EP0785563B1 - Method for fixing a first part of metal or ceramic to a second part of metal or ceramic - Google Patents

Method for fixing a first part of metal or ceramic to a second part of metal or ceramic Download PDF

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Publication number
EP0785563B1
EP0785563B1 EP96120725A EP96120725A EP0785563B1 EP 0785563 B1 EP0785563 B1 EP 0785563B1 EP 96120725 A EP96120725 A EP 96120725A EP 96120725 A EP96120725 A EP 96120725A EP 0785563 B1 EP0785563 B1 EP 0785563B1
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EP
European Patent Office
Prior art keywords
composition
ceramic
fusible conductor
fuse
ceramic member
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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.)
Expired - Lifetime
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EP96120725A
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German (de)
French (fr)
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EP0785563A1 (en
Inventor
Bernd Dr.-Ing. Fröchte
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Wickmann Werke GmbH
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Wickmann Werke GmbH
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H85/00Protective devices in which the current flows through a part of fusible material and this current is interrupted by displacement of the fusible material when this current becomes excessive
    • H01H85/02Details
    • H01H85/04Fuses, i.e. expendable parts of the protective device, e.g. cartridges
    • H01H85/041Fuses, i.e. expendable parts of the protective device, e.g. cartridges characterised by the type
    • H01H85/0411Miniature fuses
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H85/00Protective devices in which the current flows through a part of fusible material and this current is interrupted by displacement of the fusible material when this current becomes excessive
    • H01H85/02Details
    • H01H85/04Fuses, i.e. expendable parts of the protective device, e.g. cartridges
    • H01H85/05Component parts thereof
    • H01H85/143Electrical contacts; Fastening fusible members to such contacts
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H69/00Apparatus or processes for the manufacture of emergency protective devices
    • H01H69/02Manufacture of fuses
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H85/00Protective devices in which the current flows through a part of fusible material and this current is interrupted by displacement of the fusible material when this current becomes excessive
    • H01H85/02Details
    • H01H85/04Fuses, i.e. expendable parts of the protective device, e.g. cartridges
    • H01H85/041Fuses, i.e. expendable parts of the protective device, e.g. cartridges characterised by the type
    • H01H85/0411Miniature fuses
    • H01H85/0415Miniature fuses cartridge type
    • H01H85/0418Miniature fuses cartridge type with ferrule type end contacts
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H85/00Protective devices in which the current flows through a part of fusible material and this current is interrupted by displacement of the fusible material when this current becomes excessive
    • H01H85/02Details
    • H01H85/04Fuses, i.e. expendable parts of the protective device, e.g. cartridges
    • H01H85/05Component parts thereof
    • H01H85/143Electrical contacts; Fastening fusible members to such contacts
    • H01H85/157Ferrule-end contacts
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00Metal working
    • Y10T29/49Method of mechanical manufacture
    • Y10T29/49002Electrical device making
    • Y10T29/49107Fuse making

Definitions

  • the invention relates to a method for the production of an electrical fuse fixing a surface of a ceramic part on a fuse fuse, and a fuse with a ceramic first part and a second part, the an electrically conductive wire, namely the fuse element of the Fuse is.
  • ceramic material in the sense of the invention all ceramics as well as metal and glass ceramics and also glasses to understand.
  • Fastenings of this type play a part in the manufacture electrical fuses using the so-called Thick film technology plays a major role.
  • Thick film technology With thick film technology are complete circuits on a ceramic Substrate created. This is done on a ceramic substrate electrical contacts, conductor tracks and resistance layers applied and also prefabricated components or assemblies integrated into the circuit as SMD elements. For this the necessary contact points, conductor tracks and resistors as powdery layers of metal-containing mixtures applied to the surface of the ceramic. That can also in the Pastes are made that have the same mixture of materials as Wear emulsion.
  • the permanent attachment of the very fine-grained Materials are made by baking.
  • the branding or American "firing" means a process in which all components of the applied fine-grained mass with each other get connected.
  • a fuse is a fuse element in air or protective gas cheaper.
  • a first one as a carrier provided securing substrate and a second as a cover cap serving substrate in the form of two ceramic parts Burning in a paste for making electrical contacts metallized at opposite ends. A wire becomes fixed as a fuse between the two contacts. This Arrangement is permanently connected by gluing. A safe one electrical connection of the contacts to each other and to the Fusible conductor takes place in a final work step by soldering.
  • the fastening method proposed according to the invention for Manufacture of electrical fuses involves a sintering step.
  • sintering is a heat treatment described in which a powdery material mixture is not is completely melted, but only at the grain boundaries of the material mixture by diffusion and alloying connections arise.
  • the resulting connection is mechanical safe and permanent and can accordingly. for fixing of a ceramic part on a fuse element of a fuse.
  • she Depending on the composition of the mixture, it is also thermal resilient, higher than a variety of adhesives that commonly used to make such connections become.
  • the used Parts can be tubular as well as any area his.
  • ceramic materials Use in the field of electrical device fuses e.g. in the form of small pipes and flat ceramic plates with flat surface and central trough-like depression in the largest of their rectangular surface pieces.
  • the electrical conductor can also pass through before the sintering process another ceramic part to be covered.
  • This ceramic part only needs to be above the fusible conductor from a ground contact extend to the other and with these on the surfaces contact. So in a sintering process, namely through a single process step, substrate, Melting conductor and covering ceramic at the same time mechanically be firmly and electrically connected together.
  • this arrangement has the ceramic substrate between those with sinterable Mass occupied areas on a trough-like depression.
  • the covering ceramic has between those with the sinterable Earth later contacting places also one trough-like depression. So the fuse element is already at Assembly only over the two mass layers of that Substrate, and only in these places is it from the touches ceramic cover.
  • the Fusible conductor at the end of the sintering process over the two new resulting electrical contact points on both sides is mechanically connected to the carrier as with the cover and is kept self-supporting. Accordingly, the fuse element only one gas layer between its connection points surrounded with great insulation and can receive the desired switching characteristics.
  • the ceramic carrier the shape of a tube, which is connected to the sinterable mass is occupied.
  • the fuse element is through an opening is inserted and runs from the inside of the pipe Front side to the next self-supporting and only surrounded by gas.
  • the sintering process takes on the task of mechanical Attachment like the electrical contact of the Fuse element.
  • the pipe openings of this embodiment can before Sintering closed on both sides by electrically conductive caps and mechanically solid and electrical in the same sintering step conductive with the tube and with the fuse element get connected. Similar measures are also with others Embodiments conceivable.
  • the combination of materials is essential for the process in the sintered mass with regard to those to be joined Parts.
  • the mass must have metallic components for the conductive and have mechanical connection with the fuse element.
  • the components must be securely attached Mass on the surface of the ceramic of the other parts in the course enable the sintering process. So that can be used Mass to the family of "cermets", the so-called metal ceramics belong.
  • this procedure is contrary to typical cermet process the powder directly, or advantageously used in the form of a paste, and not under pressed to a blank under high pressure.
  • As a possible combination be the attachment of a silver wire to one Ceramic substrate using a sintered mass of silver, Called platinum and palladium.
  • Fig. 1 the basic attachment of the grains is one Sintered mass from a silver-palladium-platinum mass to one Silver wire shown.
  • the individual grains collide with theirs Edges and surfaces together. Sometimes they touch the surface of the silver wire. Through the sintering process there is no complete melting of those involved powdery materials, but only one Material transport between the granules, so that they attach themselves connect the contact points. Find it too Diffusion processes take place. The granules therefore lose theirs Shape not. As a result, you keep a solid and porous Mass that is well conductive and with its components the surface of the silver wire is conductively connected. In order to is a mechanically stable and electrically conductive on the wire Contact has been made.
  • Fig. 2 shows an electrical fuse.
  • sinterable mass 2 is applied on both sides Service.
  • On the ceramic top is between the mass-coated Ends of the carrier of the fuse element 3 have been placed.
  • the fuse element 3 between the contact points 4 covered by a sealing compound 5.
  • This manufacturing method for easy securing advantageously just four more steps: applying the sintered mass, Inserting the fuse element, sintering and casting.
  • the Work steps are metallizing, fixing and soldering omitted.
  • FIG. 3 shows a particularly favorable design of an SMD fuse with a fuse element 3 in a chamber.
  • ceramic substrate 1 and the cap 1 by the same shape symmetrical ceramic parts formed. With these ceramic parts only have to use the narrow side of the wider side for positioning the fuse element 3 can be distinguished over the trough 6. They are fully automatic Manufacturing no further parameters to be considered. Both parts are made on two sides with sinterable mass 2 coated and then with the between them in the Ground layer held fuse element 3 a sintering process subjected. This backup is advantageously none Post-treatment is necessary in a final step. So this process consists of only three steps. The The fuse is closed and the fuse element 3 is over the now sintered and electrically conductive contact points 4 electrically accessible.
  • this fuse does not have a fixed one Upper or lower part more. You can accordingly simply through placement machines in thick-film circuits integrated or soldered as an SMD component in printed circuits become. The production costs at Manufacturing as well as the cost of using this type of fuse significantly reduced.
  • Fig. 4 shows a basic design of a tube fuse with a ceramic, tubular support 7 attached to its End faces is covered with sinterable mass 2.
  • the fusible conductor 3 runs from the inside of the tube Face to face. It is on each face Fusible conductor 3 in contact with the sinterable mass 2. This makes it electrically like in a sintering step mechanically connected to the contact points 4, while the Mass 2 with the surface of the ceramic carrier 7 solid is connected.
  • FIG. 5 represents a supplement to the tube fuse according to FIG. 4
  • the end faces of the tube 7 by metal caps 8 have been closed before the sintering process. Only from The metal caps are for the sake of clarity 8 has been shown in FIG. 5 with a large excess.
  • Assembled fuse reliably with each other electrically also mechanically connected.

Abstract

Ceramic bodies (1) are joined together with an alloy wire (3) by using an intermediate mass (2) which is capable of being sintered.

Description

Die Erfindung betrifft ein Verfahren zur Herstellung einer elektrischen Sicherung unter Befestigung einer Oberfläche eines keramischen Teils an einem Schmelzleiter der Sicherung, und eine Schmelzsicherung mit einem keramischen ersten Teil und einem zweiten Teil, das ein elektrisch leitendes Draht, nämlich der Schmelzleiter der Sicherung ist.The invention relates to a method for the production of an electrical fuse fixing a surface of a ceramic part on a fuse fuse, and a fuse with a ceramic first part and a second part, the an electrically conductive wire, namely the fuse element of the Fuse is.

Unter einem "keramischen Werkstoff" im Sinn der Erfindung sind alle Keramiken sowie Metall- und Glaskeramiken und auch Gläser zu verstehen.Under a "ceramic material" in the sense of the invention all ceramics as well as metal and glass ceramics and also glasses to understand.

Das Verfahren erweitert die Gruppe der auf dem Gebiet der Herstellung von elektrischen Sicherungen bekannten Verbindungs- und Befestigungsverfahren. Bisher können nichtmetallische Teile wie etwa Gläser beispielsweise miteinander verklebt oder im teilerschmolzenen Zustand miteinander verbunden werden. Keramische Werkstoffe und Glaskeramiken können im feuchten Zustand zusammengesetzt und dann gemeinsam gebrannt werden. Auch ist ein Zusammenfügen von Teilen mit rauher Oberfläche durch Glaslot möglich.The procedure broadens the group of those in the field of Manufacture of electrical fuses known connection and fastening methods. So far, non-metallic Parts such as glasses glued together, for example or be connected to one another in the partially melted state. Ceramic materials and glass ceramics can be wet State put together and then burned together. Also is a joining of parts with a rough surface possible with glass solder.

Bei der Herstellung elektrischer Sicherungen ist zum Befestigen zweier metallischer Teile eine Vielzahl von Verfahren bekannt. Sie unterscheiden sich beispielsweise durch den Temperaturbereich, in dem der Befestigungsprozeß stattfindet. So werden Verfahren wie Heften, Bonden, Klemmen usw. bei normalen Umgebungstemperaturen durchgeführt, während beim Verschweißen zweier Materialien miteinander sehr hohe Temperaturen für diesen Vorgang benötigt werden. Weiter kann die Verbindung der beiden Teile auch mittels eines zusätzlichen Werkstoffes erfolgen, wie beispielsweise beim Kleben mit Leit-kleber bei normalen Temperaturen oder beim Löten bei stark erhöhter Temperatur. When making electrical fuses is to be attached two metallic parts a variety of processes known. They differ for example by the temperature range, in which the fastening process takes place. So processes such as stapling, bonding, clamping etc. in normal Ambient temperatures performed while welding two materials with each other very high temperatures for this process will be needed. The connection of the both parts are also made using an additional material, such as when gluing with conductive glue normal temperatures or when soldering at a high temperature.

Ein Großteil der vorgenannten Verfahren ist nicht mehr anwendbar bei der Verbindung von Metallen mit Nichtmetallen und konkret bei einer Befestigung eines metallischen oder metallhaltigem an einem keramischen Werkstoff.A large part of the aforementioned methods can no longer be used in the connection of metals with non-metals and specifically when attaching a metallic or metal-containing on a ceramic material.

Befestigungen dieser Art spielen unter anderem bei der Herstellung elektrischer Sicherungen unter Anwendung der sog. Dickschichttechnik eine große Rolle. Bei der Dickschichttechnik werden komplette Schaltungen auf einem keramischen Substrat erstellt. Dazu werden auf einem Keramiksubstrat elektrische Kontakte, Leiterbahnen und Widerstandsschichten aufgetragen und auch vorgefertigte Bauteile oder Baugruppen als SMD-Elemente mit in die Schaltung integriert. Hierzu werden die notwendigen Kontaktstellen, Leiterbahnen und Widerstände als pulverförmige Schichten metallhaltiger Gemische auf der Oberfläche der Keramik aufgebracht. Das kann auch in der Form von Pasten erfolgen, die die gleiche Stoffmischung als Emulsion tragen. Die dauerhafte Befestigung der sehr feinkörnigen Materialien erfolgt durch Einbrennen. Das Einbrennen oder amerikanisch "firing" bezeichnet ein Verfahren, bei dem alle Bestandteile der aufgetragenen feinkörnigen Masse miteinander verbunden werden. Das findet je nach Zusammensetzung der Gemische ab ca. 800° Celsius statt. Die Verfahrenseinheit von Auftrag der Pasten und Einbrennen ist wiederholbar. In aufeinander folgenden Schritten können auf diese Weise komplexe Strukturen auf dem Substrat aufgebaut werden. Erst nachträglich können in einem weiteren Fertigungsschritt Bauteile an den Kontakten angelötet werden, die man den hohen Temperaturen des Einbrennprozesses nicht aussetzen kann, wie z.B. Transistoren (vgl. US-A-5 363 082).Fastenings of this type play a part in the manufacture electrical fuses using the so-called Thick film technology plays a major role. With thick film technology are complete circuits on a ceramic Substrate created. This is done on a ceramic substrate electrical contacts, conductor tracks and resistance layers applied and also prefabricated components or assemblies integrated into the circuit as SMD elements. For this the necessary contact points, conductor tracks and resistors as powdery layers of metal-containing mixtures applied to the surface of the ceramic. That can also in the Pastes are made that have the same mixture of materials as Wear emulsion. The permanent attachment of the very fine-grained Materials are made by baking. The branding or American "firing" means a process in which all components of the applied fine-grained mass with each other get connected. Depending on the composition of the Mixtures take place from approx. 800 ° Celsius. The procedural unit of Application of the pastes and baking is repeatable. In each other The following steps can be complex in this way Structures are built on the substrate. Only afterwards can add components in a further production step the contacts to be soldered to the high temperatures of the stoving process, e.g. transistors (see US-A-5 363 082).

Bei der Herstellung elektrischer Sicherungen in Dickschichttechnik werden die Metallisierungen an den Enden bzw. Stirnkanten von Keramiksubstraten analog angebracht. In gleicher Weise kann bei den Sicherungen der Schmelzleiter anschließend als weitere Schicht zwischen diesen Kontakten auf den Keramikträger aufgebracht werden. Aus diesem Aufbau ergibt sich vor allem im Überlastbereich der Sicherung eine intensive Wärmeableitung vom Schmelzleiter der Sicherung zum Trägermaterial, die der Funktion dieses Bauteils als Sicherung abträglich ist.When manufacturing electrical fuses using thick-film technology become the metallizations at the ends or front edges of ceramic substrates attached analog. In the same The fuse can then be connected to the fuses as a further layer between these contacts on the ceramic carrier be applied. From this structure follows Intensive heat dissipation, especially in the overload area of the fuse from the fuse link of the fuse to the carrier material, which is detrimental to the function of this component as a fuse.

Vom Gesichtspunkt der Wärmeisolation her ist für den Aufbau einer Sicherung ein Schmelzleiter in Luft bzw. Schutzgas günstiger. Hier werden beispielsweise ein erstes als Träger vorgesehenes Sicherungssubstrat und ein zweites als Abdeckkappe dienendes Substrat in Form zweier Keramikteile durch Einbrennen einer Paste zur Herstellung elektrischer Kontakte an voneinander abgewandten Enden metallisiert. Ein Draht wird als Schmelzleiter zwischen den beiden Kontakten fixiert. Diese Anordnung wird durch Kleben dauerhaft verbunden. Eine sichere elektrische Verbindung der Kontakte untereinander und mit dem Schmelzleiter erfolgt in einem abschließenden Arbeitsschritt durch Löten.From the point of view of thermal insulation is for the construction a fuse is a fuse element in air or protective gas cheaper. Here, for example, a first one as a carrier provided securing substrate and a second as a cover cap serving substrate in the form of two ceramic parts Burning in a paste for making electrical contacts metallized at opposite ends. A wire becomes fixed as a fuse between the two contacts. This Arrangement is permanently connected by gluing. A safe one electrical connection of the contacts to each other and to the Fusible conductor takes place in a final work step by soldering.

Damit sind bislang zur Herstellung von Schmelzsicherung stets mehrschrittige Arbeitsverfahren nötig. Beispiele für mögliche Herstellungsverfahren enthalten die deutschen Gebrauchsmuster G 94 07 550.6 und G 94 10 437.9. Eines dieser Verfahren geht von an den Enden metallisierten Halbschalen aus, zwischen denen der Schmelzleiter durch Kleben an beiden Hälften fixiert wird. Die Sicherung wird durch Kleben oder Klammern zusammengefügt. In einem abschließenden Schritt wird zwischen den als Kontaktstellen dienenden Metallisierungen und dem Schmelzleiter ein sicherer elektrischer Kontakt durch Verlöten hergestellt. Damit umfaßt dieses Produktionsverfahren zum mechanischen Befestigen und zum elektrischen Verbinden mehrere Arbeitsschritte, wobei das Metallisieren der Enden der Halbschalen und das Verlöten zwei thermische Verfahren mit relativ hohen Temperaturen sind. Das Verkleben stellt einen Hilfsvorgang dar, der zusätzliche Materialien erfordert, die für die Funktion der Sicherung nicht notwendig sind.So far have always been used to manufacture fuse multi-step work procedures necessary. Examples of possible Manufacturing processes contain the German utility model G 94 07 550.6 and G 94 10 437.9. One of these procedures starts at the ends metallized half-shells, between which the fuse element is fixed by gluing on both halves. The fuse is assembled by gluing or stapling. In one final step is between the as contact points serving metallizations and the fuse element a safer electrical contact made by soldering. So that includes this production method for mechanical fastening and for electrical connection several steps, the Metallize the ends of the half shells and solder two are thermal processes with relatively high temperatures. The Gluing is an auxiliary process, the additional materials does not require that for the function of the fuse are necessary.

Auch alle anderen bisher bekannten Verfahren zum Herstellen elektrischer Sicherungen, insbesondere Gerätesicherungen aus einem oder zwei Keramik- oder Glaskörpern oder unter Verwendung von Metallkappen an den Enden erfordern eine Vielzahl einzelner, nacheinander ablaufender Schritte zum Befestigen der Komponenten.All other previously known methods of manufacture electrical fuses, especially device fuses one or two ceramic or glass bodies or using of metal caps on the ends require a variety individual, sequential steps for fastening of the components.

Daher stellt sich die Aufgabe, ein für die Herstellung elektrischer Sicherungen anwendbares Verfahren zum sicheren mechanischen Befestigen eines ersten Teils aus Metall oder aus einem keramischen Werkstoff an einem zweiten Teil aus Metall oder aus einem keramischen Werkstoff zu schaffen.Therefore, the task arises of making electrical Fuses applicable procedure for safe mechanical fastening of a first part made of metal or a ceramic material on a second part made of metal or to create from a ceramic material.

Zur Lösung der Aufgabe wird erfindungsgemäß das Verfahren nach Anspruch 1 vorgeschlagen.To achieve the object, the method according to claim 1 is proposed according to the invention.

Eine nach diesem Verfahren hergestellte Schmelzsicherung wird in Anspruch 10 definiert.A fuse made by this method is claimed in claim 10 Are defined.

Das erfindungsgemäß vorgeschlagene Befestigungsverfahren zur Herstellung von elektrischen Sicherungen umfaßt einen Sinterschritt. Mit dem Begriff "Sintern" wird eine Wärmebehandlung beschrieben, bei der ein pulverförmiges Materialgemisch nicht vollständig erschmolzen wird, sondern nur an den Korngrenzen des Materialgemisches durch Diffusion und Legieren Verbindungen entstehen. Die so entstehende Verbindung ist mechanisch sicher und dauer-haft und kann entsprechend auch. zur Befestigung eines keramischen Teiles an einem Schmelzleiter einer Sicherung verwendet werden. Sie ist -je nach Zusammensetzung des Gemisches- auch thermisch belastbar, und zwar höher als eine Vielzahl von Klebern, die üblicherweise zum Herstellen solcher Verbindungen benutzt werden. The fastening method proposed according to the invention for Manufacture of electrical fuses involves a sintering step. With the term "sintering" is a heat treatment described in which a powdery material mixture is not is completely melted, but only at the grain boundaries of the material mixture by diffusion and alloying connections arise. The resulting connection is mechanical safe and permanent and can accordingly. for fixing of a ceramic part on a fuse element of a fuse. she Depending on the composition of the mixture, it is also thermal resilient, higher than a variety of adhesives that commonly used to make such connections become.

In Erweiterung können auch mehr als zwei Teile in einem Sinterprozeß miteinander verbunden werden.In expansion, you can have more than two parts in one Sintering process.

Eine im Hinblick auf die Herstellung elektrischer Sicherungen besonders vorteilhafte Eigenschaft des Verfahrens besteht darin, daß die zur Verbindung der einzelnen Teile verwendete Masse nach dem Sintern elektrisch leitende Eigenschaften aufweist. Dadurch kann gleichzeitig mit der mechanischen Verbindung auch ein elektrischer Kontakt hergestellt werden. Für den Fall, daß auch eines der zu verbindenden Teile selbst elektrisch leitend ist, wird dieses Teil nicht nur mechanisch befestigt, sondern durch dieses Verfahren gleichzeitig mit einer Kontaktschicht versehen. Voraussetzung ist hier, daß das Teil mindestens an seiner Oberfläche elektrisch leitend ist.One in terms of making electrical fuses there is a particularly advantageous property of the method in that used to connect the individual parts Mass after sintering has electrically conductive properties. This can be done simultaneously with the mechanical connection an electrical contact can also be made. For the Case that one of the parts to be connected itself electrically is conductive, this part is not just mechanical attached, but by using this procedure at the same time provided a contact layer. The prerequisite here is that Part is electrically conductive at least on its surface.

Das Interesse gilt der Verarbeitung von Teilen mit keramischer Oberfläche durch dieses Verfahren. Die verwendeten Teile können sowohl rohrförmig als auch beliebig flächig ausgebildet sein. Hier finden keramische Werkstoffe Verwendung, auf dem Gebiet der elektrischen Gerätesicherungen z.B. in Form kleiner Rohre sowie flächige Keramikplättchen mit ebener Oberfläche sowie zentraler muldenartiger Vertiefung in der größten ihrer rechteckigen Oberflächenstücke.The interest applies to the processing of parts ceramic surface by this method. The used Parts can be tubular as well as any area his. Here you will find ceramic materials Use, in the field of electrical device fuses e.g. in the form of small pipes and flat ceramic plates with flat surface and central trough-like depression in the largest of their rectangular surface pieces.

Allen nachfolgend geschilderten Verfahren zum Herstellen von Sicherungen ist gemeinsam, daß die Sintermasse insbesondere zum Herstellen von elektrischen Kontakten an einem Substrat auf voneinander abgewandte Seiten aufgetragen wird. Die Masse umschließt hierbei diese Seiten vorteilhafterweise so, daß sie mit einem schmalen Streifen der angrenzenden Fläche(n) in Berührung steht. Nachdem die sinterbare Masse an zwei Stellen aufgebracht worden ist, wird der Schmelzleiter zwischen beiden Stellen so hinzugefügt, daß er sich in der richtigen Position sowie ebenfalls in Kontakt mit der sinterbaren Masse befindet. Der nachfolgende Sinterprozeß verbindet das Substrat mit der sinterbaren Masse und stellt damit nach außen leitende Kontakte für das Substrat her. Gleichzeitig wird der Schmelzleiter mechanisch fest sowie elektrisch leitend mit der sinterbaren Masse verbunden, so daß er nun über die beiden äußeren Kontakte elektrisch belastbar ist. Damit ist die Sicherung grundsätzlich fertig hergestellt, und zwar in einem einzigen Verfahrensschritt. Zum Schutz der Schmelzleiters kann bei einer einfachen Sicherungsbauform der Schmelzleiter auf dem Keramiksubstrat zwischen den beiden Kontaktstellen in seiner ganzen Länge mit einer elektrisch isolierenden Vergußmasse abgedeckt werden.All of the processes described below for producing Fuses have in common that the sintered mass in particular for making electrical contacts on a substrate is applied to opposite sides. The mass encloses these pages advantageously so that they with a narrow stripe of the adjacent surface (s) in Touch. After the sinterable mass in two places has been applied, the fuse element between the two Make sure that he is in the right position and also in contact with the sinterable mass. The subsequent sintering process connects the substrate with the sinterable mass and thus provides externally conductive contacts for the substrate. At the same time, the fuse element mechanically firm and electrically conductive with the sinterable Ground connected so that it now over the two outer Contacts is electrically loadable. That is the backup basically finished, in one Process step. To protect the fuse element at a simple fuse design of the fuse element on the Ceramic substrate between the two contact points in his entire length with an electrically insulating potting compound be covered.

Anstelle einer isolierenden Vergußmasse nach dem Sinterprozeß kann der elektrische Leiter vor dem Sinterprozeß auch durch ein weiteres Keramikteil abgedeckt werden. Dieses Keramikteil muß sich lediglich über dem Schmelzleiter von einer Massekontaktierung zur anderen erstrecken und mit diesen an den Oberflächen in Kontakt treten. So können in einem Sinterprozeß, nämlich durch einen einzigen Verfahrensschritt, Substrat, Schmelzleiter und abdeckende Keramik gleichzeitig mechanisch fest und elektrisch leitend miteinander verbunden werden.Instead of an insulating casting compound after the sintering process the electrical conductor can also pass through before the sintering process another ceramic part to be covered. This ceramic part only needs to be above the fusible conductor from a ground contact extend to the other and with these on the surfaces contact. So in a sintering process, namely through a single process step, substrate, Melting conductor and covering ceramic at the same time mechanically be firmly and electrically connected together.

In einer besonders vorteilhaften Ausführungsform dieser Anordnung weist das keramische Substrat zwischen den mit sinterbarer Masse belegten Stellen eine muldenartige Vertiefung auf. Die abdeckende Keramik besitzt zwischen den mit der sinterbaren Masse später in Kontakt tretenden Stellen ebenfalls eine muldenartige Vertiefung. So wird der Schmelzleiter schon beim Zusammenbau nur noch über die zwei Masseschichten von dem Substrat getragen, und nur an diesen Stellen wird er von der keramischen Abdeckung berührt. Das hat zur Folge, daß der Schmelzleiter am Ende des Sinterprozesses über die zwei neu entstandenen elektrischen Kontaktstellen auf beiden Seiten mechanisch mit dem Träger wie mit der Abdeckung verbunden ist und so freitragend gehalten wird. Demzufolge ist der Schmelzleiter zwischen seinen Anschlußstellen nur von einer Gasschicht mit großer Wärmedämmung umgeben und kann so die jeweils gewünschte Schaltcharachteristik erhalten. In a particularly advantageous embodiment of this arrangement has the ceramic substrate between those with sinterable Mass occupied areas on a trough-like depression. The covering ceramic has between those with the sinterable Earth later contacting places also one trough-like depression. So the fuse element is already at Assembly only over the two mass layers of that Substrate, and only in these places is it from the touches ceramic cover. As a result, the Fusible conductor at the end of the sintering process over the two new resulting electrical contact points on both sides is mechanically connected to the carrier as with the cover and is kept self-supporting. Accordingly, the fuse element only one gas layer between its connection points surrounded with great insulation and can receive the desired switching characteristics.

In einer weiteren Ausführungsform hat der keramische Träger die Form eines Röhrchens, das an seinen Stirnseiten mit der sinterbaren Masse belegt wird. Der Schmelzleiter wird durch eine Öffnung eingeführt und verläuft im Rohrinneren von einer Stirnseite zur nächsten freitragend und nur von Gas umgeben. Der Sinterprozeß übernimmt auch hier die Aufgabe der mechanischen Befestigung wie der elektrischen Kontaktierung des Schmelzleiters.In a further embodiment, the ceramic carrier the shape of a tube, which is connected to the sinterable mass is occupied. The fuse element is through an opening is inserted and runs from the inside of the pipe Front side to the next self-supporting and only surrounded by gas. Here, too, the sintering process takes on the task of mechanical Attachment like the electrical contact of the Fuse element.

Die Rohröffnungen dieses Ausführungsbeispiels können vor dem Sintern durch elektrisch leitende Kappen beidseitig verschlossen und im gleichen Sinterschritt mechanisch fest sowie elektrisch leitend mit dem Röhrchen und mit dem Schmelzleiter verbunden werden. Ähnliche Maßnahmen sind auch bei anderen Ausführungsformen denkbar.The pipe openings of this embodiment can before Sintering closed on both sides by electrically conductive caps and mechanically solid and electrical in the same sintering step conductive with the tube and with the fuse element get connected. Similar measures are also with others Embodiments conceivable.

Wesentlich für das Verfahren ist die Kombination der Materialien in der Sintermasse im Hinblick auf die zu verbindenden Teile. Die Masse muß metallische Bestandteile für die leitende und mechanische Verbindung mit dem Schmelzleiter aufweisen. Weiter müssen die Bestandteile eine sichere Befestigung der Masse an der Oberfläche der Keramik der übrigen Teile im Zuge des Sinterprozesses ermöglichen. Damit kann die verwendete Masse zur Familie der "Cermets", den s.g. Metallkeramiken gehören. Allerdings wird in diesem Verfahren im Gegensatz zu typischen Cermet-Verfahren das Pulver direkt, oder vorteilhafterweise in Form einer Paste verwendet, und nicht unter hohem Druck zu einem Formling gepreßt. Als eine mögliche Kombination sei die Befestigung eines Silberdrahtes an einem Keramiksubstrat unter Verwendung einer Sintermasse aus Silber, Platin und Palladium genannt.The combination of materials is essential for the process in the sintered mass with regard to those to be joined Parts. The mass must have metallic components for the conductive and have mechanical connection with the fuse element. Furthermore, the components must be securely attached Mass on the surface of the ceramic of the other parts in the course enable the sintering process. So that can be used Mass to the family of "cermets", the so-called metal ceramics belong. However, this procedure is contrary to typical cermet process the powder directly, or advantageously used in the form of a paste, and not under pressed to a blank under high pressure. As a possible combination be the attachment of a silver wire to one Ceramic substrate using a sintered mass of silver, Called platinum and palladium.

Das Verfahren wird nachstehend anhand von Ausführungsbeispielen mit Bezug auf die Zeichnungen näher erläutert. Die Zeichnungen zeigen:

Fig. 1
eine Prinzipskizze zum Sinterprozeß an einem Silberdraht mit Ag-Pd-Pt-Sintermasse;
Fig. 2
eine Schnittdarstellung eines einteiligen Gehäuses mit vergossenem Schmelzleiter;
Fig. 3
eine Schnittdarstellung eines zweiteiligen keramischen Sicherungskörpers mit einem freitragend durch Luft verlaufenden Schmelzleiter;
Fig. 4
einen Schnitt durch ein Röhrchengehäuse mit durch Sintern befestigtem und elektrisch verbundenem Schmelzleiter;
Fig. 5
einen Schnitt durch die Röhrchensicherung von Fig. 4 mit stirnseitig angebrachten und durch den Sinterprozeß befestigten und leitend verbundenen Metallkappen.
The method is explained in more detail below using exemplary embodiments with reference to the drawings. The drawings show:
Fig. 1
a schematic diagram of the sintering process on a silver wire with Ag-Pd-Pt sintered mass;
Fig. 2
a sectional view of a one-piece housing with potted fuse element;
Fig. 3
a sectional view of a two-part ceramic fuse body with a cantilevered air conductor;
Fig. 4
a section through a tube housing with sintered and electrically connected fusible conductor;
Fig. 5
a section through the tube fuse of Fig. 4 with the end face attached and fastened by the sintering process and conductively connected metal caps.

In Fig. 1 ist die prinzipielle Anlagerung der Körner einer Sintermasse aus einer Silber-Paladium-Platin-Masse an einen Silberdraht dargestellt. Die einzelnen Körner stoßen mit ihren Kanten und Flächen aneinander. Teilweise berühren sie dabei die Oberfläche des Silberdrahtes. Durch den Sintervorgang kommt es nicht zu einem vollständigen Erschmelzen der beteiligten pulverförmigen Materialien, sondern lediglich zu einem Materialtransport zwischen den Körnchen, so daß sich diese an den Kontaktstellen miteinander verbinden. Es finden dabei auch Diffusionsvorgänge statt. Die Körnchen verlieren daher ihre Form nicht. Als Ergebnis behält man eine feste und poröse Masse, die durch ihre Bestandteile selber gut leitend und mit der Oberfläche des Silberdrahtes leitend verbunden ist. Damit ist an dem Draht ein mechanisch stabiler und elektrisch leitender Kontakt angebracht worden.In Fig. 1 the basic attachment of the grains is one Sintered mass from a silver-palladium-platinum mass to one Silver wire shown. The individual grains collide with theirs Edges and surfaces together. Sometimes they touch the surface of the silver wire. Through the sintering process there is no complete melting of those involved powdery materials, but only one Material transport between the granules, so that they attach themselves connect the contact points. Find it too Diffusion processes take place. The granules therefore lose theirs Shape not. As a result, you keep a solid and porous Mass that is well conductive and with its components the surface of the silver wire is conductively connected. In order to is a mechanically stable and electrically conductive on the wire Contact has been made.

Fig. 2 zeigt eine elektrische Sicherung. Auf einem Keramiksubstrat 1 ist beidseitig sinterbare Masse 2 aufgetragen worden. Auf der Keramikoberseite ist zwischen den massebelegten Enden des Trägers der Schmelzleiter 3 aufgelegt worden. In einem einzigen Sinterschritt finden gleichzeitig Kontaktierung und Befestigung in vorstehend beschriebener Weise statt. Anschließend wird der Schmelzleiter 3 zwischen den Kontaktstellen 4 durch eine Vergußmasse 5 abgedeckt. Damit umfaßt dieses Herstellverfahren für die einfache Sicherung vorteilhafterweise nur noch vier Schritte: Auftragen der Sintermasse, Einlegen des Schmelzleiters, Sintern und Vergießen. Die Arbeitsschritte Metallisieren, Fixieren und Verlöten sind entfallen.Fig. 2 shows an electrical fuse. On a ceramic substrate 1, sinterable mass 2 is applied on both sides Service. On the ceramic top is between the mass-coated Ends of the carrier of the fuse element 3 have been placed. In a single sintering step makes contact at the same time and attachment in the manner described above. Subsequently, the fuse element 3 between the contact points 4 covered by a sealing compound 5. So that includes this manufacturing method for easy securing advantageously just four more steps: applying the sintered mass, Inserting the fuse element, sintering and casting. The Work steps are metallizing, fixing and soldering omitted.

Fig. 3 zeigt eine besonders günstige Bauform einer SMD-Sicherung mit einem Schmelzleiter 3 in einer Kammer. Zur Reduzierung der unterschiedlichen Bestandteile der Sicherung werden Keramiksubstrat 1 und die Abdeckkappe 1 durch gleichgeformte symmetrische Keramikteile gebildet. Bei diesen Keramikteilen müssen in der Produktion nur noch die schmale Seite von der breiteren Seite zur Positionierung des Schmelzleiters 3 über der Mulde 6 unterschieden werden. Es sind in einer vollautomatischen Fertigung keine weiteren Parameter zu beachten. Beide Teile werden an zwei Seiten mit sinterbarer Masse 2 beschichtet und anschließend mit dem zwischen ihnen in der Masseschicht gehaltenen Schmelzleiter 3 einem Sinterprozeß unterzogen. Bei dieser Sicherung ist vorteilhafterweise keine Nachbehandlung in einem abschließenden Schritt mehr notwendig. Dieses Verfahren besteht also nur noch aus drei Schritten. Die Sicherung ist geschlossen, und der Schmelzleiter 3 ist über die nun gesinterten und elektrisch leitenden Kontaktstellen 4 elektrisch zugänglich.3 shows a particularly favorable design of an SMD fuse with a fuse element 3 in a chamber. to Reduction of the different components of the fuse are ceramic substrate 1 and the cap 1 by the same shape symmetrical ceramic parts formed. With these ceramic parts only have to use the narrow side of the wider side for positioning the fuse element 3 can be distinguished over the trough 6. They are fully automatic Manufacturing no further parameters to be considered. Both parts are made on two sides with sinterable mass 2 coated and then with the between them in the Ground layer held fuse element 3 a sintering process subjected. This backup is advantageously none Post-treatment is necessary in a final step. So this process consists of only three steps. The The fuse is closed and the fuse element 3 is over the now sintered and electrically conductive contact points 4 electrically accessible.

Als weiteren Vorteil besitzt diese Sicherung kein fest definiertes Ober- oder Unterteil mehr. Sie kann entsprechend einfach durch Bestückungsautomaten in Dickschichtschaltungen integriert oder als SMD-Bauteil in gedruckten Schaltungen eingelötet werden. Damit werden die Produktionskosten bei der Fertigung wie auch die Kosten beim Einsatz dieser Sicherungsbauart erheblich gesenkt.As a further advantage, this fuse does not have a fixed one Upper or lower part more. You can accordingly simply through placement machines in thick-film circuits integrated or soldered as an SMD component in printed circuits become. The production costs at Manufacturing as well as the cost of using this type of fuse significantly reduced.

Fig. 4 zeigt eine Grundbauform einer Röhrchensicherung mit einem keramischen, rohrförmigen Träger 7, der an seinen Stirnseiten mit sinterbarer Masse 2 belegt ist. Durch das Innere des Röhrchen verläuft der Schmelzleiter 3 von einer Stirnseite zur anderen. An jeder Stirnseite steht der Schmelzleiter 3 in Berührung mit der sinterbaren Masse 2. Dadurch wird er in einem Sinterschritt elektrisch wie mechanisch mit den Kontaktstellen 4 verbunden, während die Masse 2 mit der Oberfläche des keramischen Trägers 7 fest verbunden wird.Fig. 4 shows a basic design of a tube fuse with a ceramic, tubular support 7 attached to its End faces is covered with sinterable mass 2. By the The fusible conductor 3 runs from the inside of the tube Face to face. It is on each face Fusible conductor 3 in contact with the sinterable mass 2. This makes it electrically like in a sintering step mechanically connected to the contact points 4, while the Mass 2 with the surface of the ceramic carrier 7 solid is connected.

Fig. 5 stellt eine Ergänzung der Röhrchensicherung nach Fig. 4 dar. Hier sind die Stirnseiten des Röhrchens 7 durch Metallkappen 8 vor dem Sinterprozeß geschlossen worden. Nur aus Gründen der Deutlichkeit der Darstellung sind die Metallkappen 8 in der Fig. 5 mit großem Übermaß dargestellt worden. In einem einzigen Sinterschritt werden alle Teile der fertig montierten Sicherung zuverlässig miteinander elektrisch wie auch mechanisch verbunden.FIG. 5 represents a supplement to the tube fuse according to FIG. 4 Here are the end faces of the tube 7 by metal caps 8 have been closed before the sintering process. Only from The metal caps are for the sake of clarity 8 has been shown in FIG. 5 with a large excess. In all parts of the are finished in a single sintering step Assembled fuse reliably with each other electrically also mechanically connected.

Claims (16)

  1. Method of manufacturing an electrical fuse by fastening a surface of a ceramic member to a fusible conductor of the fuse, wherein
    applied to at least a part of the surface of the ceramic member and/or a part of the surface of the fusible conductor there is a composition, which is securable by sintering to the surfaces to be connected together of the ceramic member and of the fusible conductor and which becomes electrically conductive as a result of sintering,
    the ceramic member and the fusible conductor are brought into contact with one another such that the composition wholly or partially engages both surfaces in the form of an intermediate layer, and
    the composition is rigidly connected to the said parts of the surface of the ceramic member and of the fusible conductor in a heat treatment suitable for sintering in a single method step,
    whereby the ceramic member is at least partially enclosed by the composition in the region of two sides of the ceramic member directed away from one another and the composition is situated on both sides in contact with the fusible conductor.
  2. Method as claimed in Claim 1, characterised in that a flat, ceramic member is used.
  3. Method as claimed in Claim 2, characterised in that the flat ceramic member has a recess in at least one of the surfaces.
  4. Method as claimed in one of Claims 1-3, characterised in that the ceramic member is covered in at least the region of the fusible conductor.
  5. Method as claimed in Claim 4, characterised in that the fusible conductor is covered by an electrically insulating potting composition.
  6. Method as claimed in Claim 5, characterised in that the flat ceramic member and the fusible conductor are covered between the contact points covered by the composition by a further member of ceramic material which may be covered by composition so that the composition layer on both sides of the ceramic member comes into contact with the corresponding surfaces of the covering member.
  7. Method as claimed in Claim 6, characterised in that the ceramic member and the further ceramic member are covered with composition at the ends and have a respective recess in their surfaces and in the centre so that at the end of the sintering process the fusible conductor extending between the ceramic member and the further ceramic member is held self-supported between the composition coatings and is electrically conductively connected to the intermediate composition layer on both sides.
  8. Method as claimed in one of Claims 1-5, characterised in that a small tube with sinterable composition in the region of the end faces is used as the ceramic member, through the opening of which the fusible conductor extends from one end face to the other.
  9. Method as claimed in one of Claims 6-8, characterised in that a cover is arranged on each side to which composition adheres and secured by sintering.
  10. Fuse with a ceramic first member (1) and a second member (3), which is an electrically conductive wire, namely the fusible conductor of the fuse, characterised in that the ceramic first member (1) is at least partially surrounded by a sintered and electrically conductive composition (2) in the region of two sides directed away from one another, whereby the composition is in contact on both sides with the second member (3), which is electrically conductive, at least on its surface, and the composition (2) and the two members (1; 3) are rigidily connected together merely by a heat treatment suitable for sintering.
  11. Fuse as claimed in Claim 10, characterised in that the ceramic first member (1) is flat, preferably with a recess (6) in the central region of at least one of its surfaces, and the fusible conductor is covered in at least the region between the contact points of the ceramic material covered by the composition.
  12. Fuse as claimed in Claim 10, characterised in that an electrically insulating potting composition (5) covers the fusible conductor (3).
  13. Fuse as claimed in Claim 10, with three members connected together, characterised in that the fusible conductor (3) is held between two ceramic members (1), which are similarly at least partially surrounded by the composition (2) in the region of two sides directed away from one another, and is electrically conductively connected.
  14. Fuse as claimed in Claim 13, characterised in that the two ceramic members (1) are flat and have a respective recess in the central region of at least one surface, the recesses (6) in the ceramic members are directed towards one another such that the third portion, which constitutes the fusible conductor (3), is held self-supported between the composition coatings (2).
  15. Fuse as claimed in Claim 10, characterised in that the fusible conductor (3) extends through the opening of a small ceramic tube (7) from one end surface to the other end surface of the small tube, which is provided at the openings with sintered and electrically conductive composition (2), and the conductor (3) is electrically conductively connected to the end surfaces.
  16. Fuse as claimed in Claim 15, characterised in that arranged and secured by sintering on each side, to which composition adheres, of the small tube (5), there is a cover, e.g. an electrically conductive cap (6).
EP96120725A 1996-01-18 1996-12-21 Method for fixing a first part of metal or ceramic to a second part of metal or ceramic Expired - Lifetime EP0785563B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19601612A DE19601612A1 (en) 1996-01-18 1996-01-18 Method of attaching a first part made of metal or ceramic to a second part made of metal or ceramic
DE19601612 1996-01-18

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EP0785563A1 EP0785563A1 (en) 1997-07-23
EP0785563B1 true EP0785563B1 (en) 2002-11-27

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EP (1) EP0785563B1 (en)
AT (1) ATE228717T1 (en)
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DE19704097A1 (en) * 1997-02-04 1998-08-06 Wickmann Werke Gmbh Electrical fuse element
DE10019121A1 (en) * 2000-04-18 2001-10-25 Moeller Gmbh Contact for electrical switch, has carrier region fabricated from one material with contacts of another material, and is produced by sintering process.
DE10056590A1 (en) * 2000-11-15 2002-05-23 Philips Corp Intellectual Pty Digital signal processing and/or storing circuit for smart card controller has at least one programmable fuse formed in multiple stages
JP4155825B2 (en) * 2001-03-02 2008-09-24 ビックマン−ベルケ ゲーエムベーハー Manufacturing method of fuse element
WO2007119358A1 (en) * 2006-03-16 2007-10-25 Matsushita Electric Industrial Co., Ltd. Surface-mount current fuse
US8154376B2 (en) * 2007-09-17 2012-04-10 Littelfuse, Inc. Fuses with slotted fuse bodies
US8081057B2 (en) * 2009-05-14 2011-12-20 Hung-Chih Chiu Current protection device and the method for forming the same
JP6007010B2 (en) * 2012-07-18 2016-10-12 矢崎総業株式会社 Electric wire fuse and manufacturing method thereof
US10276338B2 (en) 2016-06-01 2019-04-30 Littelfuse, Inc. Hollow fuse body with trench
US10325744B2 (en) * 2016-06-01 2019-06-18 Littelfuse, Inc. Hollow fuse body with notched ends

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DE1019242B (en) * 1955-06-18 1957-11-07 Steatit Magnesia Ag Method for producing a firm connection between ceramic bodies
FR2550001B1 (en) * 1983-07-29 1986-05-16 Eurofarad METHOD FOR MANUFACTURING AN ELECTRONIC COMPONENT BY ASSOCIATING ELEMENTARY CELLS, IN PARTICULAR MULTILAYERED CERAMIC CAPACITORS
US4612529A (en) * 1985-03-25 1986-09-16 Cooper Industries, Inc. Subminiature fuse
US4924203A (en) * 1987-03-24 1990-05-08 Cooper Industries, Inc. Wire bonded microfuse and method of making
JPH02288038A (en) * 1989-04-27 1990-11-28 Murata Mfg Co Ltd Fuse and its manufacture
DE9407550U1 (en) * 1993-04-21 1994-09-01 Wickmann Werke Gmbh Electrical fuse
DE9410437U1 (en) * 1993-09-10 1994-08-18 Wickmann Werke Gmbh Fuse
US5363082A (en) * 1993-10-27 1994-11-08 Rapid Development Services, Inc. Flip chip microfuse

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EP0785563A1 (en) 1997-07-23
US5926084A (en) 1999-07-20
DE59609918D1 (en) 2003-01-09
ATE228717T1 (en) 2002-12-15

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