CN1070760A - 高温超导体和其制备方法 - Google Patents

高温超导体和其制备方法 Download PDF

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CN1070760A
CN1070760A CN92108768A CN92108768A CN1070760A CN 1070760 A CN1070760 A CN 1070760A CN 92108768 A CN92108768 A CN 92108768A CN 92108768 A CN92108768 A CN 92108768A CN 1070760 A CN1070760 A CN 1070760A
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J·博克
E·普赖斯勒
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Alcatel superconductor Co.,Ltd.
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Naikesen superconducting Co.,Ltd.
Aventis Research and Technologies GmbH and Co KG
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Abstract

本发明涉及一种高温超导体，它由铋、锶、钙和铜 (有时还选用铅)的氧化物(其组成为Bi2-a+b+cPba (Sr，Ca)3-b-cCu2+dOx)以及硫酸锶和/或硫酸钡所组 成。制备所述的超导体时可以将铋、锶、钙和铜(有时 还选用铅)的氧化物，与硫酸锶和/或硫酸钡混合均 匀，将此混合物加热到870～1300℃使其熔融，硫酸 锶和/或硫酸钡含量高时，要求温度也较高，将熔融 倾入模子中慢慢固化，从模子中移出模制体使其在 700～900℃于含氧气氛中进行热处理。

Description

本发明是关于由铋、锶、钙、铜（有时还选用铅）的氧化物所组成的高温超导体和它的一种制备方法。
美国专利5，047，391揭示了制备高温超导体的一种方法这种超导体的组成为Bi2（Sr，Ca）3Cu2Ox，其中x＝8～10。在这个方法中，铋、锶、钙和铜的氧化物或碳酸盐的化学计量混合物被加热到870～1100℃，生成均匀的熔融物。将熔融物倒入模子并在其中固化。从模子中移出铸件于780-850℃热处理6～30小时，然后于600～830℃在氧气氛中处理至少6小时。用这个方法可将模制件制成片状，其边长或直径达到几个厘米，或制成棒形，长达50厘米，直径12毫米，在每一种情况下，模制体由单一相化合物组成。
所述类型的模制件在电技术中有许多应用，例如作电力输送的电流导体，作电流限制器以及构成磁屏蔽罩。但是，高温超导体在工业上使用的先决条件是在液氮温度（77K）具有约1000A/厘米2的临界电流密度。
确实，已知1厘米宽，15微米厚的载于银基片上组成为Bi2Sr2Ca Cu2Ox的带子具有1000安/厘米2的临界电流密度;但是这样的带子只能传导15安的绝对电流（参阅“Proceedings of the ICMC ’90 TopicalConference    on    Material    Aspects    of    High-Temperature    Superconductors”1991    Pages165    to    176）。这个绝对电流在薄膜的情况下甚至更低，而且讫今只可能生产几厘米尺寸的。
对以铋、锶、钙和铜的氧化物为基础的高温超导体材料制成的固体元件，已测得在77K时的电流密度数量级为102安/厘米2。
本发明的目的是提供一种基于铋、锶、钙、铜（有时还选用铅）的氧化物的高温超导体和它的制备方法。这种高温超导的临界电流密度在77K时至少1000A/厘米2，能传输至少100A的绝对电流。按照本发明的高温超导是由铋、锶、钙、铜（有时还选用铅）的氧化物（其组成为 Bi2-a+b+cPba（Sr，Ca）3-b-cCu2+dOx/式中a＝0～0.7;b+c＝0～0.5;d＝-0.1～0.1 x＝7～10，Sr∶Ca的比率为2.8∶1～1∶2.8）以及硫酸锶和/或硫酸钡所组成。
本发明的高温超导体可以在下面几个方面进一步改进：
a）a＝0;b+c＝0.25;d＝0;x＝7.9～8.5    Sr∶Ca比率从2.2∶1～1.5∶1;
b）硫酸锶含量是0.1～30%（重量），较好的是3～10%（重量）;
c）硫酸钡含量是0.1～20%（重量），较好的是3～10%（重量）。
本发明的高温超导体的制备方法可以包括把铋、锶、钙、铜（有时还选用铅）的氧化物与硫酸锶和/或硫酸钡混合均匀，加热到870-1300℃，较好的是900～1100℃;熔融此混合物;硫酸锶和/或硫酸钡的含量较高时，要求温度也较高。将熔融物倒入模子让它在其中慢慢固化，将从模子中移出的模制件在700～900℃，在含氧的气氛中进行热处理。较好的是750～870℃。
这个方法也可以设计成这样：
d）将熔融物倒入水平排列的园筒，园筒绕着它的纵轴旋转;
e）将熔融物倒入石英模子;
f）将熔融物倒入铜模子;
g）为了热处理，模制件很快地以250～350℃/小时的速率加热到700℃，高于700℃后缓慢地以5～20℃/小时的速率加热;
h）热处理在空气和氮的体积比为1∶1的气氛中进行;
i）在纯氧中进行热处理。
如果本发明的高温超导体由所谓的二层化合物（铋、锶、钙和铜的氧化物，其金属的化学计量比为2∶2∶1∶2）和硫酸锶的混合物组成，硫酸锶含量直到30%（重量）时还检测不到分解产物或其它相。
另一方面，本发明的高温超导体，它由所谓的二层化合物和硫酸钡组成，含有碱土金属铜酸盐相，例如（Sr，Ca）CuO2。
热分析研究表明，碱土金属硫酸盐与铋、锶、钙、铜（有时还选用铅）的氧化物一起熔融生成低共熔体。硫酸钡和硫酸锶的熔点，明确地说是相当地高，分别为1580和1600℃。
最后，陶瓷相的研究和用扫描电子显微镜得到的照片表明，在本发明的高温超导体中有10～100微米大小的硫酸锶和硫酸钡沉淀。
意想不到的是本发明的高温超导体，其临界湿度随着碱土金属硫酸盐的含量的增加不但不下降，在某些情况下甚至还上升。
本发明的高温超导体77K的临界电流密度约为1400A/厘米2，比先有技术中的高温超导体的值高几倍。
本发明的高温超导体的弯曲强度和弹性模量显示了令人满意的值。
本发明的高温超导体可以制成比较大的模制件，例如棒，板或园柱体，因为它们比起先有技术所制的模制件，它们脆性小，形成裂缝的倾向小。不但在熔融体固体时而且在模制件热处理的过程中都是这样。
例1（比较例）
将铋、锶、钙和铜的二元氧化物（金属的化学计算比为2∶2∶1∶2）充分混合。将1.8千克这样的混合物置于刚玉坩埚于1000℃转化成均匀的熔融体。将此均匀的熔融体通过槽口倒入直径为200毫米，深为100毫米水平排列的园柱形模子，这些模子绕着它的纵轴旋转，由于离心力的原因熔融体均匀地分布在模子的壁上。为了有利于较缓慢的冷却，在铸造后立即将一予热到600℃的管式炉推放在模子上，炉子以约2℃/分钟的速度冷却到室温。管式炉冷却后，在模子中的空心园柱体物有两条相对的相互垂直的裂缝，估计可能是严重的内在应力所致，将模制件从模子中取出时，它碎成两瓣。
例2（比较例）
重复例1，只是将1.5千克混合物转化为均匀的熔融体，在管式炉冷却后，将空心园柱体物从模子中取出，在每种情况下，它的上边和下边都有两条约1厘米长的相对的横向裂缝。
将空心的园柱体物进行热处理（750℃    24小时，850℃120小时）。热处理后，在横向裂缝的终端也形成纵向的裂缝，这些裂缝导致碎成环形断片。
例3（本发明）
重复例1，只是二元氧化物和10%（重量）硫酸锶充分混合，将2千克这种混合物加热到1050℃转化为均匀的熔融体。从模子中取出一个坚实的没有裂缝的空心园柱体，其壁厚约5毫米。
将此空心的园柱体进行热处理（750℃    24小时;850℃120小时），甚至经过这样的处理，空心园柱体仍无裂缝并且一点也没有熔开。
例4（本发明）
将例3的混合物熔融并倒入一侧封闭的石英管（内径8毫米），石英管长度为100，150，200，300，500毫米。
冷至室温后，固化的熔融体可从所有的石英管中取出，它们是坚实的、未见裂缝的棒。
将这些棒在空气/氮气混合物（体积比为1∶1）中加热，以300℃/小时的速率升温到700℃，再以10℃/小时的速率升温到850℃，在此温度保持60小时。为了确保一个尽可能均匀的温度场，热处理在多段式管式炉中进行。
所有这些棒冷却后从炉子中取出都没有裂缝。
200毫米长的棒装上触点用四点测量法，测定77K的临界电流密度为570安/厘米2·（尺度：1微伏/厘米），电位差触点之间的间隙为13厘米。
由电阻的温度依从关系测定得到电阻的总下降为89.5KΩ。
例5（比较例）
将例1的混合物熔融并倒入按照例4的各种石英管，这些石英管的一侧是封闭的。
冷到室温后，只能从100和150毫米长的石英管中取出坚实的棒，而其它的石英管中只有碎片。
例6（本发明）
铋、锶、钙和铜的二元氧化物，其金属的化学计量比为2∶2∶1∶2，与不同量的硫酸锶（0，3，6，10，15，20，25 30重量%）充分混合。不同的混合物在刚玉坩埚中于1000℃（SrSO4含量达10%），1030℃（SrSO4含量达20 20%），1100℃（SrSO4含量达30%）转化成均匀的熔融体，将每种熔融体倒入矩形铜模子中，其尺寸为15×15×60毫米3，顶部开口。为了让熔融体缓慢冷却，铸造后立即将模子放入予热到600℃的箱式炉中，然后关闭电源。
用钻石切割轮从所得的模制件切得4毫米厚的园片形样品和尺寸为45×4×3毫米3的棒。所有的样品和棒于850℃在箱式炉中一起敞空热处理24小时。
从园片形样品锯得截面积为1毫米2，长为10毫米的棒。测定这些棒的转变温度Tc和临界电流密度jc，而尺寸为45×4×3毫米3的棒则用来测定弯曲强度和弹性模量〔杨氏（Young′s）模量〕，结果总结于下表：
Figure 921087683_IMG1
例7（本发明）
重复例6，只是用硫酸钡代替硫酸锶。结果总结于下表：
Figure 921087683_IMG2
例8（比较例）
重复例6，只是用硫酸钙（无水）代替硫酸锶。结果总结于下表。
Figure 921087683_IMG3
除了所谓的二层化合物外，在X射线图中从CaSO4含量在4.4重量%以上的样品中已经辨认出一些外来的相。

Claims (11)

1、一种由铋，锶，钙，铜(有时还选用铅)的氧化物(它的组成为Bi2-a+b+cPba(Sr，Ca)3-b-cCu2+dOx
其中：a=0～0.7；b+c=0～0.5；d=-0.1～0.1；x=7～10；Sr∶Ca的比率为2.8∶1～1∶2.8以及硫酸锶和/或硫酸钡组成的高温超导体。
2、根据权利要求1的高温超导体，其特征在于a＝0;b+c＝0.25;d＝0和x＝7.9～8.5，以及Sr∶Ca的比率为2.2∶1～1.5∶1。
3、根据权利要求1或2的高温超导体，特征在于硫酸锶的含量为0.1～30重量%，较好的是3-10重量%。
4、根据权利要求1至3中至少一个权利要求的高温超导体，其特征在于硫酸钡的含量是0.1至20重量%，较好的是3～10重量%
5、根据权利要求1至4中至少一个权利要求的高温超导体的制备方法，它包括将铋、锶、钙、铜（有时还选用铅）的氧化物与硫酸锶和/或硫酸钡混合均匀，加热到870-1300℃，较好的是900-1100℃，使混合物熔融，硫酸锶和/或硫酸钡的含量较高时要求较高的温度，将熔融体倒入模子让其在其中慢慢固化，将从模子中取出的模制件在700-900℃，较好的是在750-870℃，于含氧的气氛中进行热处理。
6、根据权利要求5的方法，其特征在于把熔融体倒入绕其纵轴旋转的水平排列的圆筒中。
7、根据权利要求5或6的方法，其特征在于把熔融体倒入不英制的模子中。
8、根据权利要求5或6的方法，其特征在于把熔融体倒入铜制的模子中。
9、根据权利要求5至8中至少一个权利要求的方法，其特征在于热处理中，模制件以250至350℃/小时很快加热到700℃高于此温度时以5-20℃/小时慢慢加热。
10、根据权利要求5至9至少一个权利要求的方法，其特征在于热处理在空气和氮气的体积比为1∶1的气氛中进行。
11、根据权利要求5至9中至少一个权利要求的方法，其特征在于热处理在纯氧中进行。
CN92108768A 1991-07-26 1992-07-25 高温超导体和其制备方法 Expired - Fee Related CN1042272C (zh)

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CN1048706C (zh) * 1996-05-21 2000-01-26 浙江大学 单相性Bi2Sr2Ca2Cu3O10+δ高温超导体的分步合成方法

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DE4218950A1 (de) * 1992-06-10 1993-12-16 Hoechst Ag Verfahren zur Herstellung eines Hochtemperatursupraleiters und daraus gebildeter Formkörper
EP0611737B1 (de) * 1993-02-17 1999-05-12 Hoechst Aktiengesellschaft Verfahren zur Herstellung eines Hoch-Tc-Supraleiters als Precursormaterial für die Oxide Powder in Tube Methode (OPIT)
EP0646554A1 (de) * 1993-10-04 1995-04-05 Hoechst Aktiengesellschaft Massivteile aus Hochtemperatur-Supraleiter-Material
DE19803447A1 (de) * 1998-01-30 1999-09-16 Aventis Res & Tech Gmbh & Co Verfahren zur Herstellung von Precursormaterial für die Produktion von Hochtemperatursupraleiter-Drähten
CA2505501A1 (en) * 2004-05-04 2005-11-04 Nexans Method for mechanical stabilisation of tube-shaped superconducting ceramics and mechanically stabilised tube-shaped superconducting composite

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JPH01160861A (ja) * 1987-12-17 1989-06-23 Mitsubishi Electric Corp 超電導セラミクスの異方成長法
US4880771A (en) * 1988-02-12 1989-11-14 American Telephone And Telegraph Company, At&T Bell Laboratories Bismuth-lead-strontium-calcium-cuprate superconductors
DE68902853T2 (de) * 1988-03-21 1993-02-04 American Telephone & Telegraph Wachstum von supraleitermaterial aus einer flussmittel-schmelze, sowie fertigungsartikel.
DE3830092A1 (de) * 1988-09-03 1990-03-15 Hoechst Ag Verfahren zur herstellung eines hochtemperatursupraleiters sowie daraus bestehende formkoerper
US5157015A (en) * 1990-04-17 1992-10-20 Alfred University Process for preparing superconducting films by radio-frequency generated aerosol-plasma deposition in atmosphere
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US5059581A (en) * 1990-06-28 1991-10-22 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Passivation of high temperature superconductors

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* Cited by examiner, † Cited by third party
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CN1048706C (zh) * 1996-05-21 2000-01-26 浙江大学 单相性Bi2Sr2Ca2Cu3O10+δ高温超导体的分步合成方法

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CN1042272C (zh) 1999-02-24
EP0524442B1 (de) 1995-10-11
CA2073522A1 (en) 1993-01-27
ATE128956T1 (de) 1995-10-15
EP0524442A1 (de) 1993-01-27
JPH0735296B2 (ja) 1995-04-19
DE4124823A1 (de) 1993-01-28
KR930002278A (ko) 1993-02-22
DE59203963D1 (de) 1995-11-16
GR3017747T3 (en) 1996-01-31
KR100186833B1 (ko) 1999-04-15
ES2080991T3 (es) 1996-02-16
US5294601A (en) 1994-03-15
CA2073522C (en) 1998-07-21
JPH05194018A (ja) 1993-08-03

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