EP1255621B1 - Autoclave for the precision cleaning of objects and use of the autoclave - Google Patents

Autoclave for the precision cleaning of objects and use of the autoclave Download PDF

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Publication number
EP1255621B1
EP1255621B1 EP01953012A EP01953012A EP1255621B1 EP 1255621 B1 EP1255621 B1 EP 1255621B1 EP 01953012 A EP01953012 A EP 01953012A EP 01953012 A EP01953012 A EP 01953012A EP 1255621 B1 EP1255621 B1 EP 1255621B1
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EP
European Patent Office
Prior art keywords
solvent
autoclave
wall
autoclave according
parts
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EP01953012A
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German (de)
French (fr)
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EP1255621A1 (en
Inventor
Philipp Widmer
Carlo Devittori
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Eco2 SA
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Eco2 SA
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0021Cleaning by methods not provided for in a single other subclass or a single group in this subclass by liquid gases or supercritical fluids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/06Cleaning involving contact with liquid using perforated drums in which the article or material is placed
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/10Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations

Definitions

  • the present invention relates to an autoclave for precision cleaning of pieces by means of a solvent according to the preamble of patent claim 1 and the use of this autoclave.
  • Such an autoclave is used in the precision cleaning of high-tech products in precision, micro and nanomechanics, electronics, the ceramics industry, cermets, polymers, textile fibers, etc.
  • Organic solvents in particular chlorinated organic solvents such as trichlorethylene and perchlorethylene, chlorofluorocarbides or detergents or surfactants in Water phase.
  • This solvent as well as nitrogen protoxide, ethane, etc. can be a have good solubility in the liquid phase but they increase their solubility in vapor phase, especially in difficult to reach areas, thanks to the larger ones Diffusivity and lower viscosity that they reach in the gas state.
  • in the supercritical state temperature higher than the critical and pressure also higher than the critical one
  • the combination of both properties (low Viscosity and high density) makes them ideal solvents for precision cleaning processes, which has a high degree of cleaning in every point of the surface and in the hard-to-reach games.
  • solvents prove to be particularly effective for nonpolar or little polar polluting substances; Polar organic substances such as additives to cutting oils, salts, abrasives and metals are not noticeably solvable in solvents suitable for cleaning in the supercritical phase are. Such in the solid phase on the surfaces to be cleaned by adhesion or adsorption remaining residues must by physical means of the same be removed: For this purpose, the effectiveness of cavitation is recognized, which comes about over the areas that are immersed in a liquid are, through which propagate ultrasonic waves.
  • US Pat. No. 5,944,996 discloses a generic cleaning process using solvents, in which preferably an ultrasound treatment is also to be used.
  • the pieces to be cleaned are located in a motor-driven, rotatable drum inside the ultrasonic bath.
  • the solvent used is gaseous, liquid or preferably supercritical CO 2 .
  • this document does not disclose how to arrange an ultrasound source for use in this method.
  • US 5,759,209 discloses a purification process for which liquefied gas (preferably CO 2 ) is passed under pressure into a pressure vessel with objects to be cleaned. To clean these objects, the liquefied gas is at least initially cooled to -20 ° C to + 20 ° C and kept at a correspondingly high pressure and without any use of ultrasound in the liquid state.
  • liquefied gas preferably CO 2
  • US 4,922,939 discloses a simple device for cleaning dentures in a detergent container.
  • the objects to be cleaned are located in a drum rotatable in this container.
  • the container wall comprises Fixed paddle and the drum wall also includes paddles and openings. Through the rotation of the drum are through the mentioned paddles and openings generates strong currents and turbulences in the cleaning fluid, so that the dentures cleaned without application of ultrasound become.
  • EP 0 893 166 discloses cleaning baths with solvents whose physical State near the critical point (subcritical or supercritical) located. These cleaning baths each comprise two opposite ones Ultrasonic sources driving an intermediate propeller, whereby the cleaning effect should be improved. Also this document is silent about the exact arrangement and design of the ultrasound sources.
  • EP 0 894 542 discloses a cleaning process resulting from a washing treatment with a surface-active substance and ultrasonic cavitation as well a subsequent drying step with an organic solvent (e.g., isopropanol or acetone) or corresponding vapors. Subsequently the washing and drying device is preferably compressed air blown out.
  • an organic solvent e.g., isopropanol or acetone
  • DE 197 41 836 discloses a cleaning device designed as an ultrasonic bath with an immersed in the cleaning liquid (distilled water) Schwingerplatte to which several vibrators are attached. These Vibration generators are connected to a high frequency generator and stimulate the vibrating plate to mechanical vibrations, causing pressure fluctuations in the water. These pressure fluctuations generate in the water Over and under pressure phases, which at a corresponding frequency to the known Cause cavitation effect.
  • US 5,858,107 discloses formed as ultrasonic whistle nozzles through which liquid CO 2 is pressed. However, such nozzles are not suitable for generating ultrasonic waves in supercritical CO 2 .
  • the object of the present invention is thus to propose an autoclave according to the preamble of claim 1, which is suitable for generating ultrasonic waves in liquid and supercritical CO 2 .
  • the invention relates to an autoclave for precision cleaning of surfaces with complex shapes through the use of inert liquid or supercritical fluids as solvents, and indeed supported by irradiation of the surfaces to be cleaned with ultrasonic waves and by the resulting cavitation in a programmed movement of the to be cleaned Pieces, as well as the use of this autoclave.
  • a container is placed in the form of a drum with the pieces, which is rotatable by means of an external electric motor.
  • This drum can be with central Axes be provided or not. In it, the pieces are free, regarding the Wall of the drum to move.
  • the bases and the lateral surface of the drum are formed in the form of lattices that control the passage of ultrasonic waves and at the same time allow the solid heavy particles to separate out from the Remove the surface of the pieces.
  • the envisaged power is generally of the order of 1000 W and the frequency between 10 and 2000 kHz depending on the dimensions the solid particles to be ablated from the surface of the pieces.
  • Die Device consists of an autoclave, in which the drum, or the container 2 is introduced, in which or in which the pieces are 3, the to be subjected to the precision cleaning process.
  • the drum or the container 2 is driven by the motor 4 via an axis 5.
  • ultrasonic transducers 6 At the outer cylindrical surface of the wall 11 of the autoclave are ultrasonic transducers 6 arranged over the entire inside of the wall 11 a majority irradiate the pieces 3 radially.
  • the precision cleaning process by the action of the solvent in the liquid and / or supercritical state, or alternately in the liquid state and supercritical state.
  • the fluid can be in the autoclave after preheating or at room temperature transported the input 7 and also by evaporation via the outputs 8 and 9 are cooled. Excessive cooling of the charge chamber or Chamber 1 during the depression phase can by introducing an inert Gas with appropriate pressure through the input 10 can be avoided.
  • Temperatures, variety and duration of cleaning cycles in the liquid and supercritical phase, the movements of the drum, or the container. 2 with the pieces 3 to be cleaned (sense of rotation, change of rotation, times and speed), Pressure and amount of solvent are controlled by a computer (not shown in FIG. 1) and a specific program.
  • Both the dissolved substances in the liquid or mainly supercritical Phase, as well as the solid particles in suspension are from the charge chamber or chamber 1 transported by a fluid flow out.
  • Container 2 is rotatable in both directions of rotation, and that possibility exists to change the sense of rotation and / or the rotational speed. This happens preferably in programmed form.
  • the autoclave can also be attached to the inner wall of the container 2 or arranged on an axis blades to be a to allow guided movement of the pieces 3.
  • the ultrasonic transducers 6 can arranged on the outer wall 11 of the charge chamber or chamber 1 be, preferably at that with the greater extent.
  • the input 7 for the solvent is located at the lowest point inside the chamber 1 and the Exit 9 at the highest point. Furthermore, at the lowest point of the Chamber 1 is an outlet 8 for the solvent, which is preferably located in a position opposite the input 7. In the highest Point of the chamber 1, preferably in a 9 opposite the output Range, there may be another input 10 for a gas, preferably an inert gas, such as nitrogen, argon or helium is provided.
  • a gas preferably an inert gas, such as nitrogen, argon or helium is provided.
  • the use of the described autoclave is characterized in that the pieces to be cleaned 3 a preferably continuous flow of a fluidic solvent and / or an ultrasonic energy from a stationary source 6 is exposed, the pieces 3 be moved by movement of the container 2.
  • a solvent at a critical temperature between -70 ° and 700 ° and a critical pressure between 1 and 700 bar preferably carbon dioxide, Propane, ethane, water or nitrogen protoxide, optionally with a co-solvent supports, preferably water or an organic solvent such as preferably an alcohol, an ester, an ether or a surfactant which can be pure or dissolved in said co-solvent.
  • Cleaning cycles can with the solvent in the liquid phase or in supercritical phase are alternated.

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  • Cleaning By Liquid Or Steam (AREA)

Description

Technisches GebietTechnical area

Die vorliegende Erfindung betrifft einen Autoklav zur Präzisionsreinigung von Stücken mittels eines Lösungsmittels gemäß dem Oberbegriff des Patentanspruchs 1 sowie die Verwendung dieses Autoklav.
Anwendung findet ein solcher Autoklav bei der Präzisionsreinigung von hochtechnologischen Produkten der Präzisions-, Mikro- und Nanomechanik, der Elektronik, der keramischen Industrie, der Cermets, Polymeren, Textilfasern usw.
The present invention relates to an autoclave for precision cleaning of pieces by means of a solvent according to the preamble of patent claim 1 and the use of this autoclave.
Such an autoclave is used in the precision cleaning of high-tech products in precision, micro and nanomechanics, electronics, the ceramics industry, cermets, polymers, textile fibers, etc.

Stand der TechnikState of the art

Die Präzisionsreinigungsverfahren verwenden heutzutage organische Lösungsmittel, insbesondere chlorierte organische Lösungsmittel wie Trichlorethylen und Perchlorethylen, Chlorfluorcarbide oder auch Detergentien bzw. Tenside in Wasserphase. Precision cleaning processes today use organic solvents, in particular chlorinated organic solvents such as trichlorethylene and perchlorethylene, chlorofluorocarbides or detergents or surfactants in Water phase.

Die Verwendung von chlorierten organischen Lösungsmitteln und Freonen wurde in letzter Zeit streng beanstandet, wenn nicht sogar verboten, da sie als gesundheitsschädlich und die stratosphärische Ozonschicht zerstörend eingestuft wurden. Die Wasserphasen stellen ernsthafte Probleme bezüglich der Endqualität dar, da sie sich schwer vollständig eliminieren lassen, insbesondere aus kapillaren Leitungen und Löchern, infolge des geringen Dampfdrucks des Wassers und seiner relativ hohen Viskosität im flüssigen Zustand. Zudem erzeugen sie schmutzige Gewässer, die komplexe und kostspielige Reinigungsverfahren erforderlich machen. Schliesslich erlauben all diese Verfahren schwerlich eine Rückgewinnung von verunreinigenden Substanzen, die wieder benutzt werden könnten, insbesondere wie die bei der mechanischen Bearbeitung verwendeten Schneidöle.The use of chlorinated organic solvents and freons has recently been severely criticized, if not banned, as it is considered harmful to health and classified the stratospheric ozone layer as destructive were. The water phases pose serious end-quality problems because they are difficult to eliminate completely, especially from capillary Lines and holes, due to the low vapor pressure of the water and its relatively high viscosity in the liquid state. They also create dirty waters, which require complex and costly cleaning procedures. After all, all these methods hardly permit the recovery of contaminants Substances that could be reused, especially like the cutting oils used in mechanical processing.

Aus diesen Gründen wurden seit langem mit inerten, ungiftigen Fluiden, insbesondere mit Kohlendioxid sowohl in flüssigem als auch in superkritischem Zustand, arbeitende Präzisionsreinigungsverfahren vorgeschlagen.For these reasons, have long been with inert, non-toxic fluids, in particular with carbon dioxide in both liquid and supercritical states, working precision cleaning method proposed.

Dieses Lösungsmittel, wie auch Stickstoff-Protoxid, Ethan usw. können eine gute Lösungswirkung in flüssiger Phase haben, aber sie erhöhen ihre Lösungswirkung in Dampfphase, vor allem bei schwer erreichbaren Flächen, dank der grösseren Diffusionsfähigkeit und kleineren Viskosität, die sie im Gaszustand erreichen. Im superkritischen Zustand (Temperatur höherer als die kritische und Druck ebenfalls höher als der kritische) erreichen sie eine hohe Dichte mit nahe den für Flüssigkeiten wie das Wasser typischen Werten. Die Verbindung beider Eigenschaften (niedrige Viskosität und hohe Dichte) macht aus ihnen ideale Lösungsmittel für Präzisionsreinigungsverfahren, die einen hohen Reinigungsgrad in jedem Punkt der Oberfläche und in den schwer erreichbaren Partien garantieren müssen.This solvent, as well as nitrogen protoxide, ethane, etc. can be a have good solubility in the liquid phase but they increase their solubility in vapor phase, especially in difficult to reach areas, thanks to the larger ones Diffusivity and lower viscosity that they reach in the gas state. in the supercritical state (temperature higher than the critical and pressure also higher than the critical one) they reach a high density close to those for liquids like the water typical values. The combination of both properties (low Viscosity and high density) makes them ideal solvents for precision cleaning processes, which has a high degree of cleaning in every point of the surface and in the hard-to-reach games.

Diese Lösungsmittel erweisen sich als besonders wirksam für unpolare oder wenig polare verunreinigende Substanzen; polare organische Substanzen wie Zusätze zu Schneidölen, Salzen, Schleifmitteln und Metallen sind nicht merklich lösbar in den Lösungsmitteln, die zur Reinigung in der superkritischen Phase geeignet sind. Solche in der festen Phase an den zu reinigenden Flächen durch Adhäsion oder Adsorption zurückgebliebenen Resten müssen mit physischen Mitteln aus denselben entfernt werden: Zu diesem Zweck wird die Wirksamkeit der Kavitation erkannt, die über die Flächen zustande kommt, die in einer Flüssigkeit eingetaucht sind, durch die sich Ultraschallwellen fortpflanzen.These solvents prove to be particularly effective for nonpolar or little polar polluting substances; Polar organic substances such as additives to cutting oils, salts, abrasives and metals are not noticeably solvable in solvents suitable for cleaning in the supercritical phase are. Such in the solid phase on the surfaces to be cleaned by adhesion or adsorption remaining residues must by physical means of the same be removed: For this purpose, the effectiveness of cavitation is recognized, which comes about over the areas that are immersed in a liquid are, through which propagate ultrasonic waves.

In den Vereinigten Staaten von Amerika wurden Pionierarbeiten über Präzisionsreinigungsverfahren durch Verwendung von flüssigem und superkritischem Kohlendioxid vom National Laboratory, Los Alamos, von Autoclaves Engineering und von Hughes Aircraft angebahnt und durchgeführt, in Frankreich von CEA, Separex. Seit 1986 sind zahlreiche Patentanmeldungen eingereicht worden.In the United States, pioneering work has been done on precision cleaning processes by using liquid and supercritical Carbon dioxide from the National Laboratory, Los Alamos, by Autoclaves Engineering and initiated and carried out by Hughes Aircraft, in France by CEA, Separex. Since 1986, numerous patent applications have been filed.

Nach diesen Patenten wird die Fortpflanzung der Ultraschallwellen im Autoklav durch sich im Innern der Kammer selbst befindende Generatoren bewirkt. Nach anderen Patenten erfolgt die mechanische Entfernung der festen Teilchen und der Flüssigkeiten durch am Eingang des Lösungsmittels angeordnete Ventile, um Turbulenzen zu erzeugen, oder durch Erzeugung von Blasen, derart, dass das Lösungsmittel bei einer dem Siedepunkt nahen Temperatur gehalten wird, oder noch durch eine mittels Propellern oder festen Elementen bewirkte Bewegung des flüssigen Lösungsmittels. In anderen Fällen werden noch bezüglich der Ladung feste oder bewegliche Bürsten verwendet. According to these patents, the propagation of ultrasonic waves in the autoclave caused by itself inside the chamber itself located generators. To other patents, the mechanical removal of the solid particles and the Liquids through arranged at the entrance of the solvent valves to turbulence to generate, or by generating bubbles, such that the solvent is kept at a near the boiling point temperature, or even by a movement of the liquid effected by means of propellers or solid elements Solvent. In other cases, the charge is still solid or movable brushes used.

So ist aus US 5,944,996 ein gattungsgemässer Reinigungsprozess mit Lösungsmitteln bekannt, bei dem vorzugsweise auch eine Ultraschallbehandlung angewendet werden soll. Die zu reinigenden Stücke befinden sich in einer motorisch angetriebenen, drehbaren Trommel im Inneren des Ultraschallbades. Als Lösungsmittel wird gasförmiges, flüssiges bzw. bevorzugt superkritisches CO2 verwendet. Dieses Dokument offenbart jedoch nicht, wie eine Ultraschallquelle zur Verwendung in diesem Verfahren angeordnet bzw. ausgebildet sein soll.Thus, US Pat. No. 5,944,996 discloses a generic cleaning process using solvents, in which preferably an ultrasound treatment is also to be used. The pieces to be cleaned are located in a motor-driven, rotatable drum inside the ultrasonic bath. The solvent used is gaseous, liquid or preferably supercritical CO 2 . However, this document does not disclose how to arrange an ultrasound source for use in this method.

US 5,759,209 offenbart ein Reinigungsverfahren für welches verflüssigtes Gas (vorzugsweise CO2) unter Druck in ein Druckgefäss mit zu reinigenden Objekten geleitet wird. Zum Reinigen dieser Objekte wird das Flüssiggas zumindest anfänglich auf -20 °C bis +20 °C abgekühlt und bei entsprechend hohem Druck und ohne jede Anwendung von Ultraschall im flüssigen Zustand gehalten.US 5,759,209 discloses a purification process for which liquefied gas (preferably CO 2 ) is passed under pressure into a pressure vessel with objects to be cleaned. To clean these objects, the liquefied gas is at least initially cooled to -20 ° C to + 20 ° C and kept at a correspondingly high pressure and without any use of ultrasound in the liquid state.

US 4,922,939 offenbart eine einfache Vorrichtung zum Reinigen von Zahnprothesen in einem Reinigungsmittelbehälter. Die zu reinigenden Objekte befinden sich in einer in diesem Behälter drehbaren Trommel. Die Behälterwand umfasst fixe Paddel und die Trommelwand umfasst ebenfalls Paddel und Öffnungen. Durch die Rotation der Trommel werden durch die erwähnten Paddel und Öffnungen starke Strömungen und Turbulenzen in der Reinigungsflüssigkeit erzeugt, so dass die Zahnprothesen ohne Anwendung von Ultraschall gereinigt werden.US 4,922,939 discloses a simple device for cleaning dentures in a detergent container. The objects to be cleaned are located in a drum rotatable in this container. The container wall comprises Fixed paddle and the drum wall also includes paddles and openings. Through the rotation of the drum are through the mentioned paddles and openings generates strong currents and turbulences in the cleaning fluid, so that the dentures cleaned without application of ultrasound become.

Auch EP 0 893 166 offenbart Reinigungsbäder mit Lösungsmitteln, deren physikalischer Zustand sich nahe dem Kritischen Punkt (unterkritisch oder überkritisch) befindet. Diese Reinigungsbäder umfassen je zwei sich gegenüber liegende Ultraschallquellen, welche einen dazwischen liegenden Propeller antreiben, womit der Reinigungseffekt verbesserte werden soll. Auch dieses Dokument schweigt über die genaue Anordnung und Ausbildung der Ultraschallquellen. Also EP 0 893 166 discloses cleaning baths with solvents whose physical State near the critical point (subcritical or supercritical) located. These cleaning baths each comprise two opposite ones Ultrasonic sources driving an intermediate propeller, whereby the cleaning effect should be improved. Also this document is silent about the exact arrangement and design of the ultrasound sources.

EP 0 894 542 offenbart ein Reinigungsverfahren, das aus einer Waschbehandlung mit einer oberflächenaktiven Substanz und Ultraschallkavitation sowie aus einem anschliessenden Trocknungsschritt mit einem organischen Lösungsmittel (z.B. Isopropanol oder Aceton) oder entsprechenden Dämpfen besteht. Anschliessend wird die Wasch- und Trockenvorrichtung vorzugsweise mit Druckluft ausgeblasen.EP 0 894 542 discloses a cleaning process resulting from a washing treatment with a surface-active substance and ultrasonic cavitation as well a subsequent drying step with an organic solvent (e.g., isopropanol or acetone) or corresponding vapors. Subsequently the washing and drying device is preferably compressed air blown out.

DE 197 41 836 offenbart eine als Ultraschallbad ausgebildete Reinigungsvorrichtung mit einer in die Reinigungsflüssigkeit (destilliertes Wasser) eingetauchten Schwingerplatte, an der mehrere Schwingungserzeuger befestigt sind. Diese Schwingungserzeuger sind mit einem Hochfrequenzgenerator verbunden und regen die Schwingerplatte zu mechanischen Schwingungen an, was zu Druckschwankungen im Wasser führt. Diese Druckschwankungen erzeugen im Wasser Über- und Unterdruckphasen, die bei entsprechender Frequenz zu dem bekannten Kavitationseffekt führen.DE 197 41 836 discloses a cleaning device designed as an ultrasonic bath with an immersed in the cleaning liquid (distilled water) Schwingerplatte to which several vibrators are attached. These Vibration generators are connected to a high frequency generator and stimulate the vibrating plate to mechanical vibrations, causing pressure fluctuations in the water. These pressure fluctuations generate in the water Over and under pressure phases, which at a corresponding frequency to the known Cause cavitation effect.

US 5,858,107 offenbart als Ultraschallpfeifen ausgebildete Düsen, durch welche flüssiges CO2 gepresst wird. Solche Düsen eignen sich jedoch nicht für die Erzeugung von Ultraschallwellen in superkritischem CO2.US 5,858,107 discloses formed as ultrasonic whistle nozzles through which liquid CO 2 is pressed. However, such nozzles are not suitable for generating ultrasonic waves in supercritical CO 2 .

Die Aufgabe der vorliegenden Erfindung besteht somit darin, einen Autoklav gemäss dem Oberbegriff des Anspruchs 1 vorzuschlagen, welcher zur Erzeugung von Ultraschallwellen in flüssigem und in superkritischem CO2 geeignet ist.The object of the present invention is thus to propose an autoclave according to the preamble of claim 1, which is suitable for generating ultrasonic waves in liquid and supercritical CO 2 .

Diese Aufgabe wird gelöst, indem ein Autoklav mit den Merkmalen des Anspruchs 1 vorgeschlagen wird. Ferner wird diese Aufgabe nach der Erfindung durch die Verwendung dieses Autoklavs gemäß Patentanspruch 9 gelöst.This object is achieved by an autoclave having the features of the claim 1 is proposed. Furthermore, this object is achieved according to the invention by the use of this autoclave according to claim 9.

Weitere, erfindungsgemässe Merkmale ergeben sich aus den betreffenden abhängigen Ansprüchen. Further, inventive features revealed from the respective dependent claims.

Zeichnungdrawing

Weitere Eigenschaften und Vorteile der Erfindung werden im folgenden anhand der Beschreibung und mit Bezug auf die Zeichnung ausführlich beschrieben. Es zeigt:

  • Fig. 1 eine schematische Darstellung einer Ausführungsform der Erfindung.
  • Further characteristics and advantages of the invention will be described in detail below with reference to the description and with reference to the drawing. It shows:
  • Fig. 1 is a schematic representation of an embodiment of the invention.
  • Detaillierte Beschreibung der ErfindungDetailed description of the invention

    Gegenstand der Erfindung ist ein Autoklav zur Präzisionsreinigung von Flächen mit komplexen Formen durch Verwendung von inerten flüssigen oder superkritischen Fluiden als Lösungsmitteln, und zwar unterstützt durch Bestrahlung der zu reinigenden Flächen mit Ultraschallwellen und durch die sich daraus ergebende Kavitation bei einer programmierten Bewegung der zu reinigenden Stücke, sowie die Verwendung dieses Autoklavs.The invention relates to an autoclave for precision cleaning of surfaces with complex shapes through the use of inert liquid or supercritical fluids as solvents, and indeed supported by irradiation of the surfaces to be cleaned with ultrasonic waves and by the resulting cavitation in a programmed movement of the to be cleaned Pieces, as well as the use of this autoclave.

    Bei geeigneten Bedingungen bezüglich Temperatur, Druck und Menge des Fluids werden durch die lösende Wirkung des flüssigen und/oder superkritischen Fluids die in ihm lösbaren flüssigen oder festen verunreinigenden Substanzen aus den Oberflächen entfernt. Durch den Kavitationseffekt werden hingegen die festen unlösbaren Teilchen, wie klebende metallische Teilchen, sich aus den Schleifmittein, den organischen und anorganischen Zusätzen usw. ergebender Staub, von der Oberfläche abgetrennt und danach in Suspension durch die Fluidströmung entfernt. Für die industriellen Anwendungen der Vorrichtung nach der vorliegenden Erfindung, sowohl im kontinuierlichen als auch im diskontinuierlichen oder halbkontinuierlichen Betrieb ist davon auszugehen, dass in der Reinigungskammer eine variable Anzahl Stücke vorhanden ist, deren Oberflächen genau und regelmässig gereinigt werden sollen: Dies bedeutet, dass solche Teile derart bewegt werden, dass sie früher oder später direkt der Aktion der Ultraschallwellen ausgesetzt sind. Dies wird in einer vorzugsweise zylindrischen Kammer realisiert, die mit an der äusseren Fläche derselben Kammer angeordneten Ultraschallgeneratoren versehen ist, die sich durch die gesamte Längsfläche im Innern der Kammer fortpflanzende Ultraschallwellen erzeugen, so dass ein Kavitationseffekt im die Kammer durchfliessenden oder sich dort in flüssiger oder superkritischer Phase befindenden Fluid bewirkt wird. In der Kammer wird ein Behälter in Form einer Trommel mit den Stücken gestellt, der mit Hilfe eines äusseren Elektromotors drehbar ist. Diese Trommel kann mit mittigen Achsen versehen sein oder nicht. Darin sind die Stücke frei, sich bezüglich der Wand der Trommel zu bewegen. Die Basen und die Mantelfläche der Trommel sind in Form von Gittern ausgebildet, die den Durchgang der Ultraschallwellen und zugleich ein Ausscheiden der festen schweren Teilchen erlauben, die sich von der Fläche der Stücke ablösen.With suitable conditions regarding temperature, pressure and amount of Fluids are caused by the solvent action of the liquid and / or supercritical Fluids from the solvable in him liquid or solid contaminants removed from the surfaces. Due to the cavitation effect, however, the solid insoluble particles, such as sticky metallic particles, arising from the abrasives, the organic and inorganic additives, etc. resulting dust, from the Surface separated and then removed in suspension by the fluid flow. For industrial applications of the device according to the present invention, both continuous and discontinuous or semi-continuous Operation is assumed that in the cleaning chamber a variable Number of pieces is present, the surfaces cleaned accurately and regularly This means that such parts are moved in such a way that they Sooner or later the action of ultrasonic waves is directly exposed. this will realized in a preferably cylindrical chamber, which with on the outer surface The same chamber arranged ultrasonic generators is provided, which is ultrasonic waves propagating through the entire longitudinal surface inside the chamber generate, so that a cavitation effect in the chamber flowing through or is caused there in liquid or supercritical fluid phase. In the chamber, a container is placed in the form of a drum with the pieces, which is rotatable by means of an external electric motor. This drum can be with central Axes be provided or not. In it, the pieces are free, regarding the Wall of the drum to move. The bases and the lateral surface of the drum are formed in the form of lattices that control the passage of ultrasonic waves and at the same time allow the solid heavy particles to separate out from the Remove the surface of the pieces.

    Eine in Sinn und Geschwindigkeit geeignete, hauptsächlich während der Bestrahlung mit Ultraschall bewirkte Drehung der Trommel ermöglicht eine Aussetzung der Stücke der Bestrahlung der Ultraschallwellen und eine sich über die Oberfläche der Gesamtheit aller Stücke ausbreitende Kavitation. Dies erweist sich als besonders vorteilhaft bei einer umfangreichen Belastung mit Stücken, wie Schrauben, Kugeln, Körpern mit unregelmässiger Geometrie, da sie sich während der Bewegung gegenseitig reiben. Die Rücknahme der Stücke wird zudem dadurch erleichtert, dass sie sich im Innern einer Trommel befinden, die zu Beginn in die Kammer eingeführt und am Ende herausgenommen wird. Auch die Entfernung der festen Teile in Suspension wird durch die eine Befreiung derselben bewirkende Bewegung erleichtert. Die Möglichkeit, die Rotationsgeschwindigkeit der Trommel zu modulieren, erlaubt eine Dosierung der mechanischen Reibung zwischen den Stücken, um Schäden zu vermeiden. Bei normalen Betriebsbedingungen mit Ladungen von 40 bis 80 Kg in einer 10-Liter-Kammer können Rotationsgeschwindigkeiten von 1 bis 100 Umdrehungen pro Minute während 10 bis 20 Minuten mit 1 bis 2 Drehsinnänderungen vorgesehen werden. Die vorgesehene Leistung liegt im allgemeinen in der Grössenordnung von 1000 W und die Frequenz zwischen 10 und 2000 kHz in Abhängigkeit von den Abmessungen der von der Oberfläche der Stücke abzureibenden festen Teilchen.An appropriate in sense and speed, mainly during the irradiation Ultrasound rotation of the drum allows suspension of the pieces of irradiation of the ultrasonic waves and one over the surface the totality of all pieces of propagating cavitation. This turns out to be particularly advantageous in an extensive load with pieces, such as Screws, balls, bodies with irregular geometry, as they move during rub each other's movements. The return of the pieces is also facilitated by being inside a drum at the beginning introduced into the chamber and taken out at the end. Also the Removal of the solid parts in suspension is through the one liberation of the same facilitating movement. The possibility of the rotation speed To modulate the drum allows a dosage of mechanical Friction between the pieces to avoid damage. In normal operating conditions with loads of 40 to 80 kg in a 10-liter chamber can rotate at speeds of 1 to 100 revolutions per minute during 10 to 20 minutes with 1 to 2 changes of rotation. The envisaged power is generally of the order of 1000 W and the frequency between 10 and 2000 kHz depending on the dimensions the solid particles to be ablated from the surface of the pieces.

    Die technische Beschreibung der Erfindung ergibt sich an Hand der Fig. 1. Die Einrichtung besteht aus einem Autoklav, in welchen die Trommel, bzw. der Behälter 2 eingeführt wird, in der bzw. in welchem sich die Stücke 3 befinden, die dem Präzisionsreinigungsprozess unterworfen werden sollen. Die Trommel bzw. der Behälter 2 wird durch den Motor 4 über eine Achse 5 angetrieben. An der äusseren zylindrischen Fläche der Wand 11 des Autoklavs sind Ultraschallwandler 6 angeordnet, die über die gesamte Innenseite der Wand 11 einen Grossteil der Stücke 3 radial bestrahlen. Im Innern bzw. im Innenraum 12 des Autoklavs erfolgt daher der Präzisionsreinigungsprozess durch die Wirkung des Lösungsmittels im flüssigen und/oder superkritischen Zustand, oder abwechslungsweise im flüssigen und superkritischen Zustand.The technical description of the invention will become apparent with reference to FIG. 1. Die Device consists of an autoclave, in which the drum, or the container 2 is introduced, in which or in which the pieces are 3, the to be subjected to the precision cleaning process. The drum or the container 2 is driven by the motor 4 via an axis 5. At the outer cylindrical surface of the wall 11 of the autoclave are ultrasonic transducers 6 arranged over the entire inside of the wall 11 a majority irradiate the pieces 3 radially. Inside or in the interior 12 of the autoclave takes place therefore the precision cleaning process by the action of the solvent in the liquid and / or supercritical state, or alternately in the liquid state and supercritical state.

    Das Fluid kann im Autoklav nach Vorwärmung oder bei Raumtemperatur über den Eingang 7 befördert und zudem durch Verdampfung über die Ausgänge 8 und 9 gekühlt werden. Eine übermässige Abkühlung der Ladungskammer bzw. Kammer 1 während der Depressionsphase kann durch Einführung eines inerten Gases mit geeignetem Druck durch den Eingang 10 vermieden werden.The fluid can be in the autoclave after preheating or at room temperature transported the input 7 and also by evaporation via the outputs 8 and 9 are cooled. Excessive cooling of the charge chamber or Chamber 1 during the depression phase can by introducing an inert Gas with appropriate pressure through the input 10 can be avoided.

    Temperaturen, Abwechslung und Dauer der Reinigungszyklen in der flüssigen und superkritischen Phase, die Bewegungen der Trommel, bzw. des Behälters 2 mit den zu reinigenden Stücken 3 (Drehsinn, Drehsinnwechsel, Zeiten und Geschwindigkeit), Druck und Menge des Lösungsmittel werden durch einen Computer (nicht in Fig. 1 dargestellt) und ein spezifisches Programm geregelt.Temperatures, variety and duration of cleaning cycles in the liquid and supercritical phase, the movements of the drum, or the container. 2 with the pieces 3 to be cleaned (sense of rotation, change of rotation, times and speed), Pressure and amount of solvent are controlled by a computer (not shown in FIG. 1) and a specific program.

    Sowohl die losgelösten Substanzen in der flüssigen oder hauptsächlich superkritischen Phase, als auch die festen Teilchen in Suspension werden von der Ladungskammer bzw. Kammer 1 durch eine Fluidströmung heraus befördert.Both the dissolved substances in the liquid or mainly supercritical Phase, as well as the solid particles in suspension are from the charge chamber or chamber 1 transported by a fluid flow out.

    Die Rückgewinnung der Flüssigkeiten und der von der Oberfläche der Stücke 3 abgeriebenen festen Teile, wie auch ein Rezyklieren des Lösungsmittels erfolgen durch Druckverminderung, Filtrierung und Adsorption und Umpumpen gemäss bekannter Technologie.The recovery of the liquids and of the surface of the pieces 3 abraded solid parts, as well as a recycling of the solvent carried out by pressure reduction, filtration and adsorption and pumping according to known technology.

    Für den Fall, dass sich die Lösungsfähigkeit des inerten Fluids als ungenügend erweisen sollte, kann die Möglichkeit der Verwendung eines Mitlösungsmittels vorgesehen werden.In the event that the solubility of the inert fluid is insufficient The possibility of using a co-solvent may prove be provided.

    Eine weitere Ausführungsform zeichnet sich dadurch aus, dass der Behälter 2 in beiden Drehrichtungen drehbar ist, und dass die Möglichkeit besteht, den Drehsinn und/oder die Drehgeschwindigkeit zu ändern. Dies geschieht vorzugsweise in programmierter Form.Another embodiment is characterized in that the Container 2 is rotatable in both directions of rotation, and that possibility exists to change the sense of rotation and / or the rotational speed. this happens preferably in programmed form.

    Der Autoklav kann auch mit an der inneren Wand des Behälters 2 oder an einer Achse angeordneten Schaufeln versehen sein, um eine geführte Bewegung der Stücke 3 zu ermöglichen. Die Ultraschallwandler 6 können an der äusseren Wand 11 der Ladungskammer bzw. Kammer 1 angeordnet sein, vorzugsweise an jener mit der grösseren Ausdehnung.The autoclave can also be attached to the inner wall of the container 2 or arranged on an axis blades to be a to allow guided movement of the pieces 3. The ultrasonic transducers 6 can arranged on the outer wall 11 of the charge chamber or chamber 1 be, preferably at that with the greater extent.

    Bei einem Autoklav kann sich der Eingang 7 für das Lösungsmittel im tiefsten Punkt im Innern der Kammer 1 befinden und der Ausgang 9 im höchsten Punkt. Des Weiteren kann sich im tiefsten Punkt der Kammer 1 ein Ausgang 8 für das Lösungsmittel befinden, wobei dieser sich vorzugsweise in einer dem Eingang 7 gegenüberliegenden Lage befindet. Im höchsten Punkt der Kammer 1, vorzugsweise in einem dem Ausgang 9 gegenüberliegenden Bereich, kann ein weiterer Eingang 10 vorhanden sein, der für ein Gas, vorzugsweise ein inertes Gas, wie Stickstoff, Argon oder Helium vorgesehen ist.In an autoclave, the input 7 for the solvent is located at the lowest point inside the chamber 1 and the Exit 9 at the highest point. Furthermore, at the lowest point of the Chamber 1 is an outlet 8 for the solvent, which is preferably located in a position opposite the input 7. In the highest Point of the chamber 1, preferably in a 9 opposite the output Range, there may be another input 10 for a gas, preferably an inert gas, such as nitrogen, argon or helium is provided.

    Die Verwendung des beschriebenen Autoklavs zeichnet sich dadurch aus, dass die zu reinigenden Stücke 3 einem vorzugsweise kontinuierlichen Fluss eines fluidischen Lösungsmittels und/oder einer Ultraschallenergie aus einer stationären Quelle 6 ausgesetzt wird, wobei die Stücke 3 durch Bewegung des Behälters 2 bewegt werden.The use of the described autoclave is characterized in that the pieces to be cleaned 3 a preferably continuous flow of a fluidic solvent and / or an ultrasonic energy from a stationary source 6 is exposed, the pieces 3 be moved by movement of the container 2.

    Eine weitere Ausführungsform der Verwendung zeichnet sich dadurch aus, dass ein Lösungsmittel bei einer kritischen Temperatur zwischen -70° und 700° und einem kritischen Druck zwischen 1 und 700 bar, vorzugsweise Kohlendioxid, Propan, Ethan, Wasser oder Stickstoffprotoxid, gegebenenfalls durch ein Mitlösungsmittel unterstützt, vorzugsweise Wasser oder ein organisches Lösungsmittel wie vorzugsweise ein Alkohol, ein Ester, ein Ether oder ein Tensid verwendet wird, das rein oder im besagten Mitlösungsmittel gelöst sein kann. Another embodiment of the use is characterized in that a solvent at a critical temperature between -70 ° and 700 ° and a critical pressure between 1 and 700 bar, preferably carbon dioxide, Propane, ethane, water or nitrogen protoxide, optionally with a co-solvent supports, preferably water or an organic solvent such as preferably an alcohol, an ester, an ether or a surfactant which can be pure or dissolved in said co-solvent.

    Reinigungszyklen können mit dem Lösungsmittel in flüssiger Phase bzw. in superkritischer Phase alterniert werden.Cleaning cycles can with the solvent in the liquid phase or in supercritical phase are alternated.

    Bei einer weiteren Ausführungsform der Verwendung wird durch die Einwirkung von bezüglich Dauer, Intensität und/oder Frequenz programmierten Ultraschallwellen ein Kavitationseffekt auf den Flächen der zu reinigenden Stücke 3 bewirkt.In another embodiment of the use is programmed by the action of duration, intensity and / or frequency Ultrasonic waves a cavitation effect on the surfaces to be cleaned Pieces 3 causes.

    Claims (12)

    1. Autoclave for precision cleaning of parts (3) by means of a solvent, which may be in either liquid or supercritical phase, and by means of ultrasonic energy, the autoclave comprising a load chamber (1) in the form of a pressure chamber with an outer wall (11) surrounding an inner space (12), a container (2) arranged inside the inner space (12) and movable by means of a motor (4) and ultrasonic transducers (6), characterized in that the outer wall (11) is constructed to be massive enough to withstand internal pressures in the range 40 to 700 bar, and the ultrasonic transducers (6) being arranged on the outer surface of this massive outer wall (11).
    2. Autoclave according to Claim 1, characterized in that the load chamber (1) is cylindrical in shape and the ultrasonic transducers (6) are arranged on the cylindrical outer surface of this massive wall (11), so that a high proportion of the parts (3) can be irradiated radially through the whole cylindrical inner surface of the wall (11).
    3. Autoclave according to Claim 2, characterized in that a single ultrasonic transducer (6) is arranged on the cylindrical outer surface of this massive wall (11).
    4. Autoclave according to any one of the above Claims, characterized in that the container (2) can be rotated in either direction, is made so that it can be removed from the autoclave and is provided with walls in the form of grids to enable the transport from the load chamber (1) of solid particles that become detached from the parts (3).
    5. Autoclave according to any one of the above Claims, characterized in that the outer wall (11) is designed to withstand temperatures in the range from -70°C to 700°C.
    6. Autoclave according to any one of the above Claims, characterized in that the container (2) is equipped with paddles located on its inner wall or attached to an axle in order to impart guided movement to the parts (3).
    7. Autoclave according to any one of the above Claims, characterized in that an inlet (7) for the solvent is provided at the lowest point of the inner space (12) of the load chamber (1) and an outlet (9) at its highest point, and/or an outlet (8) for the solvent is provided at the lowest point of the load chamber (1), preferably in a position opposite the inlet (7).
    8. Autoclave according to any one of the above Claims, characterized in that at the highest point of the load chamber (1), preferably in the zone opposite to the outlet (9), an additional inlet (10) is provided intended for a gas, preferably an inert gas, such as nitrogen, argon or helium.
    9. Use of the autoclave according to any one of Claims 1 to 8 for the precision cleaning of parts (3), characterized in that the parts (3) are subjected to the action of a fluid solvent and ultrasonic energy from a stationary source, and that the parts are moved by movement of the container (2).
    10. Use of the autoclave according to Claim 9, characterized in that a solvent is used at a critical temperature between -70°C and 700°C and a critical pressure between 1 and 700 bar, this solvent being preferably carbon dioxide, propane, ethane, water or nitrogen protoxide, if necessary supported with another solvent, preferably water or an organic solvent such as preferably an alcohol, an ester, an ether or a surfactant, which may be pure or dissolved in the aforementioned solvent.
    11. Use of the autoclave according to Claim 9 or 10, characterized in that the cleaning cycles are performed with the solvent in liquid and supercritical phase alternately, and/or the load is moved in accordance with programmed movements in cycles characterized by the direction and/or speed of rotation of the container (2), the duration of the movement phase in both directions of rotation, alternation of the phases and/or number of cycles, or by pressure changes in the inner space (12) of the load chamber (1).
    12. Use of the autoclave according to any one of Claims 9 to 11, characterized in that the use of ultrasonic waves programmed with respect to duration, intensity and/or frequency exerts an effect of cavitation on the surfaces of the parts (3) to be cleaned.
    EP01953012A 2000-02-18 2001-02-06 Autoclave for the precision cleaning of objects and use of the autoclave Expired - Lifetime EP1255621B1 (en)

    Applications Claiming Priority (3)

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    CH3122000 2000-02-18
    CH312002000 2000-02-18
    PCT/IB2001/000148 WO2001060534A1 (en) 2000-02-18 2001-02-06 Device and method for the precision cleaning of objects

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    EP1255621B1 true EP1255621B1 (en) 2005-08-31

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    US7267727B2 (en) 2002-09-24 2007-09-11 Air Products And Chemicals, Inc. Processing of semiconductor components with dense processing fluids and ultrasonic energy
    US20050029492A1 (en) 2003-08-05 2005-02-10 Hoshang Subawalla Processing of semiconductor substrates with dense fluids comprising acetylenic diols and/or alcohols
    US7195676B2 (en) 2004-07-13 2007-03-27 Air Products And Chemicals, Inc. Method for removal of flux and other residue in dense fluid systems
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    US9597458B2 (en) 2009-10-29 2017-03-21 W. L. Gore & Associates, Inc. Fluoropolymer barrier materials for containers
    US11612697B2 (en) 2010-10-29 2023-03-28 W. L. Gore & Associates, Inc. Non-fluoropolymer tie layer and fluoropolymer barrier layer
    WO2012142479A1 (en) * 2011-04-15 2012-10-18 W.L. Gore & Associates, Inc. Method of reducing friction between syringe components
    DE102015222247B4 (en) * 2015-11-11 2017-10-26 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Method and device for processing capillary tubes

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    JP3209426B2 (en) * 1991-10-04 2001-09-17 シーエフエムティ インコーポレイテッド Cleaning microparts with complex shapes
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    US5783082A (en) * 1995-11-03 1998-07-21 University Of North Carolina Cleaning process using carbon dioxide as a solvent and employing molecularly engineered surfactants
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