EP1331280A1 - Verfahren zur Herstellung eines Silberrohlings sowie ein Rohrtarget - Google Patents
Verfahren zur Herstellung eines Silberrohlings sowie ein Rohrtarget Download PDFInfo
- Publication number
- EP1331280A1 EP1331280A1 EP02026718A EP02026718A EP1331280A1 EP 1331280 A1 EP1331280 A1 EP 1331280A1 EP 02026718 A EP02026718 A EP 02026718A EP 02026718 A EP02026718 A EP 02026718A EP 1331280 A1 EP1331280 A1 EP 1331280A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- silver
- casting
- calcium
- content
- aluminum
- 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.)
- Granted
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D13/00—Centrifugal casting; Casting by using centrifugal force
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D25/00—Special casting characterised by the nature of the product
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/006—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with use of an inert protective material including the use of an inert gas
Definitions
- the invention relates to a method for producing a silver blank with a silver content of ⁇ 99.99% by weight and an oxygen content of ⁇ 20 ⁇ g / g as well as a tube target for cathode sputtering systems.
- Stand casting has long been a method for producing such a silver blank known, wherein the silver is melted under an inert or reducing atmosphere to to prevent a high oxygen uptake of the silver during melting.
- the solubility for oxygen in the liquid state is approximately 40 times higher than for silver in the solid state. If a reducing or inert atmosphere is not provided, then During the melting process, oxygen from the air in high concentrations of 1000 up to 3000 ⁇ g / g absorbed extremely quickly by the silver melt. In the subsequent Solidification of the silver melt suddenly causes a large part of the oxygen absorbed released again, which leads to a violent reaction - similar to a boiling of the melt. The casting formed then usually shows a volcanic surface and high porosity.
- a high proportion of dissolved oxygen in the solidified silver cracks at the grain boundaries, which leads to fragility of the silver.
- Concentrations of dissolved oxygen are values of greater than 50 ⁇ g / g, an oxygen concentration in the range from 50 to 100 ⁇ g / g is usually present.
- the problem therefore arises of providing a method for producing a silver blank, in which the uptake of oxygen from the atmosphere is clearly hindered and thereby suppressing the formation of cracks at the grain boundaries in the silver. It posed The problem continues that the silver blank is for use as an atomizing material in a tube target should have the usual purity in the range ⁇ 99.99% by weight.
- the solidified silver meets the commercial specification for tube targets with a silver content of ⁇ 99.99% by weight.
- the method according to the invention is particularly advantageous if the casting of the silver melt takes place by centrifugal casting.
- the addition of 100 to 500 ⁇ g / g calcium or aluminum to the silver melt before centrifugal casting makes it possible to carry out the casting process in air. Setting an inert or reducing atmosphere during casting is no longer necessary.
- the melting of the silver or the silver including the Calcium and aluminum are still made under an inert or reducing atmosphere to have sufficient calcium and aluminum in the casting process in the silver. Suitable here themselves as atmospheres, particularly argon or carbon monoxide. It is also advantageous here melting the silver under a cover with coal.
- the problem is solved for the tube target by using a silver blank as the atomizing material is used, which was prepared by the inventive method.
- a silver blank has an almost pore-free and dense grain structure, it is for Excellent use as atomization material in a tube target.
- the content of calcium or aluminum in the atomizing material or silver blank ⁇ 100 ⁇ g / g, in particular ⁇ 50 ⁇ g / g, because the commercial specification requires a silver content of ⁇ 99.99% by weight for such targets.
- the silver melts with the doping elements Zr, Y, Si, Sn, Mg, Pb showed and Zn the same violent reactions as undoped silver (see experiment 1).
- the volcanic raised surface was unchanged, so that no influence of these elements on the oxygen absorption behavior of the liquid silver could be determined.
- a bending sample 1 was produced from undoped silver by melting 5 kg of silver in a carbon monoxide atmosphere, keeping the silver melt in air for 30 s and pouring the silver melt in air into a graphite mold.
- a bending sample 2 from Ca-doped silver with a Ca addition of 400 ⁇ g / g was carried out by melting 5 kg of silver and an Ag-Ca master alloy with a content of 6% by weight Ca under a carbon monoxide atmosphere, keeping the silver melt in air over 30 s and pouring the silver melt in air into a graphite mold.
- a bending sample 3 from Al-doped silver with an Al addition of 200 ⁇ g / g was carried out by melting 5 kg of silver and an Ag-Al master alloy with a content of 6 wt .-% Al in a carbon monoxide atmosphere, keeping the silver melt in air above 30 s and pouring the silver melt in air into a graphite mold.
- the middle of the solidified castings or silver blanks became 5 mm thick Sawed out slices and subjected to a bending test.
- the porosity in the silver blank rose sharply from the outer tube diameter with values of 1.3 vol.% Porosity in the direction of the inner tube diameter to values of 6.5 vol.% Porosity up to the formation of pronounced cracks in the grain structure.
- a leak test with 2 - 3 bar water pressure showed water penetration through the pipe wall, so that the presence of several continuous cracks could be determined.
- the analysis of the tubular silver blank produced showed a content of 5 - 8 ⁇ g / g dissolved oxygen and a content of 23 ⁇ g / g Ca in the grain structure.
- the silver blank was used as an atomizing material in a tube target for cathode sputtering systems. The behavior of the tube target in the coating of flat glass was flawless.
- the oxygen content of the silver it should be noted that this is not only from the used doping and their addition amounts depends, but that also the rest Experiment parameters have an influence on it. For example, with a fast Cooling of the melt means that less oxygen escapes than with slow cooling. In order to is the oxygen content of a casting with a certain doping and doping amount reproduce only if the other test parameters such as the casting process used, the casting amount, the casting atmosphere, holding times, the casting time or cooling time are largely identical. It has been shown that silver only with an oxygen content ⁇ 20 ⁇ g / g no longer tends to become brittle and the grain structure is dense and crack-free is.
- tube targets can, for example, EP 586 809 A1, US 5,354,446, US 5,591,314, FR 2745010, EP 500 774 B1, WO 97/15697 or DE 199 58 666 be removed.
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Metal Extraction Processes (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
Besonders vorteilhaft ist das erfindungsgemäße Verfahren, wenn das Gießen der Silberschmelze im Schleuderguss erfolgt. Die Zugabe von 100 bis 500 µg/g Kalzium oder Aluminium zur Silberschmelze vor dem Schleuderguss macht es möglich, den Gießvorgang an Luft vorzunehmen. Das Einstellen einer inerten oder reduzierenden Atmosphäre während des Gusses ist nicht mehr erforderlich.
- Bild 1
- einen Gefügeanschliff ( Vergrößerung 100:1 ) der Biegeprobe 1 aus Versuch 3, bei welchem deutlich Risse R an den Korngrenzen zu erkennen sind
- Bild 2
- einen Gefügeanschliff ( Vergrößerung 50:1) des Silberrohlings aus Versuch 4, 2. Abguss mit 200 µg/g Ca-Dotierung, bei welchem keine Risse vorhanden sind
- das Korngefüge zeigte im Anschliff Anrisse und aufgeweitete Korngrenzen ( siehe Bild 1 )
- das Korngefüge zeigte im Anschliff ein homogenes Gefüge mit fein verteilten, kleinen Poren
- der Ca-Gehalt betrug 98 µg/g
- der Al-Gehalt betrug 23 µg/g
Die Analyse des erzeugten rohrförmigen Silberrohlings ergab einen Gehalt von 30 - 70 µg/g gelöstem Sauerstoff im Korngefüge.
Die Porosität im Silberrohling stieg vom Rohraußendurchmesser mit Werten von 1,3 Vol.-% Porosität in Richtung des Rohrinnendurchmesser auf Werte von 6,5 Vol.-% Porosität stark an bis hin zur Bildung ausgeprägter Risse im Korngefüge.
Eine Dichtigkeitsprüfung mit 2 - 3 bar Wasserdruck zeigte einen Wasserdurchtritt durch die Rohrwandung, so dass das Vorhandensein mehrerer durchgehender Risse festgestellt werden konnte.
Die Analyse des erzeugten rohrförmigen Silberrohlings ergab einen Gehalt von 5 - 8 µg/g gelöstem Sauerstoff und einem Gehalt von 23 µg/g Ca im Korngefüge.
Bei der Bearbeitung des Silberrohlings zeigten sich weder Porosität noch Risse ( siehe Bild 2 ). Eine Dichtigkeitsprüfung mit 2 - 3 bar Wasserdruck zeigte keinen Wasserdurchtritt, die Rohrwandung war dicht.
Der Silberrohling wurde als Zerstäubungsmaterial in einem Rohrtarget für Kathodenzerstäubungsanlagen eingesetzt. Das Verhalten des Rohrtargets im Einsatz bei der Beschichtung von Flachglas war einwandfrei.
Claims (9)
- Verfahren zur Herstellung eines Silberrohlings mit einem Silbergehalt von ≥ 99,99 Gew.-% und einem Sauerstoffgehalt < 20 µg/g mit folgenden Schritten:a) Erschmelzen von Silber mit 100 bis 500 µg/g Kalzium oder Aluminium unter inerten oder reduzierenden Bedingungen, oder
Erschmelzen von Silber unter inerten oder reduzierenden Bedingungen und Zugeben von 100 bis 500 µg/g Kalzium oder Aluminium zur Silberschmelze,b) Gießen der Silberschmelze in eine Gießkokille unter Luftatmosphäre undc) Abkühlen der Silberschmelze in der Gießkokille unter Luftatmosphäre. - Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass das Gießen im Schleuderguß erfolgt.
- Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass das Gießen im Standguß erfolgt.
- Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass das Erschmelzen unter Argon-Atmosphäre erfolgt.
- Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass das Erschmelzen unter Kohlenmonoxid-Atmosphäre erfolgt.
- Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass das Silber beim Erschmelzen mit einer Kohleschicht abgedeckt wird.
- Rohrtarget für Kathodenzerstäubungsanlagen mit einem Zerstäubungsmaterial, das aus dem nach einem der Ansprüche 1 bis 6 hergestellten Silberrohling gebildet ist.
- Rohrtarget nach Anspruch 7, dadurch gekennzeichnet, dass ein Gehalt an Kalzium oder Aluminium im Zerstäubungsmaterial < 100 µg/g beträgt.
- Rohrtarget nach Anspruch 8, dadurch gekennzeichnet, dass ein Gehalt an Kalzium oder Aluminium im Zerstäubungsmaterial < 50 µg/g beträgt.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10202445A DE10202445C1 (de) | 2002-01-22 | 2002-01-22 | Verfahren zur Herstellung eines Silberrohlings sowie ein Rohrtarget |
DE10202445 | 2002-01-22 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1331280A1 true EP1331280A1 (de) | 2003-07-30 |
EP1331280B1 EP1331280B1 (de) | 2004-05-19 |
Family
ID=7712838
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP02026718A Expired - Lifetime EP1331280B1 (de) | 2002-01-22 | 2002-11-30 | Verfahren zur Herstellung eines Silberrohlings sowie ein Rohrtarget |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP1331280B1 (de) |
AT (1) | ATE267270T1 (de) |
DE (2) | DE10202445C1 (de) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2009126095A1 (en) * | 2008-04-09 | 2009-10-15 | Biopm Ab | Method of producing precious metal alloy objects |
DE102004059876B4 (de) * | 2004-12-10 | 2010-01-28 | W.C. Heraeus Gmbh | Verwendung eines Sputtertargets aus einer Silberlegierung sowie Glassubstrat mit Wärmedämmschicht |
EP2647737A1 (de) * | 2012-04-04 | 2013-10-09 | Heraeus Materials Technology GmbH & Co. KG | Planares oder rohrförmiges Sputtertarget sowie Verfahren zur Herstellung desselben |
CN103658566A (zh) * | 2013-12-31 | 2014-03-26 | 河南豫光金铅股份有限公司 | 一种生产低氧含量银锭的方法 |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6033320A (ja) * | 1983-08-04 | 1985-02-20 | Nippon Mining Co Ltd | 銅電解殿物からの高純度銀回収法 |
JPS6164830A (ja) * | 1984-09-03 | 1986-04-03 | Tanaka Kikinzoku Kogyo Kk | Ag合金の乾式精製法 |
EP0388973A1 (de) * | 1989-03-24 | 1990-09-26 | Mitsubishi Materials Corporation | Silberlegierungsblatt zur Verbindung von Sonnenzellen |
US5149498A (en) * | 1988-04-16 | 1992-09-22 | Battelle-Institut E.V. | Method of producing tarnish-resistant and oxidation-resistant alloys using zr and b |
JPH09256083A (ja) * | 1996-03-15 | 1997-09-30 | Dowa Mining Co Ltd | 高純度銀の製造方法及び製造装置 |
EP1097766A1 (de) * | 1999-11-05 | 2001-05-09 | W.C. Heraeus GmbH & Co. KG | Rohrtarget |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ATE174970T1 (de) * | 1994-10-24 | 1999-01-15 | Ivoclar Ag | Verfahren zur herstellung von metallgussteilen |
-
2002
- 2002-01-22 DE DE10202445A patent/DE10202445C1/de not_active Expired - Fee Related
- 2002-11-30 AT AT02026718T patent/ATE267270T1/de not_active IP Right Cessation
- 2002-11-30 DE DE50200464T patent/DE50200464D1/de not_active Expired - Fee Related
- 2002-11-30 EP EP02026718A patent/EP1331280B1/de not_active Expired - Lifetime
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6033320A (ja) * | 1983-08-04 | 1985-02-20 | Nippon Mining Co Ltd | 銅電解殿物からの高純度銀回収法 |
JPS6164830A (ja) * | 1984-09-03 | 1986-04-03 | Tanaka Kikinzoku Kogyo Kk | Ag合金の乾式精製法 |
US5149498A (en) * | 1988-04-16 | 1992-09-22 | Battelle-Institut E.V. | Method of producing tarnish-resistant and oxidation-resistant alloys using zr and b |
EP0388973A1 (de) * | 1989-03-24 | 1990-09-26 | Mitsubishi Materials Corporation | Silberlegierungsblatt zur Verbindung von Sonnenzellen |
JPH09256083A (ja) * | 1996-03-15 | 1997-09-30 | Dowa Mining Co Ltd | 高純度銀の製造方法及び製造装置 |
EP1097766A1 (de) * | 1999-11-05 | 2001-05-09 | W.C. Heraeus GmbH & Co. KG | Rohrtarget |
Non-Patent Citations (3)
Title |
---|
PATENT ABSTRACTS OF JAPAN vol. 009, no. 160 (C - 289) 4 July 1985 (1985-07-04) * |
PATENT ABSTRACTS OF JAPAN vol. 010, no. 230 (C - 365) 9 August 1986 (1986-08-09) * |
PATENT ABSTRACTS OF JAPAN vol. 1998, no. 01 30 January 1998 (1998-01-30) * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102004059876B4 (de) * | 2004-12-10 | 2010-01-28 | W.C. Heraeus Gmbh | Verwendung eines Sputtertargets aus einer Silberlegierung sowie Glassubstrat mit Wärmedämmschicht |
WO2009126095A1 (en) * | 2008-04-09 | 2009-10-15 | Biopm Ab | Method of producing precious metal alloy objects |
EP2647737A1 (de) * | 2012-04-04 | 2013-10-09 | Heraeus Materials Technology GmbH & Co. KG | Planares oder rohrförmiges Sputtertarget sowie Verfahren zur Herstellung desselben |
CN103658566A (zh) * | 2013-12-31 | 2014-03-26 | 河南豫光金铅股份有限公司 | 一种生产低氧含量银锭的方法 |
Also Published As
Publication number | Publication date |
---|---|
DE50200464D1 (de) | 2004-06-24 |
DE10202445C1 (de) | 2003-04-10 |
ATE267270T1 (de) | 2004-06-15 |
EP1331280B1 (de) | 2004-05-19 |
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