EP0476539B1 - Process for applying powder coatings to metallic surfaces - Google Patents
Process for applying powder coatings to metallic surfaces Download PDFInfo
- Publication number
- EP0476539B1 EP0476539B1 EP19910115563 EP91115563A EP0476539B1 EP 0476539 B1 EP0476539 B1 EP 0476539B1 EP 19910115563 EP19910115563 EP 19910115563 EP 91115563 A EP91115563 A EP 91115563A EP 0476539 B1 EP0476539 B1 EP 0476539B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- oil
- powder
- powder layer
- layer
- heating
- 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.)
- Expired - Lifetime
Links
- 239000000843 powder Substances 0.000 title claims abstract description 39
- 238000000576 coating method Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 50
- 235000019198 oils Nutrition 0.000 claims description 50
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 239000002480 mineral oil Substances 0.000 claims description 2
- 235000010446 mineral oil Nutrition 0.000 claims description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 2
- 239000008158 vegetable oil Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 claims 4
- 239000011347 resin Substances 0.000 claims 3
- 229920005989 resin Polymers 0.000 claims 3
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 239000010409 thin film Substances 0.000 claims 1
- 230000007797 corrosion Effects 0.000 abstract description 9
- 238000005260 corrosion Methods 0.000 abstract description 9
- 239000006223 plastic coating Substances 0.000 abstract description 4
- 238000003860 storage Methods 0.000 abstract description 4
- 239000007858 starting material Substances 0.000 abstract description 2
- 230000002411 adverse Effects 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 abstract 1
- 239000003973 paint Substances 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 208000014674 injury Diseases 0.000 description 2
- 239000004922 lacquer Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 239000011265 semifinished product Substances 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000007688 edging Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000002320 enamel (paints) Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000011089 mechanical engineering Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002436 steel type Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
- B05D1/04—Processes for applying liquids or other fluent materials performed by spraying involving the use of an electrostatic field
- B05D1/06—Applying particulate materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
- B05D1/12—Applying particulate materials
Definitions
- the invention relates to a method for powder coating of metal surfaces according to the preamble of claim 1.
- Such methods are used, for example, for coating metal parts in vehicle construction, in mechanical engineering, in housings for household and other devices, for metal furniture and shelves or for toys.
- the sheet In the manufacture of these metal parts, it is usually assumed that the sheet is wound as a "coil", which is oiled, painted or coated in another way to protect it from corrosion during transport and storage ("coil coating").
- the sheet is unwound from the coil and processed into the desired product by sawing, punching, drilling, folding and edging.
- the oil or paint coating also serves as a lubricant and release agent between the tool and the workpiece (sheet metal).
- an oiled coil is assumed, it is then painted or coated to protect against corrosion and to give the parts the desired color.
- a solvent-based paint is used for wet painting.
- the evaporation of the solvent is usually associated with a significant environmental impact. This can be avoided when using an electrostatic powder coating process.
- Electrostatically charged powder is sprayed onto the surface to be coated, where it adheres due to the electrostatic attraction.
- Suitable powders are, for example, polyester or epoxy resins or a mixture thereof.
- the powder layer is melted to a viscous mass by heating adheres well to the metal and results in a smooth surface.
- the coating hardens on cooling.
- edges of the sawn, punched or drilled metal parts are not coated and are therefore susceptible to rust. There is also a considerable risk of injury when handling these sharp-edged parts.
- An enamel coating method is known from US Pat. No. 4,746,533, in which a ceramic enamel powder is applied to a metal surface provided with an oil film and is then fired at a very high temperature. The oil film evaporates completely at the high firing temperature.
- JP-A-63-227 324 discloses a method for producing a plastic part by means of a shaped body.
- the molded body is first coated with a silicone oil and then with a synthetic resin solution.
- the plastic part is obtained after evaporating the solvent and separating the dried synthetic resin from the molded body, the silicone oil acting as a separating agent.
- the powder coating method according to the invention is based on an oiled metal surface.
- the powder is applied directly to the oil film. There is therefore no need to deoil the metal part to be coated.
- the invention makes it possible to coat iron materials which are provided with an oil film as corrosion protection and as a lubricant in mechanical processing steps. Since removal of the oil film is not necessary, the process is inexpensive to use and environmentally friendly.
- the method according to the invention is suitable both for coating semi-finished products, for example unprocessed flat material or coils, and for coating parts that have already been completely mechanically processed.
- the latter case is preferable if, for reasons of corrosion protection and to avoid a possible risk of injury, no uncoated edges should remain.
- the method can be applied to all metals and steel types and is also suitable for parts of any shape, for example also for profiles or pipes.
- an oil is used according to claim 3, which is stable during the heating process, as long as it remains on the surface. This includes the possibility that individual components or all of the oil diffuse and evaporate during the heating process through the powder layer or that parts or even the entire amount of oil remain on the workpiece during the heating process and mix with the powder layer. If the oil on the workpiece surface in the kiln were unstable and would burn, for example, the color of the plastic coating would be greatly influenced by the oil and in particular by the oil's conversion processes under the influence of temperature. The slightest local temperature fluctuations in the kiln would lead to an uneven structure and color of the surface. This is reliably avoided with an oil that meets the condition specified in claim 3.
- the embodiment according to claim 5 has the advantage that the electrostatically applied powder adheres as completely as possible to the workpiece surface and little powder falls off in the coating booth, which powder has to be recycled for economical powder utilization.
- a surface coating that is particularly uniform both in terms of color and in terms of thickness and structure is achieved if, according to claim 6, the surface density of the oil film is less than approx. 3 g / m 2 , preferably approx. 0.3 to 1.5 g / m 2 , and the plastic coating is at least about 50 microns, preferably about 50 microns up to about 80 microns thick.
- An oil film which remains on the surface of the cured coating according to claim 8 is an excellent lubricating film in further mechanical processing steps. For this purpose enough oil must be applied and the heat supplied by the furnace must be low enough so that there is still oil on the surface Workpiece surface remains.
- test series with which particularly preferred configurations of the method according to the invention were determined are summarized in Tables 1 and 2.
- steel test panels of type R from Q-Panel were oiled, electrostatically coated with powder and passed through a baking oven.
- the coated sample plates were assessed under a microscope with regard to their optical quality and subjected to a cupping test in accordance with DIN ISO 1520 to determine the paint adhesion.
- Table 1 shows the result of the optical assessment the hardened paint layer. The tests were carried out with different oils, which are given with their trade name, the manufacturer, the specification of the base oil and the respective viscosity at 40 ° C. The right five columns of Table 1 refer to different amounts of applied oil, to give areal densities of 0.5 to 2.5 g / m 2 in steps of 0.5 g / m 2 investigated. The table contains the symbol "x" if the oil in question has led to the formation of visible oil islands or oil inclusions in the paint layer. The paint layer then makes a "scarred” impression. An optically perfect surface is marked with the symbol "o".
- Table 1 shows that there is a high optical quality of the coated plate when the surface density of the oil is a maximum of 2.0 g / m 2 and the viscosity of the applied oil at 40 ° C is below 40 mm 2 / s, ie if the oil is very thin.
- a thin-bodied oil has the advantage that it can be applied particularly evenly and also diffuses particularly easily through the powder layer in the stoving oven and volatilizes. This is especially true when the amount applied is very small. With a surface density of 0.5 g / m 2 , optically perfect surfaces result for almost every oil.
- the optical quality of the surface is independent of whether the oil is made from mineral oil or from a vegetable oil, such as rapeseed oil.
- Table 2 shows the results of the cupping test according to DIN ISO 1520, with which the adhesion of the paint layer was measured. During the deepening test, the sample plate is deformed by a stamp and the depth of the deformation at which the lacquer layer breaks is noted. With good paint adhesion, high values are achieved.
- Table 2 lists various oils and the length of time in the stoving oven. The right five columns are arranged as in Table 1 according to the amount of oil applied. The table contains the values of the deformation in mm at which one Cracking occurred. The oven temperature was always 180 ° C. This temperature was reached by the sample plates after a residence time of 14 minutes. The cupping values were measured after a stay of 14, 16 and 18 min. In addition, for comparison, test plates were examined which were completely degreased in a conventional manner before the tests (“unoiled test plates”).
- Table 2 shows that the cupping value is 5.0 mm or more, which corresponds to a particularly good paint adhesion if the amount of oil applied does not exceed a surface density of 1.5 g / m 2 and a sufficient residence time in the oven is set.
- the sufficient residence time was 18 minutes at an oven temperature of 180 ° C.
- the amount of heat supplied to the sample plates under this condition is sufficient to essentially diffuse the oil through the powder layer and to allow it to volatilize.
- the depression value is in the order of the value for unoiled or degreased sheets, ie in the order of 10 mm. This value indicates excellent paint adhesion.
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Paints Or Removers (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Disintegrating Or Milling (AREA)
- Chemically Coating (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren zum Pulverbeschichten von Metalloberflächen nach dem Oberbegriff des Anspruchs 1. Solche Verfahren werden beispielsweise zum Beschichten von Metallteilen im Fahrzeugbau, im Maschinenbau, bei Gehäusen für Haushalts- und andere Geräte, für Metallmöbel und -regale oder auch für Spielzeug eingesetzt.The invention relates to a method for powder coating of metal surfaces according to the preamble of claim 1. Such methods are used, for example, for coating metal parts in vehicle construction, in mechanical engineering, in housings for household and other devices, for metal furniture and shelves or for toys.
Bei der Herstellung dieser Metallteile wird meist von einem als "Coil" gewickelten Blech ausgegangen, das zum Schutz vor Korrosion während Transport und Lagerung geölt, lackiert oder auf andere Weise beschichtet ist ("coil coating"). Das Blech wird vom Coil abgespult und durch Sägen, Stanzen, Bohren, Falzen und Kanten zu dem gewünschten Produkt verarbeitet. Dabei dient die Öl- oder Lackbeschichtung auch als Gleit- und Trennmittel zwischen Werkzeug und Werkstück (Blech).In the manufacture of these metal parts, it is usually assumed that the sheet is wound as a "coil", which is oiled, painted or coated in another way to protect it from corrosion during transport and storage ("coil coating"). The sheet is unwound from the coil and processed into the desired product by sawing, punching, drilling, folding and edging. The oil or paint coating also serves as a lubricant and release agent between the tool and the workpiece (sheet metal).
Wenn von einem geölten Coil ausgegangen wird, so erfolgt abschließend noch ein Lackieren oder Beschichten zum Schutz vor Korrosion und um den Teilen die gewünschte Farbe zu geben. Beim Naß-Lackieren wird dazu eine lösungsmittelhaltige Farbe verwendet. Mit der Verdunstung des Lösungsmittels ist jedoch meist eine erhebliche Umweltbelastung verbunden. Diese kann bei der Anwendung eines elektrostatischen Pulverbeschichtungsverfahrens vermieden werden.If an oiled coil is assumed, it is then painted or coated to protect against corrosion and to give the parts the desired color. For wet painting, a solvent-based paint is used. However, the evaporation of the solvent is usually associated with a significant environmental impact. This can be avoided when using an electrostatic powder coating process.
Ein solches Verfahren ist in DE-A-38 38 928 beschrieben. Dabei wird elektrostatisch aufgeladenes Pulver auf die zu beschichtende Fläche aufgesprüht, wo es aufgrund der elektrostatischen Anziehungskräfte haften bleibt. Als Pulver eignen sich beispielsweise Polyester oder Epoxidharze oder auch eine Mischung daraus. Die Pulverschicht wird durch Erhitzen zu einer viskosen Masse verschmolzen, die auf dem Metall gut haftet und eine glatte Oberfläche ergibt. Beim Abkühlen härtet die Beschichtung aus.Such a method is described in DE-A-38 38 928. Electrostatically charged powder is sprayed onto the surface to be coated, where it adheres due to the electrostatic attraction. Suitable powders are, for example, polyester or epoxy resins or a mixture thereof. The powder layer is melted to a viscous mass by heating adheres well to the metal and results in a smooth surface. The coating hardens on cooling.
Um eine einwandfreie Oberfläche zu erhalten, ist bei dem konventionellen Verfahren ein vorhergehendes Entölen der Metallteile für unerläßlich gehalten worden. Dazu sind jedoch Wasch- und Lösungsmittel notwendig, die ebenfalls eine Umweltbelastung darstellen. Außerdem ist dieser Arbeitsschritt mit erheblichen Kosten verbunden. Sie entstehen nicht nur durch die erforderliche Anlage, sondern insbesondere auch durch die Heizenergie, die notwendig ist, um die mit Lösungs- oder Waschmittel benetzten Metallteile zu trocknen. Ohne eine solche Trocknung wäre eine hohe Produktionsleistung jedoch nicht möglich.In order to obtain a perfect surface, prior de-oiling of the metal parts was considered essential in the conventional process. However, this requires washing agents and solvents, which are also environmentally harmful. This step is also associated with considerable costs. They arise not only from the required system, but in particular also from the heating energy that is required to dry the metal parts wetted with solvent or detergent. Without such drying, high production output would not be possible.
Diese Probleme werden bei der Verwendung eines lackierten bzw. beschichteten statt eines geölten Coils vermieden. Damit sind jedoch andere erhebliche Nachteile verbunden. So lassen sich beispielsweise nur mit großem Lageraufwand Produkte in einer großen Zahl verschiedener Farben herstellen. Ein Wechsel der Farbe erfordert immer auch den aufwendigen Wechsel eines Coils an der Produktionsstraße. Andererseits fällt eine Farbe an verschiedenen Coils oft unterschiedlich aus, insbesondere, wenn diese von verschiedenen Zulieferern bezogen wurden.These problems are avoided when using a painted or coated coil instead of an oiled coil. However, there are other significant disadvantages. For example, products can only be manufactured in a large number of different colors with a large amount of storage. Changing the color always requires the complex change of a coil on the production line. On the other hand, a color on different coils often turns out to be different, especially if they have been obtained from different suppliers.
Weiterhin sind bei Verwendung vorlackierter oder vorbeschichteter Bleche die Kanten der gesägten, gestanzten oder gebohrten Metallteile nicht beschichtet und damit anfällig gegen Rost. Außerdem besteht bei der Handhabung dieser scharfkantigen Teile eine erhebliche Verletzungsgefahr.Furthermore, when using pre-painted or pre-coated metal sheets, the edges of the sawn, punched or drilled metal parts are not coated and are therefore susceptible to rust. There is also a considerable risk of injury when handling these sharp-edged parts.
Diese Nachteile können vermieden werden, wenn wie oben beschrieben ein geölter Coil verwendet wird und eine Beschichtung erst nach den mechanischen Verarbeitungsschritten erfolgt. Die elektrostatische Pulverbeschichtung ist dabei besonders vorteilhaft, da die elektrischen Feldlinien so gerichtet werden können, daß sich an den Kanten des Werkstücks besonders viel Pulver anlagert. Die nach dem Aushärten entstehende Kunststoffbeschichtung ist daher dort besonders dick und führt zu abgerundeten Ecken und Kanten. Als wesentlicher Nachteil teil dieses Verfahrens verbleiben jedoch wie erwähnt die mit dem Entölen verbundenen Kosten- und Umweltprobleme.These disadvantages can be avoided if, as described above, an oiled coil is used and a coating is only carried out after the mechanical processing steps. The electrostatic powder coating is particularly advantageous because the electric field lines can be directed so that a particularly large amount of powder is deposited on the edges of the workpiece. The plastic coating created after curing is therefore particularly thick there and leads to rounded corners and edges. As a major disadvantage However, as mentioned, part of this process remains the cost and environmental problems associated with de-oiling.
Aus US-4 746 533 ist ein Emaille-Beschichtungsverfahren bekannt, bei dem ein keramisches Emaille-Pulver auf eine mit einem Ölfilm versehene Metalloberfläche aufgebracht und dann bei sehr hoher Temperatur gebrannt wird. Bei der hohen Brenntemperatur verflüchtigt sich der Ölfilm vollständig.An enamel coating method is known from US Pat. No. 4,746,533, in which a ceramic enamel powder is applied to a metal surface provided with an oil film and is then fired at a very high temperature. The oil film evaporates completely at the high firing temperature.
JP-A-63-227 324 offenbart ein Verfahren zur Herstellung eines Kunststoffteils mittels eines Formkörpers. Dabei wird der Formkörper zunächst mit einem Silikonöl und dann mit einer Kunstharz-Lösung beschichtet. Das Kunststoffteil wird nach Verdampfen des Lösungsmittels und Trennen des getrockneten Kunstharzes von dem Formkörper gewonnen, wobei das Silikonöl als Trennmittel wirkt.JP-A-63-227 324 discloses a method for producing a plastic part by means of a shaped body. The molded body is first coated with a silicone oil and then with a synthetic resin solution. The plastic part is obtained after evaporating the solvent and separating the dried synthetic resin from the molded body, the silicone oil acting as a separating agent.
Es ist die Aufgabe der Erfindung, ein Pulverbeschichtungsverfahren anzugeben, das eine umweltschonende und preisgünstige Massenfertigung erlaubt. Dabei soll ein Rostschutz des Ausgangsmaterials beibehalten werden, die Farbe exakt wiederholbar, aber ein einfacher Farbwechsel möglich sein.It is the object of the invention to provide a powder coating process which allows environmentally friendly and inexpensive mass production. A rust protection of the starting material should be maintained, the color can be exactly repeated, but a simple color change should be possible.
Diese Aufgabe wird mit der in Anspruch 1 gekennzeichneten Erfindung gelöst.This object is achieved with the invention characterized in claim 1.
Das erfindungsgemäße Pulverbeschichtungsverfahren geht von einer geölten Metalloberfläche aus. Das Pulver wird direkt auf den Ölfilm aufgebracht. Ein Entölen des zu beschichtenden Metallteils entfällt daher.The powder coating method according to the invention is based on an oiled metal surface. The powder is applied directly to the oil film. There is therefore no need to deoil the metal part to be coated.
Die Erfindung ermöglicht es, Eisenwerkstoffe zu beschichten, die mit einem Ölfilm als Korrosionsschutz und als Gleitmittel bei mechanischen Verarbeitungsschritten versehen sind. Da eine Entfernung des Ölfilms nicht notwendig ist, ist das Verfahren preiswert anzuwenden und umweltschonend.The invention makes it possible to coat iron materials which are provided with an oil film as corrosion protection and as a lubricant in mechanical processing steps. Since removal of the oil film is not necessary, the process is inexpensive to use and environmentally friendly.
Das erfindungsgemäße Verfahren eignet sich sowohl zur Beschichtung von Halbzeugen, beispielsweise unbearbeitetem Flachmaterial oder Coils, als auch zur Beschichtung von Teilen, die schon vollständig mechanisch bearbeitet sind. Der letzte Fall ist vorzuziehen, wenn aus Gründen des Korrosionsschutzes und um eine mögliche Verletzungsgefahr zu vermeiden, keine unbeschichteten Kanten zurückbleiben sollen.The method according to the invention is suitable both for coating semi-finished products, for example unprocessed flat material or coils, and for coating parts that have already been completely mechanically processed. The latter case is preferable if, for reasons of corrosion protection and to avoid a possible risk of injury, no uncoated edges should remain.
Außerdem kann das Verfahren bei allen Metallen und Stahlsorten angewendet werden und eignet sich ferner für Teile jeglicher Form, beispielsweise auch für Profile oder Rohre.In addition, the method can be applied to all metals and steel types and is also suitable for parts of any shape, for example also for profiles or pipes.
Vorteilhafte Ausgestaltungen der Erfindung sind in den Unteransprüchen angegeben.Advantageous embodiments of the invention are specified in the subclaims.
Wird beim Heizvorgang wie in Anspruch 2 angegeben so viel Wärme zugeführt, daß das Öl durch die Pulverschicht diffundiert und verdampft, so wird ein Einfluß des Öls auf die Qualität beschichteten Oberfläche der Metallteile vermieden. Die notwendige Wärmemenge (Temperatur und Dauer des Heizvorgangs) ist umso größer, je mehr Öl auf die Metalloberfläche aufgetragen wurde und je schwerer flüchtig das Öl ist. Das verdampfte Öl in der Abluft des Ofens kann verbrannt werden, wobei die entstehende Wärme zusätzlich zur Ofenheizung verwendet wird.If so much heat is supplied during the heating process as stated in claim 2 that the oil diffuses and evaporates through the powder layer, an influence of the oil on the quality of the coated surface of the metal parts is avoided. The amount of heat required (temperature and duration of the heating process) The greater the oil that has been applied to the metal surface and the less volatile the oil, the greater it is. The evaporated oil in the exhaust air from the furnace can be burned, using the heat generated in addition to heating the furnace.
Um eine einwandfreie Oberfläche zu erhalten, wird nach Anspruch 3 ein Öl verwendet, das während des Heizvorgangs stabil bzw. beständig ist, solange es auf der Oberfläche verbleibt. Dies schließt die Möglichkeit ein, daß einzelne Komponenten oder das gesamte Öl während des Aufheizvorgangs durch die Pulverschicht diffundieren und verdampfen oder daß Teile oder auch die gesamte Ölmenge während des Heizvorgangs auf dem Werkstück verbleiben und sich mit der Pulverschicht mischen. Wäre das Öl auf der Werkstückoberfläche im Brennofen instabil und würde es beispielsweise verbrennen, so würde die Farbe der Kunststoffbeschichtung stark vom Öl und insbesondere von den Umwandlungsprozessen des Öls unter Temperatureinwirkung beeinflußt. Geringste lokale Temperaturschwankungen im Brennofen würden zu einer ungleichmäßigen Struktur und Farbe der Oberfläche führen. Dies wird mit einem Öl, das die in Anspruch 3 angegebene Bedingung erfüllt, zuverlässig vermieden.In order to obtain a perfect surface, an oil is used according to claim 3, which is stable during the heating process, as long as it remains on the surface. This includes the possibility that individual components or all of the oil diffuse and evaporate during the heating process through the powder layer or that parts or even the entire amount of oil remain on the workpiece during the heating process and mix with the powder layer. If the oil on the workpiece surface in the kiln were unstable and would burn, for example, the color of the plastic coating would be greatly influenced by the oil and in particular by the oil's conversion processes under the influence of temperature. The slightest local temperature fluctuations in the kiln would lead to an uneven structure and color of the surface. This is reliably avoided with an oil that meets the condition specified in claim 3.
Verfärbt sich das Öl gemäß Anspruch 4 während des Heizvorgangs nicht, so haben geringe unvermeidbare Schwankungen der Temperatur und der Dauer des Heizvorgangs keinen Einfluß auf die Farbe des Produkts.If the oil does not change color during the heating process, slight inevitable fluctuations in the temperature and the duration of the heating process have no influence on the color of the product.
Die Ausgestaltung nach Anspruch 5 hat den Vorteil, daß das elektrostatisch aufgetragene Pulver möglichst vollständig auf der Werkstückoberfläche haften bleibt und in der Beschichtungskabine wenig Pulver abfällt, das zur wirtschaftlichen Pulverausnutzung rückgeführt werden muß.The embodiment according to claim 5 has the advantage that the electrostatically applied powder adheres as completely as possible to the workpiece surface and little powder falls off in the coating booth, which powder has to be recycled for economical powder utilization.
Eine sowohl farblich als auch bezüglich Dicke und Struktur besonders gleichmäßige Oberflächenbeschichtung wird erzielt, wenn gemäß Anspruch 6 die Flächendichte des Ölfilms kleiner als ca. 3 g/m2, vorzugsweise ca. 0,3 bis 1,5 g/m2, beträgt und die Kunststoffbeschichtung mindestens ca. 50 µm, vorzugsweise ca. 50µm bis hinauf zu ca. 80µm, dick ist. Diese Werte ergeben auch einen ausgezeichneten Korrosionsschutz bei Lagerung und Transport des Halbzeugs und garantieren bei der mechanischen Verarbeitung ausreichende Gleit- und Trenneigenschaften. Sie stellen auf diese Weise sicher, daß Werkzeug und Werkstück geschont werden.A surface coating that is particularly uniform both in terms of color and in terms of thickness and structure is achieved if, according to claim 6, the surface density of the oil film is less than approx. 3 g / m 2 , preferably approx. 0.3 to 1.5 g / m 2 , and the plastic coating is at least about 50 microns, preferably about 50 microns up to about 80 microns thick. These values also result in excellent corrosion protection Storage and transport of the semi-finished product and guarantee sufficient sliding and separating properties during mechanical processing. In this way you ensure that the tool and workpiece are protected.
Bei der Ausgestaltung nach Anspruch 7 ergibt sich ein besonders wirksamer Korrosionsschutz und es wird verhindert, daß Rost unter die Pulverbeschichtung kriechen kann. Bei konventionellen Pulverbeschichtungsverfahren, bei denen die Ölschicht entfernt wird, geschieht dies mit phosphathaltigen und/oder alkalischen Waschmitteln. Dadurch verbleibt nach dem Trocknen auf der Werkstückoberfläche eine Phosphatschicht, die einen ausgezeichneten Korrosionsschutz darstellt. Um auch bei der vorliegenden Erfindung die Korrosionsschutzeigenschaften eines Phosphatfilms zu nutzen, wird gemäß Anspruch 7 eine solche Schicht zusätzlich vor, nach oder zusammen mit dem Öl, jedoch vor dem Pulverbeschichten, aufgebracht.In the embodiment according to claim 7 there is a particularly effective corrosion protection and it is prevented that rust can crawl under the powder coating. In conventional powder coating processes, in which the oil layer is removed, this is done with phosphate-containing and / or alkaline detergents. This leaves a phosphate layer on the workpiece surface after drying, which provides excellent corrosion protection. In order to also use the corrosion protection properties of a phosphate film in the present invention, such a layer is additionally applied according to claim 7 before, after or together with the oil, but before powder coating.
Ein Ölfilm, der gemäß Anspruch 8 auf der Oberfläche der ausgehärteten Beschichtung zurückbleibt, stellt einen ausgezeichneten Gleitfilm bei weiteren mechanischen Verarbeitungsschritten dar. Zu diesem Zweck muß genug Öl aufgetragen werden, und die vom Ofen zugeführte Wärme muß niedrig genug sein, damit noch Öl auf der Werkstückoberfläche zurückbleibt.An oil film which remains on the surface of the cured coating according to claim 8 is an excellent lubricating film in further mechanical processing steps. For this purpose enough oil must be applied and the heat supplied by the furnace must be low enough so that there is still oil on the surface Workpiece surface remains.
Die Ergebnisse von Versuchsreihen, mit denen besonders bevorzugte Ausgestaltungen des erfindungsgemäßen Verfahrens ermittelt wurden, sind in den Tabellen 1 und 2 zusammengefaßt. Bei den Versuchsreihen wurden Stahl-Probeplatten des Typs R der Firma Q-Panel beölt, elektrostatisch mit Pulver beschichtet und durch einen Einbrennofen geführt. Die beschichteten Probeplatten wurden unter einem Mikroskop hinsichtlich ihrer optischen Qualität beurteilt und zur Ermittlung der Lackhaftung einer Tiefungsprüfung nach DIN ISO 1520 unterworfen.The results of test series with which particularly preferred configurations of the method according to the invention were determined are summarized in Tables 1 and 2. In the test series, steel test panels of type R from Q-Panel were oiled, electrostatically coated with powder and passed through a baking oven. The coated sample plates were assessed under a microscope with regard to their optical quality and subjected to a cupping test in accordance with DIN ISO 1520 to determine the paint adhesion.
Bei allen Versuchen wurde ein Pulver aus einer Polyester-Epoxidharz-Mischung verwendet, das so aufgetragen wurde, daß die Lackschicht nach dem Aushärten eine Dicke von etwa 70 bis 80 µm hatte.In all experiments, a powder made of a polyester-epoxy resin mixture was used, which was applied so that the lacquer layer had a thickness of about 70 to 80 microns after curing.
Tabelle 1 stellt das Ergebnis der optischen Beurteilung der gehärteten Lackschicht dar. Die Versuche wurden mit verschiedenen Ölen durchgeführt, die mit ihrer Handelsbezeichnung, dem Hersteller, der Angabe des Basisöls und der jeweiligen Viskosität bei 40°C angegeben sind. Die rechten fünf Spalten der Tabelle 1 beziehen sich auf unterschiedliche aufgetragene Ölmengen, wobei Flächendichten von 0,5 bis 2,5 g/m2 in Schritten von 0,5 g/m2 untersucht wurden. Die Tabelle enthält das Symbol "x", wenn das jeweilige Öl bei der angegebenen Ölmenge zur Bildung von sichtbaren Ölinseln bzw. Öleinschlüssen in der Lackschicht geführt hat. Die Lackschicht macht dann einen "vernarbten" Eindruck. Eine optisch einwandfreie Oberfläche ist mit dem Symbol "o" gekennzeichnet.Table 1 shows the result of the optical assessment the hardened paint layer. The tests were carried out with different oils, which are given with their trade name, the manufacturer, the specification of the base oil and the respective viscosity at 40 ° C. The right five columns of Table 1 refer to different amounts of applied oil, to give areal densities of 0.5 to 2.5 g / m 2 in steps of 0.5 g / m 2 investigated. The table contains the symbol "x" if the oil in question has led to the formation of visible oil islands or oil inclusions in the paint layer. The paint layer then makes a "scarred" impression. An optically perfect surface is marked with the symbol "o".
Tabelle 1 zeigt, daß sich eine hohe optische Qualität der lackierten Platte dann ergibt, wenn die Flächendichte des Öls maximal 2,0 g/m2 beträgt und die Viskosität des aufgetragenen Öls bei 40°C unter 40 mm2/s liegt, d.h. wenn das Öl sehr dünnflüssig ist. Ein dünnflüssiges Öl hat den Vorteil, daß es sich besonders gleichmäßig auftragen läßt und ferner im Einbrennofen besonders leicht durch die Pulverschicht diffundiert und sich verflüchtigt. Dies gilt insbesondere, wenn die aufgetragene Menge sehr gering ist. Bei einer Flächendichte von 0,5 g/m2 ergeben sich für nahezu jedes Öl optisch einwandfreie Oberflächen.Table 1 shows that there is a high optical quality of the coated plate when the surface density of the oil is a maximum of 2.0 g / m 2 and the viscosity of the applied oil at 40 ° C is below 40 mm 2 / s, ie if the oil is very thin. A thin-bodied oil has the advantage that it can be applied particularly evenly and also diffuses particularly easily through the powder layer in the stoving oven and volatilizes. This is especially true when the amount applied is very small. With a surface density of 0.5 g / m 2 , optically perfect surfaces result for almost every oil.
Die optische Qualität der Oberfläche ist unabhängig davon, ob das Öl auf Mineralölbasis oder auf Basis eines Pflanzlichen Öls, beispielsweise eines Rapsöls, hergestellt wurde.The optical quality of the surface is independent of whether the oil is made from mineral oil or from a vegetable oil, such as rapeseed oil.
Tabelle 2 zeigt die Ergebnisse der Tiefungsprüfung nach DIN ISO 1520, mit der die Haftung der Lackschicht gemessen wurde. Bei der Tiefungsprüfung wird die Probeplatte durch einen Stempel deformiert und die Tiefe der Deformation, bei der die Lackschicht reißt, notiert. Bei guter Lackhaftung werden hohe Werte erreicht.Table 2 shows the results of the cupping test according to DIN ISO 1520, with which the adhesion of the paint layer was measured. During the deepening test, the sample plate is deformed by a stamp and the depth of the deformation at which the lacquer layer breaks is noted. With good paint adhesion, high values are achieved.
In Tabelle 2 sind verschiedene Öle und die Verweildauer im Einbrennofen aufgeführt. Die rechten fünf Spalten sind wie in Tabelle 1 nach der aufgetragenen Ölmenge geordnet. Die Tabelle enthält die Werte der Deformation in mm, bei denen eine Rißbildung auftrat. Die Ofentemperatur betrug stets 180°C. Diese Temperatur wurde von den Probeplatten nach einer Verweilzeit von 14 min erreicht. Die Tiefungswerte wurden jeweils nach einer Verweildauer von 14, 16 und 18 min gemessen. Außerdem wurden zum Vergleich Probeplatten untersucht, die vor den Versuchen auf konventionelle Weise vollständig entfettet wurden ("unbeölte Probeplatten").Table 2 lists various oils and the length of time in the stoving oven. The right five columns are arranged as in Table 1 according to the amount of oil applied. The table contains the values of the deformation in mm at which one Cracking occurred. The oven temperature was always 180 ° C. This temperature was reached by the sample plates after a residence time of 14 minutes. The cupping values were measured after a stay of 14, 16 and 18 min. In addition, for comparison, test plates were examined which were completely degreased in a conventional manner before the tests (“unoiled test plates”).
Tabelle 2 zeigt, daß der Tiefungswert bei 5,0 mm oder darüber liegt, was einer besonders guten Lackhaftung entspricht, wenn die aufgetragene Ölmenge eine Flächendichte von 1,5 g/m2 nicht überschreitet und eine ausreichende Verweildauer im Ofen eingestellt wird.Table 2 shows that the cupping value is 5.0 mm or more, which corresponds to a particularly good paint adhesion if the amount of oil applied does not exceed a surface density of 1.5 g / m 2 and a sufficient residence time in the oven is set.
Im vorliegenden Fall betrug bei einer Ofentemperatur von 180°C die ausreichende Verweildauer 18 min. Die den Probeplatten unter dieser Bedingung zugeführte Wärmemenge reicht aus, um das Öl im wesentlichen durch die Pulverschicht difundieren und sich verflüchtigen zu lassen.In the present case, the sufficient residence time was 18 minutes at an oven temperature of 180 ° C. The amount of heat supplied to the sample plates under this condition is sufficient to essentially diffuse the oil through the powder layer and to allow it to volatilize.
Bei einer aufgetragenen Flächendichte des Öls von 0,5 g/m2 und der oben angegebenen Wärmemenge liegt der Tiefungswert in der Größenordnung des Wertes für unbeölte oder entfettete Bleche, d.h. in der Größenordnung von 10 mm. Dieser Wert zeigt eine hervorragende Lackhaftung an.
Claims (8)
- A method for durably powder coating a metallic surface which has been provided with an oil film, comprising the steps of:applying a resin powder layer,melting said powder layer by heating andhardening and cooling the melted layer,characterised in that
said powder layer is applied directly onto said oil film which consists of an oil on the basis of mineral oil or vegetable oil. - A method according to claim 1, characterised in that such an amount of heat is applied during said heating that the oil diffuses substantially through the powder layer and evaporates.
- A method according to claim 1 or 2, characterised in that an oil is used which is stable during said heating as far as it remains on the metal surface.
- A method according to any of claims 1 to 3, characterised in that an oil is used which is chemically stable so that it does not cause a change of the colour of the powder layer during said heating.
- A method according to any of claims 1 to 4, characterised in that the applied oil film is so thin that the adhesion of the electrostatically applied powder layer is not deteriorated.
- A method according to any of claims 1 to 5, characterised in that the surface density of the oil film is less than about 3 g/m2 and is preferably about 0.3 to 1.5 g/m2, and that the thickness of the resin layer formed by said hardening is at least about 40 µm and is preferably about 50 to 80 µm.
- A method according to any of claims 1 to 6, characterised in that an alkaline and/or phosphate layer is applied prior to said powder coating.
- A method according to any of claims 1 to 7, characterised in that a residue of said oil forms a thin film on the hardened resin surface.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19904029985 DE4029985A1 (en) | 1990-09-21 | 1990-09-21 | METHOD FOR POWDER COATING METAL SURFACES |
DE4029985 | 1990-09-21 |
Publications (3)
Publication Number | Publication Date |
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EP0476539A2 EP0476539A2 (en) | 1992-03-25 |
EP0476539A3 EP0476539A3 (en) | 1994-07-13 |
EP0476539B1 true EP0476539B1 (en) | 1996-10-09 |
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EP19910115563 Expired - Lifetime EP0476539B1 (en) | 1990-09-21 | 1991-09-13 | Process for applying powder coatings to metallic surfaces |
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US (1) | US5264254A (en) |
EP (1) | EP0476539B1 (en) |
JP (1) | JP2851728B2 (en) |
KR (1) | KR100221771B1 (en) |
AT (1) | ATE143837T1 (en) |
AU (1) | AU639138B2 (en) |
BR (1) | BR9104047A (en) |
CA (1) | CA2051879C (en) |
CZ (1) | CZ283154B6 (en) |
DE (2) | DE4029985A1 (en) |
DK (1) | DK0476539T3 (en) |
ES (1) | ES2093665T3 (en) |
GR (1) | GR3021870T3 (en) |
RU (1) | RU2004385C1 (en) |
SK (1) | SK279241B6 (en) |
ZA (1) | ZA917425B (en) |
Cited By (1)
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CN105457874A (en) * | 2015-12-10 | 2016-04-06 | 太仓贝斯特机械设备有限公司 | Electrostatic powder spraying method of aluminum material building door and window |
Families Citing this family (5)
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US5731042A (en) * | 1995-11-07 | 1998-03-24 | Glende; James A. | Protectively coated outdoor fixtures |
US6020034A (en) * | 1997-11-14 | 2000-02-01 | E. I. Du Pont De Nemours And Company | Process for producing corrosion- and creep resistant coatings |
US6676820B2 (en) * | 2001-03-02 | 2004-01-13 | Ppg Industries Ohio, Inc. | Process for electrocoating metal blanks and coiled metal substrates |
DE102004062454A1 (en) | 2004-12-20 | 2006-06-29 | Basf Ag | Process for coating metals |
KR101481316B1 (en) | 2013-09-05 | 2015-01-09 | 현대자동차주식회사 | A powder pigment composition of unification type and its preparing method |
Citations (1)
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JPS63227324A (en) * | 1987-03-16 | 1988-09-21 | Daikin Ind Ltd | Preparation of cover for enclosed packing |
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US2809906A (en) * | 1952-11-25 | 1957-10-15 | Wyandotte Chemicals Corp | Phosphating compositions |
GB1357214A (en) * | 1971-06-29 | 1974-06-19 | British Steel Corp | Method and apparatus for coating a metallic strip |
JPS5517268B2 (en) * | 1972-06-01 | 1980-05-10 | ||
US3794759A (en) * | 1972-12-26 | 1974-02-26 | Ibm | Multi-terminal communication apparatus controller |
DE2924111C2 (en) * | 1979-06-15 | 1986-07-17 | SMW Schneider & Weißhaupt GmbH, 7996 Meckenbeuren | Device for monitoring the pressure in pressurized fluid-operated chucks with clamping cylinders rotating during operation on processing machines |
DE3109713A1 (en) * | 1981-03-13 | 1982-10-21 | Resicoat Gmbh Beschichtungspulver, 7410 Reutlingen | COMPOSITE COATING AND METHOD FOR PRODUCING THE SAME |
JPS592742A (en) * | 1982-06-25 | 1984-01-09 | 藤沢薬品工業株式会社 | Vial gasket |
NZ208332A (en) * | 1983-08-02 | 1986-11-12 | American Can Co | Internally-coated deep-drawn metal container |
US4746533A (en) * | 1986-12-19 | 1988-05-24 | Mobay Corporation | Process for coating a metallic surface with a vitreous enamel |
DE3800835A1 (en) * | 1988-01-14 | 1989-07-27 | Henkel Kgaa | METHOD FOR PHOSPHATING METAL SURFACES |
DE3838928A1 (en) * | 1988-11-17 | 1990-05-23 | Columbus System Patent Ag | METHOD FOR COATING SHEET-SHAPED TAPE SHEETS WITH POWDER LACQUER AND DEVICE FOR CARRYING OUT THE METHOD |
-
1990
- 1990-09-21 DE DE19904029985 patent/DE4029985A1/en not_active Withdrawn
-
1991
- 1991-09-13 AT AT91115563T patent/ATE143837T1/en not_active IP Right Cessation
- 1991-09-13 DE DE59108255T patent/DE59108255D1/en not_active Expired - Lifetime
- 1991-09-13 DK DK91115563T patent/DK0476539T3/da active
- 1991-09-13 ES ES91115563T patent/ES2093665T3/en not_active Expired - Lifetime
- 1991-09-13 EP EP19910115563 patent/EP0476539B1/en not_active Expired - Lifetime
- 1991-09-17 AU AU84552/91A patent/AU639138B2/en not_active Ceased
- 1991-09-18 ZA ZA917425A patent/ZA917425B/en unknown
- 1991-09-19 CA CA 2051879 patent/CA2051879C/en not_active Expired - Fee Related
- 1991-09-19 JP JP23997391A patent/JP2851728B2/en not_active Expired - Lifetime
- 1991-09-20 KR KR1019910016555A patent/KR100221771B1/en not_active IP Right Cessation
- 1991-09-20 BR BR9104047A patent/BR9104047A/en not_active IP Right Cessation
- 1991-09-20 CZ CS912870A patent/CZ283154B6/en not_active IP Right Cessation
- 1991-09-20 SK SK2870-91A patent/SK279241B6/en unknown
- 1991-09-20 RU SU915001640A patent/RU2004385C1/en not_active IP Right Cessation
- 1991-09-23 US US07/763,467 patent/US5264254A/en not_active Expired - Fee Related
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1996
- 1996-12-04 GR GR960403281T patent/GR3021870T3/en unknown
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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JPS63227324A (en) * | 1987-03-16 | 1988-09-21 | Daikin Ind Ltd | Preparation of cover for enclosed packing |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105457874A (en) * | 2015-12-10 | 2016-04-06 | 太仓贝斯特机械设备有限公司 | Electrostatic powder spraying method of aluminum material building door and window |
CN105457874B (en) * | 2015-12-10 | 2018-05-11 | 太仓贝斯特机械设备有限公司 | The electrostatic powder spraying method of aluminium building doors and windows |
Also Published As
Publication number | Publication date |
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ATE143837T1 (en) | 1996-10-15 |
SK279241B6 (en) | 1998-08-05 |
JP2851728B2 (en) | 1999-01-27 |
CA2051879A1 (en) | 1992-03-22 |
DK0476539T3 (en) | 1997-03-17 |
KR100221771B1 (en) | 1999-09-15 |
AU639138B2 (en) | 1993-07-15 |
ES2093665T3 (en) | 1997-01-01 |
BR9104047A (en) | 1992-06-02 |
CA2051879C (en) | 2000-08-22 |
EP0476539A2 (en) | 1992-03-25 |
US5264254A (en) | 1993-11-23 |
EP0476539A3 (en) | 1994-07-13 |
CZ283154B6 (en) | 1998-01-14 |
DE4029985A1 (en) | 1992-03-26 |
DE59108255D1 (en) | 1996-11-14 |
KR920006530A (en) | 1992-04-27 |
RU2004385C1 (en) | 1993-12-15 |
JPH06339663A (en) | 1994-12-13 |
AU8455291A (en) | 1992-03-26 |
GR3021870T3 (en) | 1997-03-31 |
CS287091A3 (en) | 1992-04-15 |
ZA917425B (en) | 1992-05-27 |
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