EP1422308B1 - Poudre de pulvérisation pour la fabrication par pulvérisation thermique d'un revêtement de barrière thermique résistant à haute température - Google Patents

Poudre de pulvérisation pour la fabrication par pulvérisation thermique d'un revêtement de barrière thermique résistant à haute température Download PDF

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Publication number
EP1422308B1
EP1422308B1 EP03405765A EP03405765A EP1422308B1 EP 1422308 B1 EP1422308 B1 EP 1422308B1 EP 03405765 A EP03405765 A EP 03405765A EP 03405765 A EP03405765 A EP 03405765A EP 1422308 B1 EP1422308 B1 EP 1422308B1
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Prior art keywords
grains
functional material
spray powder
additive
additives
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Expired - Lifetime
Application number
EP03405765A
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German (de)
English (en)
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EP1422308A1 (fr
Inventor
Rajiv J. Dr. Damani
Kaspar Dr. Honegger
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Oerlikon Metco US Inc
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Sulzer Metco US Inc
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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
    • 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
    • C23C4/11—Oxides

Definitions

  • the invention relates to a spray powder for the production of a high-temperature resistant thermal barrier coating according to the preamble of claim 1. It also relates to processes for the production of the inventive spray powder.
  • a substrate can be coated with a thermal barrier coating, wherein the substrate is, for example, a material from which the blade of a gas turbine wheel is made.
  • a thermal barrier coating is briefly referred to as TBC ("Thermal Barrier Coating").
  • the substrate onto which the TBC is sprayed can already be coated with a single-layer or multi-layer partial coating, in particular a primer.
  • the coating material used is at least one heat-insulating functional substance which, on the one hand, has a markedly smaller thermal conductivity than the substrate and, on the other hand, forms a chemically and thermally stable phase at the high temperatures.
  • the US-A-4996117 discloses a spray powder having the enumerated in the preamble of claim 1 features, the particles in particular an agglomerate-like microstructure, each formed by a plurality of adhering grains have.
  • Another spray powder that comes from the US-A-5722379 is known, consists of particles which have a thermally decomposable core and two sheaths made of a heat-insulating functional material or of an adhesive material. Thermal spraying of these particles produces a coating with an agglomerate-like microstructure.
  • the EP-A-1 225 251 addresses the aging of the coatings:
  • the relatively low thermal conductivity of the TBC is due to inhomogeneities of the microstructure, which is due to a large number of crystal grains, with the boundary zones between the grains being decisive. In these border zones the local density is smaller than inside the crystals. Micropores and lattice defects within the grains also make a detrimental contribution to thermal conductivity.
  • the aging processes are densifications of the microstructure, which results at high temperatures due to co-sintering - namely a homogenizing growth of micropores at the grain boundaries.
  • the thermal conductivity which should remain as small as possible, increases with increasing compaction.
  • Impurities which are given by silicon, titanium, iron, nickel, sodium, lithium, copper, manganese, potassium and / or oxides of some of these elements result in amorphous phases which form thin films at the grain boundaries. Such amorphous phases promote homogenization of the coating due to co-sintering of the grains. With suitable additives, the homogenization processes can be prevented, obstructed or at least slowed down.
  • One such additive is alumina, which is in the form of precipitated crystallites. These can bind the impurities mentioned and also fix the micropores located between the grains. The alumina adsorbs silicates from the films connecting adjacent grains. This results in gap-like empty spaces between the adjacent grains, which are barriers to heat transport.
  • the object of the invention is to provide a spray powder for a coating of the type TBC whose inhomogeneity, which is related to the thermal conductivity, is particularly pronounced and thermally stable. This object is achieved by the spray powder defined in claim 1 and a process for producing this spray powder according to claim 7.
  • the spray powder is suitable for the production of a high temperature resistant thermal barrier coating.
  • This TBC can be produced on a substrate by means of a thermal spraying method.
  • the substrate may already be coated with a single-layer or multi-layer partial coating, in particular a primer.
  • At least one heat-insulating functional substance is used which on the one hand has a lower thermal conductivity than the substrate and on the other hand forms a chemically and thermally stable phase at the high temperatures.
  • the wettable powder comprises particles each having an agglomerate-like microstructure formed by a plurality of adhering grains. These grains consist of the functional substance or the functional substances.
  • This further component is on the surfaces of the functional material grains, i. H. mainly in their border zones, finely dispersed.
  • the further component in the given or in a converted form, exerts an inhibiting or inhibiting effect on sintered compounds, which can form at high temperatures between the functional material grains.
  • the spray powder according to the invention has specifically produced microstructures of its particles. These microstructures are at least partially retained in a job by thermal spraying and thus lead to a pronounced inhomogeneity, which is associated with a low thermal conductivity. This inhomogeneity has the required stability thanks to suitable additives or thanks to substances which have resulted from a conversion of the additives.
  • the spray powder according to the invention consists of particles 1 or comprises such.
  • the particles 1 each have an agglomerate-like microstructure 2, as in Fig. 1 is illustrated.
  • Fig. 2 schematically shows a cross section through an entire particle 1, which has an edge zone 10 between two dash-dotted lines 11 and 12.
  • the surface 11 is the surface of the particle 1.
  • the microstructure 2 is indicated at a point in the interior of the particle 1.
  • the particle 1 is composed of a plurality of adhering grains 3. At the surfaces 30 of the grains 3, where they are in contact with adjacent grains, micropores give low-mass boundary zones 5. Within the grains 3, which may also be polycrystalline, lattice defects, foreign ions and / or other micropores (not shown) contribute to the reduction of Thermal conductivity at.
  • Each grain 3 consists of a functional material whose function is to keep a heat flow through this functional material grain 3 small at high temperatures. There may also be various functional substances.
  • At least one additive 4 forms a further component of the particle 1. This further component is on the surfaces 30 of thejansalstoffkömern 3, ie distributed mainly in their border zones 5, finely dispersed. It exerts an inhibiting or suppressing effect on homogenizing sintering phenomena, if appropriate after conversion to another form, which occur or can occur at high temperatures on the surfaces of the functional substance grains 3. In the above conversion of the additive 4, this can first be melted and form together with material from adjacent functional material grains 3 to form a new phase. This new phase coexists with the phase of the functional material grains 3. The the sintering effect of Additive 4 is described in EP-A-1 225 251 explained.
  • the additive 4 may be secreted in a phase consisting of metal salts, these salts being thermally convertible into metal oxides. Only after a conversion of the salts by means of a thermal treatment step, the additives 4 take the effective, namely the sintering influencing form.
  • the component formed from the additive 4 or the additives has a content of not more than 5 mol%, preferably at most 3 mol%.
  • the functional material grains 3 have a mean diameter d 50 greater than 1 nm and less than 10 ⁇ m, while the particles 1 of the spray powder have a mean diameter d 50 in the range from 1 to 100 ⁇ m (50% by weight of the grains 3 or particles 1 are larger - or smaller - than the corresponding diameter d 50 ).
  • the particle diameter d 50 is preferably in the range of 40 to 90 ⁇ m.
  • the preferred range may be different, for example, between 5 and 25 microns.
  • the particles 1 of the spray powder are porous agglomerates of the functional material grains 3, each containing communicating, against the outer surface 11 of the particle 1 open pore spaces - namely the boundary zones 5 - included.
  • the additives 4 can be deposited or deposited.
  • the Indian EP-A-1 225 251 The functional material described is zirconium oxide, in particular the stabilized zirconium oxide YSZ. This is a particularly beneficial substance. But there are also others possible:
  • additive 4 for example, an Al, Mg or La oxide can be used, further an yttrium-aluminum oxide (see US-A-6203927 , Subramanian et al.) Or also a spinel, in particular magnesium-aluminum oxide.
  • nitrate or acetate salts By means of a thermal treatment of said nitrate or acetate salts results in a conversion into oxides, which are the effective additives.
  • the agglomerates are obtained by spray-drying slurries of the functional granules 3 and then sintering (calcining) the dried intermediate.
  • Each additive 4 or its converted form, which effectively influences the sintering, must not be miscible with the functional substance, so that diffusion into the functional substance is largely avoided.
  • the agglomerates are briefly brought into a plasma flame in a subsequent process step and thereby partially melted. It may thus, if appropriate, by thermal conversion from the additive at least partially arise the component that causes the inhibition of sintering.
  • a mechanically more resistant form of the powder particles 1 forms, characterized in that a partially sintered edge layer 10 is formed.

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

Claims (9)

  1. Poudre de pulvérisation pour la préparation d'un revêtement de barrière thermique résistant à haute température, un revêtement de type TBC, qui peut être produit par un procédé de pulvérisation thermique sur un substrat, où le substrat peut être déjà revêtu avec un revêtement partiel à une ou plusieurs couches, en particulier une base d'adhérence, et où au moins une substance fonctionnelle de barrière thermique est utilisée, qui présente d'une part, une conductibilité thermique plus faible que le substrat et qui forme d'autre part, une phase chimiquement et thermiquement stable à haute température, où la poudre de pulvérisation comprend des particules (1), qui présentent chaque fois, une microstructure (2) de type agglomérat, formée par un certain nombre de grains (3) adhérant les uns aux autres, ces grains consistant en la ou les substances fonctionnelles, au moins un autre composant d'un ou plusieurs additifs (4) est présent et l'autre composant exerce sous la forme donnée ou sous une forme transformée, une action inhibante ou d'arrêt, concernant les composés de frittage, qui peuvent se former à haute température entre les grains de substance fonctionnelle,
    caractérisé en ce que sur la surface (30) des grains (3), où ils sont en contact avec les grains voisins, les micropores donnent des zones de frontière (5), faiblement garnies et l'autre composant est distribué de manière finement dispersée sur la surface (30) des grains de substance fonctionnelle (3), à savoir essentiellement dans les zones de frontière (5).
  2. Poudre de pulvérisation selon la revendication 1, caractérisée en ce que sur base de tous les composants (3, 4), le composant, qui est formé à partir de l'additif (4) ou des additifs, représente une proportion non supérieure à 5% en moles, de préférence au maximum 3% en moles, en ce que les gains de substance fonctionnelle (3) ont un diamètre moyen d50 supérieur à 1 nm et inférieur à 10 µm, et en ce que les particules (1) de la poudre de pulvérisation, ont un diamètre moyen d50 situé dans l'intervalle allant de 1 à 100 µm.
  3. Poudre de pulvérisation selon la revendication 1 ou 2, caractérisée en ce que l'additif (4) ou les additifs peuvent être déposés dans une phase consistant en des sels métalliques, où ces sels peuvent être transformés thermiquement en des oxydes métalliques, de sorte que les additifs prennent la forme active, influençant le frittage, seulement après une transformation du sel par une étape de traitement thermique.
  4. Poudre de pulvérisation selon la revendication 1 ou 2, caractérisée en ce que les agglomérats, qui forment les particules (1), contiennent des espaces ouverts de pore (5), chaque fois communiquant vers la surface extérieure (11) de la particule, et en ce que dans ces espaces de pore ainsi que sur la surface extérieure, l'additif (4) ou les additifs peuvent être incorporés et respectivement, déposés.
  5. Poudre de pulvérisation selon l'une des revendications 1 à 4, caractérisée en ce que le grain de substance fonctionnelle (3) consiste en une ou plusieurs des substances suivantes:
    - l'oxyde de zirconium, en particulier un oxyde de zirconium stabilisé YSZ;
    - un matériau céramique comme le zirconate de lanthane, qui présente une structure de pyrochlore, A2B2O7, où A et B se présentent sous une forme cationique An+ et respectivement, Bm+, pour les charges n+ et m+ desquels les paires de valeurs n, m sont de 3, 4 ou 2, 5, la formule de la structure de pyrochlore s'exprime de manière générale, A2-xB2+xO7-y, et pour A et B, les éléments chimiques suivants peuvent être envisagés: A = La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb ou un mélange de ces éléments chimiques, et B = Zr, Hf, Ti;
    - une phase magnétoplumbite MMeAl11O19, avec M = La, Nd et Me = Mg, Zn, Co, Mn, Fe, Ni, Cr;
    alors que l'additif (4) ou les additifs sont par exemple, un oxyde de Al, de Mg ou de La, un oxyde d'yttrium-aluminium ou un spinelle, en particulier un oxyde de magnésium-aluminium.
  6. Poudre de pulvérisation selon l'une des revendications 1 à 5, caractérisée en ce que chaque additif (4) ou sa forme transformée, influençant activement le frittage, n'est pas miscible avec la substance fonctionnelle, de sorte qu'une diffusion dans la substance fonctionnelle ne se produit essentiellement pas.
  7. Procédé de préparation d'une poudre de pulvérisation selon l'une des revendications 1 à 6, caractérisé en ce que
    A1) dans un agglomérat poreux des grains de substance fonctionnelle (3), on introduit par un procédé d'imprégnation, au moins un des additifs (4), ou en ce que
    A2) les agglomérats sont préparés à partir d'un mélange des grains de substance fonctionnelle et d'additif finement dispersé ou d'une solution homogène ou colloïdale de l'additif, où les agglomérats sont produits de préférence, par séchage par pulvérisation d'une barbotine et ensuite, calcination.
  8. Procédé selon la revendication 7, caractérisé en ce que dans une première étape, les additifs sont introduits dans l'agglomérat poreux et respectivement, mélangés aux grains de substance fonctionnelle (3), sous forme d'une solution de sel métallique, où ces sels peuvent être transformés thermiquement en oxydes métalliques, dans une deuxième étape, le mélange est séché et dans une troisième étape, les sels sont traités à l'aide d'un traitement thermique en une forme active, influençant le frittage.
  9. Procédé selon la revendication 7 ou 8, caractérisé en ce que dans une étape suivante, les particules (1) de type agglomérat sont fondues brièvement dans une flamme de plasma.
EP03405765A 2002-11-22 2003-10-24 Poudre de pulvérisation pour la fabrication par pulvérisation thermique d'un revêtement de barrière thermique résistant à haute température Expired - Lifetime EP1422308B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP03405765A EP1422308B1 (fr) 2002-11-22 2003-10-24 Poudre de pulvérisation pour la fabrication par pulvérisation thermique d'un revêtement de barrière thermique résistant à haute température

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP02406010 2002-11-22
EP02406010 2002-11-22
EP03405765A EP1422308B1 (fr) 2002-11-22 2003-10-24 Poudre de pulvérisation pour la fabrication par pulvérisation thermique d'un revêtement de barrière thermique résistant à haute température

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EP1422308A1 EP1422308A1 (fr) 2004-05-26
EP1422308B1 true EP1422308B1 (fr) 2008-03-26

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007047629A1 (de) * 2007-04-13 2008-10-16 Stein, Ralf Verfahren zum Aufbringen einer hochfesten Beschichtung auf Werkstücke und/oder Werkstoffe
EP1980645A1 (fr) * 2007-04-13 2008-10-15 Ralf Stein Procédé d'application d'un revêtement multicouche sur des pièces à usiner et/ou matières actives
CN111777413B (zh) * 2020-07-16 2022-06-07 哈尔滨工业大学 一种等离子喷涂用纳米锆酸钆粉体的制备方法及应用
CN114041693B (zh) * 2021-12-17 2022-12-09 武汉苏泊尔炊具有限公司 炊具及其制造方法

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DE3543802A1 (de) * 1985-12-12 1987-06-19 Bbc Brown Boveri & Cie Hochtemperatur-schutzschicht und verfahren zu ihrer herstellung
US5059095A (en) * 1989-10-30 1991-10-22 The Perkin-Elmer Corporation Turbine rotor blade tip coated with alumina-zirconia ceramic
CN1195884C (zh) * 1995-11-13 2005-04-06 康涅狄格大学 用于热喷涂的纳米结构的进料
DE19542944C2 (de) * 1995-11-17 1998-01-22 Daimler Benz Ag Brennkraftmaschine und Verfahren zum Aufbringen einer Wärmedämmschicht
DE19807163C1 (de) * 1998-02-20 1999-10-28 Rainer Gadow Wärmedämmaterial und Verfahren zum Herstellen eines solchen
US6203927B1 (en) * 1999-02-05 2001-03-20 Siemens Westinghouse Power Corporation Thermal barrier coating resistant to sintering
US6544665B2 (en) * 2001-01-18 2003-04-08 General Electric Company Thermally-stabilized thermal barrier coating

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