JPH01160875A - Setter for calcining oxide superconductor - Google Patents
Setter for calcining oxide superconductorInfo
- Publication number
- JPH01160875A JPH01160875A JP62320736A JP32073687A JPH01160875A JP H01160875 A JPH01160875 A JP H01160875A JP 62320736 A JP62320736 A JP 62320736A JP 32073687 A JP32073687 A JP 32073687A JP H01160875 A JPH01160875 A JP H01160875A
- Authority
- JP
- Japan
- Prior art keywords
- oxide superconductor
- setter
- firing
- fired
- 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.)
- Pending
Links
- 239000002887 superconductor Substances 0.000 title claims abstract description 93
- 238000001354 calcination Methods 0.000 title abstract 4
- 239000000203 mixture Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000010304 firing Methods 0.000 claims description 42
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 5
- 230000007547 defect Effects 0.000 claims description 4
- 230000002950 deficient Effects 0.000 claims description 4
- 229910052788 barium Inorganic materials 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 16
- 238000011109 contamination Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000843 powder Substances 0.000 description 14
- 239000011230 binding agent Substances 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000012778 molding material Substances 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- -1 Y203 Chemical class 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Abstract
Description
【発明の詳細な説明】
［発明の目的］
（産業上の利用分野）
本発明は、被焼成物に対して汚染などの悪影響をおよぼ
すことのない酸化物超電導体焼成用セツタに関する。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Industrial Field of Application) The present invention relates to a setter for firing oxide superconductors that does not have any adverse effects such as contamination on objects to be fired.
（従来の技術）
近年、Ｂａ−Ｌａ−Ｃｕ−０系の層状ベロアスカイト型
の酸化物が高い臨界温度を有する可能性のあることが発
表されて以来、各所で酸化物超電導体の研究が行われて
いる（Ｚ、Ｐｈｙｓ、Ｂ Ｃｏｎｄｅｎｓｅｄ Ｍａｔ
ｔｅｒ６４、１８９−１９３（１９８６））。その中で
もＹ−Ｂａ−Ｃｕ−０系で代表される酸素欠陥を有する
欠陥ペロブスカイト型（（ＬｎＢａ２Ｃｕ３Ｏ７−δ型
）（δは酸素欠陥を表し通常１以下、［ｎは、Ｙ 、
Ｌａ、 Ｓｃ、 Ｎｄ、 Ｓｍ、 Ｅｕ、 Ｇｄ、Ｄｙ
、 Ｎｏ、ＥｒｌＴｍ、 ＹｂおよびＬｔｌから選ばれ
た少なくとも１種の元素、Ｂａの一部はＳｒなどで置換
可能））の酸化物超電導体は、臨界温度が９０に以上と
液体窒素の沸点以上の高い温度を示すため非常に有望な
材料として注目されている（Ｐｈｙｓ、 Ｒｅｖ、 Ｌ
ｅｔｔ。(Prior art) In recent years, since it was announced that Ba-La-Cu-0-based layered velorskite oxides may have a high critical temperature, research on oxide superconductors has been conducted in various places. (Z, Phys, B Condensed Mat
ter64, 189-193 (1986)). Among them, a defective perovskite type ((LnBa2Cu3O7-δ type)) having oxygen vacancies represented by the Y-Ba-Cu-0 system (δ represents an oxygen defect and is usually 1 or less, [n is Y,
La, Sc, Nd, Sm, Eu, Gd, Dy
, No., ErlTm, Yb, and Ltl, a part of Ba can be replaced with Sr, etc.) The oxide superconductor has a critical temperature of 90 or higher, which is higher than the boiling point of liquid nitrogen. It is attracting attention as a very promising material because it exhibits high temperatures (Phys, Rev, L
ett.
Ｖｏｌ、５８ Ｎｏ、９，９０８−９１０）。Vol. 58 No. 9, 908-910).
このような酸化物超電導体は、結晶性の酸化物であるた
め、これらを超電導部材として利用する場合には、通常
のセラミックス部材と同様に、たとえば酸化物超電導体
粉末を用い、プレス成形法などによって作製した成形体
を、あるいは酸化物超電導体粉末に有機系バインダを添
加した混合物を用い、スリツプキせスティング法、削出
成形法、押出し成形法などの各種成形法によって作製し
た成形体を、固相で焼成することによって焼結体を作製
し、この酸化物超電導体焼結体を超電導部材として利用
することが試みられている。Since such oxide superconductors are crystalline oxides, when they are used as superconducting members, they can be used in the same way as ordinary ceramic members, such as by using oxide superconductor powder and press molding. The molded body produced by the method, or the molded body produced by various molding methods such as the slip-and-sting method, the extrusion molding method, and the extrusion molding method using a mixture of oxide superconductor powder and an organic binder, is hardened. Attempts have been made to produce a sintered body by firing the phase, and to utilize this oxide superconductor sintered body as a superconducting member.
ところで、このようにして酸化物超電導体の成形体を焼
成する際には、通常のセラミックス焼結体と同様、にセ
ツタ上に成形体を載置し、この状態で焼成炉内に配置し
て焼成している。この警戒用セツタとしては、現状では
アルミナセラミックス焼結体やジルコニアセラミックス
焼結体などの耐熱性に優れた部材が使用されている。By the way, when firing an oxide superconductor molded body in this way, the molded body is placed on a setter and placed in a firing furnace in the same way as a normal ceramic sintered body. It is being fired. Currently, members with excellent heat resistance such as alumina ceramic sintered bodies and zirconia ceramic sintered bodies are used as the warning setter.
（発明が解決しようとする問題点）
しかしながら、−Ｌ述したような讐成用セッタを使用し
て作製した酸化物超電導体焼結体においては、焼成中に
酸化物超電導体と焼成用セツタとがその界面で反応し、
１９られる酸化物超電導体焼結体が焼成用セツタの構成
成分によって汚染され、充分に超電導特性を発揮できな
いという問題が発生している。(Problems to be Solved by the Invention) However, in the oxide superconductor sintered body produced using the firing setter as described above, the oxide superconductor and the firing setter are separated during firing. reacts at the interface,
A problem has arisen in that the oxide superconductor sintered body produced in the sintered body is contaminated by the constituent components of the firing setter, and cannot exhibit sufficient superconducting properties.
本発明はこのような従来の問題点を解決するためになさ
れたもので、酸化物超電導体に対して汚染などの悪影響
をおよぼすことのない酸化物超電導体焼成用セツタを提
供することを目的とする。The present invention was made to solve these conventional problems, and an object of the present invention is to provide a setter for firing oxide superconductors that does not have any adverse effects such as contamination on oxide superconductors. do.
［発明の構成］
〈問題点を解決するための手段）
本発明の酸化物超電導体焼成用セックは、酸化物超電導
体または加熱により前記酸化物超電導体となる混合物を
含有する被焼成物の前記酸化物ｉＩ！１電導体と実質的
に同一組成を有する酸化物超電導体が、少なくとも前記
被焼成物の載置面に存在していることを特徴としている
。[Structure of the Invention] <Means for Solving the Problems] The SEC for sintering an oxide superconductor of the present invention is a method for firing an oxide superconductor or a mixture that becomes the oxide superconductor by heating. Oxide II! The present invention is characterized in that an oxide superconductor having substantially the same composition as the one conductor is present at least on the mounting surface of the object to be fired.
酸化物超電導体としては、多数のものが知られているが
、臨界温度の高い、希土類元素含有のペロブスカイト型
の酸化物超電導体の使用が実用的効果が高い。ここでい
う希土類元素を含有しペロブスカイト型構造を有する酸
化物超電導体としては、超電導状態を実現できるもので
あればよく、たとえばＬｎＢａ２Ｃｕ３Ｏ７−δ系（Ｌ
ｎはＹｌＬａ、 ＳＣ。Although a large number of oxide superconductors are known, the use of perovskite-type oxide superconductors containing rare earth elements, which have a high critical temperature, have a high practical effect. The oxide superconductor containing a rare earth element and having a perovskite structure may be any material as long as it can realize a superconducting state, such as LnBa2Cu3O7-δ (LnBa2Cu3O7-δ system).
n is YlLa, SC.
Ｎｄ１５ｍ、 Ｅｕ、 Ｇｄ１Ｄｙ１Ｎｏ、 Ｅｒ、
Ｔｍ、 ＹｂＸＬｕ等の希土類元素から選ばれた少なく
とも１種の元素を、δは酸素欠陥を表し通常１以下の数
、Ｂａの一部はＳｒ、 Ｃａなどで、Ｃｕの一部はＴｉ
、 Ｖ 、 Ｃｒ、 Ｈｎ、 ｒｅ、Ｃｏ、 Ｎｉ、
Ｚｎなどで置換可能。）などの酸素欠陥を有する欠陥ペ
ロブスカイト型、５ｒ−Ｌａ−Ｃｕ−０系などの層状ペ
ロブスカイト型などの広義にペロブスカイト型を有する
酸化物が例示される。なお希土類元素は広義の定ＧＱと
し、ｓｃ、 ｙおよびＬａ系をＳむものとする。代表的
な系としてＹ−Ｂａ−Ｃｕ−０系のほかに、ＹをＥｕ、
Ｄｙ、 ｌｌｏ、’Ｅｒ、 Ｔｍ、 Ｙｂ、 Ｌｕな
どの希土類で置換した系、５ｃ−Ｂａ−Ｃｕ−０系、５
ｒ−Ｌａ−Ｃｕ−０系、さらにＳｒをＢａ、’Ｃａで置
換した系などが挙げられる。Nd15m, Eu, Gd1Dy1No, Er,
At least one element selected from rare earth elements such as Tm and YbXLu, δ represents an oxygen defect and is usually a number of 1 or less, a part of Ba is Sr, Ca, etc., and a part of Cu is Ti.
, V, Cr, Hn, re, Co, Ni,
Can be replaced with Zn, etc. Examples include oxides having a perovskite type in a broad sense, such as a defective perovskite type having oxygen defects such as ), and a layered perovskite type such as a 5r-La-Cu-0 system. Note that rare earth elements are defined as GQ in a broad sense, and sc, y, and La systems are defined as S. In addition to the Y-Ba-Cu-0 system, representative systems include Y for Eu,
Dy, llo, 'Er, Tm, Yb, system substituted with rare earth elements such as Lu, 5c-Ba-Cu-0 system, 5
Examples include the r-La-Cu-0 system and systems in which Sr is replaced with Ba or 'Ca.
このような酸化物超電導体は、たとえば以下のようにし
て作製する。Such an oxide superconductor is produced, for example, as follows.
まず、Ｙ 、 Ｂａ、 Ｃｕなどのペロブスカイト型酸
化物超電導体の構成元素を十分混合する。混合の際には
、Ｙ２０３ 、ＢａＣＯ３、ＣｕＯなどの酸化物や炭酸
塩を原料として用いることができるほか、他の焼成後酸
化物に転化する硝酸塩、水酸化物などの化合物を用いて
もよい。さらには共沈法などで得たシュウ酸塩などを用
いてもよい。次いで、前述の原料を十分に混合した後、
８５０〜９８０℃程度の温度で焼成して結晶化させ、こ
の焼成物を粉砕して酸化物超電導体粉末を作製する。First, the constituent elements of the perovskite oxide superconductor, such as Y, Ba, and Cu, are thoroughly mixed. At the time of mixing, oxides and carbonates such as Y203, BaCO3, and CuO can be used as raw materials, and other compounds such as nitrates and hydroxides that are converted into oxides after firing may also be used. Furthermore, oxalate obtained by a coprecipitation method or the like may also be used. Then, after thoroughly mixing the aforementioned raw materials,
The fired product is crystallized by firing at a temperature of about 850 to 980°C, and the fired product is pulverized to produce an oxide superconductor powder.
次に、この酸化物超電導体粉末または上述した酸化物超
電導体の原料となる混合粉末を用いて、プレス成形法な
どによって成形体を作製するか、あるいはこれらに有機
系バインダを添加・混合し、この混合物に必要に応じて
各種添加剤や分散媒などをさらに加え、プレス成形法、
射出成形法、スリップキャスティング法などの各種成形
手段によって成形体を作製する。Next, using this oxide superconductor powder or the mixed powder that is the raw material for the oxide superconductor described above, a molded body is produced by a press molding method or the like, or an organic binder is added and mixed therein, Various additives and dispersion media are further added to this mixture as necessary, and press molding is performed.
A molded body is produced by various molding methods such as injection molding and slip casting.
次いで、有機系バインダを含有する成形体は、所定の温
度で脱脂した後に、所定の温度で焼成して酸化物超電導
体焼結体を作製する。さらにこの後、この焼成工程に引
続いて、あるいは別工程として酸素を充分に供給するこ
とが可能な雰囲気中で３Ｏ０℃〜７００℃程度の温度条
件で数時間程度保持するか、または同様な雰囲気中で３
Ｏ０℃程度まで徐冷することにより超電導特性を向上さ
せて、目的とする酸化物超電導体が得られる。Next, the molded body containing the organic binder is degreased at a predetermined temperature and then fired at a predetermined temperature to produce an oxide superconductor sintered body. Furthermore, following this firing step or as a separate step, the temperature is maintained at a temperature of about 300°C to 700°C for several hours in an atmosphere where oxygen can be sufficiently supplied, or in a similar atmosphere. 3 inside
The superconducting properties are improved by slow cooling to about 00°C, and the desired oxide superconductor can be obtained.
本発明の酸化物超電導体焼成用セツタは、下記の組成物
のいずれかにより形成したもの、あるいは、下記の組成
物のいずれかを、たとえばアルミナセラミックスやジル
コニアセラミックスのような耐熱性部材を母材として、
これらの表面層として有しているものである。The setter for sintering oxide superconductors of the present invention is made of one of the following compositions, or one of the following compositions is used as a base material of a heat-resistant member such as alumina ceramics or zirconia ceramics. As,
It has as a surface layer of these.
■ 被焼成物である酸化物超電導体成形体または脱脂体
、あるいは前述した酸化物超電導体の原料となる混合物
の成形体または脱脂体と同一の焼成工程を経て実質的に
同一組成の酸化物超電導体焼結体となる酸化物超電導体
未焼結体。■ Oxide superconductors with substantially the same composition through the same firing process as the oxide superconductor molded or degreased body that is the object to be fired, or the molded body or degreased body of the mixture that is the raw material for the oxide superconductor mentioned above. An oxide superconductor unsintered body that becomes a sintered body.
■ 被焼成物である酸化物超電導体成形体または脱脂体
、あるいは前述した酸化物超電導体の原料となる混合物
の成形体または脱脂体の焼成後の組成と実質的に同一・
な組成を有する酸化物超電導体焼結体。■ The composition after firing of the oxide superconductor molded body or degreased body that is the object to be fired, or the molded body or degreased body of the mixture that is the raw material for the oxide superconductor mentioned above.
An oxide superconductor sintered body with a composition of
■ 被焼成物である酸化物超電導体焼結体と実質的に同
一な組成を有する酸化物超電導体焼結体。■ An oxide superconductor sintered body having substantially the same composition as the oxide superconductor sintered body to be fired.
なお、これらにおいて、たとえば被焼成物がＹ−Ｂａ−
Ｃｕ−０系の酸化物超電導体の場合には、このＹの一部
を他の希土類元素で置換したもののような、実質的に性
質や特性が同様なものであれば使用可能である。In addition, in these, for example, the object to be fired is Y-Ba-
In the case of a Cu-0-based oxide superconductor, it is possible to use one having substantially similar properties and characteristics, such as one in which a portion of Y is replaced with another rare earth element.
前述したように、酸化物超電導体の製造工程においては
、その製造工程の差によっていくつかの焼成処理が存在
しており、その被焼成物の焼成過程と同一の焼成過程を
経て実質的に同一な組成を有する焼成物となる組成物を
使用することが好ましい。たとえば、有機系バインダを
含有する成形体を脱脂・焼成する際には、それと同一の
成形体を用いることが好ましが、酸化物超電導体焼結体
を使用することも可能である。また、焼成時には被焼成
物と焼成用セツタとの間に、同一組成の酸化物超電導体
粉末を敷粉として使用することも好ましい。As mentioned above, in the manufacturing process of oxide superconductors, there are several firing processes depending on the manufacturing process. It is preferable to use a composition that yields a fired product having a specific composition. For example, when degreasing and firing a molded body containing an organic binder, it is preferable to use the same molded body, but it is also possible to use an oxide superconductor sintered body. Further, during firing, it is also preferable to use oxide superconductor powder of the same composition as a bedding powder between the object to be fired and the setter for firing.
また、本発明の酸化物超電導体焼成用セツタの形状とし
ては、被焼成物が載置可能な形状であればどのような形
状であってもよいが、特に焼成時の雰囲気の通過孔を有
するもの、たとえば貫通孔を有するものや多孔質なもの
が好ましい。これによって、たとえば酸素アニールの際
に被焼成物に対して酸素を均一に供給することができる
などの効果が得られる。Further, the shape of the setter for sintering an oxide superconductor of the present invention may be any shape as long as the object to be fired can be placed thereon, but in particular, the setter may have any shape as long as the object to be fired can be placed thereon. For example, a material having through holes or a porous material is preferable. As a result, effects such as being able to uniformly supply oxygen to the object to be fired can be obtained during oxygen annealing, for example.
（作 用）
本発明の酸化物超電導体焼成用セツタは、被焼成物と実
質的に同一組成の酸化物超電導体からなるものであるこ
とから、焼成時に被焼成物である酸化物超電導体を汚染
することがない。また、特に被焼成物の焼成過程と同一
の焼成過程を経て実質的に同一組成となるものであれば
、焼成時における加熱収縮率が同一であるため、被焼成
物側に歪みを生じさせることもなく、さらに焼成物の特
性を向上させることが可能である。(Function) The setter for firing an oxide superconductor of the present invention is made of an oxide superconductor having substantially the same composition as the object to be fired. No contamination. In addition, especially if the material has substantially the same composition through the same firing process as the firing process, the heat shrinkage rate during firing will be the same, so distortion will not occur in the fired product. Therefore, it is possible to further improve the properties of the fired product.
（実施例） 次に、本発明の実施例について説明する。(Example) Next, examples of the present invention will be described.
実施例１
まず、それぞれ粒径１〜５μｍとしたＢａＣ０３粉末２
ｍ０１、Ｙ２Ｏ３粉末０．５ｍｏｆ 、ＣｕＯ粉末３ｍ
ｏｌを十分混合して大気中９００℃で４８時間焼成した
後に粉砕して、欠陥ペロブスカイト型の酸化物超電導体
粉末を得た。Example 1 First, BaC03 powder 2 each having a particle size of 1 to 5 μm was prepared.
m01, Y2O3 powder 0.5mof, CuO powder 3m
The mixture was thoroughly mixed with 100 ml of ol, fired at 900° C. for 48 hours in the air, and then pulverized to obtain a defective perovskite-type oxide superconductor powder.
次に、この酸化物超電導体粉末９１重量％とバインダ成
分としてパラフィン３重量％とを充分に混合し、この混
合物を成形材料として用い、プレス成形法によって５０
＋ｕ＋ｘ ５０ｍｎ＋ｘ厚さ５ｍｍの板状成形体を作製
し、これに直径５ｍｍの貫通孔を多数形成して焼成用セ
ックとした。Next, 91% by weight of this oxide superconductor powder and 3% by weight of paraffin as a binder component were thoroughly mixed, this mixture was used as a molding material, and a 50%
+u+x A plate-shaped molded body having a thickness of 50 mm and a thickness of 5 mm was prepared, and a large number of through holes each having a diameter of 5 mm were formed therein to obtain a firing stock.
一方、前述の酸化物超電導体粉末を用いて、この酸化物
超電導体粉末９７重量％とバインダ成分としてパラフィ
ン３重量％とを充分に混合し、この混合物を成形材料と
して用い、射出成形法によって外径２９ＩＩＩＩＢ×内
径１０１１１１１１ Ｘ厚さ５＋ｎｍの被焼成物となる
円管状の成形体を作製した。On the other hand, using the above-mentioned oxide superconductor powder, 97% by weight of this oxide superconductor powder and 3% by weight of paraffin as a binder component were thoroughly mixed, and this mixture was used as a molding material and extruded by injection molding. A cylindrical molded body having a diameter of 29IIIB×inner diameter of 10111111×thickness of 5+nm was prepared to serve as an object to be fired.
次に、この成形体を、上記焼成用セツタ上に前述の酸化
物超電導体粉末を介して載置し、これを焼成炉内に設置
して、この焼成炉内に２℃／分〜３β／分で空気を供給
しながら、５５０℃まで１０℃／分で昇温し、この温度
で１時間保持して脱脂処理を行った。続いて９３Ｏ℃ま
で昇温し、この温度で酸素ガスを供給しながら３Ｏ時間
保持して焼結させた。この後、３Ｏ０℃まで酸素ガスを
供給しながら徐冷し、目的とする酸化物超電導体を得た
。Next, this molded body was placed on the above-mentioned firing setter with the oxide superconductor powder interposed therebetween, and this was placed in a firing furnace where it was heated at 2°C/min to 3β/min. The temperature was raised to 550° C. at a rate of 10° C./min while supplying air at a rate of 10° C./min, and this temperature was maintained for 1 hour to perform a degreasing treatment. Subsequently, the temperature was raised to 930° C., and sintering was carried out by maintaining this temperature for 30 hours while supplying oxygen gas. Thereafter, the mixture was slowly cooled to 300° C. while supplying oxygen gas to obtain the desired oxide superconductor.
このようにして得た酸化物超電導体をＥ ＰＭＡおよび
ＩＣＰ発光分光分析したところ、汚染もなく、また歪み
の発生も認められなかった。また、この酸化物超電導焼
結体の超電導特性を測定したところ、臨界温度９３Ｋ、
臨界電流密度５００Ａ／ｃ７と良好な結果が得られた。When the oxide superconductor thus obtained was subjected to EPMA and ICP emission spectroscopic analysis, no contamination and no distortion was observed. In addition, when we measured the superconducting properties of this oxide superconducting sintered body, we found that the critical temperature was 93K,
Good results were obtained with a critical current density of 500 A/c7.
実施例２
実施例１で作製した未焼結の焼成用セツタを、５５０℃
× １時間＋９３Ｏ℃×３Ｏ時間の条件で焼成して、こ
の実施例の焼成用セツタとした。Example 2 The unsintered firing setter produced in Example 1 was heated to 550°C.
The setter for firing of this example was obtained by firing under the conditions of × 1 hour + 930° C. × 30 hours.
次いで、この焼成用セック上に実施例１で作製した被焼
成物となる酸化物超電導体の成形体を載置し、実施例１
と同一条件で焼成して酸化物超電導体を作製した。Next, the molded body of the oxide superconductor produced in Example 1 to be the object to be fired was placed on this baking sheet, and the molded body of Example 1 was placed.
An oxide superconductor was produced by firing under the same conditions as above.
このようにして得た酸化物超電導体についても、汚染も
なく、超電導特性に優れたものであった。The oxide superconductor thus obtained was also free of contamination and had excellent superconducting properties.
［発明の効果］
以上の説明したように本発明の酸化物超電導体焼成用セ
ックによれば、焼成時にセックの構成成分による酸化物
超電導体の汚染もなく、また特に被焼成物と同一工程を
経て実質的に同一組成の焼成物となるものを使用するこ
とによって、焼成時における加熱収縮による歪みの発生
もなく、超電導特性に優れた酸化物超電導体が得られる
。[Effects of the Invention] As explained above, according to the SEC for firing an oxide superconductor of the present invention, there is no contamination of the oxide superconductor by the constituent components of the SEC during firing, and in particular, the same process as that of the object to be fired is performed. By using a fired product that has substantially the same composition over time, an oxide superconductor with excellent superconducting properties can be obtained without distortion due to heat shrinkage during firing.
出願人 株式会社 東芝 代理人 弁理士 須 山 佐 −Applicant: Toshiba Corporation Agent Patent Attorney Suyama Sa
Claims (8)
導体となる混合物を含有する被焼成物の前記酸化物超電
導体と実質的に同一組成を有する酸化物超電導体が、少
なくとも前記被焼成物の載置面に存在している酸化物超
電導体焼成用セツタ。(1) An oxide superconductor having substantially the same composition as the oxide superconductor of the to-be-fired object containing an oxide superconductor or a mixture that becomes the oxide superconductor by heating is at least A setter for firing oxide superconductor located on the mounting surface.
たは脱脂体、あるいは前記酸化物超電導体となる混合物
の成形体または脱脂体と同一の焼成工程を経て実質的に
同一組成の酸化物超電導体焼結体となる酸化物超電導体
未焼結体が、少なくとも前記被焼成物の載置面に存在し
ている特許請求の範囲第１項記載の酸化物超電導体焼成
用セッタ。(2) An oxide having substantially the same composition through the same firing process as the oxide superconductor molded body or degreased body that is the article to be fired, or the molded body or degreased body of the mixture that becomes the oxide superconductor. The setter for sintering an oxide superconductor according to claim 1, wherein the oxide superconductor unsintered body that becomes the superconductor sintered body is present at least on the mounting surface of the object to be fired.
たは脱脂体、あるいは前記酸化物超電導体となる混合物
の成形体または脱脂体の焼成後の組成と実質的に同一な
組成を有する酸化物超電導体焼結体が、少なくとも前記
被焼成物の載置面に存在している特許請求の範囲第１項
記載の酸化物超電導体焼成用セッタ。(3) Oxidation having a composition that is substantially the same as the composition after firing of the oxide superconductor molded body or degreased body that is the object to be fired, or the molded body or degreased body of the mixture that becomes the oxide superconductor. The setter for firing an oxide superconductor according to claim 1, wherein the sintered body of the oxide superconductor is present at least on the mounting surface of the object to be fired.
実質的に同一な組成を有する酸化物超電導体焼結体が、
少なくとも前記被焼成物の載置面に存在している特許請
求の範囲第１項記載の酸化物超電導体焼成用セッタ。(4) An oxide superconductor sintered body having substantially the same composition as the oxide superconductor sintered body that is the object to be fired,
The setter for firing an oxide superconductor according to claim 1, wherein the setter is present at least on the mounting surface of the object to be fired.
し第４項のいずれか１項記載の酸化物超電導体焼成用セ
ッタ。(5) A setter for firing an oxide superconductor according to any one of claims 1 to 4, which has air passage holes.
ロブスカイト型の酸化物超電導体である特許請求の範囲
第１項ないし第５項のいずれか１項記載の酸化物超電導
体焼成用セッタ。(6) The setter for firing an oxide superconductor according to any one of claims 1 to 5, wherein the oxide superconductor is a perovskite-type oxide superconductor containing a rare earth element.
Ｃｕを原子比で実質的に１：２：３の割合で含有する特
許請求の範囲第１項ないし第５項のいずれか１項記載の
酸化物超電導体焼成用セッタ。(7) The oxide superconductor according to any one of claims 1 to 5, wherein the oxide superconductor contains rare earth elements, Ba and Cu in an atomic ratio of substantially 1:2:3. A setter for firing oxide superconductors.
＿７＿−＿δ（Ｌｎは希土類元素から選ばれた少なくと
も１種の元素を、δは酸素欠陥を表す。）で示される酸
素欠陥型ペロブスカイト構造を有する特許請求の範囲第
１項ないし第５項のいずれか１項記載の酸化物超電導体
焼成用セッタ。(8) The oxide superconductor is LnBa_2Cu_3O
Any one of claims 1 to 5 having an oxygen-deficient perovskite structure represented by _7_-_δ (Ln represents at least one element selected from rare earth elements, and δ represents an oxygen defect). The setter for firing an oxide superconductor according to item 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62320736A JPH01160875A (en) | 1987-12-18 | 1987-12-18 | Setter for calcining oxide superconductor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62320736A JPH01160875A (en) | 1987-12-18 | 1987-12-18 | Setter for calcining oxide superconductor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01160875A true JPH01160875A (en) | 1989-06-23 |
Family
ID=18124730
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62320736A Pending JPH01160875A (en) | 1987-12-18 | 1987-12-18 | Setter for calcining oxide superconductor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01160875A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2744715A1 (en) * | 1996-01-05 | 1997-08-14 | Univ Princeton | PROCESS FOR PRODUCING CERAMIC SUPERCONDUCTING MONOCRYSTALS |
-
1987
- 1987-12-18 JP JP62320736A patent/JPH01160875A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2744715A1 (en) * | 1996-01-05 | 1997-08-14 | Univ Princeton | PROCESS FOR PRODUCING CERAMIC SUPERCONDUCTING MONOCRYSTALS |
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