EP2737101B1 - Beschichtungsverfahren nutzend spezielle pulverförmige beschichtungsmaterialien und verwendung derartiger beschichtungsmaterialien - Google Patents

Beschichtungsverfahren nutzend spezielle pulverförmige beschichtungsmaterialien und verwendung derartiger beschichtungsmaterialien Download PDF

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Publication number
EP2737101B1
EP2737101B1 EP12741314.4A EP12741314A EP2737101B1 EP 2737101 B1 EP2737101 B1 EP 2737101B1 EP 12741314 A EP12741314 A EP 12741314A EP 2737101 B1 EP2737101 B1 EP 2737101B1
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Prior art keywords
particles
coating material
range
spraying
value
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German (de)
English (en)
French (fr)
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EP2737101A2 (de
Inventor
Sebastian HÖFENER
Markus Rupprecht
Christian Wolfrum
Andreas Reis
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Eckart GmbH
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Eckart 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
    • 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
    • C23C4/06—Metallic material
    • C23C4/08—Metallic material containing only metal elements
    • 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
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/02—Coating starting from inorganic powder by application of pressure only
    • C23C24/04—Impact or kinetic deposition of particles
    • 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
    • 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
    • C23C4/06—Metallic material
    • 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
    • C23C4/06—Metallic material
    • C23C4/067—Metallic material containing free particles of non-metal elements, e.g. carbon, silicon, boron, phosphorus or arsenic
    • 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
    • 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
    • C23C4/123—Spraying molten metal
    • 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

Definitions

  • the present invention deals with special powder coating materials. Furthermore, the present invention encompasses the use of such powdered coating materials. Further, the present invention includes methods of substrate coating using such powdery coating materials.
  • a variety of coating techniques have been developed to provide the desired properties for the particular application.
  • Known methods use for generating the coatings, for example, kinetic energy, thermal energy or mixtures thereof, wherein the thermal energy may for example come from a conventional combustion flame or a plasma flame.
  • the latter are further distinguished in thermal and non-thermal plasmas, which have in common that a gas is partially or completely separated into free charge carriers such as ions or electrons.
  • the formation of the coating takes place by applying a powder to a substrate surface, the powder particles being greatly accelerated.
  • a heated process gas is accelerated by expansion in a Laval nozzle to supersonic speed and then injected the powder. Due to the high kinetic energy, the particles form a dense layer upon impact with the substrate surface.
  • the WO 2010/003396 A1 the use of cold gas spraying as a coating method for the application of wear protection coatings. Furthermore, there are revelations of the cold gas spraying process, for example in EP 1 363 811 A1 . EP 0 911 425 B1 and US 7,740,905 B2 ,
  • Flame spraying belongs to the group of thermal coating processes.
  • a powdery coating material is introduced into the flame of a fuel gas-oxygen mixture.
  • acetylene oxygen flames temperatures of up to about 3200 ° C. become.
  • Details on the procedure may be publications such as EP 830 464 B1 and US 5,207,382 A
  • thermal plasma spraying a powdery coating material is injected into a thermal plasma. In the typically used thermal plasma, temperatures of up to about 20,000 K are reached, whereby the injected powder melts and is deposited as a coating on a substrate.
  • thermal plasma spraying and specific embodiments as well as process parameters are known to the person skilled in the art. Exemplary will be on the WO 2004/016821 which describes the use of thermal plasma spraying to apply an amorphous coating. Further, for example, discloses EP 0 344 781 the use of flame spraying and thermal plasma spraying as a coating method using a tungsten carbide powder mixture. Specific devices for use in plasma spraying methods have been widely described in the literature, such as in US Pat EP 0 342 428 A2 . US 7,678,428 B2 . US 7,928,338 B2 and EP 1 287 898 A2 , In high velocity flame spraying, fuel is burned under high pressure, and as fuel, fuel gases, liquid fuels and mixtures thereof can be used.
  • the non-thermal plasma spraying is largely analogous to thermal plasma spraying and flame spraying.
  • a powder coating material is injected into a non-thermal plasma and applied to a substrate surface.
  • Such as the EP 1 675 971 B1 can be removed, this method is characterized by a particularly low thermal stress of the coated substrate.
  • This method, particular embodiments and corresponding process parameters are known to the skilled person from various publications. For example, this describes EP 2 104 750 A2 the application of this method and an apparatus for carrying it out. For example DE 103 20 379 A1 describes the production of an electrically heatable element using this method. Further disclosures regarding the method or devices for non-thermal plasma spraying can be found, for example, in US Pat EP 1 675 971 B1 .
  • a further object of the present invention is to provide a method by which the production of a high-quality and homogeneous coating is made possible under very mild coating conditions (temperature, velocity of the impinging particles).
  • Another object of the present invention is to provide a powdery coating material that offers advantages over the known powdered coating materials when used in the coating of substrates.
  • V m denotes the relative deformability factor.
  • d denotes the average smallest thickness of the particles, measured vertically to and in the middle half of the longitudinal axis of the particles. To determine this thickness At least 50 randomly selected particles are measured and from this the mean value is formed.
  • D 50 is the average particle size at 50% of the volume-average particle size distribution below said size lie. The determination of the D 50 is preferably carried out by means of laser granulometry, using, for example, a HELOS particle size analyzer from Sympatec GmbH, Clausthal-Zellerfeld, Germany.
  • the dispersion of a dry powder can take place here with a dispersion unit of the Rodos T4.1 type at a primary pressure of, for example, 4 bar.
  • size distribution curve of the particles can be measured, for example, with a device from the company Quantachrome (device: Cilas 1064) according to the manufacturer's instructions.
  • a device from the company Quantachrome device: Cilas 1064
  • 1.5 g of the powdered coating material are suspended in about 100 ml of isopropanol, treated for 300 seconds in an ultrasonic bath (apparatus: Sonorex IK 52, Fa. Bandelin) and then added by means of a Pasteur pipette in the sample preparation cell of the meter and measured several times. From the individual measurement results, the resulting averages are formed.
  • the evaluation of the scattered light signals is carried out according to the Fraunhofer method.
  • H X is the Mohs hardness of the particles
  • H Ag is the Mohs hardness of silver.
  • the relative ductility factor of the powdered coating material is at most 0.01.
  • the technical elastic limit of the particles of the powdery coating material is more than 45 N / mm 2 .
  • the melting point of the coating material measured in [K] is up to 60% of the temperature of the substrate-directed medium used in the coating process, for example the gas stream, the combustion flame or the plasma flame.
  • the particles of the powdered coating material comprise or are metal particles, the metal being selected from the group consisting of silver, gold, platinum, palladium, vanadium, chromium, manganese, cobalt, germanium, antimony, aluminum, zinc , Tin, iron, copper, nickel, titanium, silicon, alloys and mixtures thereof.
  • the coating process is selected from the group consisting of flame spraying, and non-thermal plasma spraying.
  • the coating process is nonthermal plasma spraying.
  • the powdery coating material has a particle size distribution with a D 50 value in the range from 1.5 to 84 ⁇ m. In certain embodiments of the aforementioned uses, the powdery coating material has a particle size distribution with a D 10 value from a range of 3.7 to 26 microns, a D 50 value from a range of 6 to 49 microns and a D 90 value from a range of 12 to 86 microns on.
  • the particles of the powdered coating material are at least partially coated. In certain of the aforementioned embodiments, the particles of the powder coating material are coated.
  • the powdery coating material is conveyed as an aerosol.
  • the medium directed to the substrate is air or was generated from air.
  • the aforementioned air can be taken from the ambient atmosphere.
  • the air is cleaned prior to its use, wherein, for example, dust and / or water vapor is separated.
  • the gaseous constituents of the air are substantially completely separated apart from nitrogen and oxygen (total amount ⁇ 0.01% by volume, preferably ⁇ 0.001% by volume).
  • powder coating material in the context of the present invention refers to a particle mixture which is applied to the substrate as a coating. It is not necessary in this case for the particles of the powdery coating material according to the invention to have a uniform thickness. Without it being to be understood as limiting the invention, it is the view of the inventors that the particles of the powdery coating material according to the invention can be mechanically deformed particularly easily and thereby significantly simpler unevenness of the substrate and fill gaps in the already applied coating, without there is a need to reflow or greatly accelerate the particles by means of a large amount of thermal energy to provide sufficient kinetic energy to deform.
  • the powdered coating material according to the invention sprays to a reduced extent from the surface of the substrate during the application of the coating.
  • the higher mechanical deformability of the particles of the invention results in a lighter conversion of the kinetic energy into a deformation of the particle, whereby the tendency for an elastic shock resulting in a Spraying the particles is reduced by the substrate to be coated, which, for example, particularly advantageous in use expensive or poorly recyclable coating materials.
  • This effect is of particular importance for processes using high gas velocities, especially for example cold gas spraying and high velocity flame spraying.
  • the particles of the powdery coating material according to the invention are therefore distinguished by the abovementioned upper limit of the relative deformability factor.
  • V m denotes the relative deformability factor.
  • d denotes the average smallest thickness of the particles, measured vertically to and in the middle half of the longitudinal axis of the particles. To determine this average thickness, at least 50 randomly selected particles are measured by means of SEM and from this the mean value is formed.
  • D 50 denotes the average particle size at which 50% of the volume-average particle size distribution lies below the stated size. The determination of the D 50 is preferably carried out by means of laser granulometry, using, for example, a HELOS particle size analyzer from Sympatec GmbH, Clausthal-Zellerfeld, Germany.
  • the mechanical deformability of the particles depends to a certain extent on the hardness of the material used. In certain embodiments, therefore, it may be preferable to introduce a correction factor based on the Mohs hardness of the material, as long as the Mohs hardness is above that of the silver. For substances with a Mohs hardness below that of silver, however, such a correction is only minor, which is why such substances the Mohs hardness of silver is used.
  • H Ag is the Mohs hardness of silver (2,7) and H X is the Mohs hardness of the material of the particles of the powdery coating material.
  • r x denotes the average proportion of the thickness of the layer X on the total particle.
  • the average thickness of the layer is preferably determined by means of SEM by measuring 50 randomly selected particles.
  • the relative deformability factor according to formula (I) or (II), optionally taking into account formula (IV), of the powdery coating material according to the invention has a relative deformability factor of at most 0.1, preferably at most 0.07 , more preferably at most 0.05, and even more preferably at most 0.03.
  • the relative deformability factor of the powdery coating material is at most 0.01, preferably at most 0.007, more preferably at most 0.005 and even more preferably at most 0.003.
  • Processes of the present invention that can be used to build coatings include cold gas spraying, thermal plasma spraying, non-thermal plasma spraying, flame spraying, and high velocity flame spraying.
  • the use of the powdery coating materials according to the invention has a particularly pronounced effect in processes in which no particularly high kinetic energies are transferred to the particles, since sufficient deformation of the particles is already achieved at significantly lower speeds.
  • the method be selected from the group consisting of thermal plasma spraying, non-thermal plasma spraying and flame spraying.
  • the method is selected from the group consisting of cold gas spraying, non-thermal plasma spraying, flame spraying and high velocity flame spraying, preferably from the group consisting of non-thermal plasma spraying and flame spraying.
  • a plasma offers the advantage that non-combustible gases can also be used as the plasma gas, thereby simplifying the apparatus and, in particular, the necessary safety precautions.
  • a harmless, easy-to-use gas is used and for special process variants small amounts of other gases to be stored in stock.
  • the method be selected from the group consisting of thermal plasma spraying and non-thermal plasma spraying.
  • non-thermal plasma spraying is used as the coating method.
  • the powdery coating materials according to the invention it is also possible to produce particularly homogeneous coatings under gentle coating conditions from substances which have a high yield strength.
  • the yield strength is a relative limit that reflects a relation between the stress applied to a material and the resulting plastic deformation. Of particular importance in this case is the 0.2% proof stress, which is also referred to as the technical elastic limit.
  • the technical elastic limit of the coating material employed is more than 45 N / mm 2 , preferably more than 70 N / mm 2 , more preferably more than 85 N / mm 2 and even more preferably more than 100 N / mm 2 .
  • the engineering elastic limit of the coating material of the invention is more than 130 N / mm 2 , preferably more than 160 N / mm 2 , more preferably more than 190 N / mm 2 and even more preferably more than 210 N / mm 2 .
  • the determination of the technical elastic limit is here according to DIN EN ISO 6892. Without it being to be understood as a limitation of the invention, it is the view of the inventors that previously used powdery coating materials were not sufficiently deformable when using gentle coating conditions when hitting the surface , Therefore, the surface structure or structure of the already applied coating could not adapt sufficiently and include cavities.
  • the average ratio of the largest thickness to the smallest thickness measured vertically to and in the middle half of the longitudinal axis of the particles is at least 1.3, preferably at least 1.4, more preferably at least 1.5, and even more preferably at least 1.6.
  • the average ratio of the thickest point to the thinnest point measured vertically to and in the middle half of the longitudinal axis of the particles be at least 1.8, preferably at least 2.0, more preferably at least 2.2, and even more preferably at least 2.4.
  • the determination of the average greatest thickness is analogous to the determination of the aforementioned average minimum thickness.
  • the average ratio of the largest thickness to the smallest thickness is calculated by the average of the ratio of at least 50 randomly selected particles.
  • the inventors have surprisingly found that the use of the inventive mechanically easily deformable powdery coating materials also the use of coating materials with an unexpectedly high melting point is made possible.
  • the at least largely sufficient energy is available to the particles of the powdery coating material selected according to the invention by the kinetic energy used in the coating process in order to transfer the particles to the substrate surface or to the substrate to adjust the gaps between already applied particles. If a thermal component is required at all, a significantly reduced amount of thermal energy is needed to allow a solid connection of the deposited particles to form a homogeneous layer.
  • powdery coating materials according to the invention can also be used to produce homogeneous layers if the melting point of the particles of the coating material measured in [K] is up to 60%, preferably up to 70%, more preferably up to 80% and even more preferably up to to 85% of the temperature measured in [K] of the medium used in the coating process, for example gas flow, the combustion flame and / or the plasma flame is.
  • particle-containing powdery coating materials to be used according to the invention can also be used for producing homogeneous layers if the melting point of the particles of the coating material measured in [K] is up to 90%, preferably up to 95%, more preferably up to 100% and even more preferably up to 105% of the temperature measured in [K] of the medium used in the coating process, for example gas flow, the combustion flame and / or the plasma flame is.
  • the abovementioned percentages refer to the ratio of the melting temperature of the coating material to the temperature of the gas stream in cold gas spraying, the combustion flame in flame spraying and high-speed flame spraying or the plasma flame in non-thermal or thermal plasma spraying in [K].
  • the resulting coating has only a few free, preferably no, particle or grain structures.
  • the "homogeneous layers” according to the invention are characterized in that the layers produced are less than 10%, preferably less than 5%, more preferably less than 3%, even more preferably less than 1% and most preferably less than 0.1%. Have cavities. In particular, it is preferred that no cavities are to be recognized.
  • the aforementioned term "cavity" in the sense of the present invention describes the proportion of the gaps enclosed in the coating on the two-dimensional surface of a transverse section of the coated substrate, based on the coating contained in the two-dimensional surface. A determination of this proportion is carried out by means of SEM at 30 randomly selected locations of the coating, wherein, for example, a length of 100 ⁇ m of the substrate coating is considered.
  • the coatings of the invention have a significantly improved thermal conductivity.
  • the coatings produced according to the invention have a thermal conductivity which is close to the thermal conductivity of a homogeneous block of the corresponding coating material due, for example, to their significantly higher homogeneity. This is attributed inter alia to the fact that no inclusions of air are included, which could hinder a heat conduction.
  • the barrier effect of the coatings according to the invention is drastically increased.
  • the coatings produced according to the invention have a denser structure, a smoother surface and a more uniform shape. Since isolated gaps in the coating represent targets for, for example, corrosion of the substrate, the coatings with denser structure and uniform shape produced according to the invention provide more reliable protection even with thin coatings, while the smoother surface offers fewer points of attack where, for example, by mechanical effects Damage to the coating occurs.
  • defined and reliable permeabilities of the coatings can be realized by the coatings produced according to the invention, since for the aforementioned reasons, for example, no indefinitely permeable gaps are present, the uniform formation of the coating provides a uniform barrier effect over the length of the coated substrate and mechanical effects not easy cause damage to the coating.
  • the determination of the size distribution of the particles is preferably carried out by means of laser granulometry.
  • the particles can be measured in the form of a powder.
  • the scattering of the irradiated laser light is detected in different spatial directions and evaluated according to the Fraunhofer diffraction theory.
  • the particles are treated mathematically as spheres.
  • the determined diameters always relate to the equivalent spherical diameter determined over all spatial directions, irrespective of the actual shape of the particles.
  • It determines the size distribution which is calculated in the form of a volume average, based on the equivalent spherical diameter.
  • This volume-averaged size distribution can be considered Cumulative frequency distribution.
  • the cumulative frequency distribution is simplified by various characteristic values, for example the D 10 , D 50 or D 90 value.
  • the measurements can be carried out, for example, using the particle size analyzer HELOS from Sympatec GmbH, Clausthal-Zellerfeld, Germany.
  • the powdery coating material has a particle size distribution with a D 50 value of at most 84 ⁇ m, preferably at most 79 ⁇ m, more preferably at most 75 ⁇ m and even more preferably at most 71 ⁇ m.
  • the powdery coating material has a particle size distribution with a D 50 value of at most 64 ⁇ m, preferably at most 61 ⁇ m, more preferably at most 59 ⁇ m and even more preferably at most 57 ⁇ m.
  • D 50 in the sense of the present invention denotes the particle size at which 50% of the aforementioned volume-average particle size distribution determined by means of laser granulometry is below the stated value. The measurements can be carried out, for example, according to the abovementioned measuring method using a particle size analyzer HELOS from Sympatec GmbH, Clausthal-Zellerfeld, Germany.
  • the powdery coating material further has a particle size distribution with a D 50 value of at least 1.5 ⁇ m, preferably at least 2 ⁇ m, more preferably at least 4 ⁇ m and even more preferably at least 6 ⁇ m.
  • the powdery coating material is a Grain size distribution having a D 50 value of at least 7 microns, preferably at least 9 microns, more preferably at least 11 microns and even more preferably at least 13 microns.
  • the powder has a particle size distribution with a D 50 value from a range of 1.5 to 84 microns, preferably from a range of 2 to 79 microns, more preferably from a range of 4 to 75 microns, and more preferably from a range of 6 to 71 microns.
  • the powder has a particle size distribution with a D 50 value in a range of 7 to 64 ⁇ m, preferably in a range of 9 to 61 ⁇ m, more preferably in a range of 11 to 59 ⁇ m and more preferably from a range of 13 to 57 microns.
  • the powder has a particle size distribution with a D 50 value in the range of 1.5 to 53 ⁇ m, preferably in the range of 2 to 51 ⁇ m, more preferably in the range of 2.5 to 50 microns, and more preferably from a range of 3 to 49 microns.
  • the powder has a particle size distribution with a D 50 value in the range from 3.5 to 48 ⁇ m, preferably in a range from 4 to 47 ⁇ m, more preferably in a range from 4, 5 to 46 microns, and more preferably from a range of 5 to 45 microns.
  • the powder has a particle size distribution with a D 50 value from a range of 9 to 84 microns, preferably from a range of 12 to 79 microns, more preferably from a range of 15 to 75 microns , more preferably from a range of 17 to 71 microns.
  • the powder has a particle size distribution with a D 50 value from a range of 19 to 64 .mu.m, preferably from a range of 21 to 61 .mu.m, more preferably from a range of 23 to 59 .mu.m and more preferably from a Range of 25 to 57 microns has.
  • the powdery coating material has a particle size distribution with a D 90 value of at most 132 ⁇ m, preferably at most 122 ⁇ m, more preferably at most 115 ⁇ m and even more preferably at most 109 ⁇ m.
  • the powdery coating material has a D 90 value of at most 97 ⁇ m, preferably at most 95 ⁇ m, more preferably at most 91 ⁇ m and even more preferably at most 89 ⁇ m.
  • D 90 in the sense of the present invention denotes the particle size at which 90% of the aforementioned volume-average particle size distribution determined by means of laser granulometry is below the stated value.
  • the measurements can be carried out, for example, according to the abovementioned measuring method using a particle size analyzer HELOS from Sympatec GmbH, Clausthal-Zellerfeld, Germany.
  • the powdery coating material has a particle size distribution with a D 90 value of at least 9 ⁇ m, preferably at least 11 ⁇ m, more preferably at least 13 ⁇ m and even more preferably at least 15 ⁇ m.
  • the powdery coating material has a particle size distribution with a D 90 value of at least 17 ⁇ m, preferably at least 19 ⁇ m, more preferably at least 21 ⁇ m and even more preferably at least 22 ⁇ m.
  • the powdery coating materials have a particle size distribution with a D 90 value in a range from 42 to 132 ⁇ m, preferably from a range from 45 to 122 ⁇ m, more preferably from a range from 48 to 115 ⁇ m and even more preferred a range of 50 to 109 microns.
  • the powdery coating material has a D 90 value in a range of 52 to 97 ⁇ m, preferably in a range of 54 to 95 ⁇ m, more preferably in a range of 56 to 91 ⁇ m, and still more preferably from a range of 57 to 89 microns.
  • the powdery coating material has a particle size distribution with a D 10 value of at most 9 ⁇ m, preferably at most 8 ⁇ m, more preferably at most 7.5 ⁇ m and even more preferably at most 7 ⁇ m.
  • the powdery coating material has a grain size distribution having a D 10 of at most 6.5 ⁇ m, preferably at most 6 ⁇ m, more preferably at most 5.7 ⁇ m, and still more preferably at most 5.4 ⁇ m having.
  • D 10 in the sense of the present invention denotes the particle size at which 10% of the aforementioned volume-average particle size distribution determined by means of laser granulometry is below the stated value.
  • the measurements can be carried out, for example, according to the abovementioned measuring method using a particle size analyzer HELOS from Sympatec GmbH, Clausthal-Zellerfeld, Germany.
  • the powdery coating materials with a high fines content also strongly tend to form fine dusts, which makes the handling of corresponding powders considerably more difficult.
  • the powdery coating material has a particle size distribution with a D 10 value of at least 0.2 ⁇ m, preferably at least 0.4 ⁇ m, more preferably at least 0.5 ⁇ m and even more preferably at least 0.6 ⁇ m exhibit.
  • the powdered coating material has a particle size distribution with a D 10 value of at least 0.7 ⁇ m, preferably 0.8 ⁇ m, more preferably 0.9 ⁇ m and even more preferably at least 1.0 ⁇ m having.
  • the powdery coating material is characterized by having a grain size distribution with a D 10 value in the range of 0.2 to 9 ⁇ m, preferably in the range of 0.4 to 8 ⁇ m, more preferably in one range from 0.5 to 7.5 microns, and more preferably from a range of 0.6 to 7 microns.
  • the powdery coating material has a grain size distribution with a D 10 value in a range of 0.7 to 6.5 ⁇ m, preferably in a range of 0.8 to 6 ⁇ m, more preferably a range of 0.9 to 5.7 microns, and more preferably from a range of 1.0 to 5.4 microns
  • the powdered coating material has a particle size distribution with a D 10 value of 3.7 to 26 ⁇ m, a D 50 value of 6 to 49 ⁇ m and a D 90 value of 12 to 86 ⁇ m having.
  • the powdery coating material has a particle size distribution having a D 10 value of 5.8 to 26 microns, a D 50 value of 11 to 46 microns and a D 90 value of 16 to 83 microns.
  • the powdery coating material has a particle size distribution with a D 10 value of 9 to 19 ⁇ m, a D 50 value of 16 to 35 ⁇ m and a D 90 value of 23 to 72 ⁇ m having.
  • the powdery coating material has a particle size distribution with a D 10 value of 0.8 to 60 ⁇ m, a D 50 value of 1.5 to 84 ⁇ m and a D 90 value of 2, 5 to 132 microns has.
  • the powdery coating material has a particle size distribution with a D 10 value of 2.2 to 56 ⁇ m, a D 50 value of 4 to 79 ⁇ m and a D 90 value of 4 to 122 has ⁇ m.
  • the powdery coating material has a particle size distribution with a D 10 value of 2.8 to 49 ⁇ m, a D 50 value of 6 to 71 ⁇ m and a D 90 value of 9 to 109 microns.
  • the powdered coating material has a particle size distribution with a D 10 value of 4.8 to 44 microns, a D 50 value 9-64 microns and a D 90 value of 13 to 97 microns having.
  • the powdery coating material has a particle size distribution with a D 10 value of 12 to 41 ⁇ m, a D 50 value of 23 to 59 ⁇ m and a D 90 value of 35 to 91 ⁇ m , In certain of the aforementioned embodiments, it is even more preferable that the powdery coating material has a Grain size distribution having a D 10 value of 15 to 39 microns, a D 50 value of 28 to 57 microns and a D 90 value of 41 to 89 microns. Further, it has been observed that the conveyability of the powdery coating material is dependent on the width of the particle size distribution.
  • the particle size of the powdery coating material is at most 2.9, preferably at most 2.6, more preferably at most 2.4, and even more preferably at most 2.1.
  • the span of the powdery coating material is at most 1.9, preferably at most 1.8, more preferably at most 1.7, and even more preferably at most 1.6.
  • the inventors have found that a very narrow chip is not necessarily required for providing the desired conveyance, which facilitates the production of the powdery coating material.
  • the span value of the powdery coating material is at least 0.4, preferably at least 0.5, more preferably at least 0.6 and even more preferably at least 0.7.
  • the span of the powdered coating material is at least 0.8, preferably at least 0.9, more preferably at least 1.0, and even more preferably at least 1.1. Based on the teachings disclosed herein, one skilled in the art may choose any combination, in particular, of the aforementioned span value limits to provide the desired combination of properties.
  • the powdery coating material has a span value from a range from 0.4 to 2.9, preferably from a range from 0.5 to 2.6, more preferably from a range from 0.6 to 2, 4 and even more preferably from a range of 0.7 to 2.1.
  • the powdery coating material has a span value in a range of 0.8 to 1.9, preferably in a range of 0.9 to 1.8, more preferably in a range of 1 , 0 to 1.7, and more preferably from 1.1 to 1.6.
  • the skilled worker is aware that based on the teachings disclosed herein, depending on the desired combination of the advantages of certain combinations of the clamping limits or ranges of values with the aforementioned preferred D 50 -Wert Schemeen are preferred.
  • the powdered coating material has a particle size distribution with a span in the range of 0.4 to 2.9 and a D 50 value in the range of 1.5 to 53 ⁇ m, preferably in a range of 2 to 51 ⁇ m, more preferably from a range of 4 to 50 ⁇ m, even more preferably from a range of 6 to 49 ⁇ m, and most preferably from a range of 7 to 48 ⁇ m.
  • the powdery coating material has a grain size distribution with a chip of one Range of 0.5 to 2.6 and a D 50 value from a range of 1.5 to 53 microns, preferably from a range of 2 to 51 microns, more preferably from a range of 4 to 50 microns, even more preferably from a range of 6 to 49 ⁇ m, and most preferably from a range of 7 to 48 ⁇ m.
  • the powdery coating material has a particle size distribution with a span of from 0.6 to 2.4 and a D 50 value in the range of 1.5 to 53 ⁇ m, preferably in the range of 2 to 51 ⁇ m, more preferably from a range of 4 to 50 ⁇ m, even more preferably from a range of 6 to 49 ⁇ m, and most preferably from a range of 7 to 48 ⁇ m.
  • the powdered coating material has a particle size distribution with a span of from 0.7 to 2.1 and a D 50 value in the range of 1.5 to 53 ⁇ m, preferably in the range of 2 to 51 microns, more preferably from a range of 4 to 50 microns, even more preferably from a range of 6 to 49 microns and most preferably from a range of 7 to 48 microns on.
  • the density of the powdery coating material can have an influence on the promotion of such powders in the form of an aerosol. Without intending to be construed as limiting the invention, it is the view of the inventors that the differences in inertia of equally sized particles of different density will result in a different behavior of the aerosol streams of powdered coating materials having identical grain size distribution. Therefore, it may be difficult to transfer production processes that have been optimized for a specific D 50 to different density powdered coating materials. In certain embodiments, it is therefore preferred that the upper limit of the Span value be dependent on the Density of the powdered coating material according to formula V is corrected.
  • spa n OK spa n O ⁇ ⁇ Alu ⁇ X 1 3
  • Span OK is the corrected upper span value
  • Span O is the upper span value
  • ⁇ Alu is the density of aluminum (2.7 g / cm 3 )
  • ⁇ X is the density of the powdered coating material used.
  • Coating processes which can be used according to the invention are known to the person skilled in the art under the name of cold gas spraying, thermal plasma spraying, non-thermal plasma spraying, flame spraying and high-speed flame spraying.
  • the cold gas spraying is characterized in that the powder to be applied is not melted in the gas jet, but that the particles are greatly accelerated and form a coating on the surface of the substrate due to their kinetic energy.
  • gases known to those skilled in the art can be used as the carrier gas, such as nitrogen, helium, argon, air, krypton, neon, xenon, carbon dioxide, oxygen or mixtures thereof. In certain variants, it is particularly preferred that are used as gas, air, helium or mixtures thereof.
  • the particles can be accelerated up to 2000 m / s. In certain variants of cold gas spraying, however, it is preferred that they have particles, for example, speeds between 300 m / s and 1600 m / s, preferably between 1000 m / s and 1600 m / s, more preferably between 1250 m / s and 1600 m / s to reach.
  • a powder is converted into the liquid or plastic state by means of a flame and then applied as a coating to a substrate.
  • a flame e.g. a mixture of oxygen and a combustible gas such as acetylene or hydrogen burned.
  • part of the oxygen is used to convey the powdery coating material into the combustion flame.
  • the particles reach in conventional variants of this process speeds between 24 to 31 m / s.
  • high-speed flame spraying converts a powder into a liquid or plastic state by means of a flame.
  • the particles are accelerated significantly faster compared to the aforementioned method.
  • a velocity of the gas stream of 1220 to 1525 m / s is called with a velocity of the particles of about 550 to 795 m / s.
  • gas velocities of over 2000 m / s are achieved.
  • the speed of the flame be between 1000 and 2500 m / s.
  • the flame temperature is between 2200 ° C and 3000 ° C.
  • the temperature of the flame is thus comparable to the temperature during flame spraying. This is achieved by combustion of the gases under a pressure of about 515 to 621 kPa followed by the expansion of the combustion gases in a nozzle.
  • coatings produced thereby have a higher density compared to, for example, coatings obtained by the flame spraying process.
  • the detonation / explosive flame spraying can be regarded as a subspecies of the high-velocity flame spraying.
  • the powdery coating material is greatly accelerated by repeated detonations of a gas mixture such as acetylene / oxygen, for example, particle velocities of about 730 m / s are achieved.
  • the detonation frequency of the method is in this case, for example, between about 4 to 10 Hz. In variants such as the so-called high-frequency gas detonation spraying but also detonation frequencies are selected by about 100 Hz.
  • the resulting layers should usually have a particularly high hardness, strength, density and good bonding to the substrate surface.
  • a disadvantage of the aforementioned method the increased security costs, and, for example, the large noise pollution due to the high gas velocities.
  • thermal plasma spraying for example, a primary gas such as argon is passed through a DC arc furnace at a rate of 40 l / min and a secondary gas such as hydrogen at a rate of 2.5 l / min, thereby generating a thermal plasma. Subsequently, the supply of, for example, 40 g / min of the pulverulent takes place Coating material by means of a carrier gas stream, which is passed into the plasma flame at a rate of 4 l / min. In conventional variants of thermal plasma spraying, the delivery rate of the powdered coating material is between 5 g / min and 60 g / min, more preferably between 10 g / min and 40 g / min.
  • argon, helium or mixtures thereof as ionizable gas.
  • the total gas flow is also preferably 30 to 150 SLPM (standard liters per minute) for certain variants.
  • the electrical power used for the ionization of the gas flow without the heat energy dissipated as a result of cooling can be selected, for example, between 5 and 100 kW, preferably between 40 and 80 kW.
  • plasma temperatures between 4000 and a few 10000 K can be achieved.
  • a non-thermal plasma is used to activate the powdery coating material.
  • the plasma used in this case is generated for example with a barrier discharge or corona discharge with a frequency of 50 Hz to 1 MHz. In certain variants of non-thermal plasma spraying, it is preferred to operate at a frequency of 10 kHz to 100 kHz.
  • the temperature of the plasma is preferably less than 3000 K, preferably less than 2500 K and more preferably less than 2000 K. This minimizes the technical complexity and keeps the energy input in the applied coating material as low as possible, which in turn allows a gentle coating of the substrate , The magnitude of the temperature of the plasma flame is thus preferably comparable to that in flame spraying or high-speed flame spraying.
  • Targeted choice of parameters also allows the generation of nonthermal plasmas with a core temperature below 1173 K or even below 773 K in the core region.
  • the measurement of Temperature in the core region takes place here, for example, with a thermocouple type NiCr / Ni and a tip diameter of 3 mm in 10 mm distance from the nozzle exit in the core of the exiting plasma jet at ambient pressure.
  • Such non-thermal plasmas are particularly suitable for coatings of very temperature-sensitive substrates.
  • the outlet opening of the plasma flame to make such that the web widths of the coatings produced are between 0.2 mm and 10 mm.
  • This allows a very accurate, flexible, energy-efficient coating with the best possible utilization of the coating material used.
  • a distance of the spray lance to the substrate for example, a distance of 1 mm is selected. This allows for the greatest possible flexibility of the coatings while ensuring high-quality coatings.
  • the distance between the spray lance and the substrate is between 1 mm and 35 mm.
  • ionizable gas various gases known to those skilled in the art and mixtures thereof can be used in the non-thermal plasma process. Examples of these are helium, argon, xenon, nitrogen, oxygen, hydrogen or air, preferably argon or air. A particularly preferred ionizable gas is air.
  • the speed of the plasma flow is below 200 m / s.
  • a flow rate for example, a value between 0.01 m / s and 100 m / s, preferably between 0.2 m / s and 10 m / s are selected.
  • the volume flow of the carrier gas is between 10 and 25 l / min, more preferably between 15 and 19 l / min.
  • the particles of the powdery coating material are preferably metallic particles or metal-containing particles.
  • the metal content of the metallic particles or metal-containing particles is at least 95% by weight, preferably at least 99% by weight, more preferably at least 99.9% by weight.
  • the metal or metals is selected from the group consisting of silver, gold, platinum, palladium, vanadium, chromium, manganese, cobalt, germanium, antimony, aluminum, zinc, tin, iron, copper, nickel, titanium, silicon , Alloys and mixtures thereof.
  • the metal or metals be selected from the group consisting of silver, gold, aluminum, zinc, tin, iron, copper, nickel, titanium, silicon, alloys, and mixtures thereof, preferably from the group consisting of silver, gold, aluminum, zinc, tin, iron, nickel, titanium, silicon, alloys and mixtures thereof.
  • the metal or the metals of the particles of the powdery coating material is selected from the group consisting of silver, aluminum, zinc, tin, copper, alloys and mixtures thereof.
  • Particularly suitable particles in specific embodiments have been found to be metallic particles or metal-containing particles in which the metal or metals are selected from the group consisting of silver, aluminum and tin.
  • the powdery coating material consists of inorganic particles, preferably from the Group consisting of carbonates, oxides, hydroxides, carbides, halides, nitrides and mixtures thereof. Particularly suitable are mineral and / or metal oxide particles.
  • the inorganic particles are alternatively or additionally selected from the group consisting of carbon particles or graphite particles.
  • Another non-inventive possibility is the use of mixtures of the metallic particles and the aforementioned inorganic particles, such as mineral and / or metal oxide particles, and / or the particles consisting of the group consisting of carbonates, oxides, hydroxides, carbides, halides , Nitrides and mixtures thereof.
  • the powdery coating material may comprise or consist of glass particles.
  • the powdery coating material comprises or consists of coated glass particles.
  • the powdery coating material comprises or consists of organic and / or inorganic salts.
  • the powdery coating material comprises or consists of plastic particles.
  • the abovementioned plastic particles are formed from, for example, pure or mixed homo-, co-, block- or prepolymers or mixtures thereof.
  • the plastic particles may be pure crystals or be mixed crystals or have amorphous phases.
  • the plastic particles can be obtained, for example, by mechanical comminution of plastics.
  • the powdery coating material comprises or consists of mixtures of particles of different materials.
  • the powdery coating material consists in particular of at least two, preferably three, different particles of different materials.
  • the particles can be produced by different methods.
  • the metal particles can be obtained by atomization or atomization of molten metal.
  • Glass particles can be produced by mechanical comminution of glass or else from the melt. In the latter case, the molten glass can also be atomized or atomized. Alternatively, molten glass can also be cut on rotating elements, such as a drum.
  • Mineral particles, metal oxide particles and inorganic particles selected from the group consisting of oxides, hydroxides, carbonates, carbides, nitrides, halides and mixtures thereof can be obtained by comminuting the naturally occurring minerals, rocks, etc. and subsequently size-classified. Size classification can be carried out, for example, by means of cyclones, air separators, screening, etc.
  • the easily deformable particles of the powdery coating material according to the invention have been provided with a coating in order, for example, to provide improved oxidation stability during storage of the powdered coating material.
  • the aforesaid coating may comprise or be made of a metal.
  • a coating of a particle may be closed or particulate, with closed structure coatings being preferred.
  • the layer thickness of such a metallic coating is preferably less than 1 ⁇ m, more preferably less than 0.8 ⁇ m and even more preferably less than 0.5 ⁇ m.
  • such coatings have a thickness of at least 0.05 ⁇ m, more preferably at least 0.1 ⁇ m.
  • particularly preferred metals for use in any of the foregoing coatings are selected from the group consisting of copper, titanium, gold, silver, tin, zinc, iron, silicon, nickel, and aluminum, preferably selected from the group of gold, silver, tin and zinc, more preferably from the group consisting of silver, tin and zinc.
  • the term main constituent in the sense of the abovementioned coating denotes that the metal in question or a mixture of the abovementioned metals represents at least 90% by weight, preferably 95% by weight, more preferably 99% by weight, of the metal content of the coating. It must be understood that in the case of a partial oxidation of the oxygen content of the corresponding oxide layer is not included.
  • the production of such metallic coatings can be carried out, for example, by means of gas-phase synthesis or wet-chemical processes.
  • the particles of the powdery coating material according to the invention are additionally or alternatively coated with a metal oxide layer.
  • this metal oxide layer consists essentially of silicon oxide, aluminum oxide, boron oxide, zirconium oxide, cerium oxide, iron oxide, titanium oxide, chromium oxide, tin oxide, molybdenum oxide, their hydrated oxides, their hydroxides and mixtures thereof.
  • the metal oxide layer consists essentially of silicon oxide.
  • the aforementioned term "consists essentially of" in the sense of the present invention means that at least 90%, preferably at least 95%, more preferably at least 98%, even more preferably at least 99% and most preferably at least 99.9% of the metal oxide layer the above-mentioned metal oxides, in each case based on the number of particles of the metal oxide layer, wherein optionally contained water is not included.
  • the determination of the composition of the metal oxide layer can be carried out by methods known to the person skilled in the art, for example sputtering in combination with XPS or TOF-SIMS.
  • the metal oxide layer is not an oxidation product of a metal core located thereunder.
  • the application of such a metal oxide layer can be carried out, for example, by the sol-gel method.
  • the substrate is selected from the group consisting of plastic substrates, inorganic substrates, cellulosic substrates, and mixtures thereof.
  • the plastic substrates may be, for example, plastic films or molded plastic.
  • the shaped bodies can have geometrically simple or complex shapes.
  • the plastic molding may be, for example, a component of the automotive industry or the construction industry.
  • the cellulose-containing substrates may be cardboard, paper, wood, wood-containing substrates, etc.
  • the inorganic substrates may be, for example, metallic substrates, such as metal sheets or metallic moldings or ceramic or mineral substrates or moldings.
  • the inorganic substrates may also be solar cells or silicon wafers onto which, for example, electrically conductive coatings or contacts are applied.
  • Substrates made of glass can also be used as inorganic substrates.
  • the glass, in particular glass panes can be provided using the method according to the invention, for example with electrochromic coatings.
  • coated by the process according to the invention substrates are suitable for very different applications.
  • the coatings have optical and / or electromagnetic effects.
  • the coatings can cause reflections or absorptions.
  • the coatings may be electrically conductive, semi-conductive or non-conductive.
  • Electrically conductive layers can be applied to components, for example in the form of printed conductors. This can be used, for example, to enable the power supply in the context of the electrical system in a motor vehicle component. Furthermore, however, such a track may also be shaped, for example, as an antenna, as a shield, as an electrical contact, etc. This is for example particularly advantageous for RFID applications (radio frequency identification). Furthermore, coatings according to the invention can be used, for example, for heating purposes or for specific heating of special components or special parts of larger components.
  • the coatings produced serve as slip layers, diffusion barriers for gases and liquids, wear and / or corrosion protection layers. Furthermore, the coatings produced can influence the surface tension of liquids or have adhesion-promoting properties.
  • the coatings produced according to the invention can furthermore be used as sensor surfaces, for example as a human-machine interface (HMI: human-machine interface), for example in the form of a touch screen.
  • HMI human-machine interface
  • the coatings can be used to shield from electromagnetic interference (EMI) or to protect against electrostatic discharge (ESD).
  • EMI electromagnetic interference
  • ESD electrostatic discharge
  • the coatings can also be used to effect electromagnetic compatibility (EMC).
  • layers can be applied by the use of the particles according to the invention, which are applied, for example, to increase the stability of corresponding components after their repair.
  • An example is repairs in the aircraft sector, for example, a loss of material due to processing steps must be compensated or a coating is to be applied, for example, for stabilization. This proves difficult for aluminum components, for example, and usually requires finishing operations such as sintering.
  • firmly adhering coatings can be applied under very gentle conditions, even without post-processing steps such as sintering being necessary.
  • the coatings serve as electrical contacts and permit electrical connection between different materials.
  • Figures 1 to 4 show a wafer, which was first coated by means of solar contact paste and subsequently by means of non-thermal plasma spraying, wherein a powdered copper coating material according to the invention was used.
  • the size distribution of the particles of the powdered coating materials used was determined by means of a HELOS instrument (Sympatec, Germany). For the measurement, 3 g of the powdered coating material was placed in the meter and sonicated for 30 seconds prior to measurement. For dispersion, a Rodos T4.1 dispersion unit was used, the primary pressure being 4 bar. The evaluation was carried out with the standard software of the device.
  • Example 1 flame spraying of copper particles
  • spherical copper particles having a relative deformability of about 0.6, with a D 50 value of 54 ⁇ m (comparative example 1.1), and copper particles with a relative deformability factor of 0, were prepared by means of an acetylene / oxygen flame. 03 and a D 50 value of 55 microns (Example 1.2 invention) applied to a plate. The resulting sheets were examined by SEM.
  • the coated sheet according to the invention is much more homogeneous in terms of its appearance and feel. SEM images of the surfaces show the formation of larger uniform areas of the coating, while the surface of the comparative example is characterized by a plurality of separated particles. Furthermore, the cross-section shows that cavities contained in the coating of the sheet according to the invention are significantly smaller.
  • the application of the powdery coating material was carried out by means of a Plasmatron plant from Inocon, Attnang-Puchheim, Austria. Argon was used as the ionizable gas. Standard process parameters were used.
  • a non-inventive powdered coating material having a relative deformability factor of 0.6 and a D 50 of 25 microns, and a powdered coating material according to the invention having a relative deformability factor of 0.009 and a D 50 of 35 microns was used.
  • the substrate was a wafer coated with solar contact paste.
  • the higher energies. which are normally chosen by the expert for applying the powdery coating materials can lead to damage of the wafer.
  • no satisfactory coatings were obtained with a powdery coating material having a relative ductility factor of 0.6 because, for example, the adhesion of the coatings was no longer satisfactory.
  • inventions allow application even under very mild conditions. For example, a very low deposition rate and / or a very low temperature can be selected.
  • Figures 1 to 4 show various sections of an applied powdered coating material according to the invention. The applied coating adapts well to the uneven surface structure of the solar contact paste and even partially penetrates into it without impairing the structure of the solar contact paste or even damaging the wafer.

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EP12741314.4A 2011-07-25 2012-07-25 Beschichtungsverfahren nutzend spezielle pulverförmige beschichtungsmaterialien und verwendung derartiger beschichtungsmaterialien Not-in-force EP2737101B1 (de)

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US11662300B2 (en) 2019-09-19 2023-05-30 Westinghouse Electric Company Llc Apparatus for performing in-situ adhesion test of cold spray deposits and method of employing
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US20140241937A1 (en) 2014-08-28
DE102011052121A1 (de) 2013-01-31
WO2013014214A2 (de) 2013-01-31
JP2014521836A (ja) 2014-08-28
EP2737101A2 (de) 2014-06-04
CN103827346A (zh) 2014-05-28
JP6092863B2 (ja) 2017-03-08
KR20140061423A (ko) 2014-05-21
WO2013014214A3 (de) 2013-06-13
US9580787B2 (en) 2017-02-28

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