EP0688879B1 - Hochvakuumanlage - Google Patents

Hochvakuumanlage Download PDF

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Publication number
EP0688879B1
EP0688879B1 EP19950107446 EP95107446A EP0688879B1 EP 0688879 B1 EP0688879 B1 EP 0688879B1 EP 19950107446 EP19950107446 EP 19950107446 EP 95107446 A EP95107446 A EP 95107446A EP 0688879 B1 EP0688879 B1 EP 0688879B1
Authority
EP
European Patent Office
Prior art keywords
vacuum
ppm
vacuum apparatus
oxygen
hydrogen
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.)
Expired - Lifetime
Application number
EP19950107446
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English (en)
French (fr)
Other versions
EP0688879A1 (de
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
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Publication of EP0688879A1 publication Critical patent/EP0688879A1/de
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Publication of EP0688879B1 publication Critical patent/EP0688879B1/de
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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 the use of a material 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.
  • a material 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.
  • 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 degree 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 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 dehydrogenation 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 the use of high-purity copper alloy material as high vacuum apparatuses which have, 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 based upon the use of 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 as high vacuum apparatuses.
  • 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 + N 2 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.
  • Table 1 below shows the composition of the ingot obtained in this manner as determined 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 used in 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.
  • Vacuum apparatus member Composition Out-gassing rate (Torr ⁇ 1/sec. ⁇ cm 2 ) Electrolytic copper purity (%) Zr (ppm) Oxygen (ppm) P (ppm) Present invention 1 99.998 3 1.8 - 1.33 x 10 -11 2 99.998 4 2.0 - 2.17 x 10 -11 3 99.998 3 1.7 - 2.34 x 10 -11 4 99.998 1 0.7 - 6.75 x 10 -12 5 99.998 7 1.8 - 8.98 x 10 -12 6 99.998 12 2.0 - 1.10 x 10 -11 7 99.998 14 2.7 - 2.14 x 10 -11 8 99.998 6 1.2 - 9.77 x 10 -12 9 99.998 11 1.5 - 7.29 x 10 -12 10 99.998 10 2.0 - 1.01 x 10 -11 Comparison 1 99.998 7 5.0 * - 6.21 x 10 -10 2 99.998 0.6 * 1.8 - 2.70 x 10 -10 3 99.998 18 * 1.2
  • use of a material as high 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 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)

Claims (3)

  1. Verwendung eines hochreinen Kupfermaterials, das vor dem Glühen (Wärmebehandlung) Wasserstoff, 3 ppm oder weniger Sauerstoff und 1 bis 15 ppm Zr enthält und eine Reinheit von 99,99 Gew.-% oder höher besitzt, als Material für die Herstellung von Hochvakuumapparaturen.
  2. Verwendung des Materials nach Anspruch 1, das 3 bis 10 ppm Zr enthält, für den gleichen Zweck wie in Anspruch 1.
  3. Verwendung des Materials nach Anspruch 1 oder 2 zur Herstellung von Energietransmitterröhren, Außenanoden, die auch als Vakuumbehälter für Mikrowellenröhren dienen, Vakuumbeschichtungsapparaturen, Kathodenzerstäubungsapparaturen und Beschleunigungshohlraumbehältern für Beschleuniger.
EP19950107446 1994-06-20 1995-05-17 Hochvakuumanlage Expired - Lifetime EP0688879B1 (de)

Applications Claiming Priority (2)

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

Publications (2)

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

Family

ID=15718373

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19950107446 Expired - Lifetime EP0688879B1 (de) 1994-06-20 1995-05-17 Hochvakuumanlage

Country Status (3)

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

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4943095B2 (ja) * 2006-08-30 2012-05-30 三菱電機株式会社 銅合金及びその製造方法
JP6720087B2 (ja) * 2015-05-21 2020-07-08 Ｊｘ金属株式会社 銅合金スパッタリングターゲット及びその製造方法
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

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2175009B (en) * 1985-03-27 1990-02-07 Mitsubishi Metal Corp Wire for bonding a semiconductor device and process for producing the same
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
JPS643903A (en) * 1987-06-25 1989-01-09 Furukawa Electric Co Ltd Thin copper wire for electronic devices and manufacture thereof
JP2726939B2 (ja) * 1989-03-06 1998-03-11 日鉱金属 株式会社 加工性，耐熱性の優れた高導電性銅合金

Also Published As

Publication number Publication date
JPH083664A (ja) 1996-01-09
DE69501569D1 (de) 1998-03-12
DE69501569T2 (de) 1998-06-10
EP0688879A1 (de) 1995-12-27

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