JPS63282169A - Production of superconductor - Google Patents
Production of superconductorInfo
- Publication number
- JPS63282169A JPS63282169A JP62116342A JP11634287A JPS63282169A JP S63282169 A JPS63282169 A JP S63282169A JP 62116342 A JP62116342 A JP 62116342A JP 11634287 A JP11634287 A JP 11634287A JP S63282169 A JPS63282169 A JP S63282169A
- Authority
- JP
- Japan
- Prior art keywords
- superconductor
- cooling
- annealing
- sintered
- oxide
- 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
Links
- 239000002887 superconductor Substances 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000000137 annealing Methods 0.000 claims abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 3
- 238000004904 shortening Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 8
- 238000007796 conventional method Methods 0.000 description 5
- 238000001354 calcination Methods 0.000 description 3
- 238000010583 slow cooling Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 206010028813 Nausea Diseases 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000008693 nausea Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N60/00—Superconducting devices
- H10N60/01—Manufacture or treatment
- H10N60/0268—Manufacture or treatment of devices comprising copper oxide
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は酸化物系超電導体の製造方法、さらに詳しく云
えば、原料焼結後のアニール処理方法に特徴を有する製
造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for manufacturing an oxide-based superconductor, and more specifically, to a manufacturing method characterized by an annealing treatment method after sintering raw materials.
超電導体は電気抵抗ゼロで電流が流れる特性を有し、と
りわけ最近見いだされた酸化物系材料（たとえばＬａ−
５ｒ−Ｃｕ−０系、Ｙ−Ｂａ−Ｃｕ−０系）は、その超
電導を示す臨界温度（以下Ｔｃと略記する）が高いこと
から非常に強い悪心がよせられている。Superconductors have the property of allowing current to flow with zero electrical resistance, and in particular, they are made of recently discovered oxide-based materials (such as La-
5r-Cu-0 series, Y-Ba-Cu-0 series) have a high critical temperature (hereinafter abbreviated as Tc) that exhibits superconductivity, which causes a strong feeling of nausea.
この酸化物系超電導体は、通常原料となる各元素を含む
化合物の配合物を混合し、仮焼した後粉砕し、成形し、
約１０００℃で焼成後、約９００℃２〜５時間空気中で
アニール処理し徐冷することによってつくられていた。This oxide-based superconductor is usually produced by mixing a compound of compounds containing various elements as raw materials, calcining it, pulverizing it, and molding it.
It was produced by firing at about 1000°C, annealing in air at about 900°C for 2 to 5 hours, and then slowly cooling.
しかしながら、前記従来法は高いアニール処理温度から
室温までその冷却温度巾が大きいため、その間の徐冷過
程が一定でなかった。その結果、製造される超電導体の
Ｔｃにバラツキが生じ、その最大と最小の差が応々にし
て１５に以上も開くことがあり、信頼性が低いという欠
点があった。However, in the conventional method, since the cooling temperature range is wide from a high annealing temperature to room temperature, the slow cooling process during that time is not constant. As a result, variations occur in the Tc of the manufactured superconductors, and the difference between the maximum and minimum values can sometimes be as large as 15 or more, resulting in low reliability.
本発明者らは前記従来法の欠点を解消するためにアニー
ル処理条件について追求したところ、富酸素雰囲気にす
れば相当低い温度でアニール処理ができ冷却温度巾を著
しく狭くできることを知見して、以下に述べる発明を完
成に導いた。The present inventors investigated the annealing treatment conditions in order to eliminate the drawbacks of the conventional method, and found that annealing can be performed at a considerably lower temperature by creating an oxygen-rich atmosphere, and the cooling temperature range can be significantly narrowed. He led to the completion of the invention described in .
すなわち本発明は所定の元素を含む化合物を混合し、成
形し、焼結し、アニール処理し、冷却してつくる酸化物
系超電導体の製造方法において、富酸素雰囲気中１００
〜６００℃でアニール処理し、冷却することを特徴とす
る酸化物系超電導体を製造する方法を要旨とするもので
ある。That is, the present invention relates to a method for producing an oxide superconductor in which a compound containing a predetermined element is mixed, molded, sintered, annealed, and cooled.
The gist of the present invention is a method for producing an oxide-based superconductor, which is characterized by annealing at ~600°C and cooling.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
本発明における富酸素雰囲気とは、空気中の酸素含有量
よりも多くの酸素を含む雰囲気を意味し、ＩＱＯｖｏ１
％酸素であることが望ましい。The oxygen-rich atmosphere in the present invention means an atmosphere containing more oxygen than the oxygen content in the air, and IQOvo1
% oxygen is preferred.
このような富酸素雰囲気のもとてのアニール処理温度は
１００〜６００℃で十分である。該温度が１００℃未満
では、Ｔｃのバラツキが大きくなり、また６００℃を超
えてもＴｃのバラツキが大きくなり、いずれも好ましく
ない。An annealing temperature of 100 to 600[deg.] C. in such an oxygen-rich atmosphere is sufficient. If the temperature is less than 100°C, there will be large variations in Tc, and if it exceeds 600°C, there will be large variations in Tc, both of which are not preferred.
冷却は徐冷、急冷いずれの方法を採用してもよくそれぞ
れの冷却法でバラツキは従来のものと比較して小さい。For cooling, either slow cooling or rapid cooling may be used, and the variation between each cooling method is smaller than that of conventional methods.
このように冷却条件が緩やかにできるのは、本発明のア
ニール処理温度が低く、冷却温度中を従来法に比較し著
しく小さくできたことに起因すると考えられる。なお、
製造工程上の時間短縮から徐冷法よりも急冷法が好まし
い。The reason why the cooling conditions can be made so gentle is considered to be that the annealing temperature of the present invention is low, and the cooling temperature can be significantly reduced compared to the conventional method. In addition,
The rapid cooling method is preferable to the slow cooling method because it saves time in the manufacturing process.
本発明で製造される酸化物系超電導体は、Ｂａ−Ｙ−Ｃ
ｕ−０系、Ｂａ−Ｌａ−Ｃｕ−０系、５ｒ−Ｌａ−Ｃｕ
−０系、Ｃａ−Ｌａ−Ｃｕ−０系等が例示される。The oxide superconductor produced in the present invention is Ba-Y-C
u-0 series, Ba-La-Cu-0 series, 5r-La-Cu
-0 series, Ca-La-Cu-0 series, etc. are exemplified.
本発明で用いる原料は超電導体を構成する所定の金属元
素を含む化合物を適宜に選択して使用すればよい。たと
えばＹ−Ｂａ−Ｃｕ−０系の超電導体を製造しようとす
る場合、ＢａＣＯ５＋Ｙｚ０３．ＣｕＯを原料とするな
どである。As the raw material used in the present invention, a compound containing a predetermined metal element constituting the superconductor may be appropriately selected and used. For example, when trying to manufacture a Y-Ba-Cu-0 based superconductor, BaCO5+Yz03. For example, CuO is used as a raw material.
原料化合物の混合、仮焼、粉砕、成形、焼結の各工程は
慣用の方法にしたがう。The steps of mixing, calcining, crushing, molding, and sintering the raw material compounds follow conventional methods.
以下、本発明を実施例に基づいて説明する。Hereinafter, the present invention will be explained based on examples.
下記手順によりＢａｏ、 ｂＹｏ、、 ４Ｃｕ０３の超
電導体を製造した。Superconductors of Bao, bYo, and 4Cu03 were manufactured by the following procedure.
原料としてＢａＣＯ５（純度９９．９ｗｔ％） 、Ｙ２
Ｏ３（純度９９．９９ｗｔ％）およびＣｕＯ（純度９９
．９９ｗｔ％）を前記組成になるように配合し、エタノ
ールを添加してボールミルで粉砕混合したのち、乾燥し
て、調整済配合物を得た。BaCO5 (purity 99.9wt%), Y2 as raw materials
O3 (purity 99.99wt%) and CuO (purity 99wt%)
．． 99 wt%) were blended to have the above composition, ethanol was added, and the mixture was ground and mixed in a ball mill, followed by drying to obtain an adjusted blend.
該酸化物を電気炉にて８００℃５時間仮焼したのち、得
られた仮焼物を乳鉢で粉砕し、所定形状に加圧成形（７
００ｋｇ／ａＪ） した。After calcining the oxide at 800°C for 5 hours in an electric furnace, the resulting calcined product was crushed in a mortar and pressure-molded into a predetermined shape (7
00kg/aJ).
得られた成形体を電気炉で９１０’Ｃ１４０時間空気中
で焼結し徐冷した。The obtained molded body was sintered in air at 910'C in an electric furnace for 140 hours and slowly cooled.
その焼結物を切断して３ｘ４ｘ３ｍの試験片を作製した
。この試験片を３個ずつ表１に示す条件でアニール処理
し、次いで冷却したのち、Ｔｃを直流四端子法で測定し
た。得られた平均値および最大値と最小値の差を同表に
併記した。The sintered product was cut into test pieces measuring 3 x 4 x 3 m. Three of these test pieces were annealed under the conditions shown in Table 1, then cooled, and Tc was measured by a DC four-terminal method. The obtained average value and the difference between the maximum value and the minimum value are also listed in the same table.
本発明は酸化物超電導体の製造方法ミ特にアニール処理
条件を改良した製造方法に係り、従来法でつくられる、
該超電導体よりも臨界温度の信転性を著しく向上させた
方法である。さらには、低温でアニール処理するので熱
エネルギー上でも本発明の方法は有利である。The present invention relates to a method for producing an oxide superconductor, particularly a method for producing an oxide superconductor with improved annealing treatment conditions.
This method significantly improves the reliability of critical temperature compared to the superconductor. Furthermore, since the annealing treatment is performed at a low temperature, the method of the present invention is advantageous in terms of thermal energy.
手 続 主甫 正 書（方式） 昭和６２年８月４日Manual (method) August 4, 1986
Claims (1)
ニール処理し冷却する酸化物系超電導体の製造方法にお
いて、富酸素雰囲気中１００〜６００℃でアニール処理
し、冷却することを特徴とする酸化物系超電導体の製造
方法。 ２）前記冷却が急冷であることを特徴とする特許請求の
範囲第一項記載の酸化物系超電導体の製造方法。[Scope of Claims] 1) A method for producing an oxide superconductor in which a compound containing a predetermined element is mixed, molded, sintered, annealed and cooled, wherein the annealing treatment is performed at 100 to 600°C in an oxygen-rich atmosphere. , a method for producing an oxide-based superconductor, characterized by cooling. 2) The method for producing an oxide superconductor according to claim 1, wherein the cooling is rapid cooling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62116342A JP2630397B2 (en) | 1987-05-13 | 1987-05-13 | Superconductor manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62116342A JP2630397B2 (en) | 1987-05-13 | 1987-05-13 | Superconductor manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63282169A true JPS63282169A (en) | 1988-11-18 |
| JP2630397B2 JP2630397B2 (en) | 1997-07-16 |
Family
ID=14684572
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62116342A Expired - Lifetime JP2630397B2 (en) | 1987-05-13 | 1987-05-13 | Superconductor manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2630397B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0721924A3 (en) * | 1988-04-08 | 1998-03-04 | Her Majesty The Queen In Right Of New Zealand | Metal oxide materials |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63282154A (en) * | 1987-05-12 | 1988-11-18 | Nec Corp | Production of oxide superconductor |
-
1987
- 1987-05-13 JP JP62116342A patent/JP2630397B2/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63282154A (en) * | 1987-05-12 | 1988-11-18 | Nec Corp | Production of oxide superconductor |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0721924A3 (en) * | 1988-04-08 | 1998-03-04 | Her Majesty The Queen In Right Of New Zealand | Metal oxide materials |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2630397B2 (en) | 1997-07-16 |
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