EP2099954A1 - Dispositif et procédé de revêtement par électrolyse - Google Patents

Dispositif et procédé de revêtement par électrolyse

Info

Publication number
EP2099954A1
EP2099954A1 EP07847339A EP07847339A EP2099954A1 EP 2099954 A1 EP2099954 A1 EP 2099954A1 EP 07847339 A EP07847339 A EP 07847339A EP 07847339 A EP07847339 A EP 07847339A EP 2099954 A1 EP2099954 A1 EP 2099954A1
Authority
EP
European Patent Office
Prior art keywords
base layer
substrate
rollers
roller
switchable
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Withdrawn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
EP07847339A
Other languages
German (de)
English (en)
Inventor
Rene Lochtman
Jürgen Kaczun
Norbert Wagner
Jürgen PFISTER
Gert Pohl
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.)
BASF SE
Original Assignee
BASF SE
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 BASF SE filed Critical BASF SE
Priority to EP07847339A priority Critical patent/EP2099954A1/fr
Publication of EP2099954A1 publication Critical patent/EP2099954A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/06—Wires; Strips; Foils
    • C25D7/0614—Strips or foils
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/16—Apparatus for electrolytic coating of small objects in bulk
    • C25D17/28—Apparatus for electrolytic coating of small objects in bulk with means for moving the objects individually through the apparatus during treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/06—Wires; Strips; Foils
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/22—Secondary treatment of printed circuits
    • H05K3/24—Reinforcing the conductive pattern
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/22—Secondary treatment of printed circuits
    • H05K3/24—Reinforcing the conductive pattern
    • H05K3/241—Reinforcing the conductive pattern characterised by the electroplating method; means therefor, e.g. baths or apparatus
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
    • H05K2203/01—Tools for processing; Objects used during processing
    • H05K2203/0104—Tools for processing; Objects used during processing for patterning or coating
    • H05K2203/0143—Using a roller; Specific shape thereof; Providing locally adhesive portions thereon
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
    • H05K2203/15—Position of the PCB during processing
    • H05K2203/1509—Horizontally held PCB

Definitions

  • the invention relates to a device and a method for the galvanic coating of a structured or full-surface base layer on a surface of a substrate, which comprises at least one electrolytic bath with at least one rotatably mounted roller switchable as a cathode, which contacts the base layer during the galvanic coating, wherein the base layer is covered by an electrolyte solution contained in the electrolyte bath and moves during the coating relative to the roller.
  • the device according to the invention and the method according to the invention are suitable, for example, for printed conductors on printed circuit boards, RFI D antennas, transponder antennas or other antenna structures, chip card modules, flat cables, seat heaters, foil conductors, printed conductors in solar cells or in LCD or plasma picture screens or galvanically produce coated products in any form. Also, the device is suitable for the production of decorative or functional surfaces on products that can be used to shield electromagnetic radiation, for heat conduction or as packaging.
  • a method and apparatus for electrolytically enhancing the thickness of an electrically conductive structure on a dielectric substrate is known, for example, from WO-A 2005/076680.
  • the device described here is suitable for the coating of flexible carriers. These are guided around a roller, on whose outer circumference rotatable cylindrical electrodes are accommodated about their longitudinal axis. The electrodes are each enclosed by shielding elements. Electrodes associated with the film on which the structure to be coated is associated are cathodically connected. Electrodes that are not in contact with the film to be coated can be replaced, for example. Preferably, the roller is only half immersed in an electrolyte solution. This avoids the deposition of metal on electrodes that are not in contact with the film.
  • the shielding elements which surround the cylindrical electrodes are made of a dielectric material, for example rubber or plastic.
  • WO-A 2005/076680 Disadvantage of the embodiment according to WO-A 2005/076680 is that this is only suitable for coating of flexible circuit carriers. Rigid circuit carriers can not be coated with the device. Another disadvantage is that the electrodes are permanently charged with voltage, so that even on electrodes, which are not in communication with the flexible supports to be coated, can deposit metal.
  • Object of the present invention is to provide a device for galvanic coating, can be coated with the structured or full-surface base layers on a surface of a substrate, which may be rigid or flexible, and in which a metal deposition on the electrode is reduced or prevented ,
  • a device for galvanic coating of a structured or full-surface base layer on a surface of a substrate which comprises at least one electrolyte bath with at least one switchable as a cathode, rotatably mounted roller which contacts the base layer during the galvanic coating.
  • the base layer is covered by an electrolyte solution contained in the electrolyte bath and moves relative to the roller during the coating.
  • the roller is switched cathodically during contact with the base layer and switched off or anodically when there is no contact with the base layer.
  • the fact that the base layer moves relative to the roller during the coating means that either the substrate with the base layer is held stationary and the roller is moved over it, or that the roller is held stationary and the substrate with the base layer is moved along the roller ,
  • Galvanically coatable structured or full-surface base layers on a surface of a substrate can be produced for example by methods known in the art of printed circuit board manufacturing.
  • a one- or two-sided copper-clad substrate is processed by the etching and resist method known to the person skilled in the art, whereby a structured, electrically coatable base layer of copper is produced.
  • all other methods known to those skilled in the art can be used.
  • Galvanically coatable structured or full-surface base layers on a surface of a substrate can furthermore be produced, for example, by providing a structured or full-surface base layer with a dispersion which is at least electroplatable particles and a matrix material containing, applied, the applied dispersion is at least partially dried and / or at least partially cured and optionally the electrically conductive particles are exposed on the surface of the remaining base layer by at least partial chemical, physical or mechanical removal of the matrix.
  • rigid or flexible carriers are suitable as the substrate on which the structured or full-surface base layer to be galvanically coated is applied.
  • the carrier is not electrically conductive. This means that the specific resistance is more than 10 9 ohm cm.
  • Suitable carriers are, for example, reinforced or unreinforced polymers, as are commonly used for printed circuit boards.
  • Suitable polymers are epoxy resins, or modified epoxy resins, for example bifunctional or polyfunctional bisphenol A or bisphenol F resins, epoxy novolac resins, brominated epoxy resins, aramid-reinforced or glass-fiber-reinforced or paper-reinforced epoxy resins (for example FR4), glass-fiber reinforced plastics, liquid cristal Polymers (LCP), polyphenylene sulfides (PPS), polyoxymethylenes (POM), polyaryl ether ketones (PAEK), polyether ether ketones (PEEK), polyamides (PA), polycarbonates (PC), polybutylene terephthalates (PBT), polyethylene terephthalates (PET), polyimides.
  • LCP liquid cristal Polymers
  • PPS polyphenylene sulfides
  • POM polyoxymethylenes
  • PAEK polyaryl ether ketones
  • PEEK polyether ether ketones
  • PA polyamides
  • PC polycarbonates
  • PBT polybutylene
  • the carrier can be both rigid and flexible.
  • the base layer preferably contains galvanically coatable particles in a matrix material.
  • a dispersion containing the electrodepositable particles in the matrix material is applied.
  • the electrolytically coatable particles may be particles of any geometry made of any arbitrary electrically conductive material, of mixtures of different electrically conductive materials or of mixtures of electrically conductive and non-conductive materials.
  • Suitable electrically conductive materials are, for example, carbon, electrically conductive metal complexes, conductive organic compounds or conductive polymers or metals, preferably zinc, nickel, copper, tin, cobalt, manganese, iron, magnesium, lead, chromium, bismuth, silver, gold, aluminum , Titanium, palladium, platinum, tantalum and alloys thereof, or metal mixtures containing at least one of these metals.
  • suitable alloys are CuZn, CuSn, CuNi, SnPb, SnBi, SnCo, NiPb, ZnFe, ZnNi, ZnCo and ZnMn. Particular preference is given to aluminum, iron, copper, nickel, zinc, carbon and mixtures thereof.
  • the electrodepositable particles have an average particle diameter of 0.001 to 100 .mu.m, preferably from 0.005 to 50 .mu.m and particularly preferably from 0.01 to 10 microns.
  • the average particle diameter can be determined by means of laser diffraction measurement, for example on a Microtrac X100 device.
  • the distribution of the particle diameter depends on their production method. Typically, the diameter distribution has only one maximum, but several maxima are also possible.
  • the surface of the electrodepositable particles may be at least partially provided with a coating ("coating"). Suitable coatings may be inorganic (for example SiC> 2 , phosphates) or organic in nature. Of course, the electrodepositable particles may also be coated with a metal or metal oxide. Also, the metal may be in partially oxidized form.
  • the electrodepositable particles can be done by a mixture of these metals. It is particularly preferred if the metals are selected from the group consisting of aluminum, iron, copper, nickel and zinc.
  • the electrodepositable particles may also include a first metal and a second metal in which the first metal is in the form of an alloy (with the first metal or one or more other metals) or the electrodepositable particles contain two different alloys.
  • the shape of the electrodepositable particles has an influence on the properties of the dispersion after a coating. With regard to the shape, numerous variants known to the person skilled in the art are possible.
  • the shape of the electrodepositable particles may be, for example, acicular, cylindrical, plate-shaped or spherical. These particle shapes represent idealized shapes, wherein the actual shape, for example due to production, may vary more or less strongly therefrom. For example, drop-shaped particles in the context of the present invention are a real deviation of the idealized spherical shape.
  • Galvanic coatable particles with different particle shapes are commercially available.
  • the individual mixing partners can also have different particle shapes and / or particle sizes. It is also possible to use mixtures of one type of electrodepositable particles having different particle sizes and / or particle shapes. In the case of different particle shapes and / or particle sizes, the metals aluminum, iron, copper, nickel and zinc as well as carbon are also preferred.
  • the electroplateable particles in the form of their powders can be added to the dispersion.
  • Such powders for example metal powders
  • Such powders are common commercial products and can easily be produced by means of known processes, for example by electrolytic deposition or chemical reduction from solutions of metal salts or by reduction of an oxidic powder, for example by means of hydrogen, by spraying or atomizing a molten metal, in particular in cooling media, for example gases or water. Preference is given to the gas and water atomization and the reduction of metal oxides.
  • Metal powders of the preferred grain size can also be made by grinding coarser metal powders. For this purpose, for example, a ball mill is suitable.
  • the carbonyl iron powder process is preferred for producing carbonyl iron powder.
  • This is done by thermal decomposition of iron pentacarbonyl. This is described, for example, in Ullman's Encyclopedia of Industrial Chemistry, 5th Edition, Vol. A14, page 599.
  • the decomposition of the iron pentacarbonyl can be carried out, for example, at elevated temperatures and elevated pressures in a heatable decomposer which comprises a tube made of a heat-resistant material such as quartz glass or V2A steel in a preferably vertical position, which consists of a heating device, for example consisting of Heating baths, heating wires or is surrounded by a heating medium flowing through a heating jacket.
  • Platelet-shaped, galvanically coatable particles can be controlled by optimized conditions in the production process or subsequently obtained by mechanical treatment, for example by treatment in a stirred ball mill.
  • the proportion of electrolytically coatable particles in the range of 20 to 98 wt .-%.
  • a preferred range of the proportion of the electrodepositable particles is 30 to 95 wt .-% based on the total weight of the dried base layer.
  • Suitable matrix materials include, for example, binders having a pigmentary anchor group, natural and synthetic polymers and their derivatives, natural resins and synthetic resins and their derivatives, natural rubber, synthetic rubber, proteins, cellulose derivatives, drying and non-drying oils and the like. These can - but need not - be chemically or physically curing, for example air-hardening, radiation-curing or temperature-curing.
  • the matrix material is a polymer or polymer mixture.
  • Preferred polymers as the matrix material are ABS (acrylonitrile-butadiene-styrene); ASA (acrylonitrile-styrene-acrylate); acrylated acrylates; alkyd resins; Alkylvinylacetate; Alkylenvi- nylacetat copolymers, in particular methylene vinyl acetate, ethylene vinyl acetate, butylene vinyl acetate; Alkylenvinylchlorid copolymers; amino resins; Aldehyde and ketone resins; Cellulose and cellulose derivatives, in particular hydroxyalkylcellulose, cellulose esters, such as acetates, propionates, butyrates, carboxyalkylcelluloses, cellulose nitrate; Epoxy acrylate; epoxy resins; modified epoxy resins, for example bifunctional or polyfunctional bisphenol A or bisphenol F resins, epoxy novolac resins, brominated epoxy resins, cycloaliphatic epoxy resins; aliphatic
  • Particularly preferred polymers as matrix material are acrylates, acrylate resins, cellulosic derivatives, methacrylates, methacrylate resins, melamine and amino resins, polyalkylenes, polyimides, epoxy resins, modified epoxy resins, for example bifunctional or polyfunctional bisphenol A or bisphenol F resins, epoxy novolak resins, brominated epoxy resins, cycloaliphatic epoxy resins; aliphatic epoxy resins, glycidyl ethers, vinyl ethers, and phenolic resins, polyurethanes, polyesters, polyvinyl acetals, polyvinyl acetates, polystyrenes, polystyrene copolymers, polystyrene acrylates, styrene-butadiene block copolymers, alkylene vinyl acetates and vinyl chloride copolymers, polyamides and their copolymers.
  • the matrix material for the dispersion is preferably thermally or radiation-curing resins, for example modified epoxy resins, such as bifunctional or polyfunctional bisphenol A or bisphenol F resins, epoxy novolac resins, brominated epoxy resins, cycloaliphatic epoxy resins; aliphatic epoxy resins, glycidyl ethers, cyanate esters, vinyl ethers, phenolic resins, polyimides, melamine resins and amino resins, polyurethanes, polyesters and cellulose derivatives.
  • modified epoxy resins such as bifunctional or polyfunctional bisphenol A or bisphenol F resins, epoxy novolac resins, brominated epoxy resins, cycloaliphatic epoxy resins; aliphatic epoxy resins, glycidyl ethers, cyanate esters, vinyl ethers, phenolic resins, polyimides, melamine resins and amino resins, polyurethanes, polyesters and cellulose derivatives.
  • the proportion of the organic binder component is from 0.01 to 60% by weight.
  • the proportion is 0.1 to 45 wt .-%, more preferably 0.5 to 35 wt .-%.
  • the dispersion containing the electrically conductive particles and the matrix material it is also possible for the dispersion to be admixed with a solvent or a solvent mixture in order to obtain the dispersion required for the respective application. drive to adjust the appropriate viscosity of the dispersion.
  • Suitable solvents are, for example, aliphatic and aromatic hydrocarbons (for example n-octane, cyclohexane, toluene, xylene), alcohols (for example methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, amyl alcohol ), polyhydric alcohols such as glycerol, ethylene glycol, propylene glycol, neopentyl glycol, alkyl esters (for example methyl acetate, ethyl acetate, propyl acetate, butyl acetate, isobutyl acetate, isopropyl acetate, 3-methylbutanol), alkoxy alcohols (for example methoxypropanol, methoxybutanol, ethoxypropanol), alkylbenzenes (for example, ethylbenzene, isopropylbenzene), butyl glycol
  • Preferred solvents are alcohols (for example, ethanol, 1-propanol, 2-propanol, butanol), alkoxyalcohols (for example, methoxypropanol, ethoxypropanol, butylglycol, butyldiglycol), butyrolactone, diglycol dialkyl ethers, diglycol monoalkyl ethers, dipropylene glycol dialkyl ethers, dipropylene glycol monoalkyl ethers, esters (for example, ethyl acetate, butyl acetate , Butyl glycol acetate, butyl diglycol acetate, diglycol alkyl ether acetates, dipropylene glycol alkyl ether acetates, DBE), ethers (for example tetrahydrofuran), polyhydric alcohols such as glycerol, ethylene glycol, propylene glycol, neopentyl glycol, ketones (for
  • alkoxy alcohols for example ethoxypropanol, butylglycol, butyldiglycol
  • polyhydric alcohols such as glycerol, esters (for example butyldiglycol acetate, butylglycol acetate, dipropylene glycol methyl ether acetates), water, cyclohexanone, butyrolactone, N- Methylpyrrolidone, DBE and mixtures thereof as a solvent particularly preferred.
  • liquid matrix materials eg liquid epoxy resins, acrylate esters
  • the respective viscosity can alternatively also be adjusted via the temperature during the application, or via a combination of solvent and temperature
  • the dispersion may further contain a dispersant component. This consists of one or more dispersants.
  • dispersants known to the person skilled in the art for use in dispersions and described in the prior art are suitable.
  • Preferred dispersants are surfactants or surfactant mixtures, for example anionic, cationic, amphoteric or nonionic surfactants.
  • the dispersant may be used in the range of 0.01 to 50% by weight based on the total weight of the dispersion.
  • the proportion is 0.1 to 25 wt .-%, particularly preferably 0.2 to 10 wt .-%.
  • the dispersion of the invention may contain a filler component.
  • This may consist of one or more fillers.
  • the filler component of the metallizable composition may contain fibrous, layered or particulate fillers or mixtures thereof. These are preferably commercially available products, such as carbon and mineral fillers.
  • fillers or reinforcing materials such as glass powder, mineral fibers, whiskers, aluminum hydroxide, metal oxides such as alumina or iron oxide, mica, quartz powder, calcium carbonate, barium sulfate, titanium dioxide or wollastonite can be used.
  • thixotropic agents for example silica, silicates, such as aerosils or bentonites or organic thixotropic agents and thickeners, such as polyacrylic acid, polyurethanes, hydrogenated castor oil, dyes, fatty acids, fatty acid amides, plasticizers, wetting agents, defoamers, Lubricants, drying agents, crosslinkers, photoinitiators, complexing agents, waxes, pigments, conductive polymer particles, can be used.
  • thixotropic agents for example silica, silicates, such as aerosils or bentonites or organic thixotropic agents and thickeners, such as polyacrylic acid, polyurethanes, hydrogenated castor oil, dyes, fatty acids, fatty acid amides, plasticizers, wetting agents, defoamers, Lubricants, drying agents, crosslinkers, photoinitiators, complexing agents, waxes, pigments, conductive polymer particles, can be used.
  • the proportion of the filler component based on the total weight of the dry coating is preferably 0.01 to 50 wt .-%. Further preferred are 0.1 to 30 wt .-%, particularly preferably 0.3 to 20 wt .-%. Furthermore, processing aids and stabilizers such as UV stabilizers, lubricants, corrosion inhibitors and flame retardants can be present in the dispersion according to the invention. Usually, their proportion based on the total weight of the dispersion 0.01 to 5 wt .-%. Preferably, the proportion is 0.05 to 3 wt .-%.
  • the structured or full-surface base layer is printed with the dispersion by any printing method on the support.
  • the printing process used to print the patterned surface is, for example, a web or sheetfed printing process, such as screen printing, gravure, flexo, letterpress, pad printing, inkjet, Lasersonic® as described in DE10051850, or offset printing.
  • Such coating methods are, for example, casting, brushing, knife coating, brushing, spraying, dipping, rolling, powdering, fluidized bed or the like.
  • the layer thickness of the structured or full surface area produced by the printing or the coating method preferably varies between 0.01 and 50 ⁇ m, more preferably between 0.05 and 25 ⁇ m and particularly preferably between 0.1 and 15 ⁇ m.
  • the layers can be applied both over the entire surface as well as structured.
  • the base layer by applying an adhesive layer and the subsequent transfer of the electrodepositable particles.
  • the material of the adhesive layer preferably corresponds to the above-described matrix material of the dispersion.
  • the adhesive layer is preferably applied by a printing process. The printing process can be the same as described above for the application of the dispersion.
  • the galvanically coatable particles can be transferred from a transfer medium to the adhesive layer, for example.
  • a transfer medium for example, any rigid or flexible carrier on which the electroformable particles can be applied can be used as the transfer medium.
  • Suitable materials for the transfer medium are, for example, metals, glass, ceramic, plastic or any composite materials.
  • the electrolytically coatable particles contained therein can be at least partially exposed in order to obtain already galvano-coatable nucleation sites, which can be found in the following galvanic coating can deposit the metal ions to form a metal layer. If the particles consist of materials which oxidize easily, it may additionally be necessary to at least partially remove the oxide layer beforehand. Depending on the implementation of the method, for example, when using acidic electrolyte solutions, the removal of the oxide layer can already take place simultaneously with the onset of galvanic coating, without an additional process step is required.
  • An advantage of exposing the particles before the galvanic coating is that, by exposing the particles, an approximately 5 to 10% by weight lower proportion of electrodepositable particles must be contained in the base layer in order to obtain a continuous electrically conductive surface, as this is the case when the particles are not exposed. Further advantages are the homogeneity and consistency of the coatings produced and the high process reliability.
  • Exposure of the electrodepositable particles can be either mechanical, for example by brushing, grinding, milling, sandblasting or supercritical carbon dioxide irradiation, physically, for example by heating, lasing, UV light, corona or plasma discharge, or chemically.
  • a chemical exposure it is preferable to use a chemical or chemical mixture suitable for the matrix material.
  • the matrix material can be at least partially dissolved and washed down by a solvent on the surface, or the chemical structure of the matrix material can be at least partially destroyed by means of suitable reagents, thereby exposing the electrodepositable particles.
  • reagents that swell the matrix material are suitable for exposing the electrodepositable particles.
  • the swelling results in cavities into which the metal ions to be deposited can penetrate from the electrolyte solution, as a result of which a larger number of electrolytically coatable particles can be metallized.
  • the adhesion, the homogeneity and the continuity of the subsequently electrodeposited metal layer are significantly better than in the methods described in the prior art. Due to the higher number of exposed, electrodepositable particles, the process speed in the metallization is also much higher, whereby additional cost advantages can be achieved.
  • the removal of the electrolessly and / or electrolytically coatable particles preferably takes place with an oxidizing agent , The oxidizing agent broken the bonds of the matrix material, whereby the binder can be peeled off and thereby the particles are exposed.
  • Suitable oxidizing agents are, for example, manganates such as potassium permanganate, potassium manganate, sodium permanganate, sodium manganate, hydrogen peroxide, oxygen, oxygen in the presence of catalysts such as manganese, molybdenum, bismuth, tungsten and cobalt salts, ozone, vanadium pentoxide, selenium dioxide, Ammonium polysulfide solution, sulfur in the presence of ammonia or amines, manganese dioxide, potassium ferrate, dichromate / sulfuric acid, chromic acid in sulfuric acid or in acetic acid or in acetic anhydride, nitric acid, hydroiodic acid, hydrobromic acid, pyridinium dichromate, chromic acid-pyridine complex, chromic anhydride, chromium ( VI) oxide, periodic acid, lead tetraacetate, quinone, methylquinone, anthraquinone, bromine, chlorine, fluorine, iron (III) salt solutions
  • manganates such as potassium permanganate, potassium manganate, sodium permanganate; Sodium manganate, hydrogen peroxide, N-methyl-morpholine N-oxide, percarbonates, for example sodium or potassium percarbonate, perborates, for example sodium or potassium perborate; Persulfates, for example sodium or potassium persulfate; Sodium, potassium and ammonium peroxodis and monosulfates, sodium hypochlorite, urea-hydrogen peroxide adducts, salts of oxohalogenic acids, such as, for example, chlorates or bromates or iodates, salts of halogenated acids, for example sodium periodate or sodium perchlorate, tetrabutylammonium peroxydisulfate, quinones , Iron (III) salt solutions, vanadium pentoxide, pyridinium dichromate, hydrochloric acid, bromine, chlorine, dichromate.
  • Iron (III) salt solutions vanadium pen
  • potassium permanganate potassium manganate, sodium permanganate, sodium manganate, hydrogen peroxide and its adducts
  • perborates percarbonates, persulfates, peroxodisulfates, sodium hypochlorite and perchlorates.
  • acidic or alkaline chemicals and / or chemical mixtures are, for example, concentrated or dilute acids, such as hydrochloric acid, sulfuric acid, phosphoric acid or nitric acid. Also organic acids, such as formic acid or acetic acid, may be suitable depending on the matrix material.
  • Suitable alkaline chemicals and / or chemical mixtures are, for example, bases, such as sodium hydroxide solution, potassium hydroxide solution, ammonium hydroxide or carbonates, for example sodium carbonate or potassium carbonate.
  • bases such as sodium hydroxide solution, potassium hydroxide solution, ammonium hydroxide or carbonates, for example sodium carbonate or potassium carbonate.
  • the temperature may be increased during the process.
  • Solvents can also be used to expose the electrodepositable particles in the matrix material.
  • the solvent must be matched to the matrix material as the matrix material must dissolve in the solvent or swell through the solvent. If a solvent is used in which the matrix material dissolves, the base layer is only brought into contact with the solvent for a short time, so that the upper layer of the matrix material is dissolved and thereby becomes detached.
  • Preferred solvents are xylene, toluene, halogenated hydrocarbons, acetone, methyl ethyl ketone (MEK), methyl isobutyl ketone (MIBK), diethylene glycol monobutyl ether.
  • MEK methyl ethyl ketone
  • MIBK methyl isobutyl ketone
  • diethylene glycol monobutyl ether diethylene glycol monobutyl ether.
  • the temperature during the dissolution process can be increased.
  • Suitable mechanical methods include, for example, brushing, grinding, abrasive polishing, or jet blasting, blasting, or supercritical carbon dioxide blasting.
  • a suitable abrasive is, for example, pumice.
  • the water jet preferably contains small solid particles, for example, pumice (Al 2 ⁇ 3 ) having an average particle size distribution of 40 to 120 .mu.m, preferably from 60 to 80 .mu.m, and quartz powder (SiO 2 ) with a particle size> 3 microns.
  • the oxide layer is at least partially removed.
  • the removal of the oxide layer can take place, for example, chemically and / or mechanically.
  • Suitable substances with which the base layer can be treated to chemically remove an oxide layer from the electrodepositable particles are, for example, acids such as concentrated or dilute sulfuric acid or concentrated or dilute hydrochloric acid, citric acid, phosphoric acid, sulfamic acid, formic acid, acetic acid ,
  • Suitable mechanical methods for removing the oxide layer from the electrodepositable particles are generally the same as the mechanical methods of exposing the particles.
  • the composition of the electrolyte solution used for coating depends on which metal the base layer is to be coated on the substrate. In principle, all metals that are nobler or equally noble as the base metal of the base layer can be used for the galvanic coating. Typical metals which are deposited by electroplating are, for example, gold, nickel, palladium, platinum, silver, tin, copper or chromium. The thicknesses of the one or more deposited layers are within the usual range known to the person skilled in the art and are not essential to the invention.
  • Suitable electrolyte solutions which can be used for coating electrically conductive structures are known to the person skilled in the art, for example, from Werner Jillek, Gustl Keller, Handbuch der Porterplattentechnik, Eugen G. Leuze Verlag, 2003, Vol. 4, pages 332 to 352.
  • the at least one roller which is mounted as cathodically switchable and rotatably, received stationary in the electrolyte bath, while the substrate is transported with the base layer through the electrolyte bath. During transport of the substrate with the base layer, the roller moves over the base layer. In this case, the base layer is contacted. As long as the roller is in contact with the base layer and is cathodically connected, metal is deposited from the electrolyte solution on the base layer. A closed metal layer is formed. In order to produce a thicker metal layer on the base layer, it is preferred that at least two cathodically switchable rollers are connected in series in the electrolyte bath.
  • the contact time of the base layer with the cathode is increased. Due to the longer contact time, more metal is deposited on the base layer. This leads to a thicker metal coating of the base layer.
  • a shield which prevents supply of electrolyte solution to the surface of the rolls.
  • the shield itself is preferably made of an electrically nonconductive material to prevent the shields from being charged negatively, so that it can settle on this metal. Suitable materials for the shields are, for example, plastics such as PVC, EPDM, silicone rubber.
  • the shields are open to the substrate with the base layer so that the roller can contact the base layer on this side.
  • a gap is formed between the shield and the surface of the substrate.
  • the gap between the shield and the surface of the substrate is closed by an elastic lip.
  • the material for the elastic lip is any elastomer that has a lower hardness than the surface of the base layer or the metallic coating. This will prevent them from being damaged. Suitable materials for the elastic lip are, for example, EPDM, silicone rubber.
  • the elastic lip closes a gap between the shield and the roller.
  • the roller By closing the gap between the roller and the shield, it is also possible for the roller to move.
  • electrolyte solution can get into the space between the shield and the roller when no substrate is in the region of the roller.
  • the gap between the shield and the surface of the substrate is largely sealed by a roller having an elastic surface.
  • the roller with an elastic surface lies on the one hand on the surface of the substrate provided with the base layer and on the other hand on the cathodically switchable roller.
  • the roller having an elastic surface it is also possible for the roller having an elastic surface to be in contact, on the one hand, with the surface of the substrate provided with the base layer and, on the other hand, with the shield.
  • the gap between the shield and the cathodically switchable roller can be largely sealed by the roller with elastic surface.
  • the roller with elastic surface rests on the one hand on the shield and on the other hand on the cathodically switchable roller.
  • the elastic lip or the elastic surface roll is arranged so that when a substrate having the patterned or full-surface base layer to be coated contacts the cathodically-switchable roll, the gap between the substrate and the roll is sealed, thereby not supplying electrolyte solution to the roll At the same time, the space between the cathodically switchable roller and the shield can be largely sealed by the elastic lip or the waist with elastic surface.
  • the space between the shield and the cathodically switchable roll surrounding the cathodically switchable roll be largely extended by the elastic lip or roll having an elastic surface - is sealed, so that as possible no electrolyte solution can flow into this room.
  • the electrolyte solution is always kept away from the surface of the cathodically switchable roller and as far as possible prevents metal deposition on the cathodically switchable roller.
  • the elastic surface roller sealing the gap between the substrate and the shield or between the cathodic switchable roller and the shield may have a non-elastic core made of, for example, metal such as steel or aluminum and an elastic coating.
  • the elastic coating is for example a coating of EPDM or silicone rubber.
  • the roller with elastic surface is made entirely of elastic material. However, this must then have a sufficiently high strength, so that it is avoided that the roller with elastic surface is at least partially squeezed and pulled between the cathodically switchable roller and the substrate.
  • the material for the roller with elastic surface if this is made entirely of elastic material, for example, the same materials as for seals are.
  • the roller can then be made of EPDM or silicone rubber, for example.
  • an anode is received in each case between the shields of two rollers.
  • the anode is preferably designed as a grid anode. This offers the advantage that electrolyte solution can be fed along the anode.
  • soluble anodes As an alternative to the possibility of supplying electrolyte, it is also possible to use soluble anodes.
  • the soluble anodes then preferably contain the metal with which the structured or full-surface base layer is galvanically coated. During the current flow, in this case the metal from the soluble anode goes into solution and then settles on the cathodically connected base layer.
  • the power supply to the individual cathodically switchable rollers is effected for example by sliding contacts.
  • the sliding contacts are preferably formed within the shield.
  • the pressing of the rollers against the sliding contacts takes place, for example, through the substrate on which the structured or full-surface base layer to be coated is located.
  • the cathodically switchable rollers are displaceable perpendicular to the surface of the substrate.
  • a force acts on the roller which removes them from the sliding contact.
  • the cathodically switchable roller is raised against this force and pressed against the sliding contact.
  • the gravitational force by which the rollers are removed from the grinding contact when there is no substrate in the area of the rollers is sufficient.
  • the force required to remove the roller from the sliding contact for example, be applied by spring elements.
  • the cathodically switchable rollers with sliding contacts it is also possible, for example, to use sensors which detect whether the roller is in contact with a base layer to be coated. As soon as it is detected that the cathodically switchable roller contacts a base layer to be coated, a voltage is applied to the cathodically switchable roller. As soon as the sensors detect that there is no contact with a base layer to be coated, the current flow is interrupted again.
  • the sensors with which it is detected whether the roller is in contact with a substrate having a structured or full-surface base layer to be coated are, for example, optical or mechanical.
  • the power can then be supplied to the roller axles via slip rings.
  • the regulation of the power supply via an optical or mechanical sensor is particularly preferred when the substrate has only a very small thickness. In this case, the thickness of the substrate would be insufficient to provide a sufficiently large stroke to push the roller against a sliding contact to produce the power supply. This is the case, for example, when the base layer to be coated is on a thin film carrier.
  • the at least one roller can also be permanently switched cathodically. Resulting metal deposits are still significantly reduced by the Ableungsvorlidept compared to systems such as are known in the prior art. This offers corresponding cost advantages, as the rollers have longer operating times and shorter maintenance intervals.
  • two rolls each lie opposite, between which the substrate is passed.
  • the base layer on the upper side and the base layer on the lower side of the substrate can be simultaneously coated.
  • Another advantage of the opposing rollers is that they can be used simultaneously for transporting the substrate through the electrolyte bath. For this purpose, at least some of the rollers are driven.
  • the transport of the substrate can also take place in that the rollers face a transport device.
  • the transport device may, for example, comprise individual driven rollers on which the substrate is conveyed.
  • the conveying device may comprise, for example, a conveyor belt on which the substrate rests. If the rollers face a conveyor, however, only one side of the substrate can be coated. In order then to coat a base layer possibly present on the underside of the substrate, it is necessary to turn over the substrate and to pass it a second time through the device for electroplating or to provide a second device through which the substrate is guided.
  • the substrate be rotated.
  • the axis of rotation about which the substrate can be rotated is arranged perpendicular to the base layer of the substrate to be coated.
  • the anode is disposed inside the rotating roller.
  • the rotating roller on which the cathodically switchable rollers are arranged designed as a hollow shaft.
  • the rollers that are not in contact with the substrate may, for example, be covered with a shield.
  • shields serve to concentrate the course of the main current on the way from the central anode to the substrate and to limit the current flow of the secondary current from the anodically connected contact rollers to the auxiliary cathodes. As a result, the current efficiency for the metallization of the substrate can be improved.
  • the shields are not required.
  • the rolls which are not in contact with the structured or full-surface base layer on the substrate are anodically switched.
  • the metal previously deposited on the roller is removed from this again.
  • the cleaning of the cathodically switchable rollers can also be done by removing the rollers outside the electrolyte bath. However, this is possible with an arrangement of the rollers in series only if no substrate is coated. In the arrangement of the cathodically switchable rollers on a rotating shaft, it is possible to remove and clean off the cathodically switchable rollers that do not contact the base layer.
  • the method according to the invention and the device according to the invention for the galvanic coating of structured or full-surface base layers on a substrate are suitable, for example, for producing printed conductors on printed circuit boards.
  • Such printed circuit boards are, for example, those with multilayer inner and multilayer outer layers, micro-via-chip-on-board, flexible and rigid printed circuit boards and are incorporated, for example, in products such as computers, telephones, televisions, automotive electrical components, keyboards, Radios, video, CD, CD-ROM and DVD players, game consoles, measuring and control devices, sensors, electrical kitchen appliances, electric toys, etc.
  • electrically conductive structures can be coated on flexible circuit carriers.
  • flexible circuit carriers are, for example, plastic films made of the materials mentioned above for the carrier, on which electrically conductive structures are printed.
  • two-dimensional or three-dimensional Molded Interconnected Devices can be produced with the method according to the invention, for example.
  • antennas with contacts for organic electronic components as well as coatings on surfaces consisting of electrically non-conductive material for electromagnetic shielding (shielding) is also possible.
  • a use is also possible in the field of flow fields of bipolar plates for use in fuel cells.
  • the scope of the inventive device and the method according to the invention enables a cost-effective production of metallized, even non-conductive substrates, in particular for use as switches and sensors, absorbers for electromagnetic radiation or gas barriers or decorative parts, especially decorative parts for motor vehicles, Sani tär-, toys , Household and office space and packaging and films.
  • Textiles can be electrically and magnetically functionalized using the method according to the invention (antennas, transmitters, RFID and transponder antennas, sensors, heating elements, anti-static (also for plastics), shielding, etc.).
  • the method according to the invention as well as the device according to the invention can likewise be used for the metallization of holes, wires, blind holes etc., for example in printed circuit boards, RFI D antennas or transponder antennas, flat cables, foil conductors with the aim of a through-connection of the upper and lower printed circuit board side. This also applies if other substrates are used.
  • the metalized articles produced in the device according to the invention or produced by the method according to the invention - if they comprise magnetizable metals - find application in areas of magnetizable functional parts, such as magnetic boards, magnetic games, magnetic surfaces, for example in refrigerator doors. They also find application in areas where one good thermal conductivity is advantageous, for example in films for seat heaters, underfloor heating and insulation materials.
  • Preferred uses of the galvanically coated surfaces according to the invention are those in which the products thus produced are printed circuit boards, RFID antennas, transponder antennas, seat heaters, flat cables, contactless chip cards, thin metal foils or polymer carriers laminated on one or two sides, foil conductors, conductor tracks in solar cells or in LCD or plasma screens or as a decorative application such as for packaging materials are used.
  • the method according to the invention and the device according to the invention for the galvanic coating of individual plates, for example for circuit boards, can be used.
  • the dimensions of the cathodically switchable rollers and the distance from roller to roller resulting from the smallest, uniformly to be electroplated structure length The smaller the smallest structure length to be electroplated, the smaller the distance between two rolls and thus also the roll diameter should be selected.
  • FIG. 1 shows a device designed according to the invention with series-connected, opposing rolls
  • FIG. 2 shows an inventively designed device in which the cathodically switchable rollers are arranged on a rotatable shaft.
  • FIG. 1 shows a device designed according to the invention with series-connected, opposing rollers.
  • a device according to the invention for electroplating 1 comprises rollers 2 which are cathodically switchable.
  • rollers 2 which are cathodically switchable.
  • Form three rollers 2 are connected in series and there are each two rollers 2 opposite.
  • the rollers 2 are located in a bath 3.
  • the bath 3 contains an electrolyte solution 5.
  • the composition of the electrolyte solution depends on which material is to be coated.
  • a metallic coating is applied by galvanic methods.
  • Typical metals which are deposited by the galvanic coating are, for example, gold, nickel, palladium, platinum, silver, tin, copper or chromium. In principle, however, all metals can be used for the galvanic coating, which are nobler or gleichedel as the base metal of the base layer. If necessary, several devices can be run through successively from the substrate to be coated. In this case, the base layer can be coated on the substrate, if necessary, in succession with different metals.
  • the device for galvanic coating 1 is supplied to a substrate 7, which has a base layer 9, which is galvanically coatable.
  • the base layer 9 can be either structured or full-surface. In the embodiment illustrated in FIG. 1, the base layer 9 is structured. Also located on both the top 11 of the substrate 7 and on the bottom 13 of the substrate 7 each have a base layer 9, which is electroplated.
  • the substrate 7 with the electrodepositable base layer 9 is in each case passed between two opposing rollers 2. By passing the substrate 7, whose direction of movement is shown by an arrow 15, the rollers 2 are displaced perpendicular to the direction of movement 15 of the substrate 7. In a first pair of rollers 17, which contacts the substrate 7 with the base layer 9, the starting position is shown in dashed lines and the position after contacting with a solid line.
  • the upper roller of the first pair of rollers 17 is raised and the lower roller of the first pair of rollers 17 is pressed down.
  • the rollers 2 of the first pair of rollers 17 are each contacted with a sliding contact 19.
  • the rollers 2 of the first pair of rollers 17 are connected cathodically.
  • the contact of the rollers 2 with the base layer 9 on the substrate 7 and the base layer 9 is connected cathodically. It separates metal from the electrolyte solution 5 on the base layer 9 from.
  • the rollers 2 are each surrounded by a shield 21. concluded.
  • electrolyte solution reaches the surface of the rollers 2.
  • elastic lips 23 are preferably formed on the shields. If there is no substrate between two rolls of a roll pair, as is the case, for example, with the second roll pair 25 or the third roll pair 27, the elastic lips 23 are preferably in contact with the roll 2. As soon as the substrate 7 with the base layer 9 is passed between two opposite rollers 2 of a pair of rollers 17, as shown in FIG.
  • the elastic lips 23 are preferably located on the upper side 11 or lower side 13 of the substrate 7. As a result, a gap between the substrate 7 and the shield 21 is closed. There can be no electrolyte solution to the roller 2. Thus, no metal can be deposited from the electrolyte solution on the roller 2.
  • a roller As an alternative to the elastic lips 23, it is also possible for a roller to be provided with an elastic surface which, on the one hand, contacts the surface of the rollers 2 and, on the other hand, the shield 21 or the substrate 7.
  • an anode 29 is received in each case between two shields 21.
  • the anode 29 is preferably designed as a grid anode.
  • the concentration of metal ions in the electrolytic solution 5 decreases due to the deposition of metal on the electrodepositable base layer 9, it is preferable that fresh electrolytic solution can be added.
  • the anodes 29 are formed as lattice anodes, it is possible to supply the electrolytic solution via the anodes 29 as indicated by the arrows 31 in FIG.
  • the supply of the electrolyte solution along the anodes 29 has the advantage that in the intermediate areas between the rollers 2 fresh electrolyte solution is added. Due to the positioning of the rollers touching, for example, as shown in Figure 1, when no substrate 7 is passed between them and otherwise contact the substrate 7, exchange of electrolyte solution in the spaces between each two adjacent rollers is only very hardly possible.
  • the individual roller pairs 17, 25, 27 are contacted successively with the base layer 9 on the substrate 7.
  • the roller pairs 17, 25, 27, between which the substrate 7 is passed, are each contacted with the corresponding sliding contacts 19.
  • the transport of the substrate 7 between the roller pairs 17, 25, 27 is effected, for example, by providing individual rollers 2 of the roller pairs 17, 25, 27 with a drive.
  • all the rollers 2 of the roller pairs 17, 25, 27 may be driven.
  • the rollers 2 are driven, which lie on the same side of the substrate 7.
  • the rollers 2 are driven on the underside 13 of the substrate 7 or the rollers 2 on the upper side 1 1 of the substrate 7.
  • the rollers 2 can either be removed for cleaning or else switched to anodic operation.
  • the Anodischschalt the rollers can be done, for example, that the sliding contacts 19 are connected anodically and a substrate without base layer is performed by the device, whereby the rollers 2 then contact the anodically connected sliding contacts 19.
  • FIG. 2 shows a second embodiment of the device according to the invention.
  • the cathodically switchable rollers 2 are arranged on a rotatable shaft 41.
  • a substrate 7 with a base layer 9 formed thereon can be coated only on one side.
  • the rollers 2 are, as in the embodiment shown in FIG. 1, enclosed by a shield 21 with elastic lips 23 formed thereon.
  • the substrate 7 with the base layer 9 to be galvanically coated is guided along the device 1.
  • at least one roller 2 contacts the base layer 9.
  • the contact between the roller 2 and the base layer 9 causes the base layer 9 to be connected in a cathodic manner.
  • Metal is deposited on the base layer 9.
  • FIG. 1 As in the embodiment shown in FIG.
  • the rotatable shaft 41, on which the rollers 2 are arranged, is preferably designed as a hollow shaft. Inside the shaft 41 is an anode 43.
  • rollers 2 which are not in contact with the base layer 9, can be switched anodically.
  • the rollers 2 are switched anodically, which are furthest removed from the base layer 9 to be coated.
  • the anodically connected rolls are provided with reference numeral 45 in FIG.
  • the anodically connected rollers 45 are preferably opposite cathodes 47, which allow a flow of current.
  • a shield 49 is preferably accommodated between the anode 43 and the anodically connected rollers 45.
  • rollers 2 which do not contact the base layer 9 and which are not connected cathodically, are preferably de-energized. These rollers may be covered by a shield 51.
  • anodically connected rollers 45 it is also possible to remove rollers 2 which are not in contact with the base layer 9 and to clean them outside the device 1.
  • the entire device 1 is covered by the electrolyte solution 5.
  • the rollers 2, which do not contact the base layer 9 on the upper side 1 1 of the substrate 7, may be outside the electrolyte solution.
  • the anode 43 is also in the electrolyte solution 5.
  • the anode 43 is not arranged as shown in Figure 2 inside the shaft 41 designed as a hollow shaft, but is located outside the shaft 41.

Abstract

L'invention concerne un dispositif de revêtement par électrolyse d'une couche de base (9) structurée ou qui s'étend sur toute la surface d'un substrat (7), et qui comprend au moins un bain d'électrolyte (3) doté d'au moins un cylindre (2) monté à rotation, apte à être raccordé comme cathode et qui pendant le revêtement par électrolyse est en contact avec la couche de base (9). La couche de base (9) est recouverte par une solution d'électrolyte (5) que contient le bain d'électrolyte (3) et se déplace par rapport au ou aux cylindres (2) pendant le revêtement. Le ou les cylindres (2) aptes à être raccordés comme cathodes sont cathodiques pendant le contact avec la couche de base (9) et dès que le contact avec la couche de base (9) est coupé, ils sont raccordés sans courant ou en anode. L'invention concerne en outre un procédé de revêtement par électrolyse d'une couche de base (9) structurée ou qui s'étend sur toute la surface d'un substrat (7). La couche de base (9) est entourée par une solution d'électrolyte (5) et est mise en contact avec au moins un cylindre (2) qui peut être raccordé comme cathode. Le cylindre (2) qui peut être raccordé comme cathode est raccordé en cathode lorsqu'il est en contact avec la couche de base (9) et est raccordé sans courant ou en anode dès que le contact avec la couche de base (9) est coupé.
EP07847339A 2006-11-28 2007-11-26 Dispositif et procédé de revêtement par électrolyse Withdrawn EP2099954A1 (fr)

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EP07847339A EP2099954A1 (fr) 2006-11-28 2007-11-26 Dispositif et procédé de revêtement par électrolyse

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EP06124862 2006-11-28
EP07847339A EP2099954A1 (fr) 2006-11-28 2007-11-26 Dispositif et procédé de revêtement par électrolyse
PCT/EP2007/062805 WO2008065069A1 (fr) 2006-11-28 2007-11-26 Dispositif et procédé de revêtement par électrolyse

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EP (1) EP2099954A1 (fr)
JP (1) JP2010511103A (fr)
KR (1) KR20090083489A (fr)
CN (1) CN101542022A (fr)
BR (1) BRPI0719665A2 (fr)
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WO2008065069A1 (fr) 2008-06-05
JP2010511103A (ja) 2010-04-08
IL198594A0 (en) 2010-02-17
BRPI0719665A2 (pt) 2013-12-17
US20090301891A1 (en) 2009-12-10
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KR20090083489A (ko) 2009-08-03
TW200829726A (en) 2008-07-16

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