un revêtment multicouche à haute résistance à l'abrasion - Google Patents

Procédé de fabrication d'un revêtment multicouche à haute résistance à l'abrasion Download PDF

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Publication number
EP1548153B1
EP1548153B1 EP04106968A EP04106968A EP1548153B1 EP 1548153 B1 EP1548153 B1 EP 1548153B1 EP 04106968 A EP04106968 A EP 04106968A EP 04106968 A EP04106968 A EP 04106968A EP 1548153 B1 EP1548153 B1 EP 1548153B1
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Prior art keywords
procedure
chosen
group
coating
thermal spray
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EP04106968A
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German (de)
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EP1548153A2 (fr
EP1548153A3 (fr
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Fabrizio Centro Sviluppo Materiali Spa Casadei
Claudio Centro Sviluppo Materiali Spa Testani
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Centro Sviluppo Materiali SpA
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Centro Sviluppo Materiali SpA
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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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/324—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal matrix material layer comprising a mixture of at least two metals or metal phases or a metal-matrix material with hard embedded particles, e.g. WC-Me
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/347—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with layers adapted for cutting tools or wear applications

Definitions

  • the present invention relates to a procedure to obtain, by means of combined thermal spray and vapour phase deposition techniques, a multilayer coating capable of improving the wear resistance of light alloy metal materials and metal matrix composite materials.
  • Wear of the material which can be defined as ablation of material due to interaction between surfaces in relative motion, is the greatest cause of the reduction and the loss of performance in mechanical and machine couplings, and therefore any decrease in this phenomenon is considered advantageous.
  • the phenomenon of wear which includes all phenomena that cause damage on the surface of two solid bodies which are in contact with each other and in relative movement, is produced in the following ways.
  • the layer of surface coating can become damaged and detach (due to friction), and in this case wear is the result of adhesion between the coatings of the bodies and is called adhesion wear.
  • wear fatigue In a second way, when the surface guarantees partial resistance to modest forms of wear, fatigue processes can arise due to stress cycles which occur during rubbing or rolling, this type of phenomenology is called wear fatigue.
  • abrasive wear which at times is very rapid, occurs.
  • the object of the present invention is to provide a procedure to improve wear resistance of light alloy metal materials or metal matrix composite materials, by application of a suitable multilayer coating on the surface thereof, capable of locally improving the characteristics of resistance of the component and therefore reducing the formation and expansion of cracks.
  • the phenomenon on which the increase in performance of components is based consists of producing a multilayer facing, with gradually increasing hardness, from the substrate to the surface.
  • the material to be coated is substantially subjected to the following operations: surface deposition, using thermal spray techniques, of a first cermet coating, with thickness ranging from 20 to 600 ⁇ m; surface finishing treatment; deposition on the first coating, using vapour phase deposition techniques, of a second nitride or carbon coating, with thickness ranging from 1 to 10 ⁇ m.
  • the surface finishing treatment according to the invention consists of mechanical machining chosen from the group comprising: polishing and/or lapping and/or grinding and/or shot blasting and/or combinations thereof.
  • the surface can also be prepared prior to the procedure of the invention and, if necessary, stabilizing heat treatment is carried out, at a temperature ranging from 20 and 800°C.
  • Surface preparation consists. for example, of a treatment chosen from the group comprising: mechanical and/or electrolytic and/or chemical cleaning and/or combinations thereof.
  • the stage of diffusion and annealing at 700-750°C for 10 hours in a protective atmosphere is performed immediately after cermet coating.
  • the thermal spray techniques according to the invention are preferably chosen from the group comprising: CAPS (Controlled Atmosphere Plasma Spray), HVOF (High Velocity Oxy Fuel), VPS (Vacuum Plasma Spray) and combinations thereof.
  • CAPS Controlled Atmosphere Plasma Spray
  • HVOF High Velocity Oxy Fuel
  • VPS Vauum Plasma Spray
  • the thermal spray techniques are applied at a temperature ranging from 50 to 350°C.
  • the cermet material used for thermal spray coating is chosen from the group comprising carbide, oxide or nitride dispersions, chosen from the group comprising WC, TiC, CrC, Al 2 O 3 , TiO2, TiN, CrN, in metal matrices, chosen from the group comprising Co, NiCr, NiCrFeBSi, NiAl, Mo, NiCoCrAlY, Ti alloys.
  • Vapour phase deposition techniques are chosen from the group comprising PVD or CVD and are preferably chosen from the group comprising: Arc-PVD, Sputtering PVD, Electron Beam PVD, CVD, also in the respective Plasma Assisted variants.
  • the material used for the coating obtained by vapour phase deposition is chosen from the group: TiN, CrN, ZrN, TiCN, TiAlN, DLC, in simple form or obtained from the combination in succession of two or more of these materials.
  • the metal material is chosen from the group comprising: aluminium alloy, titanium alloy, magnesium alloy.
  • the deposition temperature of the thermal spray coating in the case in which the metal material is aluminium alloy, ranges from 80-300°C and is preferably 150°C.
  • the deposition temperature of the thermal spray coating in the case in which the metal material is titanium alloy, ranges from 70-400°C and is preferably 150°C.
  • the metal matrix composite material is chosen from the group comprising: a matrix of Aluminium, Titanium, Magnesium, Copper, Lead, Iron or Silver reinforced with Alumina, Graphite, Silicon Carbide, Titanium Boride or Boron.
  • a further object of the present invention is the multilayer coating with high resistance to wear for light alloy metal materials and for metal matrix composite materials obtainable with the procedure indicated.
  • the present invention is used in all those cases which require the presence of components subject to cyclic application of mechanical loads, for example for applications in the aerospace, aeronautical, transport, mechanical components sectors and the like.
  • a possible example of application of the present invention is in the aircraft, car, motorcycle and bicycle components sector, for example to produce ring gears, and in any case all those components in which it is important to reduce weight and/or cost.
  • a ring gear for motorcycle applications is indicated as the first example of embodiment and has been produced on a substrate consisting of aluminium alloy AA7075. A surface preparation consisting of abrasive blasting was performed on this substrate.
  • a layer of chromium carbide cermet material in NiCr matrix was deposited on this substrate using the HVOF thermal spray procedure.
  • the layer of thermally sprayed cermet material produced has a thickness ranging from 50-300 ⁇ m.
  • the material coated with cermet was subjected to a surface finishing treatment consisting of polishing.
  • Microstructure characterization of the multilayer coating highlighted the following results: absence of unmelted particles in the cermet layer; porosity below 0.5% in the cermet layer; good degree of homogeneity of the facing along the thickness; absence of cracks; excellent adhesion of the thermally sprayed facing to the Al alloy substrate and of the thin film to the cermet layer; absence of delamination between thin film and cermet coating.
  • a gear wheel for bicycle applications is indicated as the second example of embodiment and was produced on a substrate consisting of titanium alloy Ti6A14V.
  • This substrate was subjected to surface preparation consisting of brushing, sanding and cleaning in an acetone ultrasound bath for 60 seconds.
  • a layer of cermet, based on TiN dispersed in Ti matrix was deposited on this substrate using the CAPS thermal spray technique at a temperature of 200°C.
  • the layer of thermally sprayed cermet produced has a thickness ranging from 50-300 ⁇ m.
  • the material coated with cermet was subjected to a surface finishing treatment consisting of grinding.
  • a TiN film, 2 ⁇ m thick was deposited on the surface of the material using Arc-PVD technology.
  • Microstructure characterization of the multilayer coating highlighted the following results: absence of unmelted particles in the cermet layer; porosity below 3% in the cermet layer; good degree of homogeneity of the facing along the thickness; absence of cracks; excellent adhesion of the thermally sprayed facing to the Ti alloy substrate and of the thin film to the cermet layer; absence of delamination between thin film and cermet coating.
  • the material thus obtained also improves the hot wear resistance thanks to the noteworthy reduction in porosity and cracks and, moreover, has a high level of hardness and toughness.
  • Tests were performed on these components with maximum load of 300 MPa applied to the outer layers, according to the following standard procedure: measurement of the minimum dimension; calculation of the flexural load corresponding to the maximum flexural stress of 300 MPa; application of the flexural load calculated by a balance system; start-up of the test; interruption of the test in the case of catastrophic fracture of the test piece.
  • the results were compared by performing tests on two series of samples of the same geometry manufactured with the same Titanium alloy with and without coating. The results indicate that Titanium alloy as is has a considerably lower wear resistance than can be obtained with the procedure according to the present invention adopted in the example in question.
  • a pin or tubular dowel which connects the piston to the connecting rod of a combustion engine is indicated as the second example of embodiment and was produced using the Sheet-Fibre-Sheet technique "simultaneously rolling into a spiral" a mat of SCS-6 type commercial fibres superimposed on an ultra-thin sheet of titanium alloy, for example type Ti6Al4V, above an internal spindle.
  • the internal spindle was subjected to pressure and made to expand on an external coaxial matrix.
  • the final result is a hybrid cylinder with an area with high mechanical resistance in the region subjected to the greatest mechanical loading during the test.
  • the specific mechanical properties are indicated in Figure 5 .
  • the layer of thermally sprayed cermet material produced has a thickness ranging from 50-300 ⁇ m.
  • the material coated with cermet was subjected to a surface finishing treatment consisting of grinding.
  • a CrN film with a thickness of 2 microns was deposited on the surface of the material using Arc-PVD technology.
  • Microstructure characterization of the multilayer coating highlighted the following results: absence of unmelted particles in the cermet layer; porosity below 3% in the cermet layer; good degree of homogeneity of the facing along the thickness; absence of cracks; excellent adhesion of the thermally sprayed facing to the composite material substrate and of the thin film to the cermet layer; absence of delamination between thin film and cermet coating.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Coating By Spraying Or Casting (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Laminated Bodies (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Claims (19)

  1. Procédure de production de revêtements multicouches présentant une haute résistance à l'usure, en particulier pour des matériaux métalliques en alliage léger et pour des matériaux composites à matrice métallique, caractérisée en ce que le matériau destiné à être revêtu est soumis aux opérations suivantes :
    a) dépôt sur une surface du matériau destiné à être revêtu, au moyen de techniques de pulvérisation thermique, d'un premier revêtement de cermet d'une épaisseur dans une plage de 20 à 600 µm ;
    b) application d'un traitement de finition de surface ;
    c) dépôt sur le premier revêtement, en utilisant des techniques de dépôt en phase vapeur, d'un deuxième revêtement de nitrure ou de carbone, d'une épaisseur dans une plage de 1 à 10 µm.
  2. Procédure selon la revendication 1, dans laquelle le matériau destiné à être revêtu est soumis à une préparation de surface avant l'étape a).
  3. Procédure selon la revendication 2, dans laquelle après la préparation de surface du matériau destiné à être revêtu et avant l'étape a), un traitement thermique de stabilisation est effectué à une température dans une plage de 20 à 800°C.
  4. Procédure selon la revendication 1 ou 3, dans laquelle une diffusion et un recuit à 700-750°C pendant 10 heures dans une atmosphère protectrice sont effectués entre l'étape a) et l'étape b).
  5. Procédure selon la revendication 2, dans laquelle la préparation de surface consiste en un traitement choisi parmi le groupe comprenant : un nettoyage mécanique et/ou électrolytique et/ou chimique et/ou des combinaisons de ceux-ci.
  6. Procédure selon la revendication 1, dans laquelle le traitement de finition de surface consiste en un usinage mécanique choisi parmi le groupe comprenant : un polissage et/ou un rodage et/ou un meulage et/ou un grenaillage et/ou des combinaisons de ceux-ci.
  7. Procédure selon l'une quelconque des revendications précédentes, dans laquelle les techniques de pulvérisation thermique sont préférablement choisies parmi le groupe comprenant : CAPS (projection au plasma sous atmosphère contrôlée), HVOF (oxygaz haute vélocité), VPS (projection au plasma sous vide) et des combinaisons de celles-ci.
  8. Procédure selon l'une quelconque des revendications précédentes, dans laquelle lesdites techniques de pulvérisation thermique sont appliquées à une température dans une plage de 50 à 350°C.
  9. Procédure selon l'une quelconque des revendications précédentes, dans laquelle le matériau de cermet utilisé pour le premier revêtement par pulvérisation thermique est choisi parmi le groupe comprenant des dispersions de carbure, d'oxyde ou de nitrure, choisies parmi le groupe comprenant WC, TiC, CrC, Al2O3, TiO2, TiN, CrN, dans des matrices de métal, choisies parmi le groupe comprenant des alliages de Co, NiCr, NiCrFeBSi, NiAl, Mo, NiCoCrAlY, Ti.
  10. Procédure selon la revendication 1, dans laquelle les techniques de dépôt en phase vapeur sont choisies parmi le groupe comprenant : PVD (dépôt physique en phase vapeur) ou CVD (dépôt chimique en phase vapeur).
  11. Procédure selon la revendication 10, dans laquelle les techniques de dépôt en phase vapeur sont préférablement choisies parmi le groupe comprenant : PVD à l'arc, PVD par pulvérisation cathodique, PVD par faisceau d'électrons, CVD, également dans les variantes respectives assistées par plasma.
  12. Procédure selon la revendication 11, dans laquelle le matériau utilisé pour le deuxième revêtement est choisi parmi le groupe : TiN, CrN, ZrN, TiCN, TIAIN, DLC (carbone sous forme de diamant amorphe), sous forme simple ou obtenue à partir de la combinaison en succession de deux ou plus de ces matériaux.
  13. Procédure selon l'une quelconque des revendications précédentes, dans laquelle le matériau métallique destiné à être revêtu est choisi parmi le groupe comprenant : un alliage d'aluminium, un alliage de titane, un alliage de magnésium.
  14. Procédure selon l'une quelconque des revendications 1 à 13, dans laquelle le matériau métallique est un alliage d'aluminium et la température de dépôt du revêtement par pulvérisation thermique est dans une plage de 80-300°C.
  15. Procédure selon la revendication 14, dans laquelle la température de dépôt du revêtement par pulvérisation thermique est 150°C.
  16. Procédure selon l'une quelconque des revendications 1 à 13, dans laquelle le matériau métallique est un alliage de titane et la température de dépôt du revêtement par pulvérisation thermique est dans une plage de 70-400°C.
  17. Procédure selon la revendication 16, dans laquelle la température de dépôt du revêtement est 150°C.
  18. Procédure selon l'une quelconque des revendications précédentes, dans laquelle ledit matériau composite à matrice métallique est choisi parmi le groupe comprenant : une matrice d'aluminium, de titane, de magnésium, de cuivre, de plomb, de fer ou d'argent renforcée avec de l'alumine, du graphite, du carbure de silicium, du borure de titane ou du bore.
  19. Revêtement multicouche présentant une haute résistance à l'usure pour des matériaux métalliques en alliage léger et pour des matériaux composites à matrice métallique, obtenu en utilisant la procédure selon une ou plusieurs des revendications 1 à 18.
EP04106968A 2003-12-24 2004-12-23 Procédé de fabrication d'un revêtment multicouche à haute résistance à l'abrasion Not-in-force EP1548153B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT000602A ITRM20030602A1 (it) 2003-12-24 2003-12-24 Procedimento di produzione di rivestimento multistrato
ITRM20030602 2003-12-24

Publications (3)

Publication Number Publication Date
EP1548153A2 EP1548153A2 (fr) 2005-06-29
EP1548153A3 EP1548153A3 (fr) 2007-01-24
EP1548153B1 true EP1548153B1 (fr) 2008-10-15

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Country Link
EP (1) EP1548153B1 (fr)
AT (1) ATE411413T1 (fr)
DE (1) DE602004017110D1 (fr)
IT (1) ITRM20030602A1 (fr)

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RU2449053C1 (ru) * 2011-04-05 2012-04-27 Российская Федерация, от имени которой выступает Министерство промышленности и торговли Российской Федерации (Минпромторг России) Способ нанесения износостойкого покрытия на титановые сплавы

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DE102009010110A1 (de) 2009-02-21 2010-09-02 Mtu Aero Engines Gmbh Erosionsschutz-Beschichtungssystem für Gasturbinenbauteile
DE102009010110B4 (de) * 2009-02-21 2014-08-28 MTU Aero Engines AG Erosionsschutz-Beschichtungssystem für Gasturbinenbauteile
RU2449053C1 (ru) * 2011-04-05 2012-04-27 Российская Федерация, от имени которой выступает Министерство промышленности и торговли Российской Федерации (Минпромторг России) Способ нанесения износостойкого покрытия на титановые сплавы

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ITRM20030602A1 (it) 2005-06-25

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