JPH0714494B2 - Method for manufacturing oxide superconductor - Google Patents
Method for manufacturing oxide superconductorInfo
- Publication number
- JPH0714494B2 JPH0714494B2 JP62221713A JP22171387A JPH0714494B2 JP H0714494 B2 JPH0714494 B2 JP H0714494B2 JP 62221713 A JP62221713 A JP 62221713A JP 22171387 A JP22171387 A JP 22171387A JP H0714494 B2 JPH0714494 B2 JP H0714494B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- mixed powder
- particle size
- oxide superconductor
- 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.)
- Expired - Fee Related
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
- B03C1/021—Separation using Meissner effect, i.e. deflection of superconductive particles in a magnetic field
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/16—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/18—Methods for preparing oxides or hydroxides in general by thermal decomposition of compounds, e.g. of salts or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/006—Compounds containing, besides copper, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/45—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on copper oxide or solid solutions thereof with other oxides
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Description
【発明の詳細な説明】 〔産業上の利用分野〕 この発明は、酸化物超電導体の製造方法に関するもので
ある。TECHNICAL FIELD The present invention relates to a method for producing an oxide superconductor.
第３図は例えば同一出願人による特願昭62-144401号明
細書「酸化物超電導体の製造方法」に示された従来の酸
化物超電導体の製造方法を示す説明図である。第１工程
はランタノイド金属、アルカリ土類金属の酸化物と銅の
酸化物などの素材の秤量（11）、第２工程は乳鉢中でよ
く混合（12）し、第３工程では数百℃で予備焼成（1
3）、第４工程で再び混合粉砕（14）の後、第５工程で
必要な酸化物超電導粉体を分離（15）し、第６工程で分
離された酸化物超電導粉体を必要な形に整形（16）し、
第７工程では900℃〜1100℃の温度で本焼成（17）して
合成する。FIG. 3 is an explanatory view showing a conventional method for producing an oxide superconductor, which is disclosed in, for example, Japanese Patent Application No. 62-144401 “Method for producing oxide superconductor” by the same applicant. The first step weighs materials such as lanthanoid metal, alkaline earth metal oxides and copper oxides (11), the second step mixes well (12) in a mortar, and the third step is at several hundreds of degrees Celsius. Pre-baking (1
3) After mixing and pulverizing (14) again in the 4th step, the oxide superconducting powder required in the 5th step is separated (15), and the oxide superconducting powder separated in the 6th step is formed into the required shape. Shaped (16) into
In the seventh step, main calcination (17) is performed at a temperature of 900 ° C to 1100 ° C to synthesize.
この方法は、粉体混合法と呼ばれるものである。第４図
は上記分離工程（15）の具体的な一例を説明する断面構
成図であり、図において、（１）は混合粉体収納容器，
（２）は酸化物超電導粉体，（３）は超電導を示さない
不純物，（４）は磁石，（５）は磁力線，（６）は分離
容器，（７）は仕切板，（10）は混合粉体である。分離
容器（６）の上部から混合粉体（10）を落下させると、
超電導を示す粉体（２）は、マイスナー効果により磁石
（４）から遠ざかり、分離容器（６）の仕切板（７）の
反対側に落下する。一方、超電導を示さない粉体（３）
は、そのまま落下するので、分離でき、酸化物超電導粉
体（２）のみを集めて次の整形工程（16）へ進む。な
お、粉体の分離は、酸化物超電導粉体（２）が超電導を
発揮する温度にまで冷却して行なう。This method is called a powder mixing method. FIG. 4 is a sectional configuration diagram for explaining a specific example of the separation step (15), in which (1) is a mixed powder storage container,
(2) is oxide superconducting powder, (3) is an impurity that does not show superconductivity, (4) is a magnet, (5) is a magnetic field line, (6) is a separation container, (7) is a partition plate, and (10) is It is a mixed powder. When the mixed powder (10) is dropped from the upper part of the separation container (6),
The powder (2) exhibiting superconductivity moves away from the magnet (4) due to the Meissner effect, and falls on the opposite side of the partition plate (7) of the separation container (6). On the other hand, powder that does not show superconductivity (3)
Can be separated because they fall as they are, and only the oxide superconducting powder (2) is collected and the process proceeds to the next shaping step (16). The powder is separated by cooling to a temperature at which the oxide superconducting powder (2) exhibits superconductivity.
上記のように、分離工程（15）を経て本焼成（17）して
得られた酸化物超電導体の通電特性を第２図の特性曲線
Ｉで示す。第２図において、横軸は通電電流、縦軸は、
発生電圧である。通電電流を零から徐々に上昇する。し
ばらくは超電導状態であるため、発生電圧は零である
が、Ａ点を越えると電圧が発生する。通常Ａ点は臨界電
流値と呼ばれるものである。The characteristic curve I of FIG. 2 shows the current-carrying characteristics of the oxide superconductor obtained by the main firing (17) through the separation step (15) as described above. In FIG. 2, the horizontal axis represents the energizing current and the vertical axis represents
It is the generated voltage. The energizing current gradually increases from zero. Since it is in a superconducting state for a while, the generated voltage is zero, but when point A is exceeded, a voltage is generated. Point A is usually called the critical current value.
従来の製造方法によって得られた酸化物超電導体の通電
電流特性は、特性曲線Ｉのように、臨界電流値がＡ点の
如く低く、超電導体としての特性が悪いという問題点が
あった。The current carrying characteristics of the oxide superconductor obtained by the conventional manufacturing method have a problem that the critical current value is as low as the point A as shown by the characteristic curve I and the characteristics as a superconductor are poor.
この発明は上記のような問題点を解消するためになされ
たもので、臨界電流値が高く、超電導体としての特性の
良いものを得ることを目的とする。The present invention has been made to solve the above problems, and an object thereof is to obtain a material having a high critical current value and good characteristics as a superconductor.
この発明に係る酸化物超電導体の製造方法は、複数種類
の原料を所定の割合で混合して焼成し、粉砕することに
よって酸化物超電導粉体を主成分とする混合粉体を得る
工程、前記混合粉体をふるいにかけて粒径が100μｍ以
下の混合粉体を取り出す工程、前記粒径が100μｍ以下
の混合粉体を落下させながら、該混合粉体に、磁石によ
り水平方向から磁場をかけ、前記混合粉体に含まれた酸
化物超電導粉体を該磁石とは反対の水平方向に飛ばし、
前記混合粉体に含まれた超電導を示さない不純物をその
まま下方に落下させることによって前記酸化物超電導粉
体を分離する工程、および分離された酸化物超電導体粉
体をふるいにかけて粒径が１μｍ以上のものを取り出す
工程を有することを特徴とするものである。The method for producing an oxide superconductor according to the present invention comprises a step of obtaining a mixed powder containing oxide superconducting powder as a main component by mixing and firing a plurality of kinds of raw materials at a predetermined ratio, and pulverizing the raw materials. A step of sieving the mixed powder with a particle size of 100 μm or less, dropping the mixed powder having a particle size of 100 μm or less, and applying a magnetic field from a horizontal direction to the mixed powder by a magnet; Flying the oxide superconducting powder contained in the mixed powder in the horizontal direction opposite to the magnet,
A step of separating the oxide superconducting powder by dropping the impurities not showing superconducting contained in the mixed powder as it is, and sieving the separated oxide superconducting powder so that the particle size is 1 μm or more. It is characterized by having a step of taking out the thing.
この発明における製造方法は、分離工程により不純物を
徐去すると共に、ふるいにより粒径を１〜100μｍに揃
えるのでち密で臨界電流値が高い酸化物超電導体が得ら
れる。In the production method according to the present invention, the impurities are gradually removed in the separation step, and the particle size is made uniform to 1 to 100 μm by the sieve, so that a dense oxide superconductor having a high critical current value can be obtained.
以下この発明の一実施例を図について説明する。第１図
は、この発明の一実施例による酸化物超電導体の製造方
法における一部を説明する断面構成図であり、図におい
て、（８）は穴径100μｍのふるいすなわちフィルタA,
（９）は穴径１μｍのふるいすなわちフィルタB,（21）
はＣ室，（22）はＤ室，（23）はＥ室，（24）はＦ室で
ある。An embodiment of the present invention will be described below with reference to the drawings. FIG. 1 is a cross-sectional configuration diagram for explaining a part of a method for producing an oxide superconductor according to an embodiment of the present invention. In the figure, (8) shows a sieve having a hole diameter of 100 μm, that is, a filter A,
(9) is a sieve with a hole diameter of 1 μm, namely filter B, (21)
Is room C, (22) is room D, (23) is room E, and (24) is room F.
容器（１）の中の混合粉体（10）は超電導を示す成分の
粉体（２）と超電導を示さない成分の粉体すなわち不純
物（３）が混合しているが、これらの粉体の粒度は通常
0.1μｍ以下のものから1mm程度の範囲にまで広く分布し
ている。分離容器（６）では、まず穴径が100μｍのフ
ィルタＡ（８）に、よって混合粉体（10）の粒度が100
μｍ以上のものと100μｍ以下のものとに分離する。す
なわち、100μｍ以上の粒度のものは、フィルタＡ
（８）を通過せず、右側のＣ室（21）に貯まり、100μ
ｍ未満のものはフィルタＡ（８）を通過し落下する。落
下の過程で、磁石（４）の磁力線（５）の作用と、超電
導のマイスナー効果により、超電導を示す成分の粉体
（２）のみが図面に向かって右側に遠ざかり、フィルタ
Ｂ（９）の上に落下する。フィルタＢ（９）は穴径１μ
ｍであるため、１μｍ未満の粒度のものはＥ室（23）に
落下し、１μｍ以上のものは、Ｄ室（22）に貯まるの
で、これを集めて、次の成形および焼成工程へ進む。以
上のように粒度を揃えて作るため、ち密な組織の酸化物
超電導体が得られる。The mixed powder (10) in the container (1) is a mixture of powder (2) of a component showing superconductivity and powder of a component not showing superconductivity, that is, impurities (3). Granularity is normal
Widely distributed from 0.1 μm or less to about 1 mm. In the separation container (6), first, the particle size of the mixed powder (10) is 100 because of the filter A (8) having a hole diameter of 100 μm.
Separate into those with a diameter of 100 μm or more and those with a diameter of 100 μm or less. That is, if the particle size is 100 μm or more, filter A
It does not pass through (8), accumulates in chamber C (21) on the right side, and becomes 100μ.
Those less than m pass through the filter A (8) and fall. In the process of dropping, due to the action of the magnetic field lines (5) of the magnet (4) and the Meissner effect of superconductivity, only the powder (2) of the component showing superconductivity moves away to the right toward the drawing, and the filter B (9) Fall on. Filter B (9) has a hole diameter of 1μ
Since it is m, particles having a particle size of less than 1 μm fall into the E chamber (23), and particles having a particle size of 1 μm or more are stored in the D chamber (22), which are collected and proceed to the next molding and firing step. Since the particles are made to have the same grain size as described above, an oxide superconductor having a dense structure can be obtained.
なお、超電導線の臨界電流密度向上および臨界磁界向上
の因子として、ピン止め力の大きさがあるが、このピン
止め力は酸化物超電導体の平均粒径により異なり、一般
的には、１μｍ以上が選ばれることが、文献（超電導マ
グネット研究センター報告，第３巻,P.34〜P.38,昭和61
年12月，九州大学工学部付属超電導マグネット研究セン
ター発行）に示されている。また、発明者らの実験によ
れば100μｍがその上限値であり、これにより粒径が大
きくなると、オンセットからオフセットまでの温度間隔
が著しく広い劣悪な酸化物超電導体となる可能性の高い
ことが確認された。The pinning force is a factor for improving the critical current density and the critical magnetic field of the superconducting wire. The pinning force varies depending on the average particle size of the oxide superconductor, and is generally 1 μm or more. Is selected in the literature (Superconducting Magnet Research Center Report, Volume 3, P.34 to P.38, Showa 61).
, Published by the Superconducting Magnet Research Center, Faculty of Engineering, Kyushu University). Further, according to the experiments conducted by the inventors, the upper limit value is 100 μm, and when the particle size is increased due to this, there is a high possibility that an inferior oxide superconductor having a significantly wide temperature interval from onset to offset is obtained. Was confirmed.
上記実施例により得られた酸化物超電導体の通電電流特
性を第２図の特性曲線IIで示す。この臨界電流値はＢ点
であり従来のＡ点に比べてかなり大きくなっていること
がわかる。The current carrying characteristics of the oxide superconductors obtained in the above examples are shown by characteristic curve II in FIG. This critical current value is point B, which is considerably larger than the conventional point A.
以上のように、この発明によれば、複数種類の原料を所
定の割合で混合して焼成し、酸化物超電導粉体を主成分
とする混合粉体を得る工程、および上記混合粉体に磁石
を近付け、超電導体のマイスナー効果による磁気反発力
を利用して上記酸化物超電導粉体を分離する工程、およ
びふるいにより、上記酸化物超電導粉体の粒径を１〜10
0μｍに揃える工程を施すので、臨界電流値が高く特性
の良い酸化物超電導体が得られる。As described above, according to the present invention, a step of obtaining a mixed powder containing oxide superconducting powder as a main component by mixing a plurality of kinds of raw materials at a predetermined ratio and firing the mixture, and a magnet for the mixed powder. , A step of separating the oxide superconducting powder by using the magnetic repulsion force due to the Meissner effect of the superconductor, and a sieving so that the particle size of the oxide superconducting powder is 1 to 10
Since the step of adjusting to 0 μm is performed, an oxide superconductor having a high critical current value and good characteristics can be obtained.
【図面の簡単な説明】 第１図はこの発明の一実施例による酸化物超電導体の製
造方法の一部を説明する断面構成図，第２図はこの発明
の一実施例および従来の方法により得られた酸化物超電
導体の通電電流特性を示す曲線図，第３図は従来の酸化
物超電導体の製造方法を示す工程図，第４図は第３図の
分離工程を説明する断面構成図である。 図において、（２）は酸化物超電導粉体，（３）は不純
物，（４）は磁石，（６）は分離容器，（８）はフィル
タA,（９）はフィルタB,（10）は混合粉体である。 なお、各図中、同一符号は同一、または相当部分を示す
ものとする。BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a sectional configuration view for explaining a part of a method for manufacturing an oxide superconductor according to an embodiment of the present invention, and FIG. 2 is a view showing an embodiment of the present invention and a conventional method. A curve diagram showing the energization current characteristics of the obtained oxide superconductor, FIG. 3 is a process diagram showing a conventional method for manufacturing an oxide superconductor, and FIG. 4 is a cross-sectional configuration diagram explaining the separation process of FIG. Is. In the figure, (2) is an oxide superconducting powder, (3) is an impurity, (4) is a magnet, (6) is a separation container, (8) is filter A, (9) is filter B, and (10) is It is a mixed powder. In the drawings, the same reference numerals indicate the same or corresponding parts.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｈ０１Ｌ 39/00 ＺＡＡ 9276−4Ｍ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification number Office reference number FI technical display location H01L 39/00 ZAA 9276-4M
Claims (1)
成し、粉砕することによって酸化物超電導粉体を主成分
とする混合粉体を得る工程、前記混合粉体をふるいにか
けて粒径が100μｍ以下の混合粉体を取り出す工程、前
記粒径が100μｍ以下の混合粉体を落下させながら、該
混合粉体に、磁石により水平方向から磁場をかけ、前記
混合粉体に含まれた酸化物超電導粉体を該磁石とは反対
の水平方向に飛ばし、前記混合粉体に含まれた超電導を
示さない不純物をそのまま下方に落下させることによっ
て前記酸化物超電導粉体を分離する工程、および分離さ
れた酸化物超電導粉体をふるいにかけて粒径が１μｍ以
上のものを取り出す工程を有することを特徴とする酸化
物超電導体の製造方法。1. A step of obtaining a mixed powder containing oxide superconducting powder as a main component by mixing a plurality of kinds of raw materials at a predetermined ratio, firing and pulverizing the mixed powder, and sieving the mixed powder to obtain a particle size. Of a mixed powder having a particle size of 100 μm or less, a magnetic field is applied to the mixed powder from a horizontal direction by a magnet while dropping the mixed powder having a particle size of 100 μm or less, and the oxidation contained in the mixed powder is performed. Of separating the oxide superconducting powder by flying the superconducting powder in the horizontal direction opposite to the magnet, and dropping the impurities that do not show superconductivity contained in the mixed powder downward as they are, and separation. A method for producing an oxide superconductor, comprising a step of sieving the oxide superconducting powder thus prepared to remove particles having a particle size of 1 μm or more.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62221713A JPH0714494B2 (en) | 1987-09-03 | 1987-09-03 | Method for manufacturing oxide superconductor |
| PCT/JP1988/000549 WO1988009768A1 (en) | 1987-06-09 | 1988-06-08 | Method of producing oxide superconductor |
| EP88905217A EP0317643B1 (en) | 1987-06-09 | 1988-06-08 | Method of producing oxide superconductor |
| DE88905217T DE3880973T2 (en) | 1987-06-09 | 1988-06-08 | METHOD FOR PRODUCING OXIDE-BASED SUPER LADDERS. |
| US07/315,788 US5268353A (en) | 1987-06-09 | 1988-06-08 | Method for separating superconductor powder from nonsuperconductive powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62221713A JPH0714494B2 (en) | 1987-09-03 | 1987-09-03 | Method for manufacturing oxide superconductor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6463062A JPS6463062A (en) | 1989-03-09 |
| JPH0714494B2 true JPH0714494B2 (en) | 1995-02-22 |
Family
ID=16771100
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62221713A Expired - Fee Related JPH0714494B2 (en) | 1987-06-09 | 1987-09-03 | Method for manufacturing oxide superconductor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0714494B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0711138Y2 (en) * | 1987-11-11 | 1995-03-15 | 石川島播磨重工業株式会社 | Manufacturing equipment for ceramics superconductor materials |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0616864B2 (en) * | 1987-06-01 | 1994-03-09 | 株式会社半導体エネルギー研究所 | Selection method of oxide superconducting materials |
-
1987
- 1987-09-03 JP JP62221713A patent/JPH0714494B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6463062A (en) | 1989-03-09 |
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