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EP2737099A2 - Procédé d'application d'un revêtement sur un substrat, revêtement, et utilisation de particules - Google Patents

Procédé d'application d'un revêtement sur un substrat, revêtement, et utilisation de particules

Info

Publication number
EP2737099A2
EP2737099A2 EP12741312.8A EP12741312A EP2737099A2 EP 2737099 A2 EP2737099 A2 EP 2737099A2 EP 12741312 A EP12741312 A EP 12741312A EP 2737099 A2 EP2737099 A2 EP 2737099A2
Authority
EP
European Patent Office
Prior art keywords
particles
coating
substrate
plasma
powder
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Withdrawn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
EP12741312.8A
Other languages
German (de)
English (en)
Inventor
Markus Rupprecht
Christian Wolfrum
Marco Greb
Eckart Theophile
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
Original Assignee
Eckart 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 filed Critical Eckart GmbH
Publication of EP2737099A2 publication Critical patent/EP2737099A2/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Withdrawn legal-status Critical Current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
    • 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
    • C23C16/513—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 using plasma jets
    • 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
    • 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
    • C23C4/12—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
    • C23C4/134—Plasma spraying
    • 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
    • Y10T428/254—Polymeric or resinous material

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
  • the invention relates to the use of particles which are surrounded by a shell consisting of a crosslinked polymer.
  • One known method is plasma spraying, in which a gas or gas mixture flowing through an arc of a plasma torch is ionized.
  • Ionization is a highly heated, electrically conductive gas produced at a temperature of up to 20,000 K.
  • this plasma jet powder usually injected in a particle size distribution between 5 to 120 ⁇ , which by the high
  • Plasma temperature is melted.
  • 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 carried out under normal atmosphere.
  • thermosensitive 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
  • atmospheric cold plasma also referred to as low temperature plasma
  • a method known in the art is a cold plasma jet at atmospheric
  • 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.
  • the document DE102006061435A1 teaches a method for spraying a web, in particular a printed conductor, onto a substrate by introducing into a spray lance, in which a cold plasma ( ⁇ 3000 K) is produced, a powder by means of a carrier gas, which is subsequently applied to a substrate incident.
  • a cold plasma ⁇ 3000 K
  • fine-grained powder in sizes of 0.001-100 ⁇ in a cold plasma ( ⁇ 500 ° C) are fed and as a layer on a surface
  • Higher melting point materials e.g. ceramic materials or refractory metals can not be melted in the process unless particles of very small mean diameter, i.
  • the offset in the plasma state gas flow rates and thus the plasma gas velocity is so high in the said method, that the residence time of the particles in the hot zones of the plasma is not sufficient to complete melting of the To reach particles.
  • materials with elevated melting temperature eg.
  • the references describe a preferred use of low melting metals such as tin and zinc.
  • low melting metals such as tin and zinc.
  • the effect that the particles melt to a maximum of their outer shell, can be explained by the fact that due to the conditions in the plasma is primarily an activation on the surface.
  • the specific surface area can be increased, but such powders are difficult to convey, so that they can not be industrially used industrially.
  • the object of the invention is to provide a method in which a sufficient activation of the particles is achieved while maintaining good conveyability.
  • the coating of substrates with an atmospheric cold plasma in which the material forming the layer, for example in the form of particles, which are provided with an existing of a crosslinked polymer shell, is introduced.
  • a shell can be produced, for example, by applying monomers, oligomers, polymers or mixtures of the abovementioned to the surface of the particles and crosslinking them there.
  • the present invention relates to a method for applying a coating to a substrate using cold plasma, which is characterized in that the method comprises the following steps:
  • activated particles mean that the particles can be adhesively applied to the substrate, whereby the particles can be superficially or completely softened or melted or adhere to adhere to the substrate, but the particles can also be in an energy-containing state be offset, which allows the formation of a physical or chemical bond with the substrate.
  • the coating, preferably spraying, of the coating is performed on a substrate using a longitudinally extending coating die which is moved or movable at a relative velocity relative to the substrate, in a plasma zone disposed internally one of the coating nozzle upstream electrode, a cold plasma is generated with a plasma temperature of less than 3,000 K, and wherein in the coating die by means of a
  • Carrier gas a powder is introduced, which is carried by the plasma toward a front end outlet opening from the coating die, there emerges and strikes the substrate, wherein the powder is particles with a polymer shell.
  • the cold plasma is generated in or in front of a coating nozzle and the particles are introduced into the coating nozzle via a carrier gas, wherein the coating nozzle and the substrate are movable relative to one another.
  • the coating die may be movably disposed or moved relative to the substrate or substrate relative to the coating die.
  • Coating nozzle and the substrate to be arranged movable or moved to each other.
  • the average layer thickness of the, preferably enveloping, polymer coating is less than 2 ⁇ m.
  • the cold plasma is applied by applying a pulsed DC voltage or AC voltage generates an ionizable gas.
  • the particles are platy.
  • the particles preferably the platelet-shaped particles in the plasma zone, react at least partially chemically or physically.
  • the particles at least partially melt.
  • the carrier gas is passed at a flow rate through a container in which the particles are stored as a powder, so that the powder to produce a
  • Powder dust at least partially swirled and powder dust generated in the
  • Coating nozzle is introduced.
  • the carrier gas flows through the coating nozzle with a volume flow from a range of 1 Nl / min to 15 Nl / min and preferably at pressures between 0.5 bar to 2 bar.
  • standard liters or "Nl” in the context of the present invention denotes the
  • the cold plasma is generated under pressure and the particles are then applied to the substrate, which corresponds largely to atmospheric conditions.
  • the pressure is in a range of 0.5-10 5 - 1.5 x 10 5 Pa.
  • the average thickness of the preferably enveloping polymer coating is less than 300 nm.
  • Polymer coating a polymerized (meth) acrylate resin In certain of the aforementioned embodiments, it is preferably in the Polymer coating around a polymerized acrylate resin.
  • the particles are metal particles, preferably platelet-shaped metal particles, and the metals are selected from the group consisting of aluminum, zinc, tin, titanium, iron, copper, silver, gold, tungsten, nickel, lead, platinum, silicon and alloys thereof and mixtures thereof are selected.
  • the substrate is selected from the group consisting of metals, plastics, paper, biological materials, glass, ceramics, and mixtures thereof.
  • the substrate is selected from the group consisting of metals, wood, plastics, paper, and mixtures thereof,
  • the polymer-coated particles are selected from the group consisting of oxides, carbides, silicates, nitrides, phosphates, sulfates, and mixtures thereof.
  • the present invention relates to a coating on a substrate, obtainable by a method according to any one of the preceding claims.
  • the particles are platelet-shaped metal particles and the coating has platelet-shaped metal particles at least partially intergrown with each other.
  • the coating consists of at least partially fused platelet-shaped metal particles produced by spraying the coating onto the substrate by means of a longitudinally extending coating die which is movable or moved at a relative speed relative to the substrate in a plasma zone, which is inside one of the coating nozzle
  • a cold plasma with a plasma temperature less than 3000 K is generated and wherein in the coating nozzle by means of a carrier gas, a powder is introduced, which is carried by the plasma towards a front end outlet opening from the coating die, there emerges and strikes the substrate, wherein
  • a carrier gas is passed at least partially through a powder with a polymer shell before entering the plasma zone
  • the powder is introduced into the coating nozzle with the aid of the carrier gas, c) the powder is carried by the carrier gas from the plasma in the direction of a front end outlet opening of the coating nozzle, exits there and strikes the substrate.
  • the present invention relates to the use of platelet-shaped particles, preferably of platelet-shaped metal particles, which have a
  • Polymer coating having an average thickness of less than 2 ⁇ , applying a coating to a substrate using cold plasma.
  • Diameter of the powder particles For a given powder usually can not be given a simple diameter, but the diameter has a distribution. This distribution is usually characterized by the specification of D values, for example the D50 value. These D values can be determined by means of
  • Laser granulometry can be determined for example with HELOS or CILAS devices. At the D 50 value, 50% of the aforementioned are by means of laser granulometry volume-averaged particle size distribution below the specified value.
  • 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 refer 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 be represented inter alia as a cumulative frequency curve, which is also called the cumulative frequency distribution.
  • the cumulative frequency curve in turn is usually characterized simplifying by certain characteristics, z. B.
  • the D50 or D90 value By a D90 value is meant that 90% of all particles are below the specified value. At a D50 value, 50% of all particles are below the specified value.
  • the particle diameter determines in particular the specific surface area of the individual particle and thus also the total powder.
  • specific surface is meant the outer surface referred to the mass, which describes the surface per kilogram of the powder and is defined as follows:
  • 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. For this reason, they can interact with particles in their immediate environment much more than macroparticles.
  • the apparatus comprises a jet generator having 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 having an AC or a pulsed one
  • Feed inlet via which the plasma jet particles, preferably 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 flow in a conventional jet generator is between 10 to 70 l / min, in particular between 10 to 40 l / min, at a
  • the jet generator further comprises two, in particular coaxially spaced
  • 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.
  • the 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, but in particular of less than 500 degrees Celsius (low-temperature plasma).
  • the particles By opening the feed opening in the region of the discharge gap between the electrodes of the jet generator, the particles reach a region in which a direct plasma excitation takes place through the plasma jet. By this measure, the energy input is maximized in the powder.
  • 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 location of the powder feed into the plasma flame and the location where the powder is stored are spatially separated.
  • Industrial operation requires the provision of certain amounts of powder, since otherwise, for example, an approximately continuous coating process is not feasible due to the time required for refilling the powder. A very close storage is not feasible for technical reasons, Therefore, the powder must be promoted over a certain distance. This explains the need to use powders with good pumpability.
  • the inventors have now surprisingly found that modification of the powder with a surrounding polymer shell improves the conveyability without affecting the properties of the layer.
  • the inventors have surprisingly found that the surrounding polymer shell is no longer present in the deposited layer, so that the quality of the layer is not affected.
  • the method according to the invention offers the advantage over the prior art that powders with particle sizes can be used on existing systems which can not be conveyed without the coating applied according to the invention with the powder conveyor in the system.
  • the surrounding polymer sheath so that good conveyability can be achieved without having to carry out a complex optimization of conveying units.
  • the surrounded with a polymer shell particles of the method according to the invention are characterized in that the particles of the powder are surrounded by a closed shell of a crosslinked polymer.
  • the advantage of using a crosslinked polymer is that the layer thickness of the surrounding shell can be minimized since the density of the polymer shell is maximized.
  • the average thickness of the surrounding shell is less than 2 ⁇ , preferably less than 500 nm, more preferably less than 300 nm, most preferably less than 200 nm.
  • the average thickness is on the other hand minimal 3 Nanometer (nm) is preferably 5 nm, particularly preferably 10 nm, very particularly preferably 15 nm.
  • Determination is therefore carried out by default by determining the thickness of the shell of a statistically sufficiently large number of particles surrounded by a polymer shell in SEM (scanning electron microscope) analyzes.
  • the particles are dispersed, for example in a paint and then applied to a film.
  • the film coated with the lacquer coated with a polymer shell is subsequently cut with a suitable tool so that the cut runs through the lacquer.
  • the prepared film is introduced into the SEM such that the observation direction is directed perpendicular to the cutting edge. In this way, the particles are largely viewed from the side thereof, so that the thickness of the polymer layer can be easily determined.
  • the determination is made by marking the corresponding limits by means of a suitable tool such as the software packages supplied by the manufacturer as standard with the SEM devices.
  • 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 of the polymer shell surrounding the particles is not homogeneous over all particles.
  • the fluctuation width of the polymer layer can be +/- 50% of the average thickness.
  • the polymer layer can basically consist of all organic polymers known to the person skilled in the art. Preferably, it consists of polymerized
  • Plastic resin Particularly preferably from polymerized acrylate resin.
  • the polymer shell is made of polyacrlate or polymethacrylate.
  • synthetic resin coatings consisting of e.g.
  • Epoxies polyesters, polyurethanes, or polystyrenes, and mixtures thereof.
  • crosslinked polymer shell denotes in the context of the invention that the proportion of monomers or uncrosslinked molecules in the shell less than 20 wt .-%, preferably less than 15 wt .-%, more preferably less than 10 wt .-% , Total mass of the shell.
  • the polymer coating is carried out by direct Aufpolymermaschine of the monomers on the particles.
  • the shell can be constructed from one or more monomer units. It is preferably composed of at least two monomer units.
  • Monomer units are preferably acrylate or methacrylate groups, which are characterized in that they have at least two functional acrylate or methacrylate groups.
  • the shell preferably additionally comprises organofunctional silane.
  • MetaN mono(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethyl)-(2-aminoethy
  • Resin coating According to a preferred variant is the
  • Synthetic resin coating exclusively from acrylate and / or
  • Resin coating may be included. It is inventively preferred that the acrylate and / or
  • Methacrylate each have at least three acrylate and / or methacrylate groups. With further preference these starting compounds may each also have four or five acrylate and / or methacrylate groups.
  • the use of multifunctional acrylates and / or methacrylates allows the provision of metallic effect pigments with very good chemical resistance and higher electrical resistance.
  • Metallic effect pigments of the invention are not electrically conductive, which considerably extends the possible uses of metallic effect pigments. It is thus possible to use the metallic effect pigments according to the invention,
  • the synthetic resin layer has, in particular at 2 to 4 acrylate and / or
  • Methacrylate groups per acrylate and / or methacrylate starting compound surprisingly an extraordinary tightness and strength, without being brittle.
  • extremely suitable have 3 acrylate and / or
  • Methacrylate groups per acrylate and / or methacrylate starting compound proved.
  • Synthetic resin layer comes from the metallic effect pigment surface.
  • the weight ratio of polyacrylate and / or polymethacrylate to organofunctional silane is 10: 1 to 0.5: 1. Further preferred is the weight ratio of polyacrylate and / or polymethacrylate to organofunctional silane in a range of 7: 1 to 1: 1.
  • organofunctional silane to polyacrylate and / or polymethacrylate is sufficient to apply a firmly adhering to the metallic effect pigment surface and at the same time resistant to chemicals or highly corrosive environmental conditions resin layer.
  • Metallic effect pigments of the present invention have a coating which are composed of at least two monomer components a) and b), wherein a) is at least one acrylate and / or methacrylate and b) at least one
  • organofunctional silane which preferably has at least one free-radically polymerizable functionality.
  • Component a) preferably comprises polyfunctional acrylates and / or methacrylates, the corresponding monomers having di-, tri- or polyfunctional acrylate and / or methacrylate groups.
  • Suitable difunctional acrylates a) are: allyl methacrylate, bisphenol-adimethacrylate, 1,3-butanediol dimethacrylate, 1,4-butanediol dimethacrylate,
  • Polyethylene glycol dimethacrylate polyethylene glycol 200 diacrylate, polyethylene glycol 400 diacrylate, polyethylene glycol 400 dimethacrylate, tetraethylene glycol diacrylate, tetraethylene glycol dimethacrylate, tricyclodecanedimethanol diacrylate,
  • Tripropylene glycol diacrylate Triethylene glycol dimethacrylate or mixtures thereof.
  • Pentaerythritol triacrylate trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, tris (2-hydroxyethyl) isocyanurate triacrylate, pentaerythritol tetraacrylate,
  • Acrylates which are very useful in the present invention include dipentaerythritol pentaacrylate, pentaerythritol triacrylate, pentaerythritol tetraacrylate, trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, tris (2-hydroxyethyl) isocyanurate triacrylate, 1,6-hexanediol dimethacrylate, or the like
  • organofunctional silanes b) for example
  • acrylate and / or methacrylate-functional silanes are particularly preferred.
  • organofunctional silane preferably selected from the group consisting of 2-methacryloxyethyltrimethoxysilane, 2-methacryloxyethyltriethoxysilane, 3-methacryloxypropyltriethoxysilane, 3-methacryloxypropyltrimethoxysilane,
  • the synthetic resin layer of the particles preferably to be used according to the invention preferably metallic effect pigments, preferably has an average layer thickness in a range from 20 nm to 200 nm, more preferably from 30 nm to 100 nm. According to a further variant of the invention, the average layer thickness is in a range of 40 to 70 nm. Surprisingly enough, the metallic particles preferably to be used according to the invention are preferably sufficient
  • the powder particles are preferably initially pre-loaded with a functional group-carrying silane, which is used as
  • Adhesion promoter for the polymer shell is used.
  • the functional group is more preferably acrylate or methacrylate groups.
  • the powder has particles with a size distribution with a D50 value from a range of 1 to 150 ⁇ on.
  • the size distribution between 1, 5 ⁇ and 100 ⁇ .
  • it is between 2 ⁇ and 50 ⁇ .
  • the measurements can be carried out, for example, using the particle size analyzer HELOS 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.
  • Particles can be measured, for example, with a device from the company Quantachrome (device: Cilas 1064) according to the manufacturer's instructions. For this purpose, 1, 5 g of the particles are suspended in about 100 ml of isopropanol, 300 seconds in an ultrasonic bath (device:
  • Pasteur pipette into the sample preparation cell of the measuring device and measure several times. From the individual results are the
  • the evaluation of the scattered light signals is carried out according to the Fraunhofer method.
  • the material constituting the powders may be a metal, a non-metal, a polymer or an oxide.
  • the material is a metal or a mixture of at least two metals or an alloy consisting of at least two metals.
  • the degree of purity of the individual metals is preferably more than 70 wt .-%, more preferably more than 90 wt .-%, more preferably more than 95 wt .-%, each based on the total weight of the metal, alloy or mixture.
  • the metal, the metal mixture or metal alloy can be melted under heat, for example, and then converted to powder by atomization or by application to rotating components.
  • Such produced metallic powder or metal powder have, for example, a particle size distribution with an average size (D50 value) in the range of 1 to 100 ⁇ , preferably from 2 to 80 ⁇ on.
  • the particle or particle shape of the generated metallic powder is preferably approximately spherical. However, the powder may also have particles which are irregularly shaped and / or in the form of needles, rods, cylinders or platelets.
  • 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.
  • non-metallic particles for example, these may consist of oxides or hydroxides of the metals already mentioned or of other metals, furthermore the particles may consist of glass or sheet silicates such as mica or bentonites. In addition, the particles may consist of carbides, silicates, nitrides, phosphates and sulfates.
  • the recovery and processing for the process of suitable particles may also be by other means (e.g.
  • the particles may also be organic and inorganic salts. Furthermore, 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 can also consist of mixtures of at least two materials, wherein basically all mixing ratios of the two materials are possible.
  • the amount of material that is the lowest in mass is more than 2 percent by weight, based on the total weight of the particles.
  • layers with the highest possible packing density should in principle be produced, since in most cases they have ideal application properties.
  • the highest possible packing density is synonymous with a layer that is as similar as possible to a closed, non-particulate layer, ie a layer that corresponds to the ideal base material.
  • Such layers are sought since they have the best physical and chemical properties. For example, silver traces show an increasing resistance as the packing density decreases.
  • a low packing density results especially when 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.
  • the particles tend to show such behavior if they consist of higher-melting metals (melting point> 500 ° C) and non-metallic material.
  • the energy of the plasma activates such particles only on their surface, whereby the shape of the particles as such remains in the layer formed on the substrate.
  • the inventive method can be used to coat a variety of
  • Substrates are used. 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 applications for the inventive method are also very diverse. With the method, for example, layers for applications for
  • Conductive layers produced by the process can be any material that can be used as well as the adhesion mediation. Conductive layers produced by the process can be any material that can be used as well as the adhesion mediation. Conductive layers produced by the process can be any material that can be used as well as the adhesion mediation.
  • conductive layers can also be used as shielding, as electrical contact and as antenna, in particular RFID (Radio Frequency Identification) antennas.
  • Sensor surfaces for example for HMI interfaces, control panels etc.
  • Encapsulation e.g., populated wafers
  • the layers may be applied in the form of laminar layers which cover the substrate over a large area, preferably greater than 70% of the area of the substrate.
  • the layers can also be applied in the form of patterns, which are preferably adapted to the desired functionality.
  • 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 beam generator (1) for generating a plasma jet (2) of a low-temperature plasma comprises two electrodes (4, 5) arranged in the flow of a working gas (3) and a voltage source (6) for generating a pulsed direct voltage between the electrodes (4, 5).
  • the first electrode (4) is designed as a pin electrode
  • the spaced-apart second electrode (5) is designed 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 with 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) via an inlet (21) is supplied.
  • the inlet (21) is located on a front side on the hollow cylindrical jacket (7) patch, the pin electrode (4) holding sleeve (22) made of electrically insulating material.
  • extending outlet (8) is transverse to the longitudinal extent of a feed opening (9) through which the plasma jet (2) platelet-shaped particles (10) can be fed.
  • the feed opening (9) of the jet generator is connected for this purpose via a line (12) with a swirl chamber (1 1), in the
  • the vortex chamber (1 1) is at most up to a maximum level (13) with the platelet-shaped particles (10)
  • the platelet-shaped particles (10) transversely to the propagation direction of the plasma jet (2) into a core zone (17) of the plasma jet (2), in which a temperature of less than 500 degrees Celsius prevails (low-temperature plasma ).
  • the voltage source (6) increases, during each pulse, the voltage applied between the electrodes (4, 5) until, between the electrodes (4, 5), the ignition voltage for the formation of an arc is applied between the electrodes (4, 5).
  • 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 generated which can extinguish the arc between two consecutive voltage pulses respectively.
  • 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 is a maximum of 12 kV.
  • 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 produced, in one embodiment of the invention, the possibility that the plasma jet (2) and the substrate (20), at least temporarily moved during the application of the coating relative to each other.
  • 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 a movable at least in a plane parallel to the substrate (20) plane, so that the generator with a defined Speed is movable relative to the substrate.
  • the relative movement can be webs or even full-surface coatings of the substrate produce.
  • the molten aluminum was liquid at a temperature of about 720 ° C.
  • Several nozzles which work according to an injector principle, dipped into the melt and atomize the aluminum melt vertically upwards.
  • the atomizing gas was compressed in compressors (Kaeser, Coburg, Germany) up to 20 bar and heated in gas heaters up to about 700 ° C.
  • the aluminum powder produced after spraying / atomization solidified and cooled down in the air.
  • the induction furnace was integrated in a closed system.
  • the atomization was carried out under inert gas (nitrogen).
  • the deposition of the aluminum powder was carried out first in a cyclone, wherein there deposited powdered aluminum powder had a D50 of 14-17 ⁇ .
  • Example 2 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% strength by weight ammonia solution (VWR, Germany) were added. After a short time a strong evolution of gas could be observed. Three hours after the first addition of ammonia, another 5 g of 25% strength by weight ammonia solution was added. After another three hours, again 5 g of 25 wt .-% - ammonia solution was added. The suspension was further stirred overnight.
  • VWR isopropanol
  • platelet-shaped particles 500 g of a material prepared according to Example 3 were heated for 10 minutes in a rotary kiln (Nabertherm, Germany) to 1 100 ° C. There were obtained 335 g of a white powder. This was examined as described. The results are shown in Figures 4 and 5. In contrast to the uncalcined material, the particle diameter is slightly larger and the zeta potential is positive throughout the entire pH range. The XRD analysis shows theta-Al 2 O 3 .
  • Example 5-8 Coating of particles with an acrylate shell
  • Example 5 Example 1 Ethanol 6.6 g
  • Example 7 Example 3 Ethanol 6.1 g
  • Example 8 Example 4 Ethanol 6.2 g non-metallic polymer coating
  • W .-% dispersion dispersed in 600 g of ethanol 100 ml of a solution of 0.5 g of dimethyl 2,2'-azobis (2-methylpropionate) (trade name V 601, available from WAKO Chemicals GmbH, Fuggerstrasse 12, 41468 Neuss), 1 g of methacryloxypropyltrimethoxysilane, were subsequently added over a period of 1 hour (MEMO) and 10 g of trimethylolpropane trimethacrylate (TMPTMA) in white spirit.
  • MEMO 1 hour
  • TMPTMA trimethylolpropane trimethacrylate
  • coated particles were applied by means of a Plasmatron system from Inocon, Attnang-Puchheim, Austria, argon and nitrogen being used as ionizable gases. Standard process parameters were used.
  • Examples 9-1 to 9-4 were applied to aluminum sheets, steel sheets and wafers. This showed a very uniform application of the powder, a slight overspray, a good adhesion of the layer to the surface and a color of the coating, which can be concluded with a small amount of oxidation. This was also confirmed in subsequent SEM images. Exemplary images of the spherical copper grit coating according to Example 9-1 can be found in FIGS. 3 and 4. For example, FIGS. 3 and 4. For example, FIGS. 3 and 4.
  • Coating can be achieved.
  • Surface agglomerates showed no appreciable binding to the substrate surface.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Coating By Spraying Or Casting (AREA)

Abstract

L'invention concerne un procédé d'application d'un revêtement sur un substrat au moyen d'un plasma froid, selon lequel des particules munies d'un revêtement polymère sont introduites dans un plasma froid à moins de 3 000 K, les particules ainsi activées se déposant sur le substrat. La présente invention concerne par ailleurs un revêtement de substrat qui peut être obtenu par le procédé selon l'invention. La présente invention concerne en outre l'utilisation de particules en forme de plaquettes munies d'un revêtement polymère d'une épaisseur moyenne inférieure à 2 µm pour le revêtement d'un substrat en utilisant un plasma froid.
EP12741312.8A 2011-07-25 2012-07-25 Procédé d'application d'un revêtement sur un substrat, revêtement, et utilisation de particules Withdrawn EP2737099A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102011052118A DE102011052118A1 (de) 2011-07-25 2011-07-25 Verfahren zum Aufbringen einer Beschichtung auf einem Substrat, Beschichtung und Verwendung von Partikeln
PCT/EP2012/064637 WO2013014212A2 (fr) 2011-07-25 2012-07-25 Procédé d'application d'un revêtement sur un substrat, revêtement, et utilisation de particules

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US (1) US20140170410A1 (fr)
EP (1) EP2737099A2 (fr)
JP (1) JP2014521835A (fr)
KR (1) KR20140068031A (fr)
CN (1) CN103703159A (fr)
DE (1) DE102011052118A1 (fr)
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JP2014521835A (ja) 2014-08-28
WO2013014212A3 (fr) 2013-06-20
WO2013014212A2 (fr) 2013-01-31
US20140170410A1 (en) 2014-06-19
KR20140068031A (ko) 2014-06-05
DE102011052118A1 (de) 2013-01-31
CN103703159A (zh) 2014-04-02

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