JPH04182394A - Production of single crystal superconductor - Google Patents
Production of single crystal superconductorInfo
- Publication number
- JPH04182394A JPH04182394A JP2311912A JP31191290A JPH04182394A JP H04182394 A JPH04182394 A JP H04182394A JP 2311912 A JP2311912 A JP 2311912A JP 31191290 A JP31191290 A JP 31191290A JP H04182394 A JPH04182394 A JP H04182394A
- Authority
- JP
- Japan
- Prior art keywords
- superconductor
- single crystal
- raw material
- crystal
- material powder
- 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
- 239000013078 crystal Substances 0.000 title claims abstract description 72
- 239000002887 superconductor Substances 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000000203 mixture Substances 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 32
- 238000001556 precipitation Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims description 19
- 239000012856 weighed raw material Substances 0.000 claims description 9
- 239000000758 substrate Substances 0.000 abstract description 17
- 239000000463 material Substances 0.000 abstract description 2
- 239000004570 mortar (masonry) Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract 2
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- 238000007716 flux method Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- -1 CaC01 Chemical compound 0.000 description 1
- 229910004247 CaCu Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 241000201976 Polycarpon Species 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（イ）産業上の利用分野
本発明は、超電導デバイスにおける超電導基板として使
用することができる単結晶超電導体の製造方法に関する
。DETAILED DESCRIPTION OF THE INVENTION (a) Field of Industrial Application The present invention relates to a method for producing a single crystal superconductor that can be used as a superconducting substrate in a superconducting device.
（ロ）従来の技術
超電導デバイスにおける超電導基板としては、単結晶基
板が望まれ、現在のところ、超電・淳焼結体のバルクを
スライスしたり、蒸着等による薄膜を形成することによ
り基板としている。(b) Conventional technology A single-crystal substrate is desired as a superconducting substrate in a superconducting device, and at present, the bulk of the superconductor Jun sintered body is sliced or a thin film is formed by vapor deposition. There is.
しかし、超電導焼結体のバルクをスライスしたものは、
空孔が多く緻密のものが得られないので超電導基板とし
ては好ましくなく、また、薄膜により基板を形成するに
は時間を要し、量産には不向きである。However, when the bulk of superconducting sintered body is sliced,
It is not preferred as a superconducting substrate because it has many pores and cannot be dense, and it takes time to form a substrate from a thin film, making it unsuitable for mass production.
一方、酸化物超電導体の単結晶化において、半導体製造
に用いられているブリッジマン法及びチョコラルスキー
法による単結晶作成法は、酸化物超電導材料の性質、Ｅ
極めて困難であるとされている。そこで、超電導単結晶
体を得る技術としてフラックス法が開発されている。こ
れは、まず、ある１つの組成系（例えばＢｉ ２ｓｒｃ
ａｃｕ２０＊ ）の酸化物超電導体の原料粉末（例えば
Ｂｉ、Ｏ，、ＳｒＣＯ３、ＣａＣ０１及びＣｕＯ）をそ
の組成系の組成比（例えばＢ１：Ｓｒ：Ｃａ：Ｃｕ＝２
： １ ： ］ ： ２）に秤量してアルミナのルツ
ボに入れて混合する。その後、適当な温度条件で熱処理
する。例えば室温から１時間で１０００℃に昇温しでそ
の温度を２４時間保持して原料粉末を溶融し、その後７
５０℃まで徐冷することにより、その系の超電導単結晶
を得る方法である。On the other hand, in the single crystallization of oxide superconductors, the Bridgman method and Czochralski method, which are used in semiconductor manufacturing, are used to create single crystals based on the properties of the oxide superconductor material, E
It is said to be extremely difficult. Therefore, a flux method has been developed as a technique for obtaining superconducting single crystals. This starts with a certain composition system (for example, Bi 2src
acu20*) raw material powder (e.g., Bi, O, SrCO3, CaC01, and CuO) in a compositional ratio (e.g., B1:Sr:Ca:Cu=2).
: 1 : ] : 2) Weigh and mix in an alumina crucible. Thereafter, heat treatment is performed under appropriate temperature conditions. For example, the temperature is raised from room temperature to 1000°C in 1 hour, the temperature is maintained for 24 hours to melt the raw material powder, and then 7
This is a method of obtaining a superconducting single crystal of the system by slowly cooling it to 50°C.
（ハ）発明が解決しようとする課題
前述のフラックス法により得られる単結晶の大きさは高
々０．１〜３ｍｍ角程度のものしか得られないので、超
電導デバイス用基板として使用することができなく、利
用分野が大きく制限されるという問題がある。(c) Problems to be solved by the invention Since the single crystal obtained by the above-mentioned flux method is only about 0.1 to 3 mm square at most, it cannot be used as a substrate for superconducting devices. However, there is a problem in that the field of use is greatly restricted.
本発明は、かかる点に鑑み発明さｉｔたものにして、超
電導デバイス用基板として使用することができる少なく
とも５ｍｍ角以−にの大きさの超電導基板を形成するこ
とができる単結晶超電導体の製造方法を提案しようとす
るものである。The present invention has been devised in view of the above points, and the present invention has been devised to produce a single crystal superconductor capable of forming a superconducting substrate having a size of at least 5 mm square that can be used as a substrate for a superconducting device. This is an attempt to propose a method.
（ニ）課題を解決するための手段
かかる課題を解決するために、本発明による単結晶超電
導体の製造方法は、１つの組成系の酸化物超電導体の原
料粉末をその組成系の組成比に応じて秤量し、この秤量
した原料粉末５０ｇ当り、その組成系の酸化物超電導体
の種結晶を１〜］Ｏｇの割合で混合し、その組成系の単
結晶析出温度１ｉｉｉ後の温度で溶融した後、用結晶超
、し導体を形成するものである。(d) Means for Solving the Problems In order to solve the problems, the method for manufacturing a single crystal superconductor according to the present invention includes changing the raw material powder of an oxide superconductor of one composition system to the composition ratio of that composition system. The seed crystals of the oxide superconductor of the composition were mixed at a ratio of 1 to 10 g per 50 g of the weighed raw material powder, and the mixture was melted at a temperature after the single crystal precipitation temperature of the composition. After that, a crystalline conductor is formed.
（ホ）作用
ある１つの組成系の酸化Ｏ１超Ｘ１：ｉ、専体の原料粉
末をその組成系の組成比に応じて秤量し、この秤量した
原料粉末５０ｇに対して、その組成系の酸化物超電導体
の種結晶を１〜１０ｇの割合で混合し、その組成系の単
結晶析出温度０１ｊ後の温ｌｙで溶融した後、単結晶超
電導体を形成するので、前述の従来例で得らｈるものよ
り大きい単結晶超電導１本が得られる。(e) Oxidation of one compositional system with an effect exceeding O1 A single crystal superconductor is formed by mixing 1 to 10 g of seed crystals of a physical superconductor and melting the mixture at a temperature after the single crystal precipitation temperature 01j of the composition system. One single-crystal superconductor that is larger than that of 1 h is obtained.
前記秤量した原料粉末５０ ｇ ！＝、ｋｔ して、そ
のイ１１成系の酸化物超電導体の種結晶を１ｇより少な
い割合で混合する場合には、この種結晶を混合しないと
きと同様に、高々３ｍｉ角以ドの大きさの６のしか得ら
れない。50 g of the weighed raw material powder! =, kt, and when the seed crystal of the oxide superconductor of the A11 system is mixed in a proportion less than 1 g, the size of the oxide superconductor of at most 3 mi square is the same as when this seed crystal is not mixed. I can only get 6 of these.
一方、ｄ１１記種結晶を１０ｇより多く混合するときに
は、種結晶が多いため結晶数が多くなり、単結晶にはな
らない。On the other hand, when more than 10 g of d11 seed crystals are mixed, the number of crystals increases because there are many seed crystals, and a single crystal does not form.
くべ）実施例
本発明の一実施例として、１つの組成系がＢｉ２５ｒＣ
ａＣｕ、Ｏ，である単結晶超電導体の製造方法を説明す
る。Example) As an example of the present invention, one composition system is Bi25rC.
A method for manufacturing a single crystal superconductor of aCu, O, will be described.
まず、この組成系の酸化物超電導体の原料粉末を、その
組成比に応じて秤量する。First, raw material powder for an oxide superconductor having this composition is weighed according to its composition ratio.
即ち、原料粉末として例えばＢｉ、Ｏ，、Ｓ ｒｃｏ
ｓ、ＣａＣＯ５及びＣｕＯを用い、これらの原料粉末を
その組成系の組成比Ｂｉ：Ｓｒ：Ｃａ：Ｃｕ＝２ ：
１°１：２に秤量してアルミナのルツボに入れて混合す
る。That is, as raw material powder, for example, Bi, O, S rco
s, CaCO5 and CuO, and the composition ratio of these raw material powders is Bi:Sr:Ca:Cu=2:
Weigh the ingredients at a ratio of 1°1:2 and mix them in an alumina crucible.
具体的には、純度９９．９９９％のＢｉｔＯ，を３５．
Ｏｇ、純度９９．９９％の５ｒＣＯｓを２２．１ ｇ
、純度９９．９９％のＣａＣ０１を１５．Ｏｇ、純度９
９．９９％のＣｕＯを２３．９ ｇ、それぞれ秤量し、
これらの原料粉末を混合する。この混合物にエタノール
、メタノールなどの有機溶媒を加えてスタークにて撹拌
した後、有機溶媒を蒸発させ、乳鉢にてすりつぶして粉
末状とし、原料粉末を得る。Specifically, 35% of BitO with a purity of 99.999% was used.
22.1 g of 5rCOs with 99.99% purity
, 99.99% purity CaC01. Og, purity 9
Weighed 23.9 g of 9.99% CuO,
These raw material powders are mixed. After adding an organic solvent such as ethanol or methanol to this mixture and stirring in a Stark machine, the organic solvent is evaporated and the mixture is ground in a mortar to form a powder to obtain a raw material powder.
次に、この原料粉末５０ｇ当り、従来の方法で得たＢｉ
２５ｒＣａＣｕｔ帆の種結晶を１−１０ｇの割合でアル
ミナのルツボに入れて混合するっ具体的には原料粉末５
０ｇ当り種結晶を５ｇの割合で、即ち前述の原料粉末の
量９６ｇに対して種結晶を９．６ｇ混合した。Next, per 50 g of this raw material powder, Bi obtained by the conventional method
25rCaCut sail seed crystals are mixed in an alumina crucible at a ratio of 1-10g.Specifically, raw material powder 5
Seed crystals were mixed at a ratio of 5 g per 0 g, that is, 9.6 g of seed crystals were mixed with 96 g of the aforementioned raw material powder.
続いて、このルツボを電気炉に入れて熱処理する。図面
に熱処理時間に対する熱処理温度特性を示す。この図面
から明らかなように、ます室温から単結晶超電導体の析
出温度Ｔまで１〜５時間かけて昇温する。この析出温度
Ｔは、各原料粉末の溶融温度９２５℃より高く、９５０
℃より低い温度にされる。Next, this crucible is placed in an electric furnace and heat treated. The drawing shows the heat treatment temperature characteristics with respect to heat treatment time. As is clear from this drawing, the temperature is gradually increased from room temperature to the precipitation temperature T of the single crystal superconductor over a period of 1 to 5 hours. This precipitation temperature T is higher than the melting temperature of each raw material powder, 925°C, and is 950°C.
The temperature is lower than ℃.
この析出温度Ｔの状態を２〜２・１時間保持して原料粉
末を全て溶融するとともに溶融原料を種結晶になじませ
て析出可能状態にする。This state of precipitation temperature T is maintained for 2 to 2.1 hours to melt all of the raw material powder and blend the molten raw material with the seed crystals to make it ready for precipitation.
その後、６００〜８００℃の温度まで３０〜８０時間か
けて徐冷する。この間に溶融していた原料が種結晶を核
として徐々に結晶化していき、結晶が成長する。この徐
冷の段階で温度の下げ方を２段階以−にに分けてもよい
。例えば、８００℃まで４０時間かけて降温し、その後
６００℃まで５時間かけて降温を行うなどしてもよい。Thereafter, it is slowly cooled to a temperature of 600 to 800°C over 30 to 80 hours. During this time, the molten raw material gradually crystallizes using the seed crystal as a core, and the crystal grows. The temperature may be lowered in two or more stages at this slow cooling stage. For example, the temperature may be lowered to 800°C over 40 hours, and then lowered to 600°C over 5 hours.
その後、室温まで降温して電気炉からルツボを取り出し
、ルツボを割って単結晶超電導体を取り出す。この単結
晶超電導体はその大きさが直径１０ｍｍのものであり、
単結晶超電導基板として少なくとも７ｍｍ角のらのが得
られる。従って、単結晶襞間面上・＼の電子デバイスの
バターニングが容易になる。Thereafter, the temperature is lowered to room temperature, the crucible is taken out from the electric furnace, the crucible is broken, and the single crystal superconductor is taken out. This single crystal superconductor has a diameter of 10 mm,
A square piece of at least 7 mm square can be obtained as a single-crystal superconducting substrate. Therefore, patterning of electronic devices on the interfold surfaces of the single crystal becomes easy.
次に、前述の秤量した原料粉末５０ｇに対して種結晶を
１ｇの割合で混合して単結晶超電導体を形成したところ
、直径１０ｍｍのものが得られ、単結晶超電導基板とし
て少なくとも７ｍｍ角のものが得られる。Next, when a single crystal superconductor was formed by mixing 1 g of seed crystals with 50 g of the weighed raw material powder, a single crystal superconductor with a diameter of 10 mm was obtained, and a single crystal superconducting substrate of at least 7 mm square was obtained. is obtained.
同様に、前述の秤量した原料粉末５０ｇに対して種結晶
を１０ｇの割合で混合して単結晶超電導体を形成したと
ころ、直径７ｍｍの６のが得られ、単結晶超電導基板と
して少なくとも５ｍ１ｌｌ角のものが得られる。Similarly, when a single-crystal superconductor was formed by mixing 10 g of seed crystal with 50 g of the weighed raw material powder, a single crystal superconductor with a diameter of 7 mm was obtained. You can get something.
これに対して、前述の秤量した原料粉末５０ｇに対して
種結晶を０．５ｇの割合で混合して単結晶超電導体を形
成したところ、直径５ｍｍのものが得られ、単結晶超電
導基板としては大きくても；）野角のものが得られるに
過ぎず、用結晶基板として１−分な大きさのものか得ら
れない。On the other hand, when a single crystal superconductor was formed by mixing 0.5 g of seed crystal with 50 g of the weighed raw material powder mentioned above, a single crystal superconductor with a diameter of 5 mm was obtained, which is suitable for use as a single crystal superconducting substrate. Even if it is large, it is only possible to obtain a crystal substrate with a size of 1-minute or less as a crystal substrate.
同様に、１ｔｊ述の秤量した原料粉末５０ｇ１：対して
種結晶をｌ１ｇの割合で混合シ、て超電導体を形成した
ところ、直径１０ｍｍのものが得られるが、種結晶が多
いため結晶数が多くなり、単結晶のものではなかった。Similarly, when a superconductor was formed by mixing 50 g of the weighed raw material powder described above with 1 g of seed crystals, a superconductor with a diameter of 10 mm was obtained, but due to the large number of seed crystals, the number of crystals was large. It was not a single crystal.
以−ヒの結果から、秤量した原料粉末５（Ｉｇに対する
種結晶の混合割合は、１〜１０ｇか適当である。From the results shown below, the mixing ratio of the seed crystal to the weighed raw material powder 5 (Ig) is 1 to 10 g, which is appropriate.
また、前述のようにして得た単結晶超電導体を種結晶に
用いて、−１−述した製造方法を繰り返すことにより、
さらに３０％の大型化が可能である。In addition, by repeating the manufacturing method described in -1- using the single crystal superconductor obtained as described above as a seed crystal,
Furthermore, it is possible to increase the size by 30%.
以−Ｌの実施例においては、１つの組成系がＢ ｉ 、
５ｒｃａｃｕｚ帆である場合について説明したが、Ｌ
ｎＢａ、ＣＵ、帆系（Ｌｎは、）、Ｙｂ、Ｅｒ、Ｅｕ、
Ｎｏ、Ｓｍ、＼ｄの一種又は複数種からなる） 、］’
１ＢａＣａＣｕＯ系あるいは実施例とは異なるＢ１５ｒ
ＣａＣｕ（１，系等の単結晶超電導体の形成に本発明を
適用することかできる。In the following examples, one compositional system is B i ,
Although we have explained the case where the sail is 5 rcacuz, L
nBa, CU, sail system (Ln), Yb, Er, Eu,
Consisting of one or more of No, Sm, \d) ,]'
1BaCaCuO system or B15r different from the examples
The present invention can be applied to the formation of single crystal superconductors such as CaCu(1, system).
たとえば、ＬｎＢａ＋Ｃｕ５Ｏ，系に本発明を適用する
場合には、その原料粉末（例えばＩ２Ｏ３、ＢａＣ０，
、及びＣ１１０＞を組成比Ｌｎ： Ｂａ：Ｃｕ＝ １
： ２°３．５に秤量して混合すればよく、単結晶超電
導体の析出温度Ｔを各原料粉末の溶融温度１０００℃よ
り高く、１０５０℃より低い温度に設定すればよい。For example, when applying the present invention to LnBa+Cu5O, the raw material powder (for example, I2O3, BaC0,
, and C110> with a composition ratio Ln: Ba:Cu=1
: They may be weighed and mixed at a temperature of 2°3.5°C, and the precipitation temperature T of the single crystal superconductor may be set at a temperature higher than the melting temperature of each raw material powder, 1000°C, and lower than 1050°C.
（ト）発明の効果
本発明による単結晶超電導体の製造方法は、ある１つの
組成系の酸化物超電導体の原料粉末をその組成系の組成
比に応じて秤量し、この秤量した原料粉末５０ｇ当り、
その組成系の酸化物超電導体の種結晶を１〜１０ｇの割
合で混合し、その組成系の単結晶析出温度前後の温度で
溶融した後、単結晶超電導体を形成するものであるから
、従来例で得られるものより大きい単結晶超電導体を得
ることができ、超電導デバイス用基板として使用するこ
とができる少なくとも５ｍｍ角以］、の大きさの超電導
基板として利用することができる。(G) Effects of the Invention In the method for producing a single crystal superconductor according to the present invention, raw material powder of an oxide superconductor of a certain composition system is weighed according to the composition ratio of that composition system, and 50 g of the weighed raw material powder is Hit,
Conventionally, a single crystal superconductor is formed by mixing 1 to 10 g of seed crystals of an oxide superconductor having the composition and melting the mixture at a temperature around the single crystal precipitation temperature of the composition. A single crystal superconductor larger than that obtained in the example can be obtained, and can be used as a superconducting substrate with a size of at least 5 mm square that can be used as a substrate for a superconducting device.
図面は本発明の一実施例における単結晶超電導体を形成
する熱処理時間に対する熱処理温度特性を示す。The drawing shows the heat treatment temperature characteristics with respect to the heat treatment time for forming a single crystal superconductor in one embodiment of the present invention.
Claims (1)
組成系の組成比に応じて秤量し、この秤量した原料粉末
５０ｇ当り、その組成系の酸化物超電導体の種結晶を１
〜１０ｇの割合で混合し、その組成系の単結晶析出温度
前後の温度で溶融した後、単結晶超電導体を形成する単
結晶超電導体の製造方法。(1) Weigh the raw material powder of oxide superconductor of one composition system according to the composition ratio of that composition system, and add 1 seed crystal of oxide superconductor of that composition system per 50 g of weighed raw material powder.
A method for producing a single-crystal superconductor, which comprises mixing at a ratio of ~10 g and melting at a temperature around the single-crystal precipitation temperature of the composition system to form a single-crystal superconductor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2311912A JPH04182394A (en) | 1990-11-16 | 1990-11-16 | Production of single crystal superconductor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2311912A JPH04182394A (en) | 1990-11-16 | 1990-11-16 | Production of single crystal superconductor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04182394A true JPH04182394A (en) | 1992-06-29 |
Family
ID=18022917
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2311912A Pending JPH04182394A (en) | 1990-11-16 | 1990-11-16 | Production of single crystal superconductor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04182394A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014139938A (en) * | 2010-11-05 | 2014-07-31 | Hitachi High-Technologies Corp | Ion milling system |
-
1990
- 1990-11-16 JP JP2311912A patent/JPH04182394A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014139938A (en) * | 2010-11-05 | 2014-07-31 | Hitachi High-Technologies Corp | Ion milling system |
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