EP0688879B1 - High vacuum apparatus member and vacuum apparatus - Google Patents
High vacuum apparatus member and vacuum apparatus Download PDFInfo
- 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
Links
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 19
- 229910052802 copper Inorganic materials 0.000 claims description 19
- 239000010949 copper Substances 0.000 claims description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 18
- 239000001301 oxygen Substances 0.000 claims description 18
- 229910052760 oxygen Inorganic materials 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000001133 acceleration Effects 0.000 claims description 2
- 238000000137 annealing Methods 0.000 claims description 2
- 238000004544 sputter deposition Methods 0.000 claims description 2
- 238000001771 vacuum deposition Methods 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 17
- 239000007789 gas Substances 0.000 description 9
- 229910000881 Cu alloy Inorganic materials 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000010943 off-gassing Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 3
- 238000006356 dehydrogenation reaction Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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)
Description
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.
Conventionally, 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.
Rajainmaki et al., 'The Production and application of oxygen free copper',
JOM, (March 1993), 45, (3), pages 68-70 and Helenius, A. et al;,
'Current and Future uses of oxygen free copper', Metall, (Nov. 1990), 44, (11),
pages 1067-1070, both describe the use of oxygen free copper in
high vacuum apparatus.
However, even with dehydrogenation by baking prior to use of vacuum
apparatuses manufactured using the aforementioned high-purity oxygen-free
copper, certain problems result, since hydrogen contained in the
high-purity oxygen-free copper is trapped by residual oxygen because
of its strong affinity thereto, thus rendering the dehydrogenation
more difficult. Consequently, when vacuum apparatuses manufactured
using high-purity oxygen-free copper containing such oxygen-trapped
hydrogen are used in a high vacuum, the residual hydrogen is
gradually released and causes a reduction in the degree of 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.
This object is solved in accordance with the present invention by the use of a
high-purity copper material having the features of claim 1. Preferred
applications of such material are subject matter of claims 2-3.
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.
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.
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. Therefore, the
residual trace oxygen in the high-purity copper alloy does not trap
hydrogen, and thus the hydrogen is easily removed during baking.
However, 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.
Since up to 3 ppm of oxygen in the copper alloy may combine with Zr
in the above-mentioned range of 1 to 15 ppm, the oxygen content of
the vacuum apparatus member of the present invention is preferably up
to 3 ppm.
To manufacture vacuum apparatus members containing 1 to 15 ppm of Zr
and 3 ppm or less of oxygen according to the present invention,
first, 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 vacuum apparatus material and a method
of producing it will now be explained in further detail by way of the
following example and the attached drawings which is a schematic view
of an apparatus for producing the vacuum apparatus material.
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.
First, 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 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.
The results are given in Table 1.
| Vacuum apparatus member | Composition | Out-gassing rate (Torr·1/sec.·cm2) | ||||
| Electrolytic copper purity (%) | Zr (ppm) | Oxygen (ppm) | P (ppm) | |||
| | 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 | - | 8.29 x 10-11 | |
| | 1 | 99.998 | - | 2.0 | 3.1 | 1.26 x 10-10 |
| 2 | 99.998 | - | 1.5 | 2.8 | 8.92 x 10-11 | |
| 3 | 99.998 | - | 2.5 | - | 1.94 x 10-10 | |
| (Values marked with * are outside the range of the invention) |
The results shown in Table 1 demonstrate that the vacuum apparatus
members of the present invention which contained 1 to 15 ppm of Zr
and 3 ppm or less of oxygen all had lower values for the out-gassing
rate of hydrogen gas in comparison with the vacuum apparatus members
of the conventional art which did not contain Zr, and hence the
hydrogen gas was more easily removed during the baking. In contrast,
it was shown that the removal of hydrogen gas during baking was
somewhat difficult in the case of the vacuum apparatus members for
comparison 1-2 which were outside the ranges of 1 to 15 ppm of Zr and
3 ppm or less of oxygen. Also, as observed in the case of the vacuum
apparatus member for comparison 3, a Zr content exceeding 15 ppm is
not preferred as this causes more difficult removal of hydrogen gas
during baking.
As explained above, 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.
Claims (3)
- Use of high-purity copper material containing, prior to annealing (baking), hydrogen, 3 ppm or less of oxygen and 1 to 15 ppm of Zr and having a purity of 99,99 weight % or higher as a material for the manufacture of high-vacuum apparatuses.
- The use of the material according to claim 1 containing 3 to 10 ppm of Zr for the same purpose as in claim 1.
- The use of the material according to any of claims 1 or 2 for constructing power transmitter tubes, external anodes which also serve as vacuum containers for microwave tubes, vacuum deposition and sputtering apparatuses and acceleration cavity containers for accelerators.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16059694A JPH083664A (en) | 1994-06-20 | 1994-06-20 | Vacuum device member and vacuum device |
| JP160596/94 | 1994-06-20 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0688879A1 EP0688879A1 (en) | 1995-12-27 |
| EP0688879B1 true EP0688879B1 (en) | 1998-02-04 |
Family
ID=15718373
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP19950107446 Expired - Lifetime EP0688879B1 (en) | 1994-06-20 | 1995-05-17 | High vacuum apparatus member and vacuum apparatus |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0688879B1 (en) |
| JP (1) | JPH083664A (en) |
| DE (1) | DE69501569T2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4943095B2 (en) * | 2006-08-30 | 2012-05-30 | 三菱電機株式会社 | Copper alloy and manufacturing method thereof |
| US10494712B2 (en) | 2015-05-21 | 2019-12-03 | Jx Nippon Mining & Metals Corporation | Copper alloy sputtering target and method for manufacturing same |
| JP7131376B2 (en) * | 2018-12-27 | 2022-09-06 | 三菱マテリアル株式会社 | Copper material for sputtering targets |
| CN113290217B (en) * | 2021-05-28 | 2022-09-23 | 金川集团股份有限公司 | Vacuum continuous casting process of high-purity oxygen-free copper rod |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4676827A (en) * | 1985-03-27 | 1987-06-30 | Mitsubishi Kinzoku Kabushiki Kaisha | Wire for bonding a semiconductor device and process for producing the same |
| JPS62207834A (en) * | 1986-03-10 | 1987-09-12 | Nippon Mining Co Ltd | Copper material for use in high-vacuum atmosphere |
| JPS62243727A (en) * | 1986-04-16 | 1987-10-24 | Hitachi Cable Ltd | Rolled copper foil for printed circuit board |
| JPS63312934A (en) * | 1987-06-16 | 1988-12-21 | Hitachi Cable Ltd | Lead frame material for semiconductor |
| JPS643903A (en) * | 1987-06-25 | 1989-01-09 | Furukawa Electric Co Ltd | Thin copper wire for electronic devices and manufacture thereof |
| JP2726939B2 (en) * | 1989-03-06 | 1998-03-11 | 日鉱金属 株式会社 | Highly conductive copper alloy with excellent workability and heat resistance |
-
1994
- 1994-06-20 JP JP16059694A patent/JPH083664A/en not_active Withdrawn
-
1995
- 1995-05-17 DE DE1995601569 patent/DE69501569T2/en not_active Expired - Fee Related
- 1995-05-17 EP EP19950107446 patent/EP0688879B1/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH083664A (en) | 1996-01-09 |
| DE69501569D1 (en) | 1998-03-12 |
| EP0688879A1 (en) | 1995-12-27 |
| DE69501569T2 (en) | 1998-06-10 |
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