JPH0559503A - Manufacture of cryogenic oxygen free copper - Google Patents
Manufacture of cryogenic oxygen free copperInfo
- Publication number
- JPH0559503A JPH0559503A JP22006691A JP22006691A JPH0559503A JP H0559503 A JPH0559503 A JP H0559503A JP 22006691 A JP22006691 A JP 22006691A JP 22006691 A JP22006691 A JP 22006691A JP H0559503 A JPH0559503 A JP H0559503A
- Authority
- JP
- Japan
- Prior art keywords
- free copper
- oxygen free
- copper
- oxygen
- cryogenic
- 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.)
- Pending
Links
Landscapes
- Conductive Materials (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、超伝導用の素材等に使
用する極低温用無酸素銅の製造方法に関するものであ
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing cryogenic oxygen-free copper used as a material for superconductivity.
【０００２】[0002]
【従来の技術】近年、超伝導用安定化銅材等について
は、残留抵抗の小さい無酸素銅の需要が次第に増大して
いる。2. Description of the Related Art In recent years, as for stabilized copper materials for superconductivity and the like, demand for oxygen-free copper having a small residual resistance is gradually increasing.
【０００３】これらの材料には、Ｆｅ、Ａｓ等を分離除
去した電解精製銅あるいは再電解精製銅が原料として用
いられており、この電解精製銅は、塑性加工終了後、４
００〜６００℃にて、約１時間不活性ガス中で焼鈍さ
れ、加工歪を除去して、製品化される。ただし、冷却速
度は自然放冷のままであった。For these materials, electrolytically refined copper from which Fe, As, etc. have been separated and removed, or reelectrolytically refined copper is used as a raw material.
The product is annealed in an inert gas at 00 to 600 ° C. for about 1 hour to remove work strain, and commercialized. However, the cooling rate remained as it was.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、電解精
製銅には電解液（硫酸）に起因する硫黄（Ｓ）が混入す
ることは避けられない。このＳは、焼鈍工程終了後にも
銅中に固溶しており、精製銅の残留抵抗を増加させる原
因となっていた。However, it is unavoidable that sulfur (S) resulting from the electrolytic solution (sulfuric acid) is mixed in the electrolytically refined copper. This S remained in solid solution in copper even after the annealing step was completed, which was a cause of increasing the residual resistance of the refined copper.
【０００５】本発明の目的は、前記した従来技術の欠点
を解消し、残留抵抗を大幅に減少させることができる新
規な極低温用無酸素銅の製造方法を提供することにあ
る。An object of the present invention is to solve the above-mentioned drawbacks of the prior art and to provide a novel method for producing oxygen-free copper for cryogenic temperatures, which can greatly reduce the residual resistance.
【０００６】[0006]
【課題を解決するための手段】上記課題を解決するため
の本発明の極低温用無酸素銅の製造方法の構成は、極低
温用無酸素銅の製造工程で、無酸素銅の塑性加工後に４
００〜６００℃で焼鈍し、焼鈍後の冷却は１００℃／ｈ
以下の速度で徐冷するようにしたことである。The structure of the method for producing oxygen-free copper for cryogenic use according to the present invention to solve the above-mentioned problems is as follows: Four
Annealed at 00-600 ° C, cooling after annealing is 100 ° C / h
That is, the slow cooling was performed at the following rate.
【０００７】[0007]
【作用】本発明の要旨は、Ｓを含有した銅を焼鈍後、徐
冷することにより、Ｓを粒界に析出させて、残留抵抗に
対して無害化させることにあり、これによって残留抵抗
を大幅に減少させようとするものである。The gist of the present invention is to anneal copper containing S and then gradually cool it to precipitate S at grain boundaries and render it harmless to the residual resistance. It is intended to be greatly reduced.
【０００８】残留抵抗に影響を与える不純物は、Ｃｕ中
に固溶しているＳ成分のみであり、粒界等へ析出してい
るものは無関係である。ＳのＣｕ中への固溶限は極めて
小さく、また温度依存性があることから、焼鈍温度から
徐冷することで、不純物濃度レベルのＳでも粒界等へ析
出させることができる。Impurities that affect the residual resistance are only the S component that is solid-soluted in Cu, and those that are precipitated at grain boundaries are irrelevant. Since the solid solubility limit of S in Cu is extremely small and there is temperature dependence, it is possible to precipitate S even at the impurity concentration level at grain boundaries by gradually cooling from the annealing temperature.
【０００９】焼鈍温度は５００℃以上が好ましく、５０
０℃以下では加工歪を十分に取り除くことができず、物
理的な欠陥に起因する残留抵抗が残ることになる。The annealing temperature is preferably 500 ° C. or higher, and 50
If the temperature is 0 ° C. or lower, the processing strain cannot be sufficiently removed, and residual resistance due to physical defects remains.
【００１０】冷却速度は、１００℃／ｈ以下が望まし
く、１００℃／ｈより速い場合には、Ｓの析出量が著し
く少なくなる。すなわち、冷却速度はできるだけ遅い方
が望ましい。The cooling rate is preferably 100 ° C./h or less, and when the cooling rate is higher than 100 ° C./h, the amount of precipitated S is remarkably reduced. That is, it is desirable that the cooling rate is as slow as possible.
【００１１】また、４００℃より低温では、Ｓの析出速
度がかなり小さくなり、徐冷の効果は期待できなくな
る。Further, at a temperature lower than 400 ° C., the precipitation rate of S becomes considerably small, and the effect of slow cooling cannot be expected.
【００１２】焼鈍工程中の雰囲気は、Ａｒ、Ｎ2等の不
活性ガス、還元性ガス、真空中等いずれでもよい。The atmosphere during the annealing process may be an inert gas such as Ar or N 2 , a reducing gas, or a vacuum.
【００１３】[0013]
【実施例】以下本発明にかかる実施例を表１を用いて説
明する。EXAMPLES Examples of the present invention will be described below with reference to Table 1.
【００１４】電解精製銅を原料とした無酸素銅を１ｍｍ
φ×２００ｍｍに伸線加工して（加工度９０％）、これ
をＡｒ雰囲気中で１時間焼鈍した後、各冷却速度で、徐
冷した。この時の焼鈍温度は４００〜７００℃まで変化
させた。これらの各例について、液体ヘリウム中で四端
子法により残留抵抗（Ωｃｍ）を測定した。これらの結
果を表１に示す。1 mm of oxygen-free copper made from electrolytically refined copper
The wire was drawn to φ × 200 mm (working degree 90%), annealed in Ar atmosphere for 1 hour, and then gradually cooled at each cooling rate. The annealing temperature at this time was changed to 400 to 700 ° C. For each of these examples, the residual resistance (Ωcm) was measured in liquid helium by the four-terminal method. The results are shown in Table 1.
【００１５】[0015]
【表１】 [Table 1]
【００１６】表１から判るように、実施例１〜３におい
ては、残留抵抗は５．０〜５．９×１０~9の範囲である
が、比較例１は焼鈍温度４００℃で低温のため、残留抵
抗は８．６×１０~9、また比較例２は冷却速度４００℃
／ｈのように速すぎるため、残留抵抗が７．８×１０~9
となり、実施例１〜３に比してかなり大きな値を示して
いる。As can be seen from Table 1, in Examples 1 to 3, the residual resistance was in the range of 5.0 to 5.9 × 10 to 9 , but in Comparative Example 1, the annealing temperature was 400 ° C. and the temperature was low. , The residual resistance is 8.6 × 10 9 and the cooling rate is 400 ° C. in Comparative Example 2.
/ H is too fast, so the residual resistance is 7.8 × 10 ~ 9
Which is considerably larger than those of Examples 1 to 3.
【００１７】[0017]
【発明の効果】本発明によれば、焼鈍後に徐冷すること
により、不純物のＳを結晶粒界に析出させることができ
るので、残留抵抗を大幅に減少させた極低温用無酸素銅
を容易に製造することができるようになった。EFFECTS OF THE INVENTION According to the present invention, the impurity S can be precipitated at the crystal grain boundaries by annealing and then slowly cooling it. Can now be manufactured.
【００１８】また、従来の電解精製銅を原料として使用
し、製造工程の熱処理条件を改善することで、特別な設
備の新設なしに、所期の製品が得られるので経済的効果
が著しい。Further, by using the conventional electrolytically refined copper as a raw material and improving the heat treatment conditions in the manufacturing process, the desired product can be obtained without the need to install special equipment, so that the economical effect is remarkable.
Claims (1)
の塑性加工後に４００〜６００℃で焼鈍し、焼鈍後１０
０℃／ｈ以下の冷却速度で徐冷することを特徴とする極
低温用無酸素銅の製造方法。1. A process for producing oxygen-free copper for cryogenic use, which comprises annealing at 400 to 600 ° C. after plastic working of oxygen-free copper, and annealing 10 after annealing.
A method for producing oxygen-free copper for cryogenic use, which comprises gradually cooling at a cooling rate of 0 ° C./h or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22006691A JPH0559503A (en) | 1991-08-30 | 1991-08-30 | Manufacture of cryogenic oxygen free copper |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22006691A JPH0559503A (en) | 1991-08-30 | 1991-08-30 | Manufacture of cryogenic oxygen free copper |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0559503A true JPH0559503A (en) | 1993-03-09 |
Family
ID=16745410
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP22006691A Pending JPH0559503A (en) | 1991-08-30 | 1991-08-30 | Manufacture of cryogenic oxygen free copper |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0559503A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160214217A1 (en) * | 2009-03-29 | 2016-07-28 | Montana Instruments Corporation | Low Vibration Cryocooled System for Low Temperature Microscopy and Spectroscopy Applications |
| US10451529B2 (en) | 2016-03-11 | 2019-10-22 | Montana Instruments Corporation | Cryogenic systems and methods |
| US10775285B1 (en) | 2016-03-11 | 2020-09-15 | Montana Intruments Corporation | Instrumental analysis systems and methods |
| US11125663B1 (en) | 2016-03-11 | 2021-09-21 | Montana Instruments Corporation | Cryogenic systems and methods |
| US11956924B1 (en) | 2020-08-10 | 2024-04-09 | Montana Instruments Corporation | Quantum processing circuitry cooling systems and methods |
-
1991
- 1991-08-30 JP JP22006691A patent/JPH0559503A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160214217A1 (en) * | 2009-03-29 | 2016-07-28 | Montana Instruments Corporation | Low Vibration Cryocooled System for Low Temperature Microscopy and Spectroscopy Applications |
| US9821421B2 (en) * | 2009-03-29 | 2017-11-21 | Montana Instruments Corporation | Low vibration cryocooled system for low temperature microscopy and spectroscopy applications |
| US10451529B2 (en) | 2016-03-11 | 2019-10-22 | Montana Instruments Corporation | Cryogenic systems and methods |
| US10775285B1 (en) | 2016-03-11 | 2020-09-15 | Montana Intruments Corporation | Instrumental analysis systems and methods |
| US11125663B1 (en) | 2016-03-11 | 2021-09-21 | Montana Instruments Corporation | Cryogenic systems and methods |
| US11378499B2 (en) | 2016-03-11 | 2022-07-05 | Montana Instruments Corporation | Instrumental analysis systems and methods |
| US11956924B1 (en) | 2020-08-10 | 2024-04-09 | Montana Instruments Corporation | Quantum processing circuitry cooling systems and methods |
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