DE19734211A1 - Soldering ceramic parts together or to metals - Google Patents

Soldering ceramic parts together or to metals

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Publication number
DE19734211A1
DE19734211A1 DE1997134211 DE19734211A DE19734211A1 DE 19734211 A1 DE19734211 A1 DE 19734211A1 DE 1997134211 DE1997134211 DE 1997134211 DE 19734211 A DE19734211 A DE 19734211A DE 19734211 A1 DE19734211 A1 DE 19734211A1
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Prior art keywords
soldering
ceramic
solder
metals
parts together
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DE1997134211
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DE19734211C2 (en
Inventor
Rudolf Lison
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Forschungszentrum Juelich GmbH
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Forschungszentrum Juelich GmbH
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Priority to DE1997134211 priority Critical patent/DE19734211C2/en
Publication of DE19734211A1 publication Critical patent/DE19734211A1/en
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/001—Interlayers, transition pieces for metallurgical bonding of workpieces
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    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
    • C04B37/006—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts consisting of metals or metal salts
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
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    • 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
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    • 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
    • C04B2237/125—Metallic interlayers based on noble metals, e.g. silver
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    • 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
    • C04B2237/126—Metallic interlayers wherein the active component for bonding is not the largest fraction of the interlayer
    • C04B2237/127—The active component for bonding being a refractory metal
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    • 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
    • C04B2237/34—Oxidic
    • C04B2237/343—Alumina or aluminates
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    • 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
    • C04B2237/36—Non-oxidic
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    • 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
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    • C04B2237/36—Non-oxidic
    • C04B2237/366—Aluminium nitride
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    • 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
    • C04B2237/36—Non-oxidic
    • C04B2237/368—Silicon nitride
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    • 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
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    • 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
    • C04B2237/405—Iron metal group, e.g. Co or Ni
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    • 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
    • C04B2237/60—Forming at the joining interface or in the joining layer specific reaction phases or zones, e.g. diffusion of reactive species from the interlayer to the substrate or from a substrate to the joining interface, carbide forming at the joining interface
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    • 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
    • C04B2237/72—Forming laminates or joined articles comprising at least two interlayers directly next to each other

Abstract

A process for bonding ceramic parts together or to metals involves coating the surface of a ceramic part with a reactive component and then soldering it to the similarly coated surface of another ceramic part or to the surface of a metal part.

Description

Die Erfindung betrifft ein Verfahren zum Verlöten zwei­ er Keramiken oder einer Keramik mit einem Metall.The invention relates to a method for soldering two he ceramics or a ceramic with a metal.

Bekannt ist die Herstellung einer Lötverbindung der vorgenannten Art mittels eines Aktivlotes. Unter einem Aktivlot ist ein Lot zu verstehen, das eine reaktive Komponente enthält. Wird eine Oxidkeramik verlötet, so ist unter reaktiver Komponente eine Komponente zu ver­ stehen, die eine hinreichend große Affinität zum Sauer­ stoff aufweist. Wird ein Werkstoff auf der Basis von Kohlenstoff verlötet, so ist unter reaktiver Komponente eine Komponente zu verstehen, die eine hinreichend gro­ ße Affinität zum Kohlenstoff aufweist.The production of a solder connection is known aforementioned type by means of an active solder. Under a Active solder is to be understood as a solder that is a reactive one Contains component. If an oxide ceramic is soldered, then so a component is to be ver under reactive component who have a sufficiently high affinity for sour has fabric. If a material based on Carbon is soldered under reactive component to understand a component that is sufficiently large has affinity for carbon.

Die Affinität ist hinreichend groß, wenn die Bildungs­ enthalpie der reaktiven Komponente unter den herrschen­ den Lötbedingungen kleiner ist als die Bildungsenthal­ pie der Keramik. Von folgender Bildungsreaktion wird dabei ausgegangen:
The affinity is sufficiently high if the enthalpy of formation of the reactive component under the prevailing soldering conditions is smaller than the enthalpy of formation of the ceramic. The following educational reaction is assumed:

Me'O + Me'' ⇔ Me''O + Me'.Me'O + Me '' ⇔ Me''O + Me '.

Soll also z. B. Al2O3 verlötet werden und ist Titan als reaktive Komponente vorgesehen, so lautet die Bil­ dungsreaktion:
So should z. B. Al 2 O 3 are soldered and titanium is intended as a reactive component, the formation reaction is as follows:

Al2O3 + 3 Ti ⇔ 4 Al + 3 TiO2.Al 2 O 3 + 3 Ti ⇔ 4 Al + 3 TiO 2 .

Das entstehende Al bewirkt zusammen mit dem Lot eine Benetzung der zu verlötenden Oberflächen.The resulting Al together with the solder causes one Wetting the surfaces to be soldered.

Unter Lötbedingungen sind insbesondere die Löttempera­ tur und der während der Lötung herrschende Druck der an der Reaktion beteiligten Stoffe zu verstehen.The soldering tempera in particular is under soldering conditions structure and the pressure prevailing during soldering understand the substances involved in the reaction.

Die reaktive Komponente im Aktivlot ermöglicht die Be­ netzung der zu verlötenden Oberfläche der Oxidkeramik. Diese Benetzung ist wiederum Voraussetzung für eine gu­ te Lötverbindung.The reactive component in the active solder enables the Be wetting the surface of the oxide ceramic to be soldered. This wetting is in turn a prerequisite for a gu te solder joint.

Nachteilhaft sind Aktivlote sehr teuer, da sie geson­ dert hergestellt werden müssen. Darüber hinaus sind Ak­ tivlote ungeeignet, um eine Kapillarlötung vorzunehmen. Die Aktivkomponente verbraucht sich nämlich, bevor das Lot vollständig in die Kapillare eingedrungen ist. Die vollständige Benetzung der zu verlötenden Oberflächen wird nicht erreicht. Eine Kapillarlötung kann daher praktisch nicht mit Aktivloten durchgeführt werden.Disadvantages of active solders are very expensive because must be manufactured. In addition, Ak tivlote unsuitable for capillary soldering. The active component is used up before that Lot has completely penetrated the capillary. The complete wetting of the surfaces to be soldered will not be reached. Capillary soldering can therefore practically not with active solders.

Alternativ sind CVD-Verfahren oder galvanische Verfah­ ren als Vorbereitung zum Verbinden zweier nichtmetalli­ scher Körper bekannt. Nachteilhaft müssen bei diesen Verfahren Gase oder Säuren entsorgt werden.Alternatively, CVD processes or galvanic processes as preparation for connecting two non-metallic  known body. A disadvantage of these Process gases or acids to be disposed of.

Aufgabe der Erfindung ist die Schaffung eines einfa­ chen, preiswerten, universell einsetzbaren Verfahrens zur Verlötung zweier Keramiken oder einer Keramik mit einem metallischen Werkstoff.The object of the invention is to create a simple Chen, inexpensive, universally applicable process for soldering two ceramics or one ceramic with a metallic material.

Die Aufgabe wird durch ein Verfahren mit den Merkmalen des Hauptanspruchs gelöst.The task is accomplished through a process with the characteristics of the main claim solved.

Die zu verlötende Fläche der Keramik wird mit einer re­ aktiven Komponente beschichtet. Eine Schichtdicke von wenigen Atomlagen reicht regelmäßig aus.The surface of the ceramic to be soldered is re active component coated. A layer thickness of a few atomic layers is regularly sufficient.

Die Beschichtung erfolgt vorzugsweise mechanisch, um so das Verfahren einfach und preiswert durchzuführen. Die reaktive Komponente liegt dann insbesondere als Halb­ zeug vor. Das Halbzeug wird z. B. auf der Oberfläche der Keramik verrieben. Es entsteht sofort eine dünne Schicht.The coating is preferably carried out mechanically, especially so to carry out the method easily and inexpensively. The reactive component is then in particular half stuff. The semi-finished product is e.g. B. on the surface rubbed into the ceramics. A thin one is created immediately Layer.

Beispiele für Halbzeuge sind ein Stab, ein Blech oder ein Draht. Der Draht kann in Form einer Bürste einge­ setzt werden.Examples of semi-finished products are a rod, a sheet or a wire. The wire can be turned into a brush be set.

Im nächsten Schritt wird die beschichtete Oberfläche der Keramik mit dem zu verbindenden Werkstoff verlötet. The next step is the coated surface the ceramic is soldered to the material to be joined.  

Als Lot kann ein konventionelles, also z. B. ein aus Edelmetall bestehendes Lot eingesetzt werden.A conventional, e.g. B. an off Precious metal existing solder can be used.

Die Aufgabe wird also gelöst, indem eine Beschichtung mit der reaktiven Komponente (im Unterschied zum Stand der Technik mit dem Aktivlot) getrennt vom Lötvorgang erfolgt.The task is therefore solved by a coating with the reactive component (in contrast to the state technology with the active solder) separately from the soldering process he follows.

Bei einer Kapillarlötung kann nun durch das anspruchs­ gemäße Verfahren sichergestellt werden, daß die zu ver­ lötende Oberfläche mit dem aufgeschmolzenen Lot voll­ ständig benetzt wird. Es entfällt der Einsatz eines speziellen Aktivlotes. Die Komponenten können einzeln erworben werden und für jeden einzelnen Anwendungsfall geeignet zusammengestellt werden.With a capillary soldering can now by the demanding appropriate procedures to ensure that the ver soldering surface with the melted solder full is constantly wetted. The use of a special active solder. The components can be individually can be acquired and for each individual application be put together appropriately.

Insbesondere Oxidkeramiken konnten erfolgreich mitein­ ander oder mit Metall verlötet werden.Oxide ceramics in particular were able to be successful other or with metal.

Wird beispielsweise Aluminiumoxid mit einer Nickel-Ko­ balt-Legierung verlötet, so kann als reaktive Kompo­ nente Ti, Zr, Hf, V oder Nb eingesetzt werden. Als Lot wurde dann das Silber-Kupfer-Eutektikum eingesetzt. Al­ ternativ kann z. B. ein Gold- oder Gold-Nickel-Lot vor­ gesehen werden.For example, aluminum oxide with a nickel Ko balt alloy soldered so it can be used as a reactive compo nente Ti, Zr, Hf, V or Nb can be used. As a lot the silver-copper eutectic was then used. Al ternatively z. B. before a gold or gold-nickel solder be seen.

Es ist bei der Auswahl des Lotes lediglich darauf zu achten, daß das Lot die thermodynamisch erforderlichen Löttemperaturen verträgt. So werden z. B. für eine mit Titan beschichtete Al2O3-Keramik in einem Hochvaku­ umofen bei Drücken im Bereich 10⁻4 - 10⁻5 mbar Löttempe­ raturen oberhalb von 900°C benötigt.When selecting the solder, it is only necessary to ensure that the solder can withstand the thermodynamically required soldering temperatures. So z. B. for a titanium-coated Al 2 O 3 ceramic in a high vacuum oven at pressures in the range 10⁻ 4 - 10⁻ 5 mbar soldering temperatures above 900 ° C required.

Das Lot wurde auf die beschichtete Fläche gelegt. Hier­ auf wurde der metallische Gegenstand gesetzt. Die Kera­ mik wurde dann zusammen mit dem metallischen Gegenstand auf über 900°C in einem Vakuumofen erhitzt und an­ schließend abgekühlt.The solder was placed on the coated surface. Here the metallic object was placed on. The Kera mik then became together with the metallic object heated to over 900 ° C in a vacuum oven and on finally cooled.

Die so hergestellte Lötverbindung ist mechanisch be­ lastbar und vakuumdicht.The solder connection produced in this way is mechanical resilient and vacuum-tight.

In einer vorteilhaften Ausführungsform werden die Werk­ stoffe so ausgewählt, daß die thermischen Ausdehnungs­ koeffizienten der eingesetzten Materialien weitgehend übereinstimmen. Vernachlässigbar ist dabei der Ausdeh­ nungskoeffizient der reaktiven Komponente, da von die­ ser nur wenigen Atomlagen vorliegen. Auf diese Weise werden Rißbildungen während des Abkühlens vermieden. Andernfalls kann die Keramik beschädigt oder zerstört werden.In an advantageous embodiment, the plant substances selected so that the thermal expansion coefficients of the materials used largely to match. The extent is negligible coefficient of the reactive component because of the there are only a few atomic layers. In this way cracks during cooling are avoided. Otherwise the ceramic can be damaged or destroyed become.

Al2O3 und Fe23Co28Ni weisen vergleichbare Ausdehnungs­ koeffizienten im Sinne der Erfindung auf. Diese betra­ gen im Temperaturbereich 20-300°C (5-8)10⁻6 K1 bzw. (6-8)10⁻6 K⁻1. Al 2 O 3 and Fe23Co28Ni have comparable expansion coefficients in the sense of the invention. These are in the temperature range 20-300 ° C (5-8) 10⁻ 6 K 1 or (6-8) 10⁻ 6 K⁻ 1 .

Wird das Verfahren mit Werkstoffen auf der Basis von Kohlenstoff wie z. B. mit Kohlenstoff-Fasern verstärkte Graphitkörper oder Karbide, (z. B. Borkarbide oder Si­ liziumkarbide) durchgeführt, so sind als reaktive Kom­ ponenten starke Karbidbildner vorzusehen. Titan oder Chrom sind Beispiele für starke Karbidbildner.If the process is based on materials based on Carbon such as B. reinforced with carbon fibers Graphite body or carbide, (e.g. boron carbide or Si silicon carbides) are carried out as reactive com to provide strong carbide formers. Titanium or Chromium are examples of strong carbide formers.

Wird das Verfahren mit Nitridkeramiken wie Siliziumni­ trid oder Aluminiumnitrid durchgeführt, so sind als re­ aktive Komponenten starke Nitridbildner vorzusehen. Starke Nitridbildner sind z. B. V, Ti oder Zr.If the process with nitride ceramics such as silicon Ni trid or aluminum nitride, so are as right active components to provide strong nitride formers. Strong nitride formers are e.g. B. V, Ti or Zr.

Beim anspruchsgemäßen Verfahren treten keine Umweltbe­ lastungen auf, da keine zu entsorgenden Stoffe anfal­ len. Die Beschichtung mit der reaktiven Komponente kann auf einfache Weise bei Raumtemperatur erfolgen. Zusätz­ liche Fremd- und Hilfsstoffe werden nicht benötigt. Aufwendige Techniken, wie sie bei CVD, PVD oder Metal­ lisierung angewendet werden müssen (so z. B. Abschei­ dung aus der Gasphase, Bedampfen, Kathodenzerstäubung), sind beim anspruchsgemäßen Verfahren nicht erforder­ lich. Die aufzutragende reaktive Komponente ist leicht zu beschaffen, da handelsübliche Halbzeuge eingesetzt werden können. Da sich das Lot während der Lötung nur auf der beschichteten Fläche ausbreitet, ist eine Ab­ deckung nicht zu benetzender Flächen entbehrlich. Für die Lötung können konventionelle Edelmetall-Lote einge­ setzt werden. Das Verfahren kann von einer angelernten Hilfskraft angewendet werden. Das Verfahren läßt sich problemlos mechanisieren und automatisieren. Es kann somit nicht nur in der Einzelfertigung, sondern auch in der Klein- und Großserienfertigung kostengünstig einge­ setzt werden.No environmental impact occurs in the method according to the claims burdens, since there are no substances to be disposed of len. The coating with the reactive component can easily done at room temperature. Additional Foreign and auxiliary substances are not required. Elaborate techniques such as those used in CVD, PVD or metal must be applied (such as separation formation from the gas phase, vapor deposition, cathode sputtering), are not required for the sophisticated process Lich. The reactive component to be applied is light to procure, since standard semifinished products are used can be. Because the solder only during soldering spreading on the coated surface is an ab Covering areas not to be wetted is not necessary. For The soldering can be done using conventional precious metal solders be set. The process can be done by a trained Assistant be applied. The procedure can be  mechanize and automate easily. It can thus not only in one-off production, but also in small and large series production cost-effective be set.

Claims (1)

Verfahren zum Verbinden zweier Keramiken oder einer Keramik mit einem Metall, indem eine Oberfläche ei­ ner Keramik mit einer reaktiven Komponente beschich­ tet wird und die beschichtete Oberfläche mit der Oberfläche einer weiteren, in gleicher Weise be­ schichteten Keramik oder mit der Oberfläche eines Metalls verlötet wird.Method of joining two ceramics or one Ceramic with a metal by a surface egg Coating a ceramic with a reactive component tet and the coated surface with the Surface of another, be in the same way layered ceramic or with the surface of a Metal is soldered.
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WO2002034447A1 (en) * 2000-10-24 2002-05-02 Nanogate Technologies Gmbh Soldering method for producing a ceramic-metal joint
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WO2007117988A1 (en) * 2006-03-29 2007-10-18 Honeywell International Inc. Apparatus and methods for bonding carbon-carbon composites through a reactant layer
DE102008061308A1 (en) 2008-12-11 2010-07-22 Heuberger, Martin, Dr.-Ing. About the production of metal-ceramic compounds
DE102009060938A1 (en) 2009-12-22 2011-06-30 HTM Reetz GmbH, 12555 Method for producing sealed ceramic-ceramic-compound and ceramic-metal-compound, comprises soldering the compound using a metallic solder, where the first metallic solder zone is converted in a chemical-thermal process
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