EP0688879A1 - Appareil à vide élevée - Google Patents

Appareil à vide élevée Download PDF

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Publication number
EP0688879A1
EP0688879A1 EP95107446A EP95107446A EP0688879A1 EP 0688879 A1 EP0688879 A1 EP 0688879A1 EP 95107446 A EP95107446 A EP 95107446A EP 95107446 A EP95107446 A EP 95107446A EP 0688879 A1 EP0688879 A1 EP 0688879A1
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EP
European Patent Office
Prior art keywords
ppm
vacuum
vacuum apparatus
oxygen
purity
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
Application number
EP95107446A
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German (de)
English (en)
Other versions
EP0688879B1 (fr
Inventor
Norikazu C/O Chuo-Kenkyusho Ishida
Yoshiharu C/O Chuo-Kenkyusho Mae
Kenji C/O Chuo-Kenkyusho Yajima
Takuro Iwamura
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.)
Mitsubishi Materials Corp
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Mitsubishi Materials Corp
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Publication date
Application filed by Mitsubishi Materials Corp filed Critical Mitsubishi Materials Corp
Publication of EP0688879A1 publication Critical patent/EP0688879A1/fr
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper

Definitions

  • the invention relates to a material or to members to be used for the manufacture of high-vacuum appartuses such as power transmitter tubes, external anodes which also serve as vacuum containers for microwave tubes, vacuum deposition and sputtering apparatuses, klystrons, waveguides, acceleration cavity containers for accelerators, etc., from which hydrogen is easily removed by baking, as well as to a vacuum apparatus comprising such material or members.
  • high-vacuum appartuses such as power transmitter tubes, external anodes which also serve as vacuum containers for microwave tubes, vacuum deposition and sputtering apparatuses, klystrons, waveguides, acceleration cavity containers for accelerators, etc., from which hydrogen is easily removed by baking, as well as to a vacuum apparatus comprising such material or members.
  • materials or members for the manufacture of high-vacuum apparatuses have generally been made of high-purity oxygen-free copper which satisfies required excellent electrical conductivity and thermal conductivity and includes low residual gas for preventing reduction in the degreee of vacuum in a vacuum apparatus due to residual gas in the material from which the apparatus is made.
  • Such low-residual-gas including high-purity oxygen-free copper is manufactured by degassing of normal oxygen-free copper in a reducing or vacuum atmosphere, or by addition of phophorus for deoxygenation.
  • High-purity oxygen-free copper produced in this manner contains 3 ppm or less of oxygen and 0.2 to 0.5 ppm of hydrogen, and vacuum apparatuses made of such high-purity oxygen-fee copper are subjected to dehydrogenatoina by vacuum annealing, called "baking", before use to guard against reduction in the degree of vacuum in a vacuum apparatus due to an out-gas from the material of the apparatus in a high vacuum.
  • the object of the present invention is to provide a high-purity copper alloy material suitable for high vacuum apparatuses which has after baking a reduced residual hydrogen content.
  • the inventors have conducted research aimed at producing a material suitable as vacuum apparatus member made of a copper alloy from which hydrogen is easily removed by baking, conventionally high-purity oxygen-free copper, which does not lead to a reduced degree of vacuum due to out-gassing hydrogen when used in a high vacuum, as well as a vacuum apparatus comprising such a vacuum apparatus member, and have found that a copper alloy prepared by adding 1 to 15 ppm of zirconium (Zr) to normal high-purity oxygen-free copper allows easy removal of hydrogen by baking and has a very low level of out-gassing of residual hydrogen from the material in a high vacuum, thus preventing reduction in the degree of vacuum.
  • Zr zirconium
  • the present invention has been accomplished on the basis of this finding, and is characterized by being a material having a composition of high-purity oxygen-free copper with a purity of 99.99 wt% or greater, which contains 1 to 15 ppm of Zr and 3 ppm or less of oxygen; and vacuum apparatuses constructed with the aforementioned material having a composition of high-purity copper with a purity of 99.99 wt% or greater, which contains 1 to 15 ppm of Zr and 3 ppm or less of oxygen.
  • the material of the present invention allows easy removal of hydrogen by baking when it contains 1 to 15 ppm of Zr because, since Zr is an element with a very strong affinity for oxygen, residual trace oxygen in the copper alloy combines preferentially with Zr and is not dissociated therefrom even by heating during baking. Therefor, the residual trace oxygen in the high-purity copper alloy does not trap hydrogen, and thus the hydrogen is easily removed during baking.
  • a Zr content of less than 1 ppm is not preferred since this is insufficient for combining with the residual oxygen in the copper alloy, and conversely a Zr content of more than 15 ppm is not preferred since this reduces the hydrogen-removing effect during baking.
  • the range of the Zr content is therefore established to be 1 to 15 ppm.
  • a more preferred range of the Zr content is 3 to 10 ppm.
  • the oxygen content of the vacuum apparatus member of the present invention is preferably up to 3 ppm.
  • electrolytic copper with a purity of 99.99 wt% or greater is melted in a melting furnace under constant protection with CO + N2 gas, and the resulting molten metal is poured into a ladle while Zr is added to the flow of the molten metal for adjustement of the components to a prescribed composition.
  • the apparatus shown in the drawings comprises a melting furnace 1, a spout 2, a tundish 3, an addition apparatus 4, a nozzle 5, a mold 6, a covering 7 of graphite particles and a sealing gas source 8 in order to produce an ingot 9.
  • electrolytic copper with a purity of 99.99 wt% or greater was prepared and melted in the melting furnace 1 in a CO + N2 atmosphere.
  • the resulting molten metal was passed through the spout 2 sealed with CO + N2 gas and transported to the tundish 3, and Zr was added from the addition apparatus 4 to the flowing molten metal before it reached the tundish 3.
  • the surface of the molten metal in the tundish 3 was covered with a layer of graphite particles 7 to prevent its oxidation.
  • the molten metal was then fed from the tundish 3 via the nozzle 5 to the mold 6 which was also sealed with CO + N2 gas, and an ingot 9 was obtained.
  • Table 1 below shows the composition of the ingot obtained in this manner as detrmined by measurement of the Zr and oxygen contents. Specimens of 25 mm length, 25 mm width and 8 mm thickness were cut out from the ingot, and further lathed to prepare vacuum apparatus members of the present invention (1 to 10 of Table 1), vacuum apparatus members for comparison (1 to 3 of Table 1) and vacuum apparatus members of the conventional art (1 to 3 of Table 1), each having a diameter of 20 mm and a thickness of 4 mm.
  • the vacuum apparatus material or members of the present invention 1 to 10, vacuum apparatus members for comparison 1 to 3 and vacuum apparatus members of the conventional art 1 to 3 were subjected to baking for one hour at a temperature of 500 °C in a vacuum atmosphere of 266 x 10 ⁇ 5 Pa (2 x 10 ⁇ 5 Torr) and these baked vacuum apparatus members of the present invention, vacuum apparatus members for comparison and vacuum apparatus members of the conventional art were further charged into an out-gas measuring apparatus to measure the out-gassing rate of hydrogen gas in a high-vacuum atmosphere of 133 x 10 ⁇ 10 Pa (1 x 10 ⁇ 10 Torr) while at a temperature of 500 °C.
  • Table 1 The results are given in Table 1.
  • a material for vacuum apparatus members according to the present invention offers easier removal of hydrogen during baking than vacuum apparatus members of the ceonventional art, and therefore it produces the excellent industrial effect of allowing the production of vacuum apparatuses with superior performance.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
EP19950107446 1994-06-20 1995-05-17 Appareil à vide élevée Expired - Lifetime EP0688879B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP160596/94 1994-06-20
JP16059694A JPH083664A (ja) 1994-06-20 1994-06-20 真空装置用部材および真空装置

Publications (2)

Publication Number Publication Date
EP0688879A1 true EP0688879A1 (fr) 1995-12-27
EP0688879B1 EP0688879B1 (fr) 1998-02-04

Family

ID=15718373

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19950107446 Expired - Lifetime EP0688879B1 (fr) 1994-06-20 1995-05-17 Appareil à vide élevée

Country Status (3)

Country Link
EP (1) EP0688879B1 (fr)
JP (1) JPH083664A (fr)
DE (1) DE69501569T2 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007040822B4 (de) * 2006-08-30 2013-08-14 Mitsubishi Electric Corp. Kupferlegierung und Verfahren zu deren Herstellung
US10494712B2 (en) 2015-05-21 2019-12-03 Jx Nippon Mining & Metals Corporation Copper alloy sputtering target and method for manufacturing same

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7131376B2 (ja) * 2018-12-27 2022-09-06 三菱マテリアル株式会社 スパッタリングターゲット用銅素材
CN113290217B (zh) * 2021-05-28 2022-09-23 金川集团股份有限公司 高纯无氧铜杆的真空连铸工艺

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62207834A (ja) * 1986-03-10 1987-09-12 Nippon Mining Co Ltd 高真空雰囲気中で使用する銅材
JPS62243727A (ja) * 1986-04-16 1987-10-24 Hitachi Cable Ltd プリント基板用圧延銅箔
US4717436A (en) * 1985-03-27 1988-01-05 Mitsubishi Kinzoku Kabushiki Kaisha Wire for bonding a semiconductor device
JPS63312934A (ja) * 1987-06-16 1988-12-21 Hitachi Cable Ltd 半導体用リ−ドフレ−ム材
EP0296596A1 (fr) * 1987-06-25 1988-12-28 The Furukawa Electric Co., Ltd. Fil de cuivre fin à utiliser dans les instruments eléctroniques et son procédé de fabrication
US5077005A (en) * 1989-03-06 1991-12-31 Nippon Mining Co., Ltd. High-conductivity copper alloys with excellent workability and heat resistance

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4717436A (en) * 1985-03-27 1988-01-05 Mitsubishi Kinzoku Kabushiki Kaisha Wire for bonding a semiconductor device
JPS62207834A (ja) * 1986-03-10 1987-09-12 Nippon Mining Co Ltd 高真空雰囲気中で使用する銅材
JPS62243727A (ja) * 1986-04-16 1987-10-24 Hitachi Cable Ltd プリント基板用圧延銅箔
JPS63312934A (ja) * 1987-06-16 1988-12-21 Hitachi Cable Ltd 半導体用リ−ドフレ−ム材
EP0296596A1 (fr) * 1987-06-25 1988-12-28 The Furukawa Electric Co., Ltd. Fil de cuivre fin à utiliser dans les instruments eléctroniques et son procédé de fabrication
US5077005A (en) * 1989-03-06 1991-12-31 Nippon Mining Co., Ltd. High-conductivity copper alloys with excellent workability and heat resistance

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
HELENIUS,A.,KOLEHMAINEN,M., RAJAINMAKI,H.: "Current and Future Uses of Oxygen-Free Copper", METALL, vol. 44, no. 11, pages 1067 - 1070 *
PATENT ABSTRACTS OF JAPAN vol. 12, no. 122 (C - 488) 15 April 1988 (1988-04-15) *
PATENT ABSTRACTS OF JAPAN vol. 12, no. 70 (C - 479) 4 March 1988 (1988-03-04) *
PATENT ABSTRACTS OF JAPAN vol. 13, no. 156 (C - 585) 14 April 1989 (1989-04-14) *
RAJAINMAKI,H., KOLEHMAINEN,M.,HELENIUS,A.: "The Production and Application of Oxygen-Free Copper", JOURNAL OF METALS, vol. 45, no. 3, pages 68 - 70 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007040822B4 (de) * 2006-08-30 2013-08-14 Mitsubishi Electric Corp. Kupferlegierung und Verfahren zu deren Herstellung
US10494712B2 (en) 2015-05-21 2019-12-03 Jx Nippon Mining & Metals Corporation Copper alloy sputtering target and method for manufacturing same

Also Published As

Publication number Publication date
DE69501569T2 (de) 1998-06-10
DE69501569D1 (de) 1998-03-12
EP0688879B1 (fr) 1998-02-04
JPH083664A (ja) 1996-01-09

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