DE2750436A1 - brazeable metal films prodn. on ceramics - by deposition of palladium-nickel alloy on ceramic support - Google Patents

brazeable metal films prodn. on ceramics - by deposition of palladium-nickel alloy on ceramic support

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Publication number
DE2750436A1
DE2750436A1 DE19772750436 DE2750436A DE2750436A1 DE 2750436 A1 DE2750436 A1 DE 2750436A1 DE 19772750436 DE19772750436 DE 19772750436 DE 2750436 A DE2750436 A DE 2750436A DE 2750436 A1 DE2750436 A1 DE 2750436A1
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Germany
Prior art keywords
palladium
alloy
nickel
ceramic
layer
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.)
Withdrawn
Application number
DE19772750436
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German (de)
Inventor
Wolfgang Dr Koehler
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.)
Evonik Operations GmbH
Original Assignee
Degussa GmbH
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Publication date
Application filed by Degussa GmbH filed Critical Degussa GmbH
Priority to DE19772750436 priority Critical patent/DE2750436A1/en
Publication of DE2750436A1 publication Critical patent/DE2750436A1/en
Withdrawn legal-status Critical Current

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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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • 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
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
    • C04B41/5144—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal with a composition mainly composed of one or more of the metals of the iron group
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/88—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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/09—Use of materials for the conductive, e.g. metallic pattern
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/03—Conductive materials
    • H05K2201/0302—Properties and characteristics in general
    • H05K2201/0317—Thin film conductor layer; Thin film passive component

Abstract

The palladium-nickel alloy, applied to the ceramic substrate for formation of a brazable metal film, contains 30-60 wt.% Ni. It may also contain 3-20 wt.% Cr, Mn and/or Ti. The film is applied by vapour deposition in vacuum or by cathodic sputtering. If cathodic sputtering is used, a thin Cr layer is first deposited. In an example, an Al oxide substrate is mounted on a turn table spaced 150 mm from a tungsten boat, used as evaporator. The vapour deposition vacuum is 10-4 torr, and the alloy contains 36% wt. Ni, 56% Pd and 8% Cr. The evaporator is heated for 1 min. to 1100 degrees C and then brought to 1300 degrees C.

Description

Die Erfindung betrifft ein Verfahren zur Herstellung hart-The invention relates to a method for producing hard

lötfähiger und guthaftender Metallschichten auf Keramikteilen durch Aufbringung einer nickelhaltigen Legierung.solderable and well-adhering metal layers on ceramic parts Application of an alloy containing nickel.

Es ist bekannt, lötfähige Schichten auf Keramikunterlagen durch Auftragung von metallhaltigen Einbrennpasten herzustellen. Die Haftung solcher Schichten auf der Keramikunterlage ist jedoch in vielen Fällen nicht ausreichend.It is known to apply solderable layers to ceramic substrates of metal-containing stoving pastes. The adhesion of such layers on however, the ceramic base is not sufficient in many cases.

Außerdem sind diese Schichten meist nur mit silberhaltigen Weichloten lötbar, nicht Jedoch mit Hartloten.In addition, these layers are usually only with silver-containing soft solders Solderable, but not with hard solder.

Weiterhin ist das Aufdampfen oder Aufsputtern von Nickel-oder Nickellegierungsschichten mit Eisen oder Chrom zur Lötbarmachung von Keramikteilen bekannt. In der Praxis zeigt sich Jedoch, daß diese Nickelauflagen von den verwendeten Hartloten angegriffen und aufgelöst werden.Furthermore, there is the vapor deposition or sputtering of nickel or nickel alloy layers with iron or chromium for making ceramic parts solderable. In practice However, it turns out that these nickel coatings are attacked by the brazing alloys used and be resolved.

Es war daher Aufgabe der vorliegenden Erfindung, ein Verfahren zur Herstellung von lötfähigen Metallschichten auf Keramikunterlagen zu finden, die gegen Hartlote beständig und gut haftfest auf der Unterlage sind.It was therefore an object of the present invention to provide a method for Manufacture of solderable metal layers on ceramic substrates to find that are resistant to hard solder and have good adhesion to the substrate.

Diese Aufgabe wurde erfindungsgemäß dadurch gelöst, daß auf die Keramikunterlage eine Schicht aus einer Palladium-Nickel-Legierung mit 20 bis 70 Ges.% Nickel aufgebracht wird. Besonders bewährt haben sich Legierungen, die 30 bis 60 Cew.% Nickel enthalten.This object was achieved according to the invention in that on the ceramic base a layer of a palladium-nickel alloy with 20 to 70 total% nickel is applied will. Alloys which contain 30 to 60 Cew.% Nickel have proven particularly useful.

Solche Legierungsschichten zeigen überraschenderweise eine gute Haftung auf der Keramikunterlage und sind bereits bei einer Schichtdicke von 1 bis 2/um einwandfrei hartlötbar, ohne daß die Schicht von den gebräuchlichen Hartloten aufgelöst wird. Besonders gut haftende und hartlotbeständige Schichten erhält man, wenn man der Palladium-Nlokel-Legierung zusätzlich noch insgesamt 3 bis 20 Gew.% Chrom und/oder Mangan und/oder Titan zugibt.Such alloy layers surprisingly show good adhesion on the ceramic base and are already at a layer thickness of 1 to 2 μm Can be brazed perfectly without the layer being dissolved by the conventional brazing alloys will. Layers that adhere well and are resistant to hard solder are obtained if the palladium-Nlokel alloy additionally a total of 3 to 20% by weight of chromium and / or manganese and / or titanium is added.

Vorteilhafterweise bringt man die erfindungsgemäßen Legierungsschichten durch Aufdampfen im Vakuum oder durch Sputtern auf die Keramikunterlagen auf. Ein großer Vorteil bei der Verwendung der erfindungsgemäßen Palladium-Nickel-Legierungen ist dabei ihr relativ niedriger Schmelzpunkt. Eine Palladiumlegierung mit 40 ,~ Nickel schmilzt beispielsweise bei 1237°C. Bei der Hochvakuumverdampfung wird meist bei einem Druck von etwa 1p10-4 Torr gearbeitext, bei dem der Dampfdruck von Nickel und Palladium annähernd gleich ist und der Siedepunkt bei etwa 12500C liegt. Das hat den großen Vorteil, daß die erfindungsgemäusen Legierungen sehr schnell aus der Schmelze verdampfen, während die reinen Metalle bei diesem Druck sublimieren. Durch die schnelle Verdampfung aus der Schmelze ist die Haftung der erfindungsgemäßen Legierungen auf der sehr sehr gut und besser als die der reinen Metallkomponenten.The alloy layers according to the invention are advantageously applied by vapor deposition in a vacuum or by sputtering onto the ceramic substrates. A great advantage when using the palladium-nickel alloys according to the invention is their relatively low melting point. A palladium alloy with 40, ~ For example, nickel melts at 1237 ° C. In the case of high vacuum evaporation, mostly worked at a pressure of about 1p10-4 Torr, which is the vapor pressure of nickel and palladium are approximately the same and the boiling point is about 12500C. That has the great advantage that the alloys according to the invention wear out very quickly of the melt evaporate, while the pure metals sublime at this pressure. Due to the rapid evaporation from the melt, the adhesion is according to the invention Alloys on the very very good and better than those of the pure metal components.

Der Zusatz von 3 bis 20 Gew.% Chrom und/oder Mangan und/ oder Titan verbessert die Haftfestigkeit der aufgedampften Legierungsschichten noch mehr. Beispielsweise kann man hifrfUr eine Legierung aus 54 Gew.% Palladium, 36 Gew.% Nickel und 10 Gew.% Chrom verwenden. Allerdings kann das Chrom auch vorher als Haftvermittler in dünner Schicht aus einem getrennten Verdampfer auf die Keramikunterlage aufgebracht werden.The addition of 3 to 20% by weight of chromium and / or manganese and / or titanium improves the adhesive strength of the vapor-deposited alloy layers even more. For example one can use an alloy of 54% by weight palladium, 36% by weight nickel and 10% by weight Use chrome. However, the chrome can also be used as an adhesion promoter in thinner Layer from a separate evaporator can be applied to the ceramic substrate.

Eine sehr gute Haftfestigkeit und Hartlötfähigkeit zeigen auch Palladium-Nickel-Legierungsschichten, die durch einen Sputterprozess auf die Keramikunterlagen aufgebracht wurden. Beispielsweise wird hierzu eine Palladiumlegierung mit 50 Gew.% Nickel verwendet. Beim Sputterprozess ist es besonders vorteilhaft für die Haftfestigkeit der aufgebrachten Palladium-Nickel-Legierungsschicht, wenn zuvor eine dünne Chromschicht auf die Keramikunterlage aufgesputtert wird.Palladium-nickel alloy layers also show very good adhesive strength and brazing ability, which were applied to the ceramic substrates by a sputtering process. For example a palladium alloy is used for this purpose used with 50 wt.% nickel. In the sputtering process, it is particularly advantageous for the adhesive strength of the applied Palladium-nickel alloy layer, if previously a thin layer of chrome on the ceramic base is sputtered on.

Ein weiterer Vorteil der erfindungsgemäßen Palladium-Nickel-Legierungs-Auflagen ist deren hohe Kratzfestigkeit, die weit höher ist als die der einzelnen Komponenten. Sie ist sogar beständig gegen feine Stahlwolle. Die fertigmetallisierten Keramikteile können daher ohne besondere Vorsicht gelagert werden.Another advantage of the palladium-nickel alloy coatings according to the invention is their high scratch resistance, which is far higher than that of the individual components. It is even resistant to fine steel wool. The finished metalized ceramic parts can therefore be stored without special care.

Das erfindungsgemäße Verfahren ist bei allen Keramikwerkstoffen, wie beispielsweise Aluminiumoxid, Magnesiumoxid, Siliziumnitrid oder Wolframcarbid, anwendbar. Als Hartlote können alle gebräuchlichen Hartlote verwendet werden.The inventive method is for all ceramic materials, such as for example aluminum oxide, magnesium oxide, silicon nitride or tungsten carbide, applicable. All common hard solders can be used as hard solders.

Folgende Beispiele sollen das erfindungsgemäße Verfahren näher erläutern: 1. In einer Aufdampfanlage üblicher Bauart wurden Aluminium-450 oxid-Substrate in etwa mm Abstand von dem Verdampfer (Wolframschiffohen) auf einem Drehteller montiert und bei einem Vakuum von 1u10-4 Torr mit einer Legierung aus 36 Gew.% Nickel, 56 Gew.% Palladium und 8 Gew.% Chrom bedampft. Der Verdampfer wurde zuerst etwa 1 Minute auf 11000C erhitzt und dann auf etwa 13000C gebracht, wobei die Legierung schmilzt und verdampft. Die Schichtstärke der Legierung auf den Substraten betrug etwa 1,8/um.The following examples are intended to explain the process according to the invention in more detail: 1. In a conventional type of vapor deposition system, aluminum 450 oxide substrates were made in about mm distance from the evaporator (tungsten boats) mounted on a turntable and at a vacuum of 1u10-4 Torr with an alloy of 36 wt% nickel, 56 % By weight palladium and 8% by weight chromium vapor-coated. The vaporizer was on for about 1 minute first heated to 11000C and then brought to about 13000C, melting the alloy and evaporates. The layer thickness of the alloy on the substrates was about 1.8 μm.

2. In einer Sputteranlage üblicher Bauart wurden mehrere Aluminiumoxidplättrhen zuerst unter einem Chromtarget mit einer 0,1/um starken Chromschicht und dann unter einem Pd 50 Ni-target mit einer Palladium-Nickelauflage von 1,7/um Dicke versehen.2. In a conventional type of sputtering system, several aluminum oxide plates were first placed under a chromium target with a 0.1 .mu.m thick chromium layer and then under a Pd 50 Ni target with a palladium-nickel coating of 1.7 μm thickness.

Die nach beiden Verfahren metallisierten Substratplatten lassen sich mit einem Silberhartlot der Zusammensetzung 30 % Ag, 28 % Cu, 21 % Zn und 21 ,~ Cd ohne Schwierigkeiten auf Eisenblech, Kupfer oder VA-Material bei 6800C auflöten.The substrate plates metallized by both methods can be with a silver hard solder of the composition 30% Ag, 28% Cu, 21% Zn and 21, ~ Solder Cd without difficulty on sheet iron, copper or VA material at 6800C.

Man erhält eine guthaftende Lotzone.A well-adhering solder zone is obtained.

In gleicher Auflagenstärke aufgedampfte oder aufgesputterte Nickelschichten ließen sich nicht hartlöten, das Hartlot löste die Auflage in sehr starkem Maße auf.Nickel layers vapor-deposited or sputtered with the same thickness could not be brazed, the braze dissolved the layer to a very large extent on.

Claims (5)

Verfahren zur Herstellung hartlötfähiger Metallschichten auf Keramik Patentansprüche: 1. Verfahren zur Herstellung hartlötfähiger MetallschicA-ten auf Keramik, dadurch gekennzeichnet, daß auf die Keramikunterlage eine Schicht aus einer Palladium-Nickel-Legierung mit 20 bis 70 Cew.% Nickel aufgebracht wird. Process for the production of brazeable metal layers on ceramic Claims: 1. Process for the production of brazeable MetallschicA-th Ceramic, characterized in that a layer of one on the ceramic base Palladium-nickel alloy with 20 to 70 Cew.% Nickel is applied. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Palladium-Nicke 1-Legierung 30 bis 60 % Nickel enthält. 2. The method according to claim 1, characterized in that the palladium nickel 1 alloy contains 30 to 60% nickel. 3. Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet, daß die Legierung zusätzlich noch insgesamt 3 bis 20 Gew.% Chrom und/oder mangan und/oder Titan enthält. 3. The method according to claim 1 and 2, characterized in that the Alloy additionally a total of 3 to 20% by weight of chromium and / or manganese and / or Contains titanium. 4. Verfahren nach Anspruch 1 bis 3, dadurch gekennzeichnet, daß die Aufbringung d#r Legierungsschicht durch Aufdampfen im Vakuum oder durch Sputtern erfolgt. 4. The method according to claim 1 to 3, characterized in that the Application of the alloy layer by vapor deposition in a vacuum or by sputtering he follows. 5. Verfahren nach Anspruch 1 bis 4, dadurch gekennzeichnet, daß bei Aufbringung der L?gierungsschicht durch Sputtern zuerst eine dünne Chromschicht auEgesputtert wird. 5. The method according to claim 1 to 4, characterized in that at Application of the alloy layer by sputtering first a thin chrome layer is sputtered out.
DE19772750436 1977-11-11 1977-11-11 brazeable metal films prodn. on ceramics - by deposition of palladium-nickel alloy on ceramic support Withdrawn DE2750436A1 (en)

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DE19772750436 DE2750436A1 (en) 1977-11-11 1977-11-11 brazeable metal films prodn. on ceramics - by deposition of palladium-nickel alloy on ceramic support

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0716159A1 (en) * 1994-12-07 1996-06-12 General Electric Company Brazable articles
US8308830B2 (en) 2007-05-22 2012-11-13 David Patrick Egan Coated cBN
DE102017126590A1 (en) * 2017-11-13 2019-05-16 Doduco Solutions Gmbh Method for producing a base plate for an electronic module

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0716159A1 (en) * 1994-12-07 1996-06-12 General Electric Company Brazable articles
US5626909A (en) * 1994-12-07 1997-05-06 General Electric Company Fabrication of brazable in air tool inserts
US8308830B2 (en) 2007-05-22 2012-11-13 David Patrick Egan Coated cBN
DE102017126590A1 (en) * 2017-11-13 2019-05-16 Doduco Solutions Gmbh Method for producing a base plate for an electronic module

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