EP2686460A1 - Revêtement ainsi que procédé et dispositif de revêtement - Google Patents

Revêtement ainsi que procédé et dispositif de revêtement

Info

Publication number
EP2686460A1
EP2686460A1 EP12714242.0A EP12714242A EP2686460A1 EP 2686460 A1 EP2686460 A1 EP 2686460A1 EP 12714242 A EP12714242 A EP 12714242A EP 2686460 A1 EP2686460 A1 EP 2686460A1
Authority
EP
European Patent Office
Prior art keywords
platelet
plasma jet
shaped particles
particles
coating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP12714242.0A
Other languages
German (de)
English (en)
Inventor
Michael Bisges
Christian Wolfrum
Marco Greb
Markus Rupprecht
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.)
Eckart GmbH
Maschinenfabrik Reinhausen GmbH
Original Assignee
Eckart GmbH
Reinhausen Plasma GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Eckart GmbH, Reinhausen Plasma GmbH filed Critical Eckart GmbH
Publication of EP2686460A1 publication Critical patent/EP2686460A1/fr
Withdrawn legal-status Critical Current

Links

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
    • C23C4/12—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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/14—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas designed for spraying particulate materials
    • B05B7/1404—Arrangements for supplying particulate material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/16—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas incorporating means for heating or cooling the material to be sprayed
    • B05B7/22—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas incorporating means for heating or cooling the material to be sprayed electrically, magnetically or electromagnetically, e.g. by arc
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/16—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas incorporating means for heating or cooling the material to be sprayed
    • B05B7/22—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas incorporating means for heating or cooling the material to be sprayed electrically, magnetically or electromagnetically, e.g. by arc
    • B05B7/222—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas incorporating means for heating or cooling the material to be sprayed electrically, magnetically or electromagnetically, e.g. by arc using an arc
    • B05B7/226—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas incorporating means for heating or cooling the material to be sprayed electrically, magnetically or electromagnetically, e.g. by arc using an arc the material being originally a particulate 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of 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
    • C23C4/12—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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma
    • H05H1/26—Plasma torches
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma
    • H05H1/26—Plasma torches
    • H05H1/32—Plasma torches using an arc
    • H05H1/34—Details, e.g. electrodes, nozzles
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma
    • H05H1/26—Plasma torches
    • H05H1/32—Plasma torches using an arc
    • H05H1/42—Plasma torches using an arc with provisions for introducing materials into the plasma, e.g. powder, liquid
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y10T428/256—Heavy metal or aluminum or compound thereof
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y10T428/256—Heavy metal or aluminum or compound thereof
    • Y10T428/257—Iron oxide or aluminum oxide

Definitions

  • the present invention relates to a method and a device for applying a coating to a substrate, in which by passing a working gas through an excitation zone a plasma jet of a
  • the invention relates to a coating on a substrate of at least partially intergrown platelet-shaped particles and the use of platelet-shaped particles.
  • a known method is the plasma spraying, in which a by a
  • Arc of a plasma burner flowing gas or gas mixture is ionized.
  • a highly heated, electrically conductive gas with a temperature of up to 20,000 K is generated.
  • this plasma jet powder usually injected in a particle size distribution between 5 to 120 ⁇ , which is melted by the high plasma temperature.
  • the plasma jet entrains the powder particles and places them on the substrate to be coated.
  • the plasma coating by way of plasma spraying can be under normal
  • Atmosphere done.
  • the high gas temperatures of over ⁇ ⁇ . ⁇ are required to melt the powder and thus be able to deposit as a layer. So that's it Plasma spraying energetically very expensive, creating a cost-effective
  • Coating of substrates is often not possible.
  • expensive apparatus must be used to produce the high temperatures. Due to the high temperatures, temperature-sensitive and / or very thin substrates, such as polymer films and / or paper, can not be coated. Due to the high thermal energy, such substrates are involved
  • a further disadvantage is that during plasma spraying, a high thermal load of the particles used occurs, as a result of which they can at least partially oxidize, in particular when metallic particles are used. This is particularly disadvantageous when metallic layers are to be deposited, for example, for printed conductors or as
  • Corrosion protection should be used. For these reasons, methods have been developed which use so-called atmospheric cold plasma, also referred to as low temperature plasma, to create layers on substrates.
  • a cold plasma jet is generated at atmospheric conditions by methods known in the art and introduced into the plasma jet, a powder, which is then deposited on the substrate.
  • Precursor material are fed into a plasma and reacted there, whereby only relatively low deposition rates of 300 - 400 nm / sec can be achieved. These are compared to the deposition rates, which are achieved in corresponding processes with powdery starting materials, even with the use of particles which are in the order of 100 ⁇ , by a factor of 10-1000 lower. Accordingly, is an economic
  • EP 1 675 971 B1 is another method for coating a substrate surface using a plasma jet of a
  • Low-temperature plasma known to which a fine-grained, coating-forming powder in a size of 0.001 - 100 ⁇ is supplied by means of a powder conveyor.
  • the temperature of a low-temperature plasma in the core of the plasma jet at ambient pressure reaches less than 900 degrees Celsius.
  • EP 1 675 971 B1 specifies temperatures in the core of the occurring plasma jet of up to 20,000 degrees Celsius.
  • a disadvantage is that powders of materials with higher melting points, e.g. ceramic materials or refractory metals, can not be melted in the process.
  • the speed of the plasma jet is so high that the residence time of the small particles of the powder in the hot zones of the plasma is insufficient to achieve a complete melting of the particles. Therefore, in materials having an elevated melting temperature (for example, Ag, Cu, Ni, Fe, Ti, W), at most, melting of the particle surface occurs, and a porous layer in which the particles are almost in their formation
  • the method is therefore primarily suitable for coating substrates with low-melting metals such as tin and zinc.
  • the object of the invention is to provide a generic method for applying a coating to a substrate, wherein the required Reaction energy, in particular for melting, breaking up of atomic or molecular assemblies, deagglomerating and atomizing
  • Coating materials is reduced, so that a perfect coating especially with coating materials with higher
  • Coating can be specified.
  • the object is achieved in a method of the type mentioned in that platelet-shaped particles having an average thickness H between 10 and 50,000 nanometers and a form factor F in the value range from 10 to 2000 are fed into the plasma jet directed onto the substrate.
  • the platelet-shaped particles preferably have an average thickness H of between 50 and 5,000 nm, more preferably between 100 and 2,000 nm.
  • the exact mean thickness H of the 10 platelet-shaped particles is determined by the degree of water coverage (spread to DIN 55923) and / or by scanning electron microscopy (SEM).
  • the shape factor is defined as the ratio of the mean linear expansion D to the mean thickness H of the platelet-shaped particles.
  • Form factor 10 the particles have a value for the middle
  • Length expansion D of 0.1 ⁇ on. If platelet-shaped particles with an average thickness H of 50,000 nm and a form factor 10 are used in the method according to the invention, the particles have a value for the middle one Length expansion D of 500 ⁇ on. The desired mean length expansion of the particles depends strongly on the respective
  • the feeding of the platelet-shaped particles into the plasma jet does not necessarily have to take place in the gaseous state, but can also be carried out in the liquid or solid state Feed of the platelet-shaped particles, however, by means of a carrier gas for the
  • the feed opening of the jet generator is connected via a line with a vortex chamber.
  • the vortex chamber is listed as a closed container and filled at most up to a maximum level with the platelet-shaped particles.
  • the platelet-shaped particles are acted upon by at least one gas inlet with a pressurized carrier gas, in particular in a periodic sequence, whereby the fluidized platelet-shaped particles together with the carrier gas as a mixture via at least one above the maximum level of the vortex chamber arranged outlet from the container
  • the periodic loading of the platelet-shaped particles in the vortex chamber with the carrier gas takes place at a frequency in the range of 1 Hz to 100 Hz.
  • the particles are subjected to the carrier gas in succession over several gas inlets.
  • the gas inlet (s) can open directly into the usually existing supply of platelet-shaped particles.
  • the plasma jet is generated under a pressure in a pressure range of 0.5-1.5 bar, but preferably under the conditions of ambient pressure. It is also called an atmospheric plasma. Quite surprisingly, it has been found that with the use of platelet-shaped particles, layers with outstanding properties can also be produced with metals of higher melting point and non-metals. The higher specific surface area of platelet-shaped particles compared to spherical particles is probably responsible for the very good properties.
  • platelet-shaped particles and is defined as follows:
  • nanoparticles are characterized by a reduced melting point compared to the macromaterial. Such nanoparticles have a very large surface area in relation to their volume. This means that they have far more atoms on their surface than larger particles. Since atoms on the surface are less binding partners available, as atoms in the core of the particle, such atoms are very reactive. Because of this, they can be much more involved with particles in their immediate environment Interaction occur as is the case with macroparticles.
  • the platelet-shaped particles used in the invention have a significantly increased surface area compared to mass-like spherical particles. The surface of a spherical particle with a radius of 1 ⁇ is opposite to a
  • the increased surface area of the platelet-shaped particles enhances binding between the deposited particles with each other as well as between the particles and the substrate.
  • a further advantage of the platelet-shaped particles is that their specific larger surface compared with mass-like spherical particles covers the substrate to be coated more efficiently. In particular with opaque coatings, therefore, the coating process can be done with less
  • the shape factor is defined as the ratio of the mean linear expansion D to the mean thickness H of the platelet-shaped particles. If platelet-shaped particles having an average thickness H of 10 nm and a shape factor 10 are used in the method according to the invention, the particles have a value for the mean longitudinal extent D of 0.1 ⁇ m. Be in the inventive
  • the particles When the method uses platelet-shaped particles having an average thickness H of 50,000 nm and a shape factor 10, the particles have a value for the mean longitudinal extent D of 500 ⁇ m.
  • the desired mean longitudinal expansion of the particles depends strongly on the respective coating purpose.
  • a better orientation of the platelet-shaped particles deposited on the substrate can be ensured. This is of particular interest in color coatings of surfaces.
  • the thickness distribution is an important parameter for the characterization of platelet-shaped particles according to the invention
  • Thickness distribution exist in the prior art no measuring devices that can easily determine this value. A determination is therefore made by default by determining the thickness of a statistically sufficient number
  • the particles are dispersed, for example in a paint and then applied to a film.
  • the coated film is then cut with a suitable tool so that the cut runs through the paint. Subsequently, the prepared film is introduced into the SEM such that the observation direction is perpendicular to the cut surface. In this way, the majority of the particles are viewed from the side so that their thickness can be easily determined. »The determination is carried out by default by marking the corresponding boundaries using a suitable tool such as the SEM devices of Manufacturer supplied software packages. For example, the determination can be carried out by means of a REM device of the Leo series of the manufacturer Zeiss (Germany) and the software Axiovision 4.6 (Zeiss, Germany). The thickness distribution of the platelet-shaped particles is not homogeneous. The
  • Thickness distribution is expediently represented in the form of a cumulative passage curve.
  • the mean value is the hso value of
  • the thickness distribution can also be described with the Hi 0 or H 90 value.
  • the platelet-shaped particles are preferably by means of a
  • Carrier gas is fed into the plasma jet.
  • platelet-shaped particles in the plasma jet need not necessarily be in the gaseous state, but can also be in the liquid or solid state.
  • the volume flow of the carrier gas is preferably in a range of 1 l / min to 1 5 l / min and the pressure in a range between 0.5 bar to 2 bar.
  • Homogeneous feeding of the platelet-shaped particles into a core zone of the plasma jet with a gas temperature of less than 900 degrees Celsius preferably takes place transversely to the propagation direction of the plasma jet.
  • Such platelet-shaped particles can be prepared by various methods. Depending on whether they are metallic or non-metallic materials, such as, for example, ceramic or oxidic materials, different methods of production can be used.
  • the production of metallic platelet-shaped particles preferably takes place by mechanical deformation of powders, in particular metal powders. The mechanical deformation usually takes place in mills, in particular in
  • Rotary tube ball mills etc.
  • the mechanical deformation is usually carried out by wet milling, ie by grinding the powder together with solvent, in particular organic solvent such as white spirit, and in the presence of lubricants or wetting and / or dispersing additives such as oleic acid, stearic acid etc ..
  • the grinding takes place in Presence of grinding media, usually grinding balls, wherein the ball diameter is usually in a range of 0.1 to 10 mm, preferably from 0.2 to 4.0 mm.
  • the grinding media are usually made of ceramic, glass or metal, such as steel.
  • steel balls are used as grinding bodies.
  • Such a deformation is described for example in DE 10 2007 062 942 A1, the content of which is hereby incorporated by reference.
  • the powder used is preferably classified by size and this is then mechanically deformed to obtain platelet-shaped particles in a size distribution with a D50 value from 0.5 to 200 ⁇ m.
  • the classification can be carried out, for example, with air classifiers, cyclones, sieves and / or other known devices.
  • the metal particles can be measured in the form of a dispersion of particles.
  • the scattering of the irradiated laser light is in
  • the particles are treated mathematically as spheres.
  • the determined diameters always relate to the equivalent spherical diameter averaged over all spatial directions, irrespective of the actual shape of the metal 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 i.a. when
  • Summed passage curve are shown.
  • the sum curve in turn is usually characterized simplifying by certain characteristics, z.
  • the D50 or D90 value By a D90 value is meant that 90% of all particles are below the specified value. In other words, 10% of all Particles above the specified value. At a D50 value, 50% of all particles are below and 50% of all particles are above the specified value.
  • the powder may first be ground and then classified by size in order to obtain the platelet-shaped particles according to the invention having a size distribution with a D50 value from a range from 1 to 150 ⁇ m.
  • the size distribution between 1, 5 ⁇ and 100 ⁇ . According to a very preferred embodiment, it is between 2 ⁇ and 50 ⁇ .
  • the degree of purity of the metals is preferably more than 70 wt .-%, more preferably more than 90 wt .-%, particularly preferably more than 95 wt .-%, each based on the total weight of the metal, the alloy or
  • the metal the metal mixture or metal alloy can be melted under heat, for example, and then converted into a powder by atomization or by application to rotating components.
  • metallic powders produced in this way have a particle size distribution with an average size (D 50 value) in the range from 1 to 100 ⁇ m, preferably from 2 to 80 ⁇ m.
  • non-metallic layers are to be applied to substrates, preferably non-metallic platelet-shaped particles are used in the
  • Coating process used In this case, completely oxidized or even partially oxidized, e.g. only surface-oxidized educts are used. Such can be generated by targeted oxidation of metallic platelet-shaped particles. This oxidation can be carried out by all methods known to the person skilled in the art. Further oxidation is possible in particular in oxygen-containing plasmas and, depending on the amount of energy input and the coating material, the rule. By adjusting the oxygen content in the working gas, oxidation can optionally be controlled.
  • the metallic particles may be by gas phase oxidation and / or by Liquid phase oxidation are oxidized.
  • the oxidation is carried out in a liquid or by combustion in a gas stream.
  • the oxidation is carried out in a liquid phase or liquid
  • this is preferably done by first distributing the powder in the liquid phase or liquid. This can be done with or without addition of excipients and with or without the input of energy.
  • the dispersion takes place without the addition of auxiliaries and with stirring.
  • the liquid can be an inert
  • the dispersion either begins immediately or is initiated by the addition of an oxidizing agent and / or oxidation catalyst and / or by increasing the temperature.
  • the oxidation may already begin during the dispersion. Whether the oxidation reaction starts immediately depends on the chosen combination of liquid / metallic powder and possibly catalyst presence.
  • the oxidation is preferably started by adding an oxidizing agent and / or oxidation catalyst.
  • an oxidizing agent is sulfuric acid, potassium permanganate, hydrogen peroxide and other oxidizing agents known to those skilled in the art.
  • oxidation catalysts are metals, metal salts, acids and bases. In particular, in the case of the addition of acids and bases, the addition is preferably carried out so that a pH value suitable for the oxidation reaction is set in the reaction mixture.
  • the reaction is preferably maintained until the metal is at least 90% by weight, more preferably at least 95% by weight, even more preferably at least 99% by weight, based on the total weight the metallic particle is present in a non-zero oxidation state.
  • particles are completely present as metal oxide after the oxidation treatment.
  • the metal oxide content can be determined experimentally by methods known to the person skilled in the art.
  • the temperature can be raised, lowered or kept constant.
  • a further addition of one or more oxidizing agents and / or oxidation catalysts can take place, whereby the oxidation process can be controlled.
  • additional chemical reactions may be initiated and / or further reaction components.
  • Components for example metals or metal oxides, are incorporated into the resulting metal oxide particles, for example as doping.
  • the chemical and physical properties of the metal oxide particles, their size and their morphology can be adjusted specifically. Preference is given to
  • the metal oxide particles can be separated from the liquid in which the oxidation was carried out.
  • the separation can be carried out by directly removing the liquid from the reaction mixture. This can be done by methods known in the art such as thermal drying, preferably in a reduced pressure atmosphere.
  • the separation of the liquid takes place after a first concentration of the solid has been carried out by a simple process, in particular by filtration.
  • the metal oxide particles may optionally be subjected to annealing, i. be supplied to an additional temperature treatment.
  • annealing or this temperature treatment in particular the chemical composition and / or the crystal structure of the above
  • metal oxide particles are changed.
  • the temperatures of such a temperature treatment are typically above 200 ° C but below the melting or decomposition temperature.
  • the duration is typically a few minutes to a few hours.
  • aluminum hydroxide prepared by reacting aluminum metal powder in water by heating
  • Alumina are converted. With further temperature treatment in the range between 800 ⁇ ⁇ and 1300 ⁇ ⁇ , the crystal structure of the
  • Alumina can be adjusted specifically. Thus, for example, converts v- Al 2 O 3 upon heating to temperatures greater than 800 ° C in oc-Al 2 O 3 in order.
  • non-metallic platelet-shaped particles can also be produced directly.
  • platelet particles can be made from crystalline, semi-crystalline or amorphous material.
  • glass flakes are produced in which a jet of molten glass is poured onto a rotating, cup or cup-shaped vessel. Due to the rotation of the vessel, the glass melt is squirted out of the vessel in the form of a thin lamella. During this process, the melt solidifies, forming platelet-shaped particles of glass.
  • non-metallic platelet-shaped particles may be obtained by mechanical delamination of layered materials, e.g. Phyllosilicates, are generated.
  • the platelet-shaped particles may consist of different materials.
  • metallic particles these may consist, for example, of aluminum, zinc, tin, titanium, iron, copper, silver, gold, tungsten, nickel, lead, platinum, silicon, further alloys or mixtures thereof.
  • aluminum, copper, zinc and tin or alloys or mixtures thereof are particularly preferred.
  • non-metallic particles these may consist, for example, of oxides or hydroxides of the metals already mentioned or of other metals.
  • the particles may consist of glass, layer silicates such as mica or bentonites.
  • the particles may consist of carbides, silicates and sulfates.
  • the recovery and processing for the process of suitable particles may also be by other means (e.g., artificially by crystallization, drawing, etc.), breeding methods, or conventional scouring and flotation, etc.).
  • the particles may also be organic and inorganic salts.
  • the particles may consist of pure or mixed homo-, co-, block- or prepolymers or plastics or mixtures thereof, but also be organic pure or mixed crystals or amorphous phases.
  • the particles may also consist of mixtures of at least two materials.
  • the platelet-shaped particles have at least one, preferably enveloping coating.
  • the at least simple coating can be, for example, a protective layer against corrosion, which is also referred to as a corrosion protection layer.
  • the platelet-shaped particles according to the invention can, for example, with be provided at least one metal oxide layer.
  • Metal oxides, metal hydroxides and / or metal oxide hydrates are preferably carried out by precipitation, by sol-gel methods or by wet-chemical oxidation of the particle surface.
  • Oxides, hydroxides and / or hydrated oxides of silicon, aluminum, cerium, zirconium, yttrium, chromium and / or mixtures / admixtures thereof are preferably used for the metal oxide coating.
  • oxides, hydroxides and / or hydrated oxides of silicon and / or aluminum are used. Most preferred are oxides, hydroxides and / or hydrated oxides of silicon.
  • the layer thicknesses of the metal oxide layers are in the range from preferably 5 to 150 nm, preferably from 10 to 80 nm, more preferably from 1 5 to 50 nm.
  • a protective layer against corrosion a protective layer of organic polymers can also be applied.
  • Polyacrylate and / or polymethacrylate coatings have proven to be very suitable.
  • passivation layers can also be applied.
  • the mechanism of action of the passivation layers is complex. For inhibitors, it is mostly based on steric effects.
  • the inhibitors are usually in low concentrations of the order of 1 wt .-% to 1 5 wt .-%, based on the
  • the following coating substances are preferably used:
  • R alkyl, aryl, alkylaryl, aryl-alkyl and alkyl ethers, in particular ethoxylated alkyl ethers and
  • R1 may be the same or different than R2.
  • each alkyl is branched or
  • R1 may be the same or different from R2.
  • Heterocycles such as thiourea derivatives, sulfur and / or nitrogen compounds of higher ketones, aldehydes and / or alcohols
  • the passivating inhibitor layer can also consist of the aforementioned substances. Preference is given to organic phosphonic acids and / or phosphoric esters or mixtures thereof.
  • Amine compounds have these preferably organic radicals having more than 6 carbon atoms. Preference is given to the abovementioned amines together with organic phosphonic acids and / or phosphoric esters or mixtures thereof used.
  • Passivating anticorrosion coatings which ensure particularly good corrosion protection in the case of platelet-shaped metallic particles, comprise or consist of silicon oxide, preferably silicon dioxide,
  • Chromium alumina preferably by chromating, chromium oxide, zirconium oxide, cerium oxide, alumina, polymerized plastic resin (s), phosphate, phosphite or borate compounds or mixtures thereof.
  • silicon dioxide layers and chromium aluminum oxide layers Preference is given to silicon dioxide layers and chromium aluminum oxide layers (chromating). Further preferred are cerium oxide, hydroxide or
  • the SiCV layers are preferably by sol-gel method with
  • average layer thicknesses of 10-150 nm and preferably 15-40 nm in organic solvents.
  • the listed coatings can be combined, so that, for example, in a particular embodiment of the invention particles a coating of a Si0 2 layer with subsequently applied
  • the highest possible packing density of the deposited particles is equal to a layer that is as similar as possible to a closed, non-particulate layer, thus a layer that corresponds to the ideal base material.
  • a high packing density is achieved if the particles retain their shape and structure as far as possible during the coating process and are still present as individual particles, in particular in the resulting layer. Such behavior is demonstrated by the particles as described, if they are made of higher-melting metals (melting point> 500 ° C) and non-metallic
  • the coatings which can be produced by the process according to the invention on the substrate of platelet-shaped particles which are at least partially intergrown with one another can be produced without a binder between the coating and the substrate.
  • the prerequisite for the production of coatings without binder between layer and substrate is the use of
  • the device comprises a jet generator with an inlet for the supply of a flowing working gas and an outlet for a guided from the working gas plasma jet, the beam generator two connectable to an AC or a pulsed DC voltage source electrodes to form a
  • the plasma jet platelet-shaped particles can be fed.
  • the working gas of the device are supplied via the inlet ionizable gases, in particular pressurized air, nitrogen, argon, carbon dioxide or hydrogen.
  • the working gas is previously cleaned so that it is free of oil and lubricant.
  • the gas stream in a conventional jet generator is between 1 0 to 70 l / min, in particular between 1 0 to 40 l / min, at a speed of the working gas between 1 0 to 1 00 m / s, in particular between 10 to 50 m / s.
  • the beam generator further comprises two, in particular coaxially spaced apart electrodes, which are connected to an AC voltage, but in particular a pulsed DC voltage source. Between the electrodes, the discharge path is formed.
  • the pulsed DC voltage of the DC voltage source is preferably between 500 V to 12 kV.
  • the pulse frequency is between 10 to 100 kHz, but in particular between 10 to 50 kHz.
  • Electrons and the heavy ions can form. This results in a low temperature load of the injected platelet-shaped particles.
  • Coating process with the jet generator according to the invention is preferably controlled such that the plasma jet of
  • Low temperature plasma in the core zone has a gas temperature of less than
  • the platelet-shaped particles reach a region in which a direct plasma excitation takes place through the plasma jet.
  • the required reaction energy is kept as low as possible.
  • the feed opening is located immediately adjacent to the outlet for the plasma jet in the region of the discharge path.
  • the feed is below the outlet of the device, which is basically possible, it is only an indirect
  • Plasma excitation by the gas-guided plasma jet which is energetically unfavorable.
  • the method of the invention can be used to coat a variety of substrates.
  • Substrates may be, for example, metals, wood, plastics or paper.
  • the substrates can be present in the form of geometrically complex shapes, such as components or finished goods but also as a film or sheet.
  • the coatings which can be produced by the process according to the invention on the substrate of platelet-shaped particles which are at least partially intergrown with one another can be produced without a binder between the coating and the substrate.
  • a prerequisite for the production of coatings without binder between layer and substrate is the use of platelet-shaped particles of a
  • optically and electromagnetically reflecting or absorbing optically conductive, semiconducting or insulating layers, diffusion barriers for gases and liquids,
  • conductive layers can also be used as shields, as electrical contacts, as sensor surfaces and as antennas, in particular RFID (radio
  • Frequency Identification antennas
  • the coatings can be applied over a large area, so that they cover the substrate to a large extent (greater than 70% of the surface of the substrate).
  • the layers can also be applied over a small area, in particular in the form of webs or as sub-areas, which cover less than 10% of the area of the substrate.
  • a relative movement between the substrate and the beam generator during the coating is not required.
  • the layers can also be applied in the form of patterns, which are preferably adapted to the desired functionality. The generation of geometric patterns can also be done, for example, by the use of masks.
  • the apparatus comprises a jet generator with an inlet for the supply of a flowing working gas and an outlet for a plasma jet guided by the working gas, the jet generator two with an AC or a pulsed
  • the working gas of the device are supplied via the inlet ionizable gases, in particular pressurized air, nitrogen, argon, carbon dioxide or hydrogen.
  • the working gas is previously cleaned so that it is free of oil and lubricant.
  • the gas stream in a conventional jet generator is between 10 to 70 l / min, in particular between 10 to 40 l / min, at a
  • Speed of the working gas between 10 to 100 m / s, in particular between 10 to 50 m / s.
  • the jet generator further comprises two, in particular coaxially spaced electrodes arranged with an AC voltage,
  • the pulsed DC voltage of the DC voltage source is preferably between 500 V to 12 kV.
  • the pulse frequency is between 10 to 100 kHz, but in particular between 10 to 50 kHz. Due to the pulsed operation of the DC voltage source is thereof
  • Coating process with the jet generator according to the invention is preferably controlled such that the plasma jet of the low-temperature plasma in the core zone has a gas temperature of less than 900 degrees Celsius,
  • the feed opening in the region of the discharge gap between the electrodes of the jet generator, the platelet-shaped particles reach a region in which a direct plasma excitation takes place through the plasma jet.
  • the required reaction energy is kept as low as possible.
  • the feed opening is located immediately adjacent to the outlet for the plasma jet in the region of the discharge path. Is this done?
  • the feeding of the platelet-shaped particles preferably takes place by means of a carrier gas for the platelet-shaped particles.
  • the vortex chamber is listed as a closed container and at most up to a maximum level with the
  • the platelet-shaped particles are acted upon by at least one gas inlet with a pressurized carrier gas, in particular in a periodic sequence, whereby the fluidized platelet-shaped particles together with the carrier gas as a mixture over at least one above the maximum level of the vortex chamber arranged outlet from the container in the direction of the feed opening of the jet generator flow.
  • the periodic loading of the platelet-shaped particles in the vortex chamber with the carrier gas takes place at a frequency in the range from 1 Hz to 100 Hz.
  • Gas inlets with the carrier gas applied can open directly into the usually existing supply of platelet-shaped particles.
  • the gas inlet or inlets it is also possible to arrange the gas inlet or inlets above the maximum fill level of the particles in the vortex chamber so that the carrier gas strikes the surface of the particles.
  • the size-thickness ratio of a particle sample from the examples listed was determined from the evaluation of SEM images.
  • the longitudinal diameter was determined by means of Cilas 1064 and the thickness of a statistical number (at least 100) of particles and calculated the average size-thickness ratio by quotient of longitudinal diameter to thickness.
  • Separation of the aluminum powder was carried out first in a cyclone, wherein there deposited powdered Aluminiumgr imagine a D50 14-17 ⁇ possessed.
  • a multicyclone was used in succession, the pulverulent aluminum powder deposited in this having a D50 of 2.3 to 2.8 ⁇ m.
  • the gas-solid separation was carried out in a filter (Fa. Alpine, Thailand) with metal elements (Pall). Here was the finest fraction
  • platelet-shaped particles (aluminum): In a 5 L glass reactor, 300 g of a shaped aluminum powder described in Example 2 were dispersed in 1000 ml of isopropanol (VWR, Germany) by stirring with a propeller stirrer. The suspension was heated to 78 ° C. Subsequently, 5 g of a 25 wt .-% ammonia solution (VWR, Germany) were added. After a short time, a strong gas evolution was possible to be watched. Three hours after the first addition of ammonia, another 5 g of 25% by weight ammonia solution was added. After a further three hours, 5 g of 25% by weight ammonia solution were again added. The suspension was further stirred overnight.
  • VWR isopropanol
  • Example 4 Preparation of non-metallic platelet-shaped particles (aluminum oxide) by temperature treatment of non-metallic
  • platelet-shaped particles (aluminum hydroxide).
  • Material Difference to the uncalcined. Material is the particle diameter slightly larger and the zeta potential in the entire pH range positive.
  • the XRD analysis shows theta-AI203.
  • FIG. 1 shows a schematic representation of an embodiment of a
  • Figure 2 is an enlarged view of the beam generator of Figure 1 in
  • the first electrode 4 is designed as a pin electrode, while the spaced second
  • Electrode 5 is formed as an annular electrode. The distance between the tip of the pin electrode 4 and the ring electrode 5 forms a discharge path 16.
  • a jacket 7 of electrically conductive material is arranged concentrically to the pin electrode 4 and insulated from the pin electrode 4.
  • the annular electrode 5, opposite end face of the jet generator 1, the working gas 3 is supplied via an inlet 21.
  • the inlet 21 is located on a frontally placed on the hollow cylindrical jacket 7, the pin electrode 4-holding sleeve 22 of electrically insulating material.
  • a feed opening 9 Immediately adjacent to the extending in the axial direction of the jet generator 1 outlet 8 is transverse to the longitudinal extent of a feed opening 9, via which the plasma jet 2 platelet-shaped particles 10 are fed.
  • the feed opening 9 of the jet generator 1 is connected for this purpose via a line 12 with a vortex chamber 1 1, are stored in the platelet-shaped particles 10.
  • the vortex chamber 1 1 is filled at most up to a maximum level 13 with the platelet-shaped particles 10. Below the maximum level 13 opens in the vortex chamber 1 1, an inlet 23 for a carrier gas 14 under a
  • the particles 10 are fluidized in the space above the maximum level 20 and reach via an outlet 15, the conduit 12 and the feed opening 9 in the discharge path 16 of the jet generator. 1
  • Voltage source 6 increases, during each pulse, the voltage applied between the electrodes 4, 5, to between the electrodes 4, 5, the ignition voltage for the formation of an arc between the electrodes 4, 5 is applied. Due to the conductive shell 7, it also leads to discharges in the direction of the inner
  • Electrodes 4, 5 conductive.
  • the voltage source 6 is preferably designed such that it generates a voltage pulse with an ignition voltage for the arc discharge and a pulse frequency which causes the arc to extinguish between two consecutive voltage pulses. As a result, there is a pulsed gas discharge in the plasma jet 2.
  • the pulse frequency is preferably in a range between 10 kHz to 100 kHz, in the illustrated embodiment at 50 kHz.
  • the voltage of the voltage source 6 is a maximum of 12 kV. As working gas 3 compressed air is used, with 40 l / min are supplied in the normal operating condition.
  • Embodiment not only a punctiform coating on the substrate 20 is to be generated, it is in an embodiment of the invention the possibility that the plasma jet 2 and the substrate 20, during the application of the
  • Relative movement can be effected by moving the substrate 20, for example on a movable table in the horizontal plane.
  • the beam generator 1 is arranged on an XY moving unit that is movable at least in a plane parallel to the substrate 20, so that the generator can be moved relative to the substrate at a defined speed.
  • Relative movement can be webs or even full-surface coatings of the substrate 20 produce.

Abstract

L'invention concerne un procédé et un dispositif pour appliquer un revêtement sur un substrat (20). Un faisceau (2) d'un plasma à basse température est produit par guidage d'un gaz de travail (3) à travers une zone d'excitation. Le faisceau de plasma est dirigé sur le substrat (20) et des particules (10) en forme de plaquette ayant une épaisseur moyenne (H) entre 10 et 50 000 nanomètres et un facteur de forme (F) dans la plage de valeurs de 10 à 2000 sont introduites dans le faisceau plasma (2). L'introduction dans le faisceau de plasma (2) a lieu à l'aide d'un gaz porteur (14). Le faisceau de plasma (2) est produit par excitation du gaz de travail (3) au moyen d'une tension alternative ou d'une tension continue pulsée.
EP12714242.0A 2011-03-16 2012-03-15 Revêtement ainsi que procédé et dispositif de revêtement Withdrawn EP2686460A1 (fr)

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DE102011001312 2011-03-16
DE102011001982 2011-04-12
PCT/EP2012/054530 WO2012123530A1 (fr) 2011-03-16 2012-03-15 Revêtement ainsi que procédé et dispositif de revêtement

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EP (1) EP2686460A1 (fr)
JP (1) JP5888342B2 (fr)
KR (1) KR20140052982A (fr)
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WO (1) WO2012123530A1 (fr)

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WO2012123530A1 (fr) 2012-09-20
JP5888342B2 (ja) 2016-03-22
KR20140052982A (ko) 2014-05-07
CN103415644B (zh) 2016-11-09
JP2014511941A (ja) 2014-05-19
US20140023856A1 (en) 2014-01-23

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