ES2205290T3 - PROCESS TO TREAT THE SURFACE OF ARTICLES MADE OF TITANIUM AND ITS ALLOYS. - Google Patents
PROCESS TO TREAT THE SURFACE OF ARTICLES MADE OF TITANIUM AND ITS ALLOYS.Info
- Publication number
- ES2205290T3 ES2205290T3 ES98102510T ES98102510T ES2205290T3 ES 2205290 T3 ES2205290 T3 ES 2205290T3 ES 98102510 T ES98102510 T ES 98102510T ES 98102510 T ES98102510 T ES 98102510T ES 2205290 T3 ES2205290 T3 ES 2205290T3
- Authority
- ES
- Spain
- Prior art keywords
- sealed
- process according
- neutral atmosphere
- container
- molded
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/24—Nitriding
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Electrochemistry (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
- Apparatus For Disinfection Or Sterilisation (AREA)
- Dental Tools And Instruments Or Auxiliary Dental Instruments (AREA)
Abstract
SE DESCRIBE UN PROCEDIMIENTO Y APARATO PARA TRATAR, EN ATMOSFERA CONTROLADA, LA SUPERFICIE DE ARTICULOS REALIZADOS CON TITANIO Y SUS ALEACIONES, PARTICULARMENTE PARA PROTESIS Y SIMILARES EN LA CAVIDAD ORAL. TODAS LAS OPERACIONES EXIGIDAS PARA OBTENER UN ARTICULO ACABADO SE DESARROLLAN BAJO ATMOSFERA NEUTRA Y CONTROLADA, CON EL FIN DE OBTENER UN ARTICULO ACABADO PROTEGIDO POR UNA PELICULA FUERTEMENTE ADHERIDA Y QUE TIENE UN ASPECTO DELGADO Y FINO.A PROCEDURE AND APPARATUS ARE DESCRIBED TO TREAT, IN CONTROLLED ATMOSPHERE, THE SURFACE OF ARTICLES MADE WITH TITANIUM AND ITS ALLOYS, PARTICULARLY FOR PROTESIS AND SIMILAR IN ORAL CAVITY. ALL THE OPERATIONS REQUIRED TO OBTAIN A FINISHED ARTICLE ARE UNDERTAKEN UNDER NEUTRAL AND CONTROLLED ATMOSPHERE, IN ORDER TO OBTAIN A FINISHED ARTICLE PROTECTED BY A STRONGLY ADHERED FILM AND THAT HAS A THIN AND FINE ASPECT.
Description
Proceso para tratar la superficie de artículos hechos de titanio y sus aleaciones.Process to treat the surface of articles Made of titanium and its alloys.
La presente invención se refiere a un proceso para tratar en una atmósfera controlada la superficie de piezas y artículos hechos de titanio y sus aleaciones o metales similares. Los artículos se forman preferentemente mediante moldeo a la cera perdida, en particular para su utilización en dentistería protésica, ortodoncia y similares.The present invention relates to a process to treat the surface of parts in a controlled atmosphere and Articles made of titanium and its alloys or similar metals. The items are preferably formed by wax molding lost, particularly for use in dentistry prosthetic, orthodontics and the like.
Es bien conocido que el titanio tiene unas propiedades peculiares tales como la afinidad con O_{2} y H, y se oxida fácilmente a elevada temperatura con independencia de la presión parcial del O_{2}.It is well known that titanium has some peculiar properties such as affinity with O2 and H, and it easily oxidizes at high temperature regardless of partial pressure of O2.
Por consiguiente, el moldeo que utiliza el método tradicional a la cera perdida exige trabajar en una atmósfera neutra (de argón u otros gases nobles).Therefore, the molding that uses the method traditional lost wax requires working in an atmosphere neutral (from argon or other noble gases).
Hoy hay comercializados aparatos automáticos equipados con un arco eléctrico para fundir el material y adaptados para verter el titanio fundido en un cilindro de moldeo en una atmósfera neutra, tal como un gas inerte.Today there are commercialized automatic devices equipped with an electric arc to melt the material and adapted to pour the molten titanium into a molding cylinder in a neutral atmosphere, such as an inert gas.
Estos aparatos son satisfactorios pero su difusión es algo limitada debido a los elevados costes de la planta y a la demanda limitada (en la actualidad) ya que ahora los talleres especializados sólo suministran piezas "pasivadas", es decir, piezas que han sido sometidas a un tratamiento superficial de pasivación que es completamente inadecuado.These devices are satisfactory but their diffusion is somewhat limited due to high plant costs and to the limited demand (at present) since now the specialized workshops only supply "passivated" parts, it is that is, parts that have undergone a surface treatment of passivation that is completely inappropriate.
De hecho, esa pasivación es decididamente cuestionable desde el punto de vista estético ya que confiere al artículo un aspecto grisáceo oscuro y mate; en realidad, implica una oxidación profunda que carece de calidad estética.In fact, that passivation is decidedly questionable from the aesthetic point of view as it confers on article a dark gray and matt appearance; actually implies a deep oxidation that lacks aesthetic quality.
Se ha objetado fuertemente la mala biocompatibilidad del oro y de sus aleaciones, así como de las aleaciones de Cr, Co, Ag y Ga y otros metales actualmente utilizados en los dispositivos protésicos y en dispositivos para corregir defectos para su uso en la cavidad oral.The bad one has been strongly objected biocompatibility of gold and its alloys, as well as the Cr, Co, Ag and Ga alloys and other metals currently used in prosthetic devices and devices for Correct defects for use in the oral cavity.
Por consiguiente, es deseable proporcionar a los operadores médicos alternativas viables al uso del oro, cromo-cobalto y también del llamado acero "quirúrgico" que hasta hoy ha sido parte principal de la mayoría de los materiales utilizados en el campo de la prótesis dental, la corrección ortodóntica y la implantación debajo del periostio.Therefore, it is desirable to provide the alternative medical operators viable to the use of gold, chrome-cobalt and also called steel "surgical" that until now has been a main part of the most of the materials used in the field of prostheses Dental, orthodontic correction and implantation under the periosteum.
Como ya se ha mencionado, hay aparatos conocidos para moldear artículos de titanio en una atmósfera neutra utilizando un arco eléctrico para fundir el material y utilizando óxido de zirconio como revestimiento del cilindro de moldeo. Aunque los resultados son aceptables en general, este proceso conocido se lleva a cabo después de la fusión y con el cilindro lleno de metal fundido, lo que no es recomendable. La temperatura del cilindro es alta, alrededor de 800°C, y no es conveniente abrir la máquina de fusión y moldeo para extraer el cilindro y sumergirlo en agua, renunciando así a la atmósfera controlada. De esta manera, se consigue un enfriamiento rápido del metal con una oxidación simultánea (profunda o superficial) del artículo, y una fuerte contaminación de hidrógeno, lo que hace el artículo quebradizo y provoca la formación de óxidos superficiales de color gris oscuro que son estéticamente muy desagradables (pasivación).As already mentioned, there are known devices to mold titanium items in a neutral atmosphere using an electric arc to melt the material and using Zirconium oxide as coating of the molding cylinder. Even if the results are generally acceptable, this known process is carried out after melting and with the cylinder full of metal cast, which is not recommended. The temperature of the cylinder is high, around 800 ° C, and it is not convenient to open the machine melting and molding to extract the cylinder and immerse it in water, thus giving up the controlled atmosphere. In this way, it achieves rapid cooling of the metal with oxidation simultaneous (deep or superficial) of the article, and a strong hydrogen pollution, what the brittle article does and causes the formation of dark gray surface oxides which are aesthetically very unpleasant (passivation).
En M. J. Donachie: "Titanium - A Technical Guide" 1988, ASM, Metals Park, Ohio, EE.UU., se describe un proceso de moldeo para producir piezas fundidas fundiendo titanio con un arco en el vacío en un crisol de cobre refrigerado con agua.In M. J. Donachie: "Titanium - A Technical Guide "1988, ASM, Metals Park, Ohio, USA, describes a molding process to produce castings melting titanium with a vacuum arc in a chilled copper crucible with Water.
La oxidación y la nitruración del titanio para mejorar la resistencia y la protección contra el desgaste son conocidas por "ASM Handbook, 10^{th} Ed. Vol. 5, Surface Engineering" 1994, ASM International, Metals Park, Ohio, EE.UU.Oxidation and nitriding of titanium for improve resistance and wear protection are known for "ASM Handbook, 10th Ed. Vol. 5, Surface Engineering "1994, ASM International, Metals Park, Ohio, USA
La GB 2 244 019 y la GB 2 244 019 describen un método para moldear metales dentales con un aparato de moldeo que comprende una cámara de moldeo herméticamente sellada en una atmósfera de gas inerte.GB 2 244 019 and GB 2 244 019 describe a method for molding dental metals with a molding apparatus that comprises a tightly sealed molding chamber in a atmosphere of inert gas.
La FR 2695581 describe un tratamiento de un metal sensible a la oxidación llevado a cabo en un recinto aislado. Consiste en introducir el metal en ese recinto, producir un vacío parcial, fundir el metal, introducir la masa fundida en un molde y dejarlo solidificar. El recinto, después de ser puesto en vacío parcial, se limpia por medio de un gas inerte.FR 2695581 describes a metal treatment Oxidation sensitive carried out in an isolated enclosure. It consists of introducing the metal into that enclosure, producing a vacuum partial, melt the metal, introduce the melt into a mold and Let it solidify. The enclosure, after being empty partial, it is cleaned by means of an inert gas.
En la GB 732298 se describe un ejemplo de un aparato para moldear metales como titanio y sus aleaciones.In GB 732298 an example of a apparatus for molding metals such as titanium and its alloys.
El objeto de la presente invención es superar los inconvenientes anteriores proporcionando un proceso mejorado para el tratamiento superficial de artículos hechos de titanio y de sus aleaciones.The object of the present invention is to overcome previous issues providing an improved process for surface treatment of articles made of titanium and its alloys
Este objeto se consigue mediante un proceso según la reivindicación 1.This object is achieved by a process according to claim 1
De acuerdo con la invención, todas las operaciones requeridas para obtener un artículo acabado se realizan en una atmósfera neutra y controlada en un solo aparato de manera que se obtiene una pieza acabada que está protegida por una película fuertemente adherente y que tiene un buen aspecto antes de ser transferida a una atmósfera normal y después al ambiente de la cavidad oral.According to the invention, all operations required to obtain a finished item are performed in a neutral and controlled atmosphere in a single device so that you get a finished piece that is protected by a strongly adherent film and that looks good before be transferred to a normal atmosphere and then to the environment of the oral cavity.
La pieza se somete luego a oxidación anódica o nitruración en una atmósfera de amoníaco, lo que permite la formación adecuada de un revestimiento protector de óxido y nitruro que tiene una fuerza de adherencia a la pieza del orden de 1400 kg/mm^{2}.The piece is then subjected to anodic oxidation or nitriding in an atmosphere of ammonia, which allows proper formation of a protective coating of oxide and nitride which has a force of adhesion to the piece of the order of 1400 kg / mm2.
Se describirá ahora en detalle el proceso de la invención con especial referencia al dibujo adjunto, que muestra un diagrama de bloques de un aparato adaptado para realizar el proceso.The process of the invention with special reference to the attached drawing, which shows a block diagram of an apparatus adapted to perform the process.
Este aparato comprende sustancialmente un recipiente sellado 1 provisto de una cubierta transparente de manera que todas las fases de trabajo pueden ser comprobadas y controladas visualmente, y dotado de guantes de goma inflexados para manipular los artículos.This apparatus substantially comprises a sealed container 1 provided with a transparent cover of so that all work phases can be checked and visually controlled, and equipped with inflated rubber gloves To manipulate the items.
El aparato está provisto además de una botella de un gas inerte y de una válvula manorreductora asociada; está provisto también de una bomba de vacío y un dispositivo de Getter 3 adaptado para provocar una rápida y completa oxidación del metal contenido dentro del aparato, eliminando así todas las moléculas residuales de O_{2} dentro del recipiente sellado 1.The device is also provided with a bottle of an inert gas and an associated pressure reducing valve; is also equipped with a vacuum pump and a Getter 3 device adapted to cause rapid and complete oxidation of the metal contained within the apparatus, thus eliminating all the molecules residuals of O2 within the sealed container 1.
El recipiente sellado 1 contiene además un cilindro de alta temperatura 5 donde se moldea el artículo, un tanque 7 que contiene un baño líquido (por ej., aceite) en el que el artículo puede enfriarse rápidamente, y un brazo 6 para retirar el artículo del cilindro 5 y sumergirlo en el baño de aceite del tanque 7 en el que se enfría rápidamente en ausencia de contaminantes.The sealed container 1 also contains a high temperature cylinder 5 where the article is molded, a tank 7 containing a liquid bath (e.g. oil) in which the item can be cooled quickly, and an arm 6 to remove the cylinder 5 article and immerse it in the oil bath of the tank 7 in which it cools quickly in the absence of pollutants
Dentro del recipiente 1 del aparato se proporciona además una estación de acabado 9 (zona de enfriamiento), una estación de limpieza con chorro de arena (11) y una estación de decapado (13).Inside the container 1 of the apparatus also provides a finishing station 9 (zone of cooling), a sandblasting station (11) and a pickling station (13).
Aunque el riesgo de contaminar el artículo enfriado rápidamente es muy pequeño, no obstante, de acuerdo con la invención, todas las fases posteriores de acabado (9), la limpieza con chorro de arena (11) y el decapado (13) se realizan en el ambiente neutro proporcionado en el recipiente 1.Although the risk of contaminating the article Quickly cooled is very small, however, according to the invention, all subsequent phases of finishing (9), cleaning with sandblasting (11) and pickling (13) are performed in the neutral environment provided in container 1.
Dentro del recipiente 1 se incluye una estación 15 adicional (si se requiere) para pulir mecánicamente el artículo, una estación 17 para operaciones de (micro)soldadura y una estación (que no se muestra) para operaciones de soldadura por puntos. Todas las operaciones antes mencionadas de pulir y soldar se llevan a cabo en la atmósfera neutra.Inside the container 1 a station is included 15 additional (if required) to mechanically polish the item, a station 17 for (micro) welding operations and a station (not shown) for welding operations by points. All aforementioned polishing and welding operations They are carried out in the neutral atmosphere.
El recipiente 1 contiene además un dispositivo de oxidación anódica 19 y un dispositivo 21 para nitrurar el artículo en una atmósfera de amoníaco. Mediante estas operaciones, se forma un revestimiento de óxido o un revestimiento de nitruro sobre la superficie del artículo 23 ó 25, teniendo dicho revestimiento una fuerza de adherencia (cohesión) comprendida entre 1000 y 2000 kg/mm^{2}, y preferentemente del orden de 1400 kg/mm^{2}. Después de este o estos tratamiento(s), el artículo 23 (o 25) puede ser expuesto a la atmósfera o a agentes contaminantes sin el riesgo de verse sometido a ulteriores reacciones químicas o químico-físicas no deseadas en la superficie o en el cuerpo del artículo. De esta manera, el artículo puede mantener indefinidamente el aspecto estético que hace a ese artículo preferible a los que se hacen con otros materiales o por un proceso diferente. Esas cualidades son, por ejemplo, una coloración rosada cuando el artículo tiene que casar con la mucosa gingival o una coloración lechosa cuando los dispositivos ortodónticos están situados sobre el esmalte de las coronas dentales naturales.The container 1 also contains a device for anodic oxidation 19 and a device 21 for nitriding the article in an atmosphere of ammonia. Through these operations, it is formed an oxide coating or a nitride coating on the surface of article 23 or 25, said coating having a adhesion force (cohesion) between 1000 and 2000 kg / mm2, and preferably of the order of 1400 kg / mm2. After this or these treatment (s), article 23 (or 25) can be exposed to the atmosphere or to pollutants without the risk of being subjected to further chemical reactions or chemical-physical unwanted on the surface or in the article body. In this way, the article can keep indefinitely the aesthetic aspect that makes that article preferable to those made with other materials or by a process different. Those qualities are, for example, a pink coloring when the item has to marry the gingival mucosa or a milky coloring when orthodontic devices are located on the enamel of natural dental crowns.
Claims (8)
- --
- proporcionar un recipiente sellado;provide a sealed container;
- --
- obtener una atmósfera neutra en dicho recipiente sellado por medio de un gas inerte, una bomba de vacío y un dispositivo de Getter, comprendiendo dicho dispositivo de Getter un metal adaptado para provocar una oxidación rápida y completa, eliminando así sustancialmente todas las moléculas residuales de O_{2} dentro del recipiente sellado;get one neutral atmosphere in said sealed vessel by means of a gas inert, a vacuum pump and a Getter device, comprising said Getter device a metal adapted to cause a rapid and complete oxidation, thus substantially eliminating all the residual molecules of O2 inside the container sealed;
- --
- formar un dispositivo protésico en un cilindro de moldeo de alta temperatura en dicho recipiente sellado en la atmósfera neutra así obtenida;To form a prosthetic device in a high temperature molding cylinder in said vessel sealed in the neutral atmosphere as well obtained;
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- sumergir dicho dispositivo moldeado en un baño de enfriamiento rápido en dicho recipiente sellado en la misma atmósfera neutra, provocando con ello el enfriamiento rápido del dispositivo moldeado en dicho recipiente sellado en la misma atmósfera neutra;dip said molded device in a fast cooling bath in said sealed container in the same neutral atmosphere, thereby causing rapid cooling of the molded device in said container sealed in the same neutral atmosphere;
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- someter posteriormente dicho dispositivo moldeado a oxidación anódica en dicho recipiente sellado en la misma atmósfera neutra, formando con ello un revestimiento protector sobre la superficie de dicho dispositivo moldeado.submit subsequently said device molded to anodic oxidation in said sealed vessel in the same neutral atmosphere, forming with it a protective coating on the surface of said molded device
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP19980102510 EP0938940B1 (en) | 1998-02-13 | 1998-02-13 | A process for treating the surface of articles made of titanium and alloys thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| ES2205290T3 true ES2205290T3 (en) | 2004-05-01 |
Family
ID=8231401
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| ES98102510T Expired - Lifetime ES2205290T3 (en) | 1998-02-13 | 1998-02-13 | PROCESS TO TREAT THE SURFACE OF ARTICLES MADE OF TITANIUM AND ITS ALLOYS. |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0938940B1 (en) |
| DE (1) | DE69817320T2 (en) |
| ES (1) | ES2205290T3 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111455427A (en) * | 2020-05-26 | 2020-07-28 | 东莞金稞电子科技有限公司 | Gradual change treatment process for sand surface and high gloss surface of aluminum alloy surface |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB732298A (en) * | 1952-05-03 | 1955-06-22 | Nat Lead Co | Apparatus for casting refractory metals |
| JP2912940B2 (en) * | 1990-05-18 | 1999-06-28 | 株式会社ジーシー | Dental metal casting method |
| JP2912941B2 (en) * | 1990-05-18 | 1999-06-28 | 株式会社ジーシー | Dental metal casting method |
| IT1257103B (en) * | 1992-09-16 | 1996-01-05 | PROCESSING PROCESS OF METAL MATERIALS IN A CONTROLLED ATMOSPHERE. |
-
1998
- 1998-02-13 EP EP19980102510 patent/EP0938940B1/en not_active Expired - Lifetime
- 1998-02-13 ES ES98102510T patent/ES2205290T3/en not_active Expired - Lifetime
- 1998-02-13 DE DE69817320T patent/DE69817320T2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| EP0938940B1 (en) | 2003-08-20 |
| DE69817320T2 (en) | 2004-06-17 |
| EP0938940A1 (en) | 1999-09-01 |
| DE69817320D1 (en) | 2003-09-25 |
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