EP0977909B1 - Thin, fine pored metal layer - Google Patents
Thin, fine pored metal layer Download PDFInfo
- Publication number
- EP0977909B1 EP0977909B1 EP98916815A EP98916815A EP0977909B1 EP 0977909 B1 EP0977909 B1 EP 0977909B1 EP 98916815 A EP98916815 A EP 98916815A EP 98916815 A EP98916815 A EP 98916815A EP 0977909 B1 EP0977909 B1 EP 0977909B1
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- Prior art keywords
- layer
- suspension
- metal layer
- thickness
- metal
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- 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.)
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
- B22F5/106—Tube or ring forms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/002—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Definitions
- the invention relates to an open metal layer Porosity.
- Porous metal layers consisting of fabric and nonwoven are known of the type mentioned, in particular can be used as a filter.
- a metallic fleece If a metallic fleece is used, it can small pore sizes in the micrometer range can be achieved. Then the fleece thickness is at least one half a millimeter. The layer thicknesses of the aforementioned Furthermore, nonwovens cannot be manufactured very precisely. Relatively large tolerances have to be accepted become.
- Ceramics and plastics used as filter materials are also relatively thick, however, and it occurs a correspondingly large flow resistance. Also ductility is not guaranteed. For many purposes further represents the brittleness of the ceramic Material is a disadvantage.
- plastic is used as filter material, so are no increased operating temperatures possible.
- Plastic is not a suitable filter material for application purposes because it does not meet the requirements can be sterilized, e.g. B. in medical or required in the food sector are. The filter can be used again Cases not possible.
- EP 570 889 67 describes a process for the production a porous layer on a metal surface, where a mixture of binder, metallic Powder and brazing filler made of metal powder with specific grain size as a suspension on the metal surface is applied. This will then heated and sintered.
- DE-A 2 323 878 describes a method for coating described a metal substance. This will start with a binder solution with volatile and low volatility Components applied to the metal substrate. Subsequently we applied metal powder to this layer. First, the volatile components evaporated. Then, by heating too the volatile components evaporate. Another Heating leads to the formation of one with the metal substrate connected porous metal layer.
- a method is also known from FR-A 2 520 265 for the production of a particle-bound heat pipe wick on inner walls of a heat pipe.
- the particles e.g. B. +325 stainless steel microspheres up to -100 mesh (44 - 149 ⁇ m) in a suitable diameter Binder solution suspended and on the heat pipe wall painted.
- the binder is at 400 ° C evaporated under reduced pressure.
- the green layer thus obtained is at 1250 ⁇ 50 ° C for Sintered for 2 hours.
- the object of the invention is to produce a temperature-resistant, sterilizable, simple and reproducible metal layer to be produced with continuous Porosity that is ductile, mechanically stable and elastic is and at - if they are used as a filter will occur - low flow pressure losses. Microfiltration tasks with the metal layer are also intended can be perceived.
- the object of the invention is achieved by a maximum 500 ⁇ m thick metal layer, in other words through solved a metal foil that has an effective pore diameter has up to a twelfth, preferably up to a fifteenth of the layer thickness of the Metal layer.
- the channels are here as pores to understand who is going through the layer Create open porosity. Occasional "cavities" due to inhomogeneities there are no pores in the The meaning of the claim.
- the layer thickness one according to the invention from particles or from powder produced porous layer at least three times is larger than the average particle diameter.
- the effective Pore diameter in particular up to a quarter, preferably up to a fifth of the average particle or powder grain diameter of the used Powder.
- the effective size of the pores is the cause continuous (open) porosity, up to 500/12 mm, i.e. up to approx. 40 ⁇ m. Expressed differently this means that substances smaller than approx. 40 ⁇ m to be able to pass through the metal layer.
- the layer thickness should at least three times as thick as the powder diameter, So be at least 150 ⁇ m to inhomogeneities cavity problems due to the material are reliable to avoid.
- the effective pore diameter of the The layer is then regularly up to 50/4 ⁇ m (3 * 50/12 ⁇ m), preferably up to 50/5 ⁇ m (3 * 50/15 ⁇ m).
- the layer thickness of the metal foil maximum 100 ⁇ m, preferably not more than 50 ⁇ m.
- the effective pore size in the aforementioned sense is maximum in all cases 1/12 of the layer thickness.
- the metal allows elevated temperatures, behaves ductile, mechanically stable and elastic. About that the material can also be easily sterilized.
- the Layer thickness of the layer or film can be compared to a fleece or a fabric within narrow tolerance limits getting produced.
- the manufacture is also special inexpensive compared to a fabric.
- the layer consists of metals that are sinterable are.
- the sophisticated metal layer can be characterized by film casting known in the ceramic field become.
- a pouring slurry is first in other words, a suspension is provided.
- the Slurry has metal powder.
- the average diameter of the metal powder is less than a third the layer thickness to be produced.
- the ratio of metal powder to layer thickness ensures that the layer consists of several layers There are powder grains. So are going through the layer Avoided "holes" that are significantly larger than the desired effective pore size. The more Layers of powder are possible, the more reliable kicking no "holes going through”.
- a metal layer should therefore preferably consist of 5 to 10 Powder layers should be built up.
- the slip consists of a solvent, Dispersant, binder and if necessary from a substance to adjust the viscosity of the slip to an applied pouring or spraying device.
- the thinner the pouring slot in one pouring device used the thinner must be the slip. This adjustment is made if necessary through the substance to adjust the viscosity.
- Isopropanol is particularly suitable as solvent, but also toluene, water etc. Can be used as a dispersant Phthalic acid bis (2 ethylhexyl ester) can be used.
- Phthalic acid bis (2 ethylhexyl ester) can be used.
- polyvinyl butyral is suitable as a binder.
- a substance to adjust the viscosity to equipment Conditions can be used fish oil.
- the slip When selecting the slip, make sure that that the subsequent sintering interferes as little as possible becomes. Carbon, oxygen or nitrogen are allowed in the sintered product therefore in not too high concentrations occur. Are oxide, carbide, nitride formations to avoid during sintering.
- the slip should therefore consist of substances that are used for compliance of the above requirements thermally light are decomposable.
- the slip preferably also contains a release agent like polyethylene glycol.
- the release agent causes a dried one made from the slip Layer of a carrier sufficiently uncomplicated can be solved.
- the slip is applied in layers on a carrier.
- a carrier z. B. a plastic or metal foil.
- the slip is dried and removed from the carrier, or detached if a self-supporting metal layer to be manufactured. Then this green compact sintered.
- the layer can in an advantageous further process step be calibrated by rolling. On in this way, for example, a 117 ⁇ m thick film rolled to exactly 100 ⁇ m thickness.
- the metal layer can be produced reproducibly in terms of its thickness become.
- the pore size can be rolled defined shrink. It can have a defined pore size be produced reproducibly.
- the flow resistance or the flow rate is consequently at the layer produced according to the method can be calibrated.
- the demanding layer can be used as a filter, for sound insulation purposes or used with flame arrestors become.
- Layer firmly connected to the inner wall of a pipe.
- the tube is continuously porous and can, for example can be used as a filter.
- the effective pore size in the tube is then preferably larger than that of the metallic Layer to low flow resistance to get.
- the tube then acts as a carrier.
- the suspension is processed using a tube fed into the tube with the open porosity.
- the The tube is moved in a defined manner in the tube. To this Wise is an even distribution of the suspension ensured in the pipe.
- a spray head is inserted into the pipe.
- the spray head or the pipe rotates.
- the Sprayed inside walls of the pipe corresponds the spray process known from DE 41 20 706. It is particularly useful for pipes with an inner diameter of more than 50 mm.
- a pipe wall 2 is shown in sections open porosity shown in cross section, on the according to the process a metal layer 1 as an inner coating has been applied.
- the inside coating is in in the manner shown in the figure, a maximum of 500 ⁇ m thick.
- film casting is a slick manufactured with the following components:
- the sample is mixed for 2-2.5 hours, e.g. in the tumble mixer and then immediately on a film casting bench poured to thicknesses of e.g. 60 ⁇ m, 120 ⁇ m or thicker (tested up to 400 ⁇ m).
- the sintering process follows.
- sintering was carried out at 950 ° C for 1-3 hours in a vacuum ( ⁇ 10 -2 mbar), argon or argon + 4% by volume hydrogen in a tube furnace.
- the product is a flexible, porous metal foil with a relative density between 55% and 69%.
- the pore maximum for the powder mentioned is about 5-7 ⁇ m in diameter.
- the desired film shape cut out with a punching or cutting tool: here ⁇ 93 mm with punching tool.
- a punching or cutting tool here ⁇ 93 mm with punching tool.
- 1-2 Hours of drying time (here 2 hours) is the PE film from peeled off the green sheet.
- the sintering was carried out at 950 ° C, Carried out in vacuo for 1 hour.
- the product has one relative density of 63% and a pore maximum at approx. 6 microns.
- the binder solution is a 9% shellac solution (shellac ethanol).
- the spray suspension consists of a mixture of powder and binder solution in a ratio of 1: 2.
- Powder and binder solution are homogenized in a tumble mixer for 8 hours.
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- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Powder Metallurgy (AREA)
- Filtering Materials (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
Description
Die Erfindung betrifft eine Metallschicht mit offener Porosität.The invention relates to an open metal layer Porosity.
Bekannt sind aus Gewebe und Vlies bestehende poröse Metallschichten der eingangs genannten Art, die insbesondere als Filter eingesetzt werden.Porous metal layers consisting of fabric and nonwoven are known of the type mentioned, in particular can be used as a filter.
Bei Filtern sind kleine Schichtdicken anzustreben, um unerwünschte Strömungswiderstände zu minimieren. Es gibt ca. 100 µm dünne, aus Gewebe bestehende metallische Filter, die dann allerdings nachteilhaft verhältnismäßig große Poren aufweisen. Auch müssen zur Herstellung entsprechend dünne und daher teure Drähte verwendet werden. Die hieraus hergestellten Gewebe sind folglich ebenfalls entsprechend teuer.In the case of filters, small layer thicknesses should be aimed at to minimize unwanted flow resistance. It are about 100 µm thin, metallic fabric Filters, which are then disadvantageously proportionate have large pores. Also need to manufacture accordingly thin and therefore expensive wires used become. The fabrics made from it are consequently also correspondingly expensive.
Wird ein metallisches Vlies eingesetzt, so können zwar kleine Porengrößen im Mikrometerbereich erzielt werden. Dann beträgt die Vliesdicke jedoch wenigstens einen halben Millimeter. Die Schichtdicken der vorgenannten Vliese können ferner nicht sehr genau gefertigt werden. Verhältnismäßig große Toleranzen müssen hingenommen werden.If a metallic fleece is used, it can small pore sizes in the micrometer range can be achieved. Then the fleece thickness is at least one half a millimeter. The layer thicknesses of the aforementioned Furthermore, nonwovens cannot be manufactured very precisely. Relatively large tolerances have to be accepted become.
Alternativ zum Metall werden u. a. Keramiken und Kunststoffe als Filtermaterialien verwendet. Keramische Filter sind jedoch ebenfalls relativ dick, und es tritt ein entsprechend großer Strömungswiderstand auf. Auch ist die Duktilität nicht gewährleistet. Für viele Einsatzzwecke stellt des weiteren die Sprödigkeit des keramischen Werkstoffs einen Nachteil dar.As an alternative to metal, a. Ceramics and plastics used as filter materials. Ceramic filter are also relatively thick, however, and it occurs a correspondingly large flow resistance. Also ductility is not guaranteed. For many purposes further represents the brittleness of the ceramic Material is a disadvantage.
Wird Kunststoff als Filtermaterial eingesetzt, so sind keine erhöhten Betriebstemperaturen möglich. Für einige Anwendungszwecke stellt Kunststoff kein geeignetes Filtermaterial dar, da dieser nicht den Anforderungen entsprechend sterilisiert werden kann, die z. B. im medizinischen oder im Lebensmittelbereich erforderlich sind. Die Wiedereinsetzbarkeit des Filters ist in diesen Fällen nicht möglich.If plastic is used as filter material, so are no increased operating temperatures possible. For some Plastic is not a suitable filter material for application purposes because it does not meet the requirements can be sterilized, e.g. B. in medical or required in the food sector are. The filter can be used again Cases not possible.
Aus EP 570 889 67 ist ein Verfahren zur Herstellung einer porösen Schicht auf einer Metalloberfläche bekannt, bei dem eine Mischung aus Binder, metallischem Pulver und hartlötendem Füller aus Metallpulver mit spezifischer Korngröße als Suspension auf die Metalloberfläche aufgebracht wird. Diese wird anschließend aufgeheizt und gesintert.EP 570 889 67 describes a process for the production a porous layer on a metal surface, where a mixture of binder, metallic Powder and brazing filler made of metal powder with specific grain size as a suspension on the metal surface is applied. This will then heated and sintered.
In DE-A 2 323 878 wird ein Verfahren zur Beschichtung einer Metallsubstanz beschrieben. Dabei wird zunächst eine Bindemittellösung mit leicht- und schwerflüchtigen Bestandteilen auf das Metallsubstrat aufgebracht. Anschließend wir Metallpulver auf diese Schicht aufgebracht. Zunächst werden die leichtflüchtigen Komponenten verdampft. Anschließend werden durch Erwärmung auch die schwerflüchtigen Komponenten verdampft. Eine weitere Erwärmung führt zu der Bildung einer mit dem Metallsubstrat verbundenen porösen Metallschicht.DE-A 2 323 878 describes a method for coating described a metal substance. This will start with a binder solution with volatile and low volatility Components applied to the metal substrate. Subsequently we applied metal powder to this layer. First, the volatile components evaporated. Then, by heating too the volatile components evaporate. Another Heating leads to the formation of one with the metal substrate connected porous metal layer.
Aus US-A 3 855 638 ist eine chrirurgische metallische Prothese mit einer porösen metallischen Schicht bekannt. Die den Zwischenraum bildenden Poren sind dabei größer als 20 µm, aber vorteilhaft maximal 50 µm groß. Die Schichtdicke variiert von 100 µm bis 1000 µm. Für die Herstellung wird eine wäßrige Aufschlämmung, enthaltend Metallpulver und Binder, auf die metallische Prothese aufgebracht, erwärmt, um das Wasser zu entfernen, und anschließend gesintert, wobei der organische Binder ausgetrieben wird.From US-A 3 855 638 is a surgical metallic Known prosthesis with a porous metallic layer. The pores forming the space are included larger than 20 µm, but advantageously a maximum of 50 µm in size. The layer thickness varies from 100 µm to 1000 µm. For the preparation will contain an aqueous slurry Metal powder and binder, on the metallic Prosthesis applied, heated to remove the water, and then sintered, the organic Binder is driven out.
Ebenfalls bekannt ist aus FR-A 2 520 265 ein Verfahren
zur Herstellung eines teilchengebundenen Wärmerohrdochts
auf Innenwänden eines Wärmerohres. Dabei werden
die Teilchen, z. B. rostfreie Stahlmikrokugeln von +325
bis -100 mesh (44 - 149 µm) Durchmesser in einer geeigneten
Bindemittellösung suspendiert und auf die Wärmerohrwand
aufgestrichen. Das Bindemittel wird bei
400 °C unter vermindertem Druck verdampft. Anschließend
wird die so erhaltene Grünschicht bei 1250 ± 50 °C für
2 Stunden gesintert.A method is also known from FR-
Aufgabe der Erfindung ist die Herstellung einer temperaturbeständigen, sterilisierbaren, einfach und reproduzierbar herzustellenden Metallschicht mit durchgehender Porosität, die duktil, mechanisch stabil und elastisch ist und bei der - sofern sie als Filter eingesetzt wird - geringe Strömungsdruckverluste auftreten. Ferner sollen Mikrofiltrationsaufgaben mit der Metallschicht wahrgenommen werden können.The object of the invention is to produce a temperature-resistant, sterilizable, simple and reproducible metal layer to be produced with continuous Porosity that is ductile, mechanically stable and elastic is and at - if they are used as a filter will occur - low flow pressure losses. Microfiltration tasks with the metal layer are also intended can be perceived.
Die Aufgabe der Erfindung wird durch eine maximal 500 µm dicke Metallschicht, mit anderen Worten durch eine Metallfolie gelöst, die einen effektiven Porendurchmesser aufweist, der bis zu einem Zwölftel, vorzugsweise bis zu einem Fünfzehntel der Schichtdicke der Metallschicht beträgt. Als Poren sind hier die Kanäle zu verstehen, die die durch die Schicht hindurchgehende offene Porosität erzeugen. Gelegentliche "Hohlräume" aufgrund von Inhomogenitäten stellen keine Poren im Sinne des Anspruchs dar.The object of the invention is achieved by a maximum 500 µm thick metal layer, in other words through solved a metal foil that has an effective pore diameter has up to a twelfth, preferably up to a fifteenth of the layer thickness of the Metal layer. The channels are here as pores to understand who is going through the layer Create open porosity. Occasional "cavities" due to inhomogeneities there are no pores in the The meaning of the claim.
Die vorgenannten Hohlräume aufgrund von Inhomogenitäten spielen erfahrungsgemäß keine Rolle, wenn die Schichtdicke einer erfindungsgemäß aus Partikeln bzw. aus Pulver hergestellten porösen Schicht wenigstens dreimal größer als der mittlere Partikeldurchmesser ist. Wird die anspruchsgemäße Schicht aus Partikeln oder Pulvern erfindungsgemäß hergestellt, so beträgt der effektive Porendurchmesser insbesondere bis zu einem Viertel, vorzugsweise bis zu einem Fünftel des mittleren Partikel- bzw. Pulverkörnerdurchmessers des eingesetzten Pulvers.The aforementioned cavities due to inhomogeneities Experience has shown that it does not matter if the layer thickness one according to the invention from particles or from powder produced porous layer at least three times is larger than the average particle diameter. Becomes the sophisticated layer of particles or powders produced according to the invention, the effective Pore diameter in particular up to a quarter, preferably up to a fifth of the average particle or powder grain diameter of the used Powder.
Liegt beispielsweise eine 500 µm dicken Metallschicht vor, so beträgt die effektive Größe der Poren, die die durchgehende (offene) Porosität bewirken, bis zu 500/12 mm, also bis zu ca. 40 µm. Anders ausgedrückt bedeutet dies, daß Substanzen kleiner als ca. 40 µm sein müssen, um die Metallschicht passieren zu können.For example, there is a 500 µm thick metal layer before, the effective size of the pores is the cause continuous (open) porosity, up to 500/12 mm, i.e. up to approx. 40 µm. Expressed differently this means that substances smaller than approx. 40 µm to be able to pass through the metal layer.
Wurde eine Metallschicht aus Pulvern der Größe 50 µm erfindungsgemäß hergestellt, so sollte die Schichtdicke wenigstens dreimal so dick wie der Pulverdurchmesser, also wenigstens 150 µm betragen, um auf Inhomogenitäten des Materials zurückzuführende Hohlraumprobleme zuverlässig zu vermeiden. Der effektive Porendurchmesser der Schicht beträgt dann regelmäßig bis zu 50/4 µm (3*50/12 µm), vorzugsweise bis zu 50/5 µm (3*50/15 µm). Was a metal layer from powders size 50 microns Made according to the invention, the layer thickness should at least three times as thick as the powder diameter, So be at least 150 µm to inhomogeneities cavity problems due to the material are reliable to avoid. The effective pore diameter of the The layer is then regularly up to 50/4 µm (3 * 50/12 µm), preferably up to 50/5 µm (3 * 50/15 µm).
In einer vorteilhaften Ausgestaltung der Erfindung beträgt
die Schichtdicke der Metallfolie maximal 100 µm,
vorzugsweise nicht mehr als 50 µm. Die effektive Porengröße
im vorgenannten Sinne beträgt in allen Fällen maximal
1/12 der Schichtdicke.In an advantageous embodiment of the invention
the layer thickness of the metal foil maximum 100 µm,
preferably not more than 50 µm. The effective pore size
in the aforementioned sense is maximum in all
Das Metall erlaubt erhöhte Temperaturen, verhält sich duktil, mechanisch stabil und ist elastisch. Darüber hinaus ist das Material problemlos sterilisierbar. Die Schichtdicke der Schicht bzw. Folie kann im Vergleich zu einem Vlies oder einem Gewebe in engen Toleranzgrenzen hergestellt werden. Auch ist die Herstellung insbesondere im Vergleich zu einem Gewebe kostengünstig.The metal allows elevated temperatures, behaves ductile, mechanically stable and elastic. About that the material can also be easily sterilized. The Layer thickness of the layer or film can be compared to a fleece or a fabric within narrow tolerance limits getting produced. The manufacture is also special inexpensive compared to a fabric.
Die Schicht besteht aus Metallen, die sinterfähig sind. Metalle, die diese Eigenschaft im Sinne des Anspruchs aufweisen, bilden während eines Sinterungsprozesses Sinterbrücken zwischen einzelnen metallischen Pulverkörnern. Stahl, Edelstahl, Bronze und Nickel bilden Sinterbrücken im vorgenannten Sinne. Diese lassen sich besser als Reaktivmetalle wie Aluminium und Titan sintern.The layer consists of metals that are sinterable are. Metals that have this property in mind of the claim, form during a sintering process Sintered bridges between individual metallic Powder grains. Steel, stainless steel, bronze and Nickel form sintered bridges in the aforementioned sense. These are better than reactive metals like aluminum and titanium sinter.
Die anspruchsgemäße Metallschicht kann durch das aus dem keramischen Bereich bekannte Foliengießen hergestellt werden. Hierfür wird zunächst ein Gießschlicker, mit anderen Worten eine Suspension bereitgestellt. Der Schlicker weist Metallpulver auf. Der mittlere Durchmesser des Metallpulvers ist kleiner als ein Drittel der herzustellenden Schichtdicke zu wählen. The sophisticated metal layer can be characterized by film casting known in the ceramic field become. For this, a pouring slurry is first in other words, a suspension is provided. The Slurry has metal powder. The average diameter of the metal powder is less than a third the layer thickness to be produced.
Das genannte Verhältnis von Metallpulver zur Schichtdicke stellt sicher, daß die Schicht aus mehreren Lagen Pulverkörnern besteht. So werden durch die Schicht hindurchgehende "Löcher" vermieden, die erheblich größer als die gewünschte effektive Porengröße sind. Je mehr Lagen Pulver möglich sind, desto zuverlässiger treten keine "hindurchgehenden Löcher" auf.The ratio of metal powder to layer thickness ensures that the layer consists of several layers There are powder grains. So are going through the layer Avoided "holes" that are significantly larger than the desired effective pore size. The more Layers of powder are possible, the more reliable kicking no "holes going through".
Nachteilhaft nimmt mit der Anzahl der Pulverlagen der Strömungswiderstand zu. Nach derzeitigem Kenntnisstand sollte eine Metallschicht daher bevorzugt aus 5 bis 10 Pulverlagen aufgebaut sein.Disadvantageously increases with the number of powder layers Flow resistance too. According to the current state of knowledge a metal layer should therefore preferably consist of 5 to 10 Powder layers should be built up.
Der Schlicker besteht neben dem Pulver aus einem Lösungsmittel, Dispergator, Binder und erforderlichenfalls aus einer Substanz zur Anpassung der Viskosität des Schlickers an eine eingesetzte Gieß- oder Sprühvorrichtung.In addition to the powder, the slip consists of a solvent, Dispersant, binder and if necessary from a substance to adjust the viscosity of the slip to an applied pouring or spraying device.
Je dünner beispielsweise der Ausgußschlitz bei einer verwendeten Gießvorrichtung ist, desto dünnflüssiger muß der Schlicker sein. Diese Anpassung erfolgt im Bedarfsfall durch die Substanz zur Anpassung der Viskosität.For example, the thinner the pouring slot in one pouring device used, the thinner must be the slip. This adjustment is made if necessary through the substance to adjust the viscosity.
Als Lösungsmittel eignet sich insbesondere Isopropanol, aber auch Toluol, Wasser etc.. Als Dispergator kann Phtalsäurebis-(2 ethylhexylester) eingesetzt werden. Als Binder eignet sich beispielsweise Polyvinylbutyral. Als Substanz zur Anpassung der Viskosität an apparative Gegebenheiten kann Fischöl verwendet werden. Isopropanol is particularly suitable as solvent, but also toluene, water etc. Can be used as a dispersant Phthalic acid bis (2 ethylhexyl ester) can be used. For example, polyvinyl butyral is suitable as a binder. As a substance to adjust the viscosity to equipment Conditions can be used fish oil.
Bei der Auswahl des Schlickers ist darauf zu achten, daß die nachfolgende Sinterung möglichst wenig behindert wird. Kohlenstoff, Sauerstoff oder Stickstoff dürfen im Sinterprodukt daher in nicht zu hohen Konzentrationen auftreten. Oxid-, Carbid-, Nitridbildungen sind während der Sinterung zu vermeiden. Der Schlicker sollte also aus Substanzen bestehen, die zwecks Einhaltung der vorgenannten Anforderungen thermisch leicht zersetzbar sind.When selecting the slip, make sure that that the subsequent sintering interferes as little as possible becomes. Carbon, oxygen or nitrogen are allowed in the sintered product therefore in not too high concentrations occur. Are oxide, carbide, nitride formations to avoid during sintering. The slip should therefore consist of substances that are used for compliance of the above requirements thermally light are decomposable.
Soll eine freitragende Schicht hergestellt werden, so enthält der Schlicker vorzugsweise noch ein Trennmittel wie Polyethylenglykol. Das Trennmittel bewirkt, daß eine getrocknete, aus dem Schlicker hergestellte Schicht von einem Träger ausreichend komplikationslos gelöst werden kann.If a self-supporting layer is to be produced, then the slip preferably also contains a release agent like polyethylene glycol. The release agent causes a dried one made from the slip Layer of a carrier sufficiently uncomplicated can be solved.
Der Schlicker wird auf einen Träger schichtförmig aufgetragen. Als Träger eignet sich z. B. eine Kunststoff- oder Metallfolie.The slip is applied in layers on a carrier. As a carrier z. B. a plastic or metal foil.
Der Schlicker wird getrocknet und vom Träger abgezogen, bzw. abgelöst, falls eine freitragende Metallschicht hergestellt werden soll. Anschließend wird dieser Grünling gesintert.The slip is dried and removed from the carrier, or detached if a self-supporting metal layer to be manufactured. Then this green compact sintered.
Alternativ kann die anspruchsgemäße, poröse Metallfolie mittels des aus DE 41 20 706 bekannten Spray-Verfahrens aus der Suspension, also aus dem Schlicker hergestellt werden.Alternatively, the sophisticated, porous metal foil by means of the spray process known from DE 41 20 706 made from the suspension, i.e. from the slip become.
Die Schicht kann in einem vorteilhaften weiteren Verfahrensschritt durch Walzen kalibriert werden. Auf diese Weise wurde beispielsweise eine 117 µm dicke Folie auf exakt 100 µm Dicke gewalzt. Die Metallschicht kann so hinsichtlich ihrer Dicke reproduzierbar hergestellt werden.The layer can in an advantageous further process step be calibrated by rolling. On in this way, for example, a 117 µm thick film rolled to exactly 100 µm thickness. The metal layer can be produced reproducibly in terms of its thickness become.
Alternativ läßt sich mittels Walzens die Porengröße definiert verkleinern. Es kann so eine definierte Porengröße reproduzierbar hergestellt werden. Der Strömungswiderstand bzw. die Durchflußrate ist folglich bei der verfahrensgemäß herstellten Schicht kalibrierbar.Alternatively, the pore size can be rolled defined shrink. It can have a defined pore size be produced reproducibly. The flow resistance or the flow rate is consequently at the layer produced according to the method can be calibrated.
Die anspruchsgemäße Schicht kann als Filter, zu Schallschutzzwecken oder bei Flammenrückschlagsperren eingesetzt werden.The demanding layer can be used as a filter, for sound insulation purposes or used with flame arrestors become.
In einer weiteren Ausgestaltung der Erfindung ist die Schicht fest mit der Innenwand eines Rohres verbunden. Das Rohr ist durchgehend porös, und kann beispielsweise als Filter eingesetzt werden. Die effektive Porengröße im Rohr ist dann vorzugsweise größer als die der metallischen Schicht, um zu geringen Strömungswiderständen zu gelangen. Das Rohr fungiert dann also als Träger.In a further embodiment of the invention Layer firmly connected to the inner wall of a pipe. The tube is continuously porous and can, for example can be used as a filter. The effective pore size in the tube is then preferably larger than that of the metallic Layer to low flow resistance to get. The tube then acts as a carrier.
Zur Herstellung eines solchen Rohres mit poröser Innenschicht wird z. B. zunächst eine Suspension (Schlicker) wie in DE 41 20 706 hergestellt. Diese Suspension wird dosiert in ein rotierendes, je nach Anwendungszweck poröses Rohr eingespeist. Durch Rotation des Rohres wird die Suspension gleichmäßig und schichtförmig auf der Innenwand abgeschieden. Während des Rotationsvorgangs trocknet die Suspension. Ist die gewünschte Schichtdicke erreicht, so wird die Zufuhr der Suspension gestoppt. Sobald der Trocknungsvorgang beendet ist, wird die Rotation beendet. Anschließend wird das Rohr mit der getrockneten Suspension, also mit dem Grünling gesintert.To manufacture such a tube with a porous inner layer z. B. first a suspension (slip) as produced in DE 41 20 706. This suspension will dosed in a rotating, depending on the application Porous tube fed. By rotating the pipe becomes the suspension evenly and in layers on the Separated inside wall. During the rotation process dries the suspension. Is the desired layer thickness reached, the supply of the suspension is stopped. As soon as the drying process is finished the rotation ends. Then the pipe with the dried suspension, i.e. with the green body sintered.
In einer vorteilhaften Ausführungsform des vorgenannten Herstellungsverfahrens wird im Falle eines porösen Rohres dieses von außen abgedichtet. So wird verhindert, daß Suspension im Übermaß in die Poren des Rohres eindringen kann, wenn diese größer als der Pulverdurchmesser sind.In an advantageous embodiment of the above Manufacturing process is in the case of a porous tube this sealed from the outside. This prevents that excess suspension penetrate into the pores of the tube can if this is larger than the powder diameter are.
In einer weiteren vorteilhaften Ausführungsform des Verfahrens wird die Suspension mittels eines Röhrchens in das Rohr mit der offenen Porosität eingespeist. Das Röhrchen wird definiert in dem Rohr bewegt. Auf diese Weise wird eine gleichmäßige Verteilung der Suspension im Rohr sichergestellt.In a further advantageous embodiment of the The suspension is processed using a tube fed into the tube with the open porosity. The The tube is moved in a defined manner in the tube. To this Wise is an even distribution of the suspension ensured in the pipe.
In einer alternativen Ausführungsform des Verfahrens wird ein Sprühkopf in das Rohr eingeführt. Der Sprühkopf oder das Rohr rotiert. Auf diese Weise werden die Innenwände des Rohrs besprüht. Dieses Verfahren entspricht dem aus DE 41 20 706 bekannten Spray-Verfahren. Es wird insbesondere bei Rohren mit einem Innendurchmesser von mehr als 50 mm eingesetzt. In an alternative embodiment of the method a spray head is inserted into the pipe. The spray head or the pipe rotates. In this way, the Sprayed inside walls of the pipe. This procedure corresponds the spray process known from DE 41 20 706. It is particularly useful for pipes with an inner diameter of more than 50 mm.
In der Figur wird ausschnittsweise ein Rohrwand 2 mit
offener Porosität im Querschnitt gezeigt, auf der verfahrensgemäß
eine Metallschicht 1 als Innenbeschichtung
aufgebracht worden ist. Die Innenbeschichtung ist in
der aus der Figur ersichtlichen Weise maximal 500 µm
dick.In the figure, a
Die Erfindung wird anhand der nachfolgenden Beispiele näher erläutert.The invention is illustrated by the following examples explained in more detail.
Für die Herstellungsart "Foliengießen" wird ein Schlikker mit folgenden Bestandteilen hergestellt:For the production type "film casting" is a slick manufactured with the following components:
Einwaage von 100 g Edelstahlpulver, mittlerer Pulverdurchmesser
≤ 16 µm
Die Einwaage wird 2-2,5 h gemischt, z.B. im Taumelmischer und dann unmittelbar auf einer Foliengießbank ausgegossen auf Dicken von z.B. 60 µm, 120 µm oder dikker (erprobt bis 400 µm). The sample is mixed for 2-2.5 hours, e.g. in the tumble mixer and then immediately on a film casting bench poured to thicknesses of e.g. 60 µm, 120 µm or thicker (tested up to 400 µm).
Nach dem Trocknen (ca. 3 h) und Abziehen der Schicht folgt der Sinterprozeß. Hier wurden Sinterungen bei 950° C für 1-3 Stunden in Vakuum (< 10-2 mbar), Argon oder Argon + 4 Vol.-% Wasserstoff in einem Rohrofen durchgeführt. Das Produkt ist eine flexible, poröse Metallfolie mit einer relativen Dichte zwischen 55 % und 69 %. Das Porenmaximum liegt bei dem genannten Pulver bei einem Durchmesser von ca. 5-7 µm.After drying (approx. 3 h) and stripping the layer, the sintering process follows. Here, sintering was carried out at 950 ° C for 1-3 hours in a vacuum (<10 -2 mbar), argon or argon + 4% by volume hydrogen in a tube furnace. The product is a flexible, porous metal foil with a relative density between 55% and 69%. The pore maximum for the powder mentioned is about 5-7 µm in diameter.
Für eine Herstellung mittels des aus DE 41 20 706 bekannten Spray-Verfahrens wird zunächst die Spritzsuspension durch Mischung von Binderlösung und Pulver im Verhältnis 2 : 1 (Vol. Anteile) hergestellt. Als Binderlösung wurde eine 9%ige (Gew.-%) Schellack-Ethanollösung verwendet und als Metallpulver ein gasverdüstes Edelstahlpulver 316 L mit einem Korndurchmesser < 16 µm.For a production by means of that known from DE 41 20 706 The spray process is first the spray suspension by mixing binder solution and powder in Ratio 2: 1 (vol. Shares) produced. As a binder solution became a 9% (wt%) shellac ethanol solution used and as a metal powder a gas atomized 316 L stainless steel powder with a grain diameter <16 microns.
Nach ca. 8 h Homogenisierung im Taumelmischer kann die Suspension unmittelbar in einer geeigneten Anlage verspritzt werden.After about 8 hours of homogenization in the tumble mixer, the The suspension is sprayed directly into a suitable system become.
Das geschieht durch Aufspritzen von 50 - 200 µm dicken Schichten auf Polyethylen-Folien (PE-HD 0,2 mm).This is done by spraying 50 - 200 µm thick Layers on polyethylene foils (PE-HD 0.2 mm).
Nach Antrocknen (5-10 min) wird die gewünschte Folienform mit einem Stanz- oder Schneidewerkzeug ausgeschnitten: hier Ø 93 mm mit Stanzwerkzeug. Nach 1-2 Stunden Trockenzeit (hier 2 h) wird die PE-Folie von der Grünfolie abgezogen. Die Sinterung wurde bei 950°C, 1 Stunde im Vakuum durchgeführt. Das Produkt hat eine relative Dichte von 63% und ein Porenmaximum bei ca. 6 µm.After drying (5-10 min) the desired film shape cut out with a punching or cutting tool: here Ø 93 mm with punching tool. After 1-2 Hours of drying time (here 2 hours) is the PE film from peeled off the green sheet. The sintering was carried out at 950 ° C, Carried out in vacuo for 1 hour. The product has one relative density of 63% and a pore maximum at approx. 6 microns.
Für eine Innenbeschichtung von porösen Trägerrohren wurde als Pulverwerkstoff Edelstahl 316 L, ØPulverkörner< 5 µm eingesetzt. Die Binderlösung ist eine 9%ige Schellacklösung (Schellack-Ethanol). Die Spritzsuspension besteht aus einer Mischung aus Pulver und Binderlösung im Verhältnis 1 : 2.For an inner coating of porous carrier tubes, stainless steel 316 L, Ø powder grains <5 µm was used as the powder material. The binder solution is a 9% shellac solution (shellac ethanol). The spray suspension consists of a mixture of powder and binder solution in a ratio of 1: 2.
Pulver und Binderlösung werden 8 Stunden im Taumelmischer homogenisiert. Zur Innenbeschichtung wird das zu beschichtende Rohr (hier Øi = 15 mm, Länge = 400 mm) in Rotation versetzt (hier ca. 60 Umdrehungen/min) und über einen mit konstanter Geschwindigkeit verfahrbaren Dosierkopf (Ø 3 mm) Suspension in das Rohr eindosiert. Nach ca. 5 minütiger Trockenzeit wird das Rohr in den Sinterofen eingesetzt und bei 950° C, 1 Stunde lang im Vakuum gesintert. Innenbeschichtungen mit Porositäten zwischen 30 und 50% wurden so in einem Dickebereich zwischen 20 und 300 µm hergestellt.Powder and binder solution are homogenized in a tumble mixer for 8 hours. For the internal coating, the pipe to be coated (here Ø i = 15 mm, length = 400 mm) is set in rotation (here approx. 60 revolutions / min) and suspension is metered into the pipe via a dosing head (Ø 3 mm) that can be moved at constant speed , After a drying time of approx. 5 minutes, the tube is inserted into the sintering furnace and sintered at 950 ° C. for 1 hour in a vacuum. Inner coatings with porosities between 30 and 50% were produced in a thickness range between 20 and 300 µm.
Claims (5)
- Method for producing a sintered metal layer with open porosity, with the following steps:a suspension comprising metal powder, dispersant and substances for adjusting viscosity is applied in the form of a layer to a substrate,the thickness of the layer of suspension applied to the substrate is chosen so that the thickness of the metal layer after sintering is at least three times the mean powder diameter of the metal powder,the suspension is dried on the substrate,the dried metal layer is stripped from the substrate prior to sintering,the metal layer is sintered.
- Method for producing a metal layer with open porosity on the internal wall of a tube which has through-going porosity, with the following steps:a suspension comprising metal powder, dispersant and substances for adjusting viscosity is applied in the form of a layer to the internal wall of a tube,the thickness of the layer of suspension applied to the internal wall of the tube is chosen so that the thickness of the metal layer after sintering is at least three times the mean powder diameter of the metal powder,the suspension is dried and then sintered.
- Method according to the preceding Claim wherein the tube rotates during application and drying of the suspension.
- Method according to either of the preceding Claims 2 and 3 wherein the external wall of the porous tube is sealed with a sealing medium until the suspension is dried.
- Metal layer with open porosity, obtained in accordance with any one of Claims 2 to 4, and with a maximum layer-thickness of 500 µm, wherein the effective diameter of the through-going pores is not more than one twelfth of the layer-thickness, the metal layer being formed as the internal wall of a tube with through-going porosity.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19716595 | 1997-04-21 | ||
DE19716595A DE19716595C1 (en) | 1997-04-21 | 1997-04-21 | Thin metal inner layer with fine porosity for a pipe |
PCT/DE1998/000594 WO1998048077A1 (en) | 1997-04-21 | 1998-02-27 | Thin, fine pored metal layer |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0977909A1 EP0977909A1 (en) | 2000-02-09 |
EP0977909B1 true EP0977909B1 (en) | 2002-06-12 |
Family
ID=7827146
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP98916815A Expired - Lifetime EP0977909B1 (en) | 1997-04-21 | 1998-02-27 | Thin, fine pored metal layer |
Country Status (4)
Country | Link |
---|---|
EP (1) | EP0977909B1 (en) |
AT (1) | ATE219166T1 (en) |
DE (3) | DE19716595C1 (en) |
WO (1) | WO1998048077A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7306753B2 (en) | 1999-12-29 | 2007-12-11 | Gkn Sinter Metals Gmbh | Method of making a thin porous layer |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10041992A1 (en) * | 2000-08-26 | 2002-03-14 | Gkn Sinter Metals Gmbh | Module for use as a filter, catalyst or heater and process for its manufacture |
DE10123199B4 (en) * | 2001-05-12 | 2005-02-24 | Gkn Sinter Metals Gmbh | Process for producing at least partially internally coated tubular bodies with a coating of a sinterable material |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
NL219239A (en) * | 1956-07-25 | |||
FR2031787A5 (en) * | 1969-02-07 | 1970-11-20 | Onera (Off Nat Aerospatiale) | |
CA962806A (en) * | 1970-06-04 | 1975-02-18 | Ontario Research Foundation | Surgical prosthetic device |
DE2323878A1 (en) * | 1973-05-11 | 1974-11-21 | Union Carbide Corp | METHOD AND DEVICE FOR COATING METAL SUBSTRATES |
JPS5788967A (en) * | 1980-11-21 | 1982-06-03 | Showa Alum Corp | Formation of porous layer on metallic surface |
IT1206312B (en) * | 1982-01-22 | 1989-04-14 | Thermo Electron Corp | METHOD TO FORM A WICK FOR A HEAT TUBE. |
DE4000302C1 (en) * | 1990-01-08 | 1991-07-25 | Degussa Ag, 6000 Frankfurt, De | |
DE4120706C2 (en) * | 1991-06-22 | 1994-10-13 | Forschungszentrum Juelich Gmbh | Process for the production of porous or dense sintered workpieces |
FR2701719B1 (en) * | 1993-02-19 | 1995-04-14 | Maubeuge Fer | Methods and installations for continuously producing several coatings based on metallic alloy on a steel strip. |
-
1997
- 1997-04-21 DE DE19716595A patent/DE19716595C1/en not_active Expired - Fee Related
- 1997-04-21 DE DE19758454A patent/DE19758454A1/en not_active Withdrawn
-
1998
- 1998-02-27 WO PCT/DE1998/000594 patent/WO1998048077A1/en active IP Right Grant
- 1998-02-27 DE DE59804429T patent/DE59804429D1/en not_active Expired - Lifetime
- 1998-02-27 EP EP98916815A patent/EP0977909B1/en not_active Expired - Lifetime
- 1998-02-27 AT AT98916815T patent/ATE219166T1/en active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7306753B2 (en) | 1999-12-29 | 2007-12-11 | Gkn Sinter Metals Gmbh | Method of making a thin porous layer |
Also Published As
Publication number | Publication date |
---|---|
DE59804429D1 (en) | 2002-07-18 |
ATE219166T1 (en) | 2002-06-15 |
WO1998048077A1 (en) | 1998-10-29 |
DE19716595C1 (en) | 1998-09-03 |
DE19758454A1 (en) | 1998-10-22 |
EP0977909A1 (en) | 2000-02-09 |
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