JPH01234327A - Production of oxide superconductor - Google Patents
Production of oxide superconductorInfo
- Publication number
- JPH01234327A JPH01234327A JP5960788A JP5960788A JPH01234327A JP H01234327 A JPH01234327 A JP H01234327A JP 5960788 A JP5960788 A JP 5960788A JP 5960788 A JP5960788 A JP 5960788A JP H01234327 A JPH01234327 A JP H01234327A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- temperature
- oxide superconductor
- superconductor
- heat
- 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
- 239000002887 superconductor Substances 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000000843 powder Substances 0.000 claims abstract description 22
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 14
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 7
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 7
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 5
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 5
- 239000000155 melt Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 abstract description 11
- 238000001816 cooling Methods 0.000 abstract description 8
- 238000002844 melting Methods 0.000 abstract description 8
- 230000008018 melting Effects 0.000 abstract description 8
- 235000010216 calcium carbonate Nutrition 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 5
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 2
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 abstract description 2
- 230000008023 solidification Effects 0.000 abstract 1
- 238000007711 solidification Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 230000007423 decrease Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000012768 molten material Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000010949 copper Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 239000005751 Copper oxide Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 2
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 2
- 229940112669 cuprous oxide Drugs 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229910016335 Bi—Ca Inorganic materials 0.000 description 1
- 229910001006 Constantan Inorganic materials 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Landscapes
- 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〕
この発明は、Ｂｉ −Ｃａ −Ｓｒ −Ｃｕ −０系酸
化物超伝導体の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing a Bi-Ca-Sr-Cu-0 based oxide superconductor.
（従来の技術）
最近、酸化物高温超伝導体の一種として、Ｂｉ −Ｃａ
−Ｓｒ −Ｃｕ −０系のものが新しく開発された。こ
のＢ＋ −ｃａ −ｓｒ −ｃｕ −ｏ系酸化物超伝導
体は、従来のＹ −ｔｔａ＝ｃｕ−ｏ系酸化物超伝導体
に比べてより高い温度で超伝導を示し、しかも超伝導特
性の安定性が良好であると伝えられている。(Prior art) Recently, as a type of oxide high temperature superconductor, Bi-Ca
-Sr-Cu-0 series has been newly developed. This B+ -ca-sr-cu-o oxide superconductor exhibits superconductivity at higher temperatures than the conventional Y-tta=cu-o oxide superconductor, and has excellent superconducting properties. It is reported to have good stability.
このＢｉ −Ｃａ −Ｓｒ −Ｃｕ −０系酸化物超伝
導体１４造する方法としては、酸化ビスマス、炭酸カル
シウム、炭酸ストロンチウムおよび酸化銅の粉末を所定
量混合し、これを仮焼したのら、粉砕し、さらにプレス
成形してのら本焼成し、冷却する従来のＹ−Ｂａ−Ｃｕ
−０系超伝導体の製造と同様のいわゆる粉末焼結法が用
いられている。The method for producing the Bi-Ca-Sr-Cu-0-based oxide superconductor 14 is as follows: mixing a predetermined amount of powders of bismuth oxide, calcium carbonate, strontium carbonate, and copper oxide, calcining the mixture, and then calcining the mixture. Conventional Y-Ba-Cu is crushed, press-molded, fired, and cooled.
A so-called powder sintering method similar to that used for producing -0 series superconductors is used.
しかしながら、このような粉末焼結法によって得られた
Ｂｉ −Ｃａ −Ｓｒ −Ｃｕ −０系酸化物超伝導体
にあっては、第１図曲線Ｂで示すように冷却に伴って電
気抵抗がスムーズにゼロにならず尾を引いてしまう特性
を有し、臨界温度が実際には低（なる不具合がある。However, in the Bi-Ca-Sr-Cu-0 based oxide superconductor obtained by such a powder sintering method, the electrical resistance smoothly decreases as it cools, as shown by curve B in Figure 1. It has the characteristic that it does not reach zero but has a tail, and the critical temperature is actually low.
また、上述のように粉末焼結法自体工程数が多く、製造
が面倒である問題点もある。Further, as mentioned above, the powder sintering method itself has a problem that the number of steps is large and manufacturing is troublesome.
この発明では、酸化ビスマス、炭酸カルシウム、炭酸ス
トロンチウムおよび酸化銅の混合粉末を溶融し、この溶
融物を急冷して固形化したのら熱処理することにより上
記課題を解決するようにした。In this invention, the above-mentioned problem is solved by melting a mixed powder of bismuth oxide, calcium carbonate, strontium carbonate, and copper oxide, rapidly cooling the melt, solidifying it, and then heat-treating it.
以下、この発明の製造方法の一例を説明する。An example of the manufacturing method of the present invention will be described below.
まず、出発原料として、酸化ビスマス（Ｂｉ２０３）粉
末、炭酸カルシウム（ｃａｃｏ３ ）粉末、炭酸ストロ
ンチウム（ＳｒＣ（ｈ ）粉末、酸化第一銅（ＣＵＯ）
粉末を用意し、これらの化合物粉末を所定の割合、例え
ば原子比でＢｉ：Ｃａ：Ｓｒ：Ｃｕ＝１ ： １ ：１
：２で混合し、混合粉末とする。これらの化合物粉末の
純度は９９．９％以上のものが好ましく、粉末粒径は１
〜５μｍ程度のものが好ましい。First, as starting materials, bismuth oxide (Bi203) powder, calcium carbonate (caco3) powder, strontium carbonate (SrC(h) powder, cuprous oxide (CUO))
Powders are prepared, and these compound powders are mixed in a predetermined ratio, for example, in an atomic ratio of Bi:Ca:Sr:Cu=1:1:1.
: Mix in step 2 to make a mixed powder. The purity of these compound powders is preferably 99.9% or more, and the powder particle size is 1
A thickness of approximately 5 μm is preferable.
ついで、この混合粉末ｉ白金るつぼ、アルミするつぼな
どのるつぼに入れ、電気炉などの加熱炉中で１１００〜
１２００℃の温度範囲で加熱し溶融する。溶融温度が１
１００℃未満では溶融、混合が不充分となり、また１２
００℃を越えると試料の蒸発が顕著となって不都合とな
る。溶融時間は３０分程度で十分である。また、溶融雰
囲気は酸素含有雰囲気でよい。Next, this mixed powder is placed in a crucible such as a platinum crucible or an aluminum crucible, and heated in a heating furnace such as an electric furnace at 1100~
Heat and melt in a temperature range of 1200°C. Melting temperature is 1
Below 100°C, melting and mixing will be insufficient, and 12
If the temperature exceeds 00°C, evaporation of the sample becomes noticeable, which is inconvenient. A melting time of about 30 minutes is sufficient. Further, the melting atmosphere may be an oxygen-containing atmosphere.
ついで、この溶融物を急冷し、所望の形状に固形化する
。急冷の方法としては例えば常温の厚鉄板上に溶融物を
すばやく流し、上から常温の鉄板を置いて軽く加圧する
と同時に冷却し、フィルム状物を得る方法、溶融物をる
つぼ底部から帯状に冷却回転ロール上に流延して冷部し
、リボン状物を得る方法、溶融物をるつぼ底部から糸状
に流し出し、ただちに液化窒素中に浸漬し冷却して、糸
状物を得る方法などが用いられ、この時の冷却速度を１
秒当り約１０３〜１０”Ｃとすることが好ましい。This melt is then rapidly cooled and solidified into the desired shape. Rapid cooling methods include, for example, quickly pouring the molten material onto a thick iron plate at room temperature, placing the iron plate at room temperature on top, applying light pressure, and cooling at the same time to obtain a film-like material, or cooling the molten material in a band from the bottom of the crucible. The methods used include a method in which the melt is cast onto a rotating roll and cooled to obtain a ribbon-like product, and a method in which the melt is poured out in the form of threads from the bottom of the crucible and immediately immersed in liquefied nitrogen and cooled to obtain a thread-like product. , the cooling rate at this time is 1
Preferably, it is about 10 3 to 10”C per second.
このようにして急冷して得られた急冷物を電気炉などを
用いて熱処理する。ここでの熱処理温度は７５０〜８８
０℃の範囲とされる。熱処理温度が７５０℃未満である
と超伝導相の発現がなく、８８０℃を越えると急冷物の
部分溶解が生じて不都合である。好ましい熱処理温度は
８００〜８５０℃である。熱処理時間は１〜２４時間程
度とされ、熱処理雰囲気は空気中、酸素ガス中などの酸
素含有雰囲気とされる。The quenched material obtained by quenching in this manner is heat treated using an electric furnace or the like. The heat treatment temperature here is 750-88
It is assumed to be in the range of 0°C. If the heat treatment temperature is less than 750°C, no superconducting phase will develop, and if it exceeds 880°C, partial melting of the quenched material will occur, which is disadvantageous. The preferred heat treatment temperature is 800-850°C. The heat treatment time is about 1 to 24 hours, and the heat treatment atmosphere is an oxygen-containing atmosphere such as air or oxygen gas.
熱処理終了後は、熱処理物を電気炉に入れたまま冷却す
るか、または炉から取り出して空気中放冷するかあるい
は液化窒素中に投入して急冷するなどの方法で冷却し、
目的のＢｉ −Ｃａ−Ｓｒ−Ｃｕ−０系酸化物超伝導体
を得る。After the heat treatment is completed, the heat-treated product is cooled while it is still in the electric furnace, or it is taken out of the furnace and left to cool in the air, or it is cooled by quenching by placing it in liquefied nitrogen.
The desired Bi-Ca-Sr-Cu-0 based oxide superconductor is obtained.
このような製造方法にあっては、得られる超伝導体の潤
度−抵抗特性が良好で、温度降下に対応してスムーズに
電気抵抗がゼロとなり、臨界温度（Ｔｃ ＞曲線が電気
抵抗ゼロ近傍で尾を引くことがない。また、急冷方法を
種々選択することにより、種々の形状の超伝導体を得る
ことができ、例えばフィルム状、リボン状、線状のもの
が得られ、さらには基板上に膜状の超伝導体を形成する
こともできる。さらに、従来の粉末焼結法に比較して工
程数が少なく、製造が極めて簡便である。In such a manufacturing method, the obtained superconductor has good moisture-resistance characteristics, the electrical resistance smoothly decreases to zero as the temperature decreases, and the critical temperature (Tc > the curve approaches zero electrical resistance). In addition, by selecting various quenching methods, it is possible to obtain superconductors in various shapes, such as films, ribbons, and wires. A film-like superconductor can also be formed thereon.Furthermore, the number of steps is small compared to the conventional powder sintering method, and manufacturing is extremely simple.
（実施例）
Ｂｉ、 ０３ 、ＣａＣＯ３、ＳｒＣＯ３、ＣｕＯの粉
末を、原子比テＢｉ：Ｃａ：Ｓｒ：Ｃｕ＝１ ： １
： １ ： ２となるように坪量混合し、この混合粉末
を白金るつぼに入れ、電気炉中で４度１１５０℃で３０
分間溶融した。この溶融物を鉄板上に流し出してプレス
し、急冷して厚さｌｌｌｌ１ｍのシート状の急冷物を得
た。ついで、この急冷物を電気炉内で空気中、温度８０
０℃、時間２４時間の条件で熱処理し、電気炉内で室温
まで冷却して、シート状の試料を得た。(Example) Powders of Bi, 03, CaCO3, SrCO3, and CuO were prepared in an atomic ratio of Bi:Ca:Sr:Cu=1:1.
: 1 : 2, put this mixed powder into a platinum crucible, and heat it in an electric furnace at 1150℃ for 30 minutes.
It melted for a minute. This molten material was poured onto an iron plate, pressed, and rapidly cooled to obtain a sheet-like quenched product with a thickness of 1 m. Next, this quenched material is heated to a temperature of 80°C in air in an electric furnace.
The sample was heat-treated at 0° C. for 24 hours and cooled to room temperature in an electric furnace to obtain a sheet-like sample.
このシート状の試料について、温度降下に伴う電気抵抗
変化、温度降下に伴う帯磁率変化および臨界電流密度を
測定した。電気抵抗変化は幅３ＩＩｎ、長さ１０＃ＩＩ
Ｉ、厚さ１Ｎの試料について直流四端子法（電流５ｎＡ
）にて測定した。温度測定には銅−コンスタンタン熱電
対を用いた。また、帯磁率は相互インダクタンスを測定
することにより求めた。For this sheet-like sample, changes in electrical resistance due to temperature drop, changes in magnetic susceptibility due to temperature drop, and critical current density were measured. Electrical resistance change is width 3IIn, length 10#II
I, DC four-terminal method (current 5 nA) for a sample with a thickness of 1N
). A copper-constantan thermocouple was used for temperature measurement. Moreover, the magnetic susceptibility was determined by measuring mutual inductance.
臨界電流密度の測定は直流四端子法により、測定温度７
７Ｋ、零磁場で行った。The critical current density was measured using the DC four-terminal method at a measurement temperature of 7.
It was performed at 7K and zero magnetic field.
結果を第１図ないし第３図に示す。The results are shown in Figures 1 to 3.
第１図のグラフは、電気抵抗変化を示し、グラフ中曲線
Ａはこの実験例によって得られた試料についてのもので
、曲ｔｉ！Ｂは従来の粉末焼結法で得られた８ｉ −Ｃ
ａ −ｓｒ −Ｃｕ −０系超伝導体についてのもので
ある。このグラフより、この発明の方法によれば電気抵
抗が１９度降下に対応してスムーズに低下する超伝導体
が得られることがわかる。なお、この試料の臨界温度（
Ｔｃ ）は８６にであった。The graph in FIG. 1 shows the change in electrical resistance, and the curve A in the graph is for the sample obtained in this experimental example, and the curve ti! B is 8i-C obtained by conventional powder sintering method
This is about an a-sr-Cu-0 based superconductor. From this graph, it can be seen that according to the method of the present invention, a superconductor whose electrical resistance smoothly decreases in response to a 19 degree drop can be obtained. Note that the critical temperature of this sample (
Tc) was 86.
第２図は帯磁率変化を示し、８５に以下で帯磁率が急激
に低下しており、この温度以下で超伝導相が形成されて
いることが確認された。FIG. 2 shows the change in magnetic susceptibility, and the magnetic susceptibility decreases rapidly below 85°C, confirming that a superconducting phase is formed below this temperature.
第３図は臨界電流密度ＬＪＣ）を示し、この試料では臨
界電流密度が１０２Ａ／ｃｉであった。FIG. 3 shows the critical current density (LJC), and in this sample, the critical current density was 102 A/ci.
まｌＣ％熱処理時の熱処理温度を８２０℃および８５０
℃とした試料についても同様の結果が得られた。The heat treatment temperature during heat treatment was 820℃ and 850℃.
Similar results were obtained for samples kept at ℃.
以上説明したように、この発明の酸化物超伝導体の製造
方法は、酸化ビスマス粉末、炭酸カルシウム粉末、炭酸
ストロンチウム粉末および酸化銅粉末を混合し、この混
合粉末を１１００〜１２００℃で溶融し、この溶融物を
急冷して固形化したのち、７５０〜８８０℃で熱処理す
るものであるので、製造が従来の粉末焼結法に比べて極
めて簡便であり、また急冷方法を選択することにより線
状、膜状、テープ状等の任意の形状のものが得られる。As explained above, the method for producing an oxide superconductor of the present invention involves mixing bismuth oxide powder, calcium carbonate powder, strontium carbonate powder, and copper oxide powder, melting this mixed powder at 1100 to 1200°C, This molten material is rapidly cooled to solidify and then heat-treated at 750 to 880°C, making production extremely simple compared to the conventional powder sintering method. , film-like, tape-like, or other arbitrary shapes can be obtained.
さらに、（ηられる超伝導体は特性も良好であるなどの
効果が得られる。Furthermore, the superconductor with (η) has good characteristics and other effects.
第１図ないし第３図はいずれもこの発明の実験例で得ら
れた測定結果を示すグラフであり、第１図は電気抵抗変
化を、第２因は帯磁率変化を、第３図は臨界電流密度を
示す。
不１化牢（ａ、ｕ）
抵抗、（ｍＱ ｃｍ）
第３図
電＞ｉ ’１９ （４７ｃｍ２）
手粘に打ｌ↑正書 （自発）
昭和６３年ダ月７０Figures 1 to 3 are graphs showing measurement results obtained in experimental examples of the present invention. Figure 1 shows changes in electrical resistance, changes in magnetic susceptibility as the second factor, and Figure 3 shows changes in criticality. Indicates current density. Non-uniform prison (a, u) Resistance, (mQ cm) Figure 3 Den>i '19 (47cm2) Hand punch l ↑ Original text (self-motivated) Da 70, 1988
Claims (1)
チウム粉末および酸化銅粉末を混合し、この混合粉末を
１１００〜１２００℃で溶融し、この溶融物を急冷して
固形化したのち、７５０〜８８０℃で熱処理することを
特徴とする酸化物超伝導体の製造方法。Bismuth oxide powder, calcium carbonate powder, strontium carbonate powder, and copper oxide powder are mixed, this mixed powder is melted at 1100 to 1200°C, this melt is rapidly cooled to solidify, and then heat treated at 750 to 880°C. A method for producing an oxide superconductor, characterized in that:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5960788A JPH01234327A (en) | 1988-03-14 | 1988-03-14 | Production of oxide superconductor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5960788A JPH01234327A (en) | 1988-03-14 | 1988-03-14 | Production of oxide superconductor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01234327A true JPH01234327A (en) | 1989-09-19 |
Family
ID=13118111
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5960788A Pending JPH01234327A (en) | 1988-03-14 | 1988-03-14 | Production of oxide superconductor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01234327A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01212226A (en) * | 1988-02-18 | 1989-08-25 | Sanyo Electric Co Ltd | Production of oxide superconducting material |
| JPH0579608A (en) * | 1991-03-25 | 1993-03-30 | Foster Wheeler Energy Corp | Fluidized bed combustion device with large number of furnace areas and method thereof |
-
1988
- 1988-03-14 JP JP5960788A patent/JPH01234327A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01212226A (en) * | 1988-02-18 | 1989-08-25 | Sanyo Electric Co Ltd | Production of oxide superconducting material |
| JPH0579608A (en) * | 1991-03-25 | 1993-03-30 | Foster Wheeler Energy Corp | Fluidized bed combustion device with large number of furnace areas and method thereof |
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