JPH03215342A - Production of oxide-based superconducting sintered molded article - Google Patents
Production of oxide-based superconducting sintered molded articleInfo
- Publication number
- JPH03215342A JPH03215342A JP2006798A JP679890A JPH03215342A JP H03215342 A JPH03215342 A JP H03215342A JP 2006798 A JP2006798 A JP 2006798A JP 679890 A JP679890 A JP 679890A JP H03215342 A JPH03215342 A JP H03215342A
- Authority
- JP
- Japan
- Prior art keywords
- crucible
- oxide
- molded article
- current value
- molded body
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000002887 superconductor Substances 0.000 claims abstract description 22
- 229910001316 Ag alloy Inorganic materials 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000000748 compression moulding Methods 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 abstract description 19
- 239000000956 alloy Substances 0.000 abstract description 6
- 229910017944 Ag—Cu Inorganic materials 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 229910045601 alloy Inorganic materials 0.000 abstract 1
- 230000006835 compression Effects 0.000 abstract 1
- 238000007906 compression Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 27
- 238000002844 melting Methods 0.000 description 13
- 230000008018 melting Effects 0.000 description 13
- 229910052709 silver Inorganic materials 0.000 description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 8
- 238000009792 diffusion process Methods 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- 239000008188 pellet Substances 0.000 description 7
- 238000005275 alloying Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000010304 firing Methods 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 3
- 230000002265 prevention Effects 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 229910017980 Ag—Sn Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- BSWGGJHLVUUXTL-UHFFFAOYSA-N silver zinc Chemical compound [Zn].[Ag] BSWGGJHLVUUXTL-UHFFFAOYSA-N 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、酸化物系超電導焼結成型体の製造法に関し、
特に銀合金溶融体の特性の利用により目的製品における
超電導特性の劣化を防止しながら高い臨界電流値を有す
る超電導焼結成型体を得る方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing an oxide-based superconducting sintered body,
In particular, the present invention relates to a method of obtaining a superconducting sintered molded body having a high critical current value while preventing deterioration of superconducting properties in a target product by utilizing the characteristics of a silver alloy melt.
［従来技術〕
従来、Ｙ（イットリウム）系酸化物超電導体の製造にお
いて、高い臨界電流値（Ｊ ｃ）を有する焼結成型体を
得る方法としては、酸化物超電導体の原料粉末や合成粉
末を金型ブレスあるいは静水圧プレス等で成型した後、
適当な焼成条件下で焼成して焼結成型体を得る方法が一
般的である。[Prior art] Conventionally, in the production of Y (yttrium)-based oxide superconductors, the method of obtaining a sintered molded body having a high critical current value (Jc) was to use raw material powder or synthetic powder of oxide superconductor. After molding with a mold press or isostatic press,
A common method is to obtain a sintered molded body by firing under appropriate firing conditions.
しかしながらこの方法で焼結成型体をつくる場合には、
超電導体の結晶粒間でジョセフソン結合を作り易いため
、高い臨界電流値を持つものを得ることができなかった
。However, when making a sintered molded body using this method,
Because Josephson bonds are easily formed between superconductor grains, it has not been possible to obtain a superconductor with a high critical current value.
他の方法として、使用する酸化物超電導体粉末の表面を
前処理段階で予め酸エッチング、またはアルカリエッチ
ングで処理することにより表面の未反応相を取り除いた
合成粉末を金型プレスあるいは静水圧プレス等で成型し
た後、適当な焼成条件下で焼成して成型体を得る方法も
公知である。As another method, the surface of the oxide superconductor powder to be used is pretreated with acid etching or alkali etching to remove the unreacted phase on the surface, and then the synthetic powder is processed by mold pressing or isostatic pressing. There is also a known method in which a molded product is obtained by molding the material and then firing it under appropriate firing conditions.
しかしながら、この方法で得られる焼結成型体は、結晶
粒子間にジョセフソン接合ができてしまい、臨界電流値
が低下することが知られている。However, it is known that in the sintered molded body obtained by this method, Josephson junctions are formed between crystal grains, resulting in a decrease in critical current value.
更に他の方法として、酸化物超電導体の原料粉末または
合成粉末をるつぼに入れ、１．２００℃〜１．５００℃
の温度で部分的に、あるいは全体的に溶融させた後に、
冷却し、次いで９００〜１．０００℃で超電導結晶を包
晶反応で生成させて成型体を得る方法も知られている。Still another method is to put raw material powder or synthetic powder of oxide superconductor into a crucible and heat it to 1.200°C to 1.500°C.
After being partially or totally melted at a temperature of
A method is also known in which a molded body is obtained by cooling and then generating superconducting crystals by a peritectic reaction at 900 to 1,000°C.
しかしながらこの方法によって得られる成型体は、臨界
電流値に関しては好ましい値を示すが、原料粉としてＹ
，Ｂ ａ ２ Ｃ ｕ ３ ０ｔ−＊を用いた場合には
、これがｐｔるつぼと１．２００℃付近で反応すること
によって、Ｙ，Ｂａ２Ｃｕ．ＰｔＯ．。が生成して非超
電導体となるほか、ＭｇＯあるいはＡｊ！ ２０．るつ
ぼを用いた場合には、酸化物超電導体がるつぼに拡散し
たり、あるいは逆にるつぼ材が超電導材に拡散したりす
るためにるつぼと接合したり、超電導特性の劣化が生じ
たりする。However, although the molded body obtained by this method shows a favorable critical current value, Y
, Ba2Cu30t-* is used, it reacts with a PT crucible at around 1.200°C to form Y, Ba2Cu. PtO. . In addition to forming a non-superconductor, MgO or Aj! 20. When a crucible is used, the oxide superconductor diffuses into the crucible, or conversely, the crucible material diffuses into the superconducting material, resulting in bonding with the crucible and deterioration of superconducting properties.
上述の問題点を解決する一手段として、本発明者は先の
出願に係る特願平１−２３２３８７号「酸化物系超電導
焼結成型体の製法」において、酸化物超電導体粉末を予
め圧縮成型して仮焼した後、該仮焼体を銀浴中あるいは
銀浴上に配置して焼成することによって高い臨界電流値
を有する成型体を得る技術を開示した。As a means to solve the above-mentioned problems, the present inventor has developed a method of compression molding oxide superconductor powder in advance in the earlier application No. 1-232387 entitled "Method for producing oxide-based superconducting sintered body". The present invention discloses a technique for obtaining a molded body having a high critical current value by placing the calcined body in or on a silver bath and firing the calcined body.
しかしながらその後の研究により、上記作製法では、基
板からの拡散（不純物）や融着かなくなり、質の向上が
計られるという利点を有するものの、銀の融点が９６０
℃と高いために、仮焼体を浮かしている銀浴から銀を抜
く時にるつぼと接合する等の問題も一部あり、特に仮焼
体が大きい場合には、処理が困難であるということがわ
かった。However, subsequent research has shown that although the above manufacturing method has the advantage of eliminating diffusion (impurities) and fusion from the substrate and improving quality, the melting point of silver is 960.
℃, there are some problems such as bonding with the crucible when removing silver from the silver bath in which the calcined body is floating, and processing is difficult especially when the calcined body is large. Understood.
［発明が解決しようとする課題］
上述のように高い臨界電流値を持つ焼結成型体の得られ
る溶融法や部分溶融法は、るつぼとの接合や拡散がなけ
れば優れた焼結成型法の一つであり、また本発明者の上
記先行出願に係る銀浴法も同様に優れた焼結法の一つで
あるが、るつぼとの接合を完全に防止する上では若干の
問題があるため、更なる改良が求められていた。[Problems to be Solved by the Invention] As mentioned above, the melting method or partial melting method for obtaining a sintered molded body with a high critical current value is not an excellent sintered molding method unless there is bonding with a crucible or diffusion. The silver bath method according to the above-mentioned prior application of the present inventor is also one of the excellent sintering methods, but there are some problems in completely preventing bonding with the crucible. , further improvements were required.
［課題を解決するための手段］
本発明者らは斯る課題を解決するために鋭意研究したと
ころにより、るつぼ内に予め配置した銀合金を接合防止
材として使用し、９６０℃以下の温で焼結することによ
って酸化物超電導体の仮焼体とるつぼとが接合せずに、
しかも超電導特性を損なわずに高い臨界電流値を持つ成
型体を得ることができることを見い出して本発明を達成
することができた。[Means for Solving the Problems] In order to solve the problems, the present inventors conducted extensive research and found that a silver alloy placed in advance in a crucible was used as a bonding prevention material, and a silver alloy was used at a temperature of 960°C or less. By sintering, the calcined body of the oxide superconductor and the crucible do not bond together,
Moreover, the present invention was achieved by discovering that a molded body having a high critical current value can be obtained without impairing the superconducting properties.
すなわち本発明は、酸化物超電導体粉末を予め圧縮成型
した成型体または該成型体を仮焼した仮焼体を作製した
後、これらを銀合金浴上あるいは銀合金浴中に配置して
、９６０℃以下で焼成することにより高い臨界電流値を
有する成型体を得ることを特徴とする酸化物系超電導焼
結成型体の製造法に関するものである。That is, in the present invention, after producing a molded body by compression-molding oxide superconductor powder in advance or a calcined body by calcining the molded body, these are placed on or in a silver alloy bath, and then heated at 960° C. The present invention relates to a method for producing an oxide-based superconducting sintered molded body, which is characterized in that a molded body having a high critical current value is obtained by firing at a temperature of 0.degree. C. or lower.
［作 用］
本発明法においては、酸化物超電導体粉末としてＹ（イ
ットリウム）系酸化物のＹ１Ｂａ２（ｕ３０ｔ−ｘ粉を
用い、溶融法あるいは部分溶融法で臨界電流値の向上を
図っている。すなわち、Ｙ ，Ｂ ａ ２ Ｃ ｕ ３
０ ７−ｘを１．３００℃以上で卑全な溶融状態とす
る溶融法によって、あるいは１ ． ２００℃以下でＹ
２ Ｂ ａ Ｉ Ｃ ｕ ，Ｏ，の固相と残部の液相と
を生ぜしめた部分溶融状態から９００〜ｔ．ｏｏｏ℃の
温度で包晶反応を行い、固相表面でのＹ１Ｂａ２Ｃｕ，
０７−ｘの結晶化を図る部分溶融法によって所望の臨界
電流値をもつ焼結成型体の製造を図っている。従来行わ
れてきた通常の溶融法あるいは部分溶融法ではこの段階
でるつぼ材の材料の一部がＹＩ Ｂ ａ ２ Ｃ ｕ
ｉ ０７−ｘ ヘ拡散したり、また、取出し時にるつぼ
自体と酸化物超電導体とが接合して分離不可能になった
りするが、本発明法においてはるつぼ中に銀合金材を予
め配置して接合防止材として働くようにしているため上
記のような問題は生じない。[Function] In the method of the present invention, Y1Ba2 (u30t-x powder) of Y (yttrium)-based oxide is used as the oxide superconductor powder, and the critical current value is improved by a melting method or a partial melting method. That is, Y , Ba 2 Cu 3
1.07-x by a melting method that brings it into a base molten state at 1.300°C or higher, or 1. Y below 200℃
2 B a I Cu , O, from a partially molten state that produced a solid phase and a liquid phase at 900 to 900 t. A peritectic reaction is carried out at a temperature of ooo℃, and Y1Ba2Cu,
We are attempting to manufacture a sintered molded body having a desired critical current value by a partial melting method for crystallizing 07-x. In the conventional melting method or partial melting method, a part of the crucible material is converted into YI B a 2 Cu at this stage.
i 07-x may diffuse into the crucible, or the crucible itself and the oxide superconductor may bond together and become impossible to separate when taken out, but in the method of the present invention, the silver alloy material is placed in the crucible in advance. Since the material acts as a bonding prevention material, the above-mentioned problem does not occur.
尚、本発明法において使用する銀合金材の合金元素とし
て好ましいものは、Ｃｕｓ Ｇｅｓ ＰｂｓＳ ｎ ｓ
Ｇ ａ ｓ Ｉ ｎ −， Ｓ ｂ ｓ Ｚ ｎか
らなる群より選ばれた金属であり、これらは銀と合金化
することによって銀の融ヘ，を９６０℃以下にすること
ができる合金元素である。In addition, preferred alloying elements for the silver alloy material used in the method of the present invention are Cus Ges PbsS n s
It is a metal selected from the group consisting of G a s I n -, S b s Z n, and these are alloying elements that can reduce the melting temperature of silver to 960 ° C or less by alloying with silver. .
これら合金元素の添加によって、銀の融点が９００℃以
下となるようにすることが特に好ましいが、そのために
加えるべき合金元素の添加量は合金元素の種類によって
異なる。例えば、Ａｇ−Ｃｕ系ではＣｕを６％（重量％
、以下同じ）以上、Ａｇ Ｇｅ系ではＧｅをＢ％以上
、Ａｇ−Ｐｂ系ではｐｂをｌＯ％以上、Ａｇ−Ｓｎ系で
はＳｎを１０％以上、Ａｇ−Ｇａ系ではＧａを５％以上
、ＡｇＩｎ系ではＩｎをｌＯ％以上、Ａｇ−Ｓｂ系では
ｓｂを１０％以上、Ａｇ−Ｚｎ系ではＺｎを７％以上、
それぞれ添加することにより銀合金の融点が９００℃以
下となるように調製できることを確認した。It is particularly preferable to adjust the melting point of silver to 900° C. or less by adding these alloying elements, but the amount of the alloying element to be added for this purpose differs depending on the type of alloying element. For example, in the Ag-Cu system, Cu is 6% (weight%
, hereinafter the same) above, for Ag Ge system, Ge is B% or more, for Ag-Pb system, pb is 10% or more, for Ag-Sn system, Sn is 10% or more, for Ag-Ga system, Ga is 5% or more, and AgIn For systems, In is 10% or more, for Ag-Sb systems, sb is 10% or more, for Ag-Zn systems, Zn is 7% or more,
It was confirmed that the melting point of the silver alloy could be adjusted to 900° C. or lower by adding each of them.
これらの銀合金材は、酸化物超電導体粉末をプレス成型
したものを１．２００℃以上で焼成する際、該成型体と
るつぼ材との間にあって、るつぼ材と超電導体材との相
互拡散を防ぐ役割をするばかりでなく、９００〜ｔ，ｏ
ｏｏ℃の間で行う結晶化反応の際もるつほ材との接合を
防止する働きをする。When press-molding oxide superconductor powder is fired at 1.200°C or higher, these silver alloy materials are present between the molded body and the crucible material to prevent mutual diffusion between the crucible material and the superconductor material. Not only does it play a role in preventing, but also
It also functions to prevent bonding with the rutsuho material during the crystallization reaction that takes place at temperatures between 0.0 and 0.0°C.
このようにして得られた結晶化したＹＩ Ｂａ２Ｃｕ３
０７−ｔの焼結材（バルク材）を取り出すには、９６０
℃以下、好ましくは９００℃以下で銀合金を融かして取
り除き、徐冷する。これによって容易に超電導焼結体を
取り出すことができる。The crystallized YI Ba2Cu3 thus obtained
To take out the sintered material (bulk material) of 07-t, use 960
The silver alloy is melted and removed at a temperature of 0.degree. C. or less, preferably 900.degree. C. or less, and then slowly cooled. This allows the superconducting sintered body to be easily taken out.
以下、実施例をもって詳細に説明する。Hereinafter, a detailed explanation will be given using examples.
［実施例１］
Ｙ２Ｂａ，Ｃｕ，０５とＢａＣｕＯ２ＣｕＯの３Ｉｌ１
ａアンダー粉をＹ：Ｂａ：Ｃｕ−１：２：３の組成に配
合した混合粉を金型プレス内で１ ｔｏｎ／Ｃ■２の圧
力をかけて成型した後９５０℃にて２０時間焼成し、１
インチペレットを予め作製した。[Example 1] 3Il1 of Y2Ba, Cu, 05 and BaCuO2CuO
A mixed powder containing under powder with a composition of Y:Ba:Cu-1:2:3 was molded in a mold press under a pressure of 1 ton/C2, and then baked at 950℃ for 20 hours. ,1
Inch pellets were prepared in advance.
次いでＡｌｌ２（ｈるつぼにＡ ｇ ｌｏｏｇとＰｂｌ
Ｏｇとを入れ、その上に上記の１インチペレットを置い
て、加熱炉中で１．１００℃で２時間加熱した。Then All2 (A g loog and Pbl in the crucible
The above 1-inch pellet was placed on top of the 1-inch pellet, and heated at 1.100° C. for 2 hours in a heating furnace.
次いで炉内温度を９８０℃にして酸素雰囲気中に５０時
間保持して、Ｙ１Ｂ ａ ２ Ｃ ｕ ３ ０７−Ｉ＋
の結晶化を図った。結晶化が終了した後、温度を９００
℃に下げて、るつぼ内の焼結体を取り出した。Next, the temperature inside the furnace was raised to 980°C, maintained in an oxygen atmosphere for 50 hours, and Y1B a 2 Cu 3 07-I+
We attempted to crystallize the After crystallization is completed, the temperature is increased to 900°C.
℃, and the sintered body in the crucible was taken out.
次いで、残ったＹＩ Ｂ ａ ２ Ｃ ｕ ３ ０７−
ｘの焼結体をｌ”ｃ／ｓｉｎの割合で徐冷して、６００
℃の温度で２０時間、酸素雰囲気の条件下で保持した後
、炉浄を行った。Then, the remaining YI Ba 2 Cu 3 07-
The sintered body of x was slowly cooled at a rate of l"c/sin,
After being maintained in an oxygen atmosphere at a temperature of .degree. C. for 20 hours, the furnace was cleaned.
この焼結体には、るつぼ材であるＡＩ２０ｓや銀合金浴
のｐｂの拡散が少量しか認められず、また、該焼結体の
臨界電流値はｉｏ３Ａ／ｃ■２であり、Ｙ系酸化物超電
導体としては優れた焼結体であることが確認された。In this sintered body, only a small amount of diffusion of AI20s, which is the crucible material, and PB from the silver alloy bath was observed, and the critical current value of the sintered body was io3A/c2, and Y-based oxide It was confirmed that the sintered body is an excellent superconductor.
［実施例２］
実施例１で作製した１インチベレットをＡ＃２０３るつ
ぼにＡ ｇ １００ｇとＣｕｌ（Ｉｇとを入れたものの
上に置いて、加熱炉中にて１．１００℃で２時間加熱し
た。[Example 2] The 1-inch pellet produced in Example 1 was placed in an A#203 crucible containing 100 g of Ag and Cul (Ig), and heated in a heating furnace at 1.100°C for 2 hours. did.
次いで炉内温度を９８０℃にして酸素雰囲気中に５０時
間保持して、Ｙ，Ｂａ２ Ｃｕ，ｏ７−１の結晶化を図
った。結晶化が終了した後、温度を９００”Ｃに下げて
、るつぼ内の焼結体を取り出した。Next, the temperature in the furnace was raised to 980° C. and maintained in an oxygen atmosphere for 50 hours to crystallize Y, Ba2 Cu, o7-1. After crystallization was completed, the temperature was lowered to 900''C and the sintered body in the crucible was taken out.
次いで、残ったＹ ＩＢ ａ ２ Ｃ ｕ ３ ０ ７
−ｘの焼結体を１℃／ａｋｉｎの割合で徐冷して、６０
０℃の温度で２０時間、酸素雰囲気の条件下で保持した
後、炉浄を行った。Then, the remaining Y IB a 2 Cu 3 0 7
-x sintered body was slowly cooled at a rate of 1°C/akin, and
After being maintained in an oxygen atmosphere at a temperature of 0° C. for 20 hours, the furnace was cleaned.
この焼結体には、るつぼ材であるＡＩ２０ｑや銀合金浴
のＣｕの拡散が少量しが認められず、また、該焼結体の
臨界電流値は１Ｇ’Ａ／ｃ■２であり、Ｙ系酸化物超電
導体としては優れた焼結体であることが確認された。In this sintered body, a small amount of diffusion of AI20q, which is the crucible material, and Cu from the silver alloy bath was not observed, and the critical current value of the sintered body was 1 G'A/c2, and Y It was confirmed that the sintered body is an excellent oxide superconductor.
［実施例３］
実施例１で作製したｌインチペレットをＡｌ２０，るつ
ぼにＡ ｇ １００ｇとＺｎ８ｇとを加えたものの上に
置いて、加熱炉中にて１ ， １００℃で２時間加熱し
た。[Example 3] The 1-inch pellet produced in Example 1 was placed on an Al20 crucible containing 100 g of Ag and 8 g of Zn, and heated in a heating furnace at 1,100° C. for 2 hours.
次いで炉内温度を９８０℃にして酸素雰囲気中に５０時
間保持して、Ｙ １Ｂ ａ ２ Ｃ ｕ ３ Ｏｆ−Ｉ
１の結晶化を図った。結晶化が終了した後、温度を９０
０℃に下げて、るつぼ内の焼結体を取り出した。Next, the temperature inside the furnace was raised to 980°C and maintained in an oxygen atmosphere for 50 hours, and Y 1B a 2 Cu 3 Of-I
We attempted to crystallize 1. After crystallization is completed, the temperature is increased to 90
The temperature was lowered to 0° C., and the sintered body in the crucible was taken out.
次いで、残ったＹ１Ｂａ２Ｃｕｓ Ｏｔ−ｘの焼結体を
ｌ”ｃ／ｗｉｎの割合で徐冷して、６００℃の温度で２
０時間、酸素雰囲気の条件下で保持した後、炉浄を行っ
た。Next, the remaining sintered body of Y1Ba2Cus Ot-x was slowly cooled at a rate of 1"c/win, and was heated at a temperature of 600°C for 2
After maintaining the furnace under oxygen atmosphere conditions for 0 hours, the furnace was cleaned.
この焼結体には、るつぼ材であるＡ＃２０ｉや銀合金浴
のＺｎの拡散が少量しか認められず、また、該焼結体の
臨界電流値は１０’Ａ／ｅｓ２であり、Ｙ系酸化物超電
導体としては優れた焼結体であることが確認された。In this sintered body, only a small amount of diffusion of Zn from the crucible material A#20i and the silver alloy bath was observed, and the critical current value of the sintered body was 10'A/es2. It was confirmed that the sintered body is an excellent oxide superconductor.
［比較例１］
実施例１と同様に作製したＹ（ Ｂａ２Ｃｕ３０７−１
の１インチペレットを、直接ＡＮ２０３るつぼ内に入れ
て、加熱炉中で１，２００℃の温度で１時間加熱したと
ころ、該るつぼにＹ，Ｂａ２Ｃｕ３０７−ｘのベレット
が融着してしまい取れなくなってしまった。[Comparative Example 1] Y (Ba2Cu307-1
When a 1-inch pellet of Y,Ba2Cu307-x was directly placed in an AN203 crucible and heated in a heating furnace at a temperature of 1,200℃ for 1 hour, the Y,Ba2Cu307-x pellet was fused to the crucible and could not be removed. Oops.
また、冷却後取り外したＹ，Ｂａ２ Ｃｕ３０フー．の
焼結体をＥＰＭＡで調べたところ、焼結体中にＡＩ２０
３が拡散しているのが認められた。In addition, the Y, Ba2 Cu30 fu. which was removed after cooling. When examining the sintered body using EPMA, it was found that AI20 was found in the sintered body.
3 was observed to be spreading.
この焼結体の臨界電流値は８０Ａ／ｃｍ２であった。The critical current value of this sintered body was 80 A/cm2.
［発明の効果］
本発明法では、上述のように予めるつぼ中に入れておい
たＡｇとＰｂ，Ｃｕ，ＺｎＳＳｎＳＧｅｓＧａ，Ｉｎ，
Ｓｂ等とが融解して生じた銀合金材を接合と拡散防止の
ための隔離媒体として利用するため、酸化物超電導体と
るつぼ材との接合および材質の相互拡散を防止すること
ができるばかりでなく、得られた焼結体の劣化がなく高
い臨界電流値を有する焼結成型体が得られる。[Effect of the invention] In the method of the present invention, Ag and Pb, Cu, ZnSSnSGesGa, In, which have been placed in a pot in advance as described above,
Since the silver alloy material produced by melting Sb etc. is used as an isolation medium for bonding and diffusion prevention, it is possible to bond the oxide superconductor and crucible material and prevent mutual diffusion of the materials. Therefore, a sintered molded body having a high critical current value without deterioration of the obtained sintered body can be obtained.
Claims (1)
該成形体を仮焼した仮焼体を銀合金浴上あるいは銀合金
浴中に配置して、９６０℃以下で焼成することにより高
い臨界電流値を有する成型体を得ることを特徴とする酸
化物系超電導焼結成型体の製法。A molded body obtained by compression molding oxide superconductor powder in advance or a calcined body obtained by calcining the molded body is placed on or in a silver alloy bath and fired at a temperature of 960°C or less to obtain a high critical current value. A method for producing an oxide-based superconducting sintered body, characterized by obtaining a molded body having the following properties.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006798A JP3010363B2 (en) | 1990-01-16 | 1990-01-16 | Manufacturing method of oxide superconducting sintered compact |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006798A JP3010363B2 (en) | 1990-01-16 | 1990-01-16 | Manufacturing method of oxide superconducting sintered compact |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03215342A true JPH03215342A (en) | 1991-09-20 |
| JP3010363B2 JP3010363B2 (en) | 2000-02-21 |
Family
ID=11648199
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2006798A Expired - Fee Related JP3010363B2 (en) | 1990-01-16 | 1990-01-16 | Manufacturing method of oxide superconducting sintered compact |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3010363B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0530370A1 (en) * | 1991-03-14 | 1993-03-10 | International Superconductivity Technology Center | Process for producing oxide superconductor |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4174332B2 (en) * | 2003-01-23 | 2008-10-29 | 財団法人国際超電導産業技術研究センター | Oxide superconductor manufacturing method, oxide superconductor and its precursor support base material |
-
1990
- 1990-01-16 JP JP2006798A patent/JP3010363B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0530370A1 (en) * | 1991-03-14 | 1993-03-10 | International Superconductivity Technology Center | Process for producing oxide superconductor |
| EP0530370A4 (en) * | 1991-03-14 | 1993-11-24 | International Superconductivity Technology Center | Method of making oxide superconductor |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3010363B2 (en) | 2000-02-21 |
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