DE1038973B - Process for producing vacuum-tight connections between ceramic tubes and sleeves or lids made of metal - Google Patents

Process for producing vacuum-tight connections between ceramic tubes and sleeves or lids made of metal

Info

Publication number
DE1038973B
DE1038973B DEL27136A DEL0027136A DE1038973B DE 1038973 B DE1038973 B DE 1038973B DE L27136 A DEL27136 A DE L27136A DE L0027136 A DEL0027136 A DE L0027136A DE 1038973 B DE1038973 B DE 1038973B
Authority
DE
Germany
Prior art keywords
titanium
metal
solder
sleeves
tight connections
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.)
Pending
Application number
DEL27136A
Other languages
German (de)
Inventor
Dipl-Ing Guenther Dobke
Rudolf Heller
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Licentia Patent Verwaltungs GmbH
Original Assignee
Licentia Patent Verwaltungs GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Licentia Patent Verwaltungs GmbH filed Critical Licentia Patent Verwaltungs GmbH
Priority to DEL27136A priority Critical patent/DE1038973B/en
Publication of DE1038973B publication Critical patent/DE1038973B/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
    • C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
    • C04B37/026—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used consisting of metals or metal salts
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
    • C04B2237/12—Metallic interlayers
    • C04B2237/122—Metallic interlayers based on refractory metals
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32—Ceramic
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/40—Metallic
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/59—Aspects relating to the structure of the interlayer
    • C04B2237/592—Aspects relating to the structure of the interlayer whereby the interlayer is not continuous, e.g. not the whole surface of the smallest substrate is covered by the interlayer
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/76—Forming laminates or joined articles comprising at least one member in the form other than a sheet or disc, e.g. two tubes or a tube and a sheet or disc
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/76—Forming laminates or joined articles comprising at least one member in the form other than a sheet or disc, e.g. two tubes or a tube and a sheet or disc
    • C04B2237/765—Forming laminates or joined articles comprising at least one member in the form other than a sheet or disc, e.g. two tubes or a tube and a sheet or disc at least one member being a tube

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Products (AREA)

Description

Es ist bereits ein Verfahren zur Herstellung von vakuumdichten Verbindungen zwischen Keramikrohren und Hülsen oder Deckeln aus Metall vorgeschlagen, bei dem die Metallhülse und der Keramikkörper sich nicht berühren und durch ein Lot miteinander verbunden werden. Hierbei wird das in einem Schmelzofen verflüssigte Bindemittel über ein Gießrohr in den Verbindungsspalt gegossen.It is already a method of making vacuum-tight connections between ceramic tubes and sleeves or covers made of metal are proposed, in which the metal sleeve and the ceramic body do not touch each other and are connected by a plumb line. This is all in one Melting furnace, liquefied binder is poured into the connecting gap via a pouring pipe.

Es ist weiterhin bekannt, daß Titan ein chemisch sehr aktives Metall ist. Man hat aus diesem Grunde bereits Titanhydrid als Aufstrich auf die Keramik verwendet oder als metallisches Titan aufgedampft, um eine gute Metall-Keramik-Lotverbindung zu erhalten. Bei diesem Verfahren muß man jedoch das Mengenverhältnis Titanhydrid-Lotmetall genau abstimmen, um homogene, gut haftende und vakuumdichte Schichten zu erhalten. Titanhydrid ist aber sehr empfindlich gegen Verunreinigungen, so daß nur bei sehr hohem Vakuum oder sehr reinem Schutzgas gearbeitet werden kann. Aus diesem Grunde hat sich das Verfahren mehr im Fertigungsbetrieb durchgesetzt. It is also known that titanium is a very chemically active metal. For this reason one has Titanium hydride has already been used as a spread on the ceramic or has been vapor-deposited as metallic titanium, to achieve a good metal-ceramic solder joint. With this procedure, however, you have to Precisely adjust the quantity ratio of titanium hydride to solder metal in order to ensure homogeneous, well-adhering and vacuum-tight Get layers. But titanium hydride is very sensitive to impurities, so only it is possible to work with a very high vacuum or very pure protective gas. Because of this, has the process is more prevalent in the manufacturing plant.

Gegenstand der Erfindung ist ein Verfahren zur Herstellung von vakuumdichten Verbindungen zwischen Keramikrohren und Hülsen oder Deckeln aus Metall, bei dem der Zwischenraum zwischen Metallhülse und Keramikkörper durch ein Lot ausgefüllt wird mit dem Kennzeichen, daß das in einem Schmelzofen verflüssigte Lot kurz vor der Verbindungsstelle über metallisches Titan fließt.The invention relates to a method for producing vacuum-tight connections between Ceramic tubes and sleeves or covers made of metal, in which the space between the metal sleeve and ceramic body is filled by a solder with the label that it is in a melting furnace Liquefied solder flows over metallic titanium just before the connection point.

Der Erfindung liegt die Erkenntnis zugrunde, daß Legierungen von Titan und Silber nicht stabil sind, sondern Titan nach einem Auslösungsvorgang wieder ausscheidet. Das Lot, ζ. B. Silber, darf bei der Reaktionstemperatur nicht vollkommen mit dem Titan zusammenschmelzen. Diese Tatsache wird aber erfindungsgemäß dadurch vermieden, daß das Lot an dem metallischen Titan, das beispielsweise als Ring vor dem Verbindungsspalt liegt, vorbeifließt. Hierdurch geht eine geringe Menge Titan in dem Silber in Lösung, die Schmelze bleibt aber reaktionsfähig, und die Ausscheidung des Titans erfolgt unmittelbar an der zu verlötenden Keramikfläche. Es hat sich als vorteilhaft erwiesen, vor dem Verbindungsspalt und somit vor dem Titan den Zuflußkanal zu verengen und dadurch die Strömungsgeschwindigkeit auf ein möglichst geringes Maß herabzusetzen. Eine Ventilvorrichtung an dem Boden des Lötofens verhindert, daß das Lot vor dem Verschmelzungsvorgang mit dem Titan in Kontakt kommt.The invention is based on the knowledge that alloys of titanium and silver are not stable, but titanium precipitates again after a release process. The plumb bob, ζ. B. silver, allowed at the reaction temperature do not completely fuse with the titanium. But this fact is according to the invention thereby avoided that the solder on the metallic titanium, for example as a ring lies in front of the connecting gap, flows past. This causes a small amount of titanium to go into the silver in solution, but the melt remains reactive and the titanium precipitates immediately on the ceramic surface to be soldered. It has been found to be advantageous in front of the connecting gap and thus narrowing the inflow channel in front of the titanium and thereby reducing the flow velocity to as much as possible to reduce to a small degree. A valve device at the bottom of the soldering furnace prevents the solder comes into contact with the titanium before the fusion process.

Die Zeichnung zeigt ein Ausführungsbeispiel der Erfindung. Das Keramikrohr 1 soll mit dem Deckel 2 und der Hülse 3 durch Lot verbunden werden. Da bei Strorneinführungen mit größerem Durchmesser, z. B.The drawing shows an embodiment of the invention. The ceramic tube 1 should be connected to the cover 2 and the sleeve 3 are connected by solder. Since with current inlets with a larger diameter, z. B.

von vakuumdichten Verbindungenof vacuum-tight connections

zwischen Keramikrohren und Hülsenbetween ceramic tubes and sleeves

oder Deckeln aus Metallor lids made of metal

Anmelder:Applicant:

LICENTIA Patent-Verwaltungs-G.m.b.H., Hamburg 36, Hohe Bleichen 22LICENTIA Patent-Verwaltungs-G.m.b.H., Hamburg 36, Hohe Bleichen 22

Dipl.-Ing. Günther Dobke, Berlin-Grunewald,Dipl.-Ing. Günther Dobke, Berlin-Grunewald,

und Rudolf Heller, Berlin-Reinickendorf,and Rudolf Heller, Berlin-Reinickendorf,

sind als Erfinder genannt wordenhave been named as inventors

100 mm und mehr, die Konzentrierung der Teile während der Lötung nicht mehr gesichert ist, wird sie durch mechanische Mittel herbeigeführt. Zu diesem Zweck ist ein zweiteiliger Graphitring 4 vorgesehen, der bei Lottemperatur zugleich das Keramikrohr und das Ende des Metallzylinders eng umschließt. Der am Keramikrohr anliegende Rand des Graphitringes bildet gleichzeitig den äußeren Abschluß des Verbindungsspaltes 5. Mittels eines weiteren Graphitringes 6 wird der halbierte Graphitring 4 zusammengehalten und somit der Metallzylinder zu dem Keramikrohr 1 konzentriert. Der genaue Abstand zwischen den beiden Graphitringen 4 wird beispielsweise durch vier auf den Umfang verteilte Exzenterzapfen 7 abgestimmt. Innerhalb des Keramikrohres 1 sind zwei Lotvorratsgefäße 8 und 9 übereinander eingesetzt und von einem Ofen 10 umgeben. Die Lotvorratsgefäße sind über je ein Kupplungsrohr 11 und 12 und über je eine in den Einsatzringen 13 und 14 vorgesehene Nut 15 mit dem Raum des Verbindungsspaltes 5 verbunden. Wird durch den Ofen 10 das Lot in den Vorratsgefäßen 8 und 9 geschmolzen, dann fließt es über das Kupplungsrohr und die Nut in den Verbindungsspalt und füllt diesen vollkommen aus. In der Nut 15 ist nun erfindungsgemäß ein Titanring 18 vorgesehen, über den das flüssige Lot fließt und das zum Teil durch das Silberlot gelöst wird. Ein Ventil 19 in dem Löttiegel 8 bzw. 9 verhindert die Berührung des Silberlotes mit dem Titan vor dem Verschmelzungsvorgang. 100 mm and more, the concentration of the parts is no longer ensured during soldering, it becomes brought about by mechanical means. A two-part graphite ring 4 is provided for this purpose, which at the same time tightly encloses the ceramic tube and the end of the metal cylinder at soldering temperature. The on Ceramic tube adjacent edge of the graphite ring at the same time forms the outer closure of the connecting gap 5. The halved graphite ring 4 is held together by means of a further graphite ring 6 and thus the metal cylinder is concentrated to the ceramic tube 1. The exact distance between the two Graphite rings 4 are matched, for example, by four eccentric pins 7 distributed around the circumference. Within the ceramic tube 1, two solder storage vessels 8 and 9 are inserted one above the other and from surrounded by an oven 10. The solder storage vessels are each via a coupling tube 11 and 12 and via each a groove 15 provided in the insert rings 13 and 14 is connected to the space of the connecting gap 5. If the solder in the storage vessels 8 and 9 is melted by the furnace 10, it overflows the coupling tube and the groove in the connecting gap and fills this completely. In the groove 15 a titanium ring 18 is now provided according to the invention, over which the liquid solder flows and that in part is solved by the silver solder. A valve 19 in the soldering pot 8 or 9 prevents contact with the Silver solder with the titanium before the fusion process.

Der das Keramikrohr umschließende Teil, der Metallzylinder, besteht oft aus einheitlichem Material, z. B. Eisen. Unter Umständen ist es jedoch vorteil-The part surrounding the ceramic tube, the metal cylinder, often consists of a uniform material, z. B. iron. However, it may be advantageous

809 637/428809 637/428

haft, Schrumpfringe 16 und 17 mit besonderen thermischen Eigenschaften vorzusehen.liable to provide shrink rings 16 and 17 with special thermal properties.

Es hat sich als vorteilhaft erwiesen, das ganze Verfahren in einem elektrisch beheizten, sauerstofffreien Ofen, z. B. einem Vakuumofen, vorzunehmen. Es werden so die zu verbindenden Teile gleichmäßig erwärmt, und es wird verhindert, daß das Lot an weniger erwärmten Teilen zu früh erstarrt und den Spalt nicht mehr voll ausfüllen kann. Gleichzeitig wird eine Oxydierung der Metall- und Graphitteile vermieden.It has proven advantageous to do the whole process in an electrically heated, oxygen-free one Furnace, e.g. B. a vacuum furnace to make. The parts to be connected are heated evenly, and it is prevented that the solder solidifies too early on less heated parts and the gap can no longer fill in full. At the same time, oxidation of the metal and graphite parts is avoided.

Claims (4)

PatentansprOchE:Patent claims: 1. Verfahren zum Herstellen von vakuumdichten Verbindungen zwischen Keramikrohren und Hülsen oder Deckeln aus Metall, bei dem der Zwischenraum zwischen Metallhülse und Keramikkörper durch ein Lot ausgefüllt wird, dadurch gekennzeichnet, daß das in einem Schmelzofen verflüssigte Lot kurz vor der Verbindungsstelle über metallisches Titan fließt.1. Process for making vacuum-tight connections between ceramic tubes and sleeves or lids made of metal, in which the space between the metal sleeve and ceramic body is filled in by a solder, characterized in that the liquefied in a melting furnace Solder flows over metallic titanium just before the connection point. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Titan vor dem Verbindungsspalt in einer Verengung des Zuflußkanals angeordnet wird.2. The method according to claim 1, characterized in that the titanium in front of the connecting gap is arranged in a constriction of the inflow channel. 3. Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet, daß das Lot vor dem Verschmelzungsprozeß durch ein Ventil von dem Titan ferngehalten wird.3. The method according to claim 1 and 2, characterized in that the solder before the fusion process is kept away from the titanium by a valve. 4. Verfahren nach Anspruch 1 bis 3, dadurch gekennzeichnet, daß das Titan in Ringform verwendet wird.4. The method according to claim 1 to 3, characterized in that the titanium is used in a ring shape will. Hierzu 1 Blatt Zeichnungen1 sheet of drawings © 809 637/425 9.58© 809 637/425 9.58
DEL27136A 1957-03-15 1957-03-15 Process for producing vacuum-tight connections between ceramic tubes and sleeves or lids made of metal Pending DE1038973B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEL27136A DE1038973B (en) 1957-03-15 1957-03-15 Process for producing vacuum-tight connections between ceramic tubes and sleeves or lids made of metal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEL27136A DE1038973B (en) 1957-03-15 1957-03-15 Process for producing vacuum-tight connections between ceramic tubes and sleeves or lids made of metal

Publications (1)

Publication Number Publication Date
DE1038973B true DE1038973B (en) 1958-09-11

Family

ID=7264074

Family Applications (1)

Application Number Title Priority Date Filing Date
DEL27136A Pending DE1038973B (en) 1957-03-15 1957-03-15 Process for producing vacuum-tight connections between ceramic tubes and sleeves or lids made of metal

Country Status (1)

Country Link
DE (1) DE1038973B (en)

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