EP2104748B1 - Procédé pour un procédé de projection thermique - Google Patents

Procédé pour un procédé de projection thermique Download PDF

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Publication number
EP2104748B1
EP2104748B1 EP07856100.8A EP07856100A EP2104748B1 EP 2104748 B1 EP2104748 B1 EP 2104748B1 EP 07856100 A EP07856100 A EP 07856100A EP 2104748 B1 EP2104748 B1 EP 2104748B1
Authority
EP
European Patent Office
Prior art keywords
cooling
coating
layer
substrate
oxide
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.)
Not-in-force
Application number
EP07856100.8A
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German (de)
English (en)
Other versions
EP2104748A2 (fr
Inventor
Robert Vassen
Karl-Heinz Rauwald
Detlev STÖVER
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.)
Forschungszentrum Juelich GmbH
Original Assignee
Forschungszentrum Juelich GmbH
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Publication of EP2104748A2 publication Critical patent/EP2104748A2/fr
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Publication of EP2104748B1 publication Critical patent/EP2104748B1/fr
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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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/129—Flame spraying
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134—Plasma spraying
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/18—After-treatment

Definitions

  • the invention relates to a coating method, in particular a thermal spraying method.
  • a single or several adherent layers of formless material are applied to the surface of a workpiece. It may be a thin layer or a thick layer, the distinction is not well defined and is based on the coating process and application.
  • the coating methods themselves differ on the one hand in the type of layer application in chemical, mechanical, thermal and thermomechanical processes, and on the other hand on the initial state of the material to be applied.
  • gaseous application such as chemical vapor deposition (CVD or chemical vapor deposition) or physical vapor deposition (also known as PVD)
  • liquid application such as painting, spraying, and Thermal spraying including flame spraying, high-speed flame spraying, wire arc spraying and plasma spraying and also the fixed application method as in sintering processes.
  • thermal spraying is understood to mean different spraying processes, which differ in the type of spray additive material (wire or powder), the production or the energy source.
  • the spray additive As an energy source for the on or melting of the spray additive usually serve electronic arc, laser beam, fuel gas-oxygen flame or kerosene-oxygen high-velocity flame, high-kinetic gases and the plasma jet.
  • the density of the coating, the adhesion of the sprayed layer and the adhesive tensile strength between the coating and the base material usually result from the energy which is coupled with the particle velocity and temperature.
  • Thermal spraying processes are characterized in that the material intended for the coating strikes a substrate in the form of meltable particles and forms a layer there. Both the thermal energy sources used to produce the molten particles, such as plasmas, arcs or combustion processes and the thermal energy content of the particles themselves, regularly lead to a heating of the substrate. This heating often has negative consequences, such as distortion, corrosion or oxidation of the substrate.
  • cooling is typically used in thermal spraying.
  • the cooling used is usually via cooling nozzles, through which the substrate with a cooling medium, such as. B. compressed air is blown.
  • the cooling nozzles are fixedly directed to the substrate or they are arranged next to the burner and move accordingly with this.
  • WO 2004005575 a device for internal coating of cavities by thermal spraying with two cooling lances is known, which are arranged on opposite sides of the burner. In part, both cooling methods are used simultaneously. It's over C. Coddet, Surface & Coatings Technology 201 (2006) 1969-1974 Also known cooling methods that are used in conjunction with preheating prior to thermal spraying. These are for temperature management in the layer / substrate interconnections and are designed to maintain the substrate temperature at the ambient (room temperature) level.
  • EP 1 712 962 A a method for coating a metallic substrate by means of a thermal spraying process is already known in which the three process parameters deposition rate, deposition rate and cooling rate are controlled by the temperature is measured during deposition at different points of the metallic substrate, the averaged temperature with a Target range specification is compared and adjusted in case of deviations of at least one of the aforementioned process parameters so that the average temperature of the substrate is guided into the desired value range.
  • the cooling itself is done with the help of a CO 2 jet.
  • the nominal temperature range is between 80 ° C and 300 ° C.
  • EP 0 872 563 A A method for coating a substrate by means of a thermal spraying process is described, in which cooling of the substrate and the deposited layer takes place with CO 2 .
  • the object of the invention is to provide a coating method which permits the production of layers having a good bond between the individual spray lamellae without preheating methods and thus makes it possible in a simple manner to deposit high-density, thin layers but also thicker, segmented layers. It is another object of the invention to provide an apparatus for performing this method.
  • the coating is carried out in such a way that cooling is controlled in such a way that only those areas in which coating has been carried out immediately before are specifically cooled.
  • This can be expediently implemented, for example, in such a way that the use of the cooling nozzles fastened to the burner is coordinated with the burner movement.
  • a burner is provided with at least two cooling nozzles. During the coating, however, only the cooling nozzle is activated in each case, which are located behind the burner in the direction of movement. This advantageously allows a crossing of the substrate at least in two directions, z. B. in the form of a meander. In terms of plant technology, this can be achieved by valve control of the cooling nozzles in accordance with the burner movement.
  • the process can be transferred accordingly.
  • a plurality of cooling nozzles may be appropriate, so that a drive over in several directions in space is possible, if a corresponding Control of the cooling nozzles for a defined downstream cooling of the just deposited spray spot ensures.
  • Suitable cooling media are both gases, such as CO 2 , compressed air, nitrogen, helium or water vapor, as well as liquids, such as water in question. Further, a solid such. As CO 2 snow, also suitable.
  • the targeted cooling has a decisive influence on the layer formation of the coating. Due to the exclusive subsequent cooling it is avoided that the already deposited layer, or the substrate, is cooled immediately before the layer deposition. In addition, the substrate temperature is adjusted by the targeted cooling dosing so that even after cooling, there is a relation to the ambient temperature elevated temperature. In the first injection process, this can be done advantageously by preheating with the burner without particle injection. As a result of the elevated temperatures of the substrate compared with the prior art, it is now achieved that the newly deposited layers can advantageously be deposited with a high density. The subsequent, targeted cooling now leads to the fact that the permissible temperatures of the substrate are not exceeded, but on the other hand, a sufficiently high temperature level can be adjusted to achieve a layer deposition with high density.
  • the temperatures of the substrate are advantageously 200 to 800 K above the ambient temperature, ideally between 300 and 600 K above the ambient temperature.
  • the temperatures of the substrate are advantageously 200 to 800 K above the ambient temperature, ideally between 300 and 600 K above the ambient temperature.
  • the cooling time of the splats can be estimated from the lamella thickness, which is typically 5 ⁇ m, divided by the root of the thermal diffusivity (depending on the material, typically 10 -6 m 2 / s), which gives about 5 ms.
  • the targeted cooling further includes that the diameter of the flow of the cooling gas medium is matched to the spray spot size.
  • the cooled area should not be larger than the spray spot.
  • the profile of the cooling flow should accordingly be only a few millimeters in diameter.
  • the choice of the material of the coating depends inter alia on the application of the coating.
  • a particularly suitable material for an ion-conducting membrane for a solid electrolyte fuel cell is to be mentioned with yttrium-stabilized zirconium oxide (YSZ).
  • YSZ YSZ
  • insulating layers can be prepared, for. Using powders comprising alumina, spinel compounds, steatites, forsterites, porcelan, pyrochlors, mullites, magnesia, zircon, zirconia (unstabilized and stabilized) and titania.
  • thermal spraying methods such as high-speed flame spraying, can be used in addition to plasma spraying, using the described cooling, to deposit high-density layers at low thermal stress of the substrate.
  • the method according to the invention combines the advantages of an overall increased temperature level of the substrate with a defined cooling following directly on the spray spot removal in order to achieve particularly advantageous gas-tight, thin or even highly segmented thicker layers.
  • FIG. 1 is a schematic representation of the movement of the burner during thermal spraying with according to the disclosure of the invention specified cooling.
  • a burner with two cooling nozzles is used on each side of the burner.
  • the cooling is activated according to the burner movement during the coating process by selectively activating the left or the right cooling nozzle, whichever is located in the burner direction behind the burner.
  • the burner movement is always only in one direction, here from left to right, provided. Therefore, according to the invention, only the left cooling nozzle is always activated, which in this case is arranged behind the burner during the coating process in the burner direction.
  • FIG. 3 shows the microstructures of thermally sprayed layers, left with the targeted, cooling according to the invention in the wake, right with cooling before coating. It can be seen clearly the strong improvement of the microstructure in the inventive method.
  • Deposited deposited layers were prepared with a TRIPLEX II burner using yttria-stabilized zirconia (YSZ) powder. For coating both layers, identical plasma spray conditions were used set.
  • YSZ yttria-stabilized zirconia
  • the application efficiency ie the layer thickness deposited per coating cycle, is significantly increased, as is the result of the significantly greater layer thickness in FIG FIG. 2 a is apparent.
  • a layer was subsequently deposited on a stainless steel substrate at a robot speed of 250 mm / s with the CO 2 cooling according to the invention.
  • the spray distance was 100 mm
  • the process gases used were 50 standard liters per minute (slpm) of Ar and He.
  • the coating temperature was between 700 and 800 ° C
  • a preheat cycle heated the substrate to about 500 ° C.
  • the layer was deposited by passing four times with the burner. With the hot spray parameters used an extremely dense layer with a high density of segmentation cracks (> 3.5 per mm) could be deposited. Furthermore, this layer shows no delamination cracks, as seen from FIG. 4a ) is recognizable.
  • a second layer was deposited on a bondcoat (NiCOCrAlY) coated superalloy substrate (IN738) in accordance with the present invention.
  • This layer has a reduced segmentation crack density in accordance with what has been said above, and likewise no delamination cracks or the extremely high density of the layer between segmentation cracks should be emphasized.
  • a thin layer of YSZ using fused and crushed powders with the use of a CO 2 was prepared in the wake of cooling by means of atmospheric plasma spraying.
  • the spray distance was in this case 95 mm, the burner power about 61 kW.
  • the temperature of the substrate during coating was about 450 ° C, preheated to about 400 ° C.
  • the layer shows a high density and no segmentation cracks, such as FIG. 5 can be seen.
  • a thermal spraying method was used in which instead of a flowable powder, a suspension z. B. from partially stabilized zirconium oxide was used and the cooling was carried out according to the invention in the wake.
  • the high segmentation crack densities achievable via suspension plasma spraying could be further increased.
  • regularly high density layers can be achieved in which gas tightness below 0.1 mbar 1 / s / cm 2 , preferably below 10 -3 mbar 1 / s / cm 2 can be achieved.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Coating By Spraying Or Casting (AREA)

Claims (14)

  1. Procédé de revêtement d'un substrat à l'aide d'un procédé de projection thermique, dans le cadre duquel on utilise un refroidissement,
    caractérisé en ce
    - que ne sont refroidies de manière ciblée que les zones, dans lesquelles un revêtement a été réalisé directement au préalable,
    - en ce que la zone du refroidissement est ajustée de manière à ne pas être plus grande que la zone de l'éclaboussure, et
    - en ce que la température de la couche/du composite de substrat est d'au moins 200 K au-dessus de la température ambiante aussi bien au cours du revêtement qu'à l'issue d'un refroidissement défini de la couche déposée.
  2. Procédé selon la revendication 1, dans le cadre duquel la température de la couche/du composite de substrat est d'au moins 300 à 600 K au-dessus de la température ambiante.
  3. Procédé selon la revendication 1 ou 2, dans le cadre duquel un laps de temps inférieur à 100 ms, en particulier inférieur à 10 ms et en particulier compris entre 0,1 et 5 ms s'écoule après la projection, entre la projection et le refroidissement défini de ladite couche déposée.
  4. Procédé selon l'une quelconque des revendications 1 à 3, dans le cadre duquel le substrat est préalablement chauffé avant le revêtement à l'aide d'une torche à plasma avec un refroidissement activé ultérieurement mais sans injection de poudre.
  5. Procédé selon la revendication 4, dans le cadre duquel le substrat est préalablement chauffé à au moins 200 K au-dessus de la température ambiante, avant le revêtement, à l'aide d'une torche à plasma avec un refroidissement activé ultérieurement mais sans injection de poudre.
  6. Procédé selon l'une quelconque des revendications 1 à 5, dans le cadre duquel la zone du refroidissement correspond à l'éclaboussure.
  7. Procédé selon l'une quelconque des revendications 1 à 6, dans le cadre duquel la sortie du milieu de refroidissement se fait directement à côté de l'éclaboussure.
  8. Procédé selon l'une quelconque des revendications 1 à 7, dans le cadre duquel on utilise en tant que milieu de refroidissement un gaz, en particulier du CO2, de l'air comprimé, de l'azote, de l'hélium ou de la vapeur d'eau, ou un liquide, en particulier de l'eau, ou un solide, en particulier de la neige carbonique.
  9. Procédé selon l'une quelconque des revendications 1 à 8, dans le cadre duquel la vitesse relative entre le substrat et la torche est supérieure à 100 mm/s, de préférence est comprise entre 250 et 1 000 mm/s.
  10. Procédé selon l'une quelconque des revendications 1 à 9, dans le cadre duquel on produit un revêtement à partir d'oxyde de zirconium stabilisé avec de l'yttrium (YSZ) ou à partir d'autres substances actives oxydées, en particulier à partir d'une pérovskite, d'un aluminate, d'un spinelle ou d'un pyrochlore.
  11. Procédé selon l'une quelconque des revendications 1 à 10, dans le cadre duquel on utilise en tant que procédé de projection thermique un procédé de projection atmosphérique (APS) ou une projection à la flamme à haute vitesse (HVOF).
  12. Procédé selon l'une quelconque des revendications 1 à 11, dans le cadre duquel on produit, en particulier par un passage unique, le revêtement sous la forme d'une couche étanche au gaz présentant une épaisseur de couche totale inférieure à 100 µm.
  13. Procédé selon l'une quelconque des revendications 1 à 13, dans le cadre duquel on fabrique le revêtement
    a) sous la forme d'une membrane conductrice d'ions pour une pile à combustible à électrolyte solide comprenant du YSZ ou
    b) sous la forme d'une membrane de séparation de gaz, comprenant un oxyde conducteur de mélange ou un conducteur de protons, ou
    c) sous la forme d'une couche isolante, comprenant un oxyde d'aluminium, un composé de spinelle, une stéatite, une fostérite, une porcelaine, un pyrochlore, une mullite, un oxyde de magnésium, un zirconium, un oxyde de zirconium ou un oxyde de titane non stabilisé ou stabilisé, ou
    d) sous la forme d'une couche de protection anticorrosion.
  14. Procédé selon l'une quelconque des revendications 1 à 13, dans le cadre duquel on produit, en particulier par un passage unique, un revêtement segmenté présentant une épaisseur de couche supérieure à 100 µm.
EP07856100.8A 2006-12-21 2007-12-13 Procédé pour un procédé de projection thermique Not-in-force EP2104748B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006061977A DE102006061977A1 (de) 2006-12-21 2006-12-21 Verfahren und Vorrichtung für thermisches Spritzverfahren
PCT/DE2007/002250 WO2008074301A2 (fr) 2006-12-21 2007-12-13 Procédé et dispositif pour un procédé de projection thermique

Publications (2)

Publication Number Publication Date
EP2104748A2 EP2104748A2 (fr) 2009-09-30
EP2104748B1 true EP2104748B1 (fr) 2015-01-14

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Application Number Title Priority Date Filing Date
EP07856100.8A Not-in-force EP2104748B1 (fr) 2006-12-21 2007-12-13 Procédé pour un procédé de projection thermique

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EP (1) EP2104748B1 (fr)
DE (1) DE102006061977A1 (fr)
WO (1) WO2008074301A2 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20190078463A1 (en) * 2017-09-08 2019-03-14 United Technologies Corporation Segmented Ceramic Coatings and Methods

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2615022C2 (de) * 1976-04-07 1978-03-02 Agefko Kohlensaeure-Industrie Gmbh, 4000 Duesseldorf Verfahren zum Beschichten einer Oberfläche mittels eines Strahles aus erhitztem Gas und geschmolzenem Material
CH656560A5 (de) * 1982-03-19 1986-07-15 Castolin Sa Verfahren zum auftragen einer schutzschicht durch thermisches spritzen.
JPS61501397A (ja) * 1984-03-12 1986-07-10 コミツサレ・ア・レナジイ・アトミツク　エタブリスマン・ドウ・カラクテ−ル・サイエンテイフイツク・テクニツク・エ・アンドウストリ− 部品の表面処理およびとくに熱吹付けにより部品上に次いで蒸着される被膜の密着を改善するためのこの処理の使用
FR2756756B1 (fr) * 1996-12-09 1999-01-15 Inst Polytechnique De Sevenans Procede et dispositif pour la realisation d'un revetement sur un substrat
FR2762667B1 (fr) 1997-04-28 1999-05-28 Air Liquide Dispositif et procede de traitement thermique
US6103315A (en) * 1998-04-13 2000-08-15 General Electric Co. Method for modifying the surface of a thermal barrier coating by plasma-heating
EP0960955A1 (fr) * 1998-05-26 1999-12-01 Universiteit Gent Procédé et appareillage pour la production d'un revêtement dur par projection à chalumeau
DE10230847B3 (de) 2002-07-04 2004-02-05 Universität Stuttgart Institut für Fertigungstechnologie keramischer Bauteile Verfahren und Vorrichtung zur Innenbeschichtung von Hohlräumen durch thermisches Spritzen
US8715772B2 (en) 2005-04-12 2014-05-06 Air Products And Chemicals, Inc. Thermal deposition coating method

Also Published As

Publication number Publication date
EP2104748A2 (fr) 2009-09-30
DE102006061977A1 (de) 2008-06-26
WO2008074301A2 (fr) 2008-06-26
WO2008074301A3 (fr) 2009-06-04

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