CN1290124C - 基于化合物MgB2的超导线和带的生产方法 - Google Patents

基于化合物MgB2的超导线和带的生产方法 Download PDF

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CN1290124C
CN1290124C CNB021077843A CN02107784A CN1290124C CN 1290124 C CN1290124 C CN 1290124C CN B021077843 A CNB021077843 A CN B021077843A CN 02107784 A CN02107784 A CN 02107784A CN 1290124 C CN1290124 C CN 1290124C
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克劳斯·菲舍尔
沃尔夫冈·哈斯勒
玛吉塔·舒泊特
汉斯－彼德·特林克斯
安德列亚斯·吉姆贝尔
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Abstract

本发明涉及以“粉末-在-管-技术”生产超导线和带的方法，其包括如下步骤：提供一普通导电材料的外管；向所述外管加入以下材料以形成结合物，a)含有完全反应的MgB2化合物的粉状超导化合物或b)含有由Mg、B以及反应的MgB2化合物构成的粉状机械合金混合物的粉状超导化合物初产品；或基于Mg与B粉的混合物的粉状超导化合物初产品；对该结合物进行重新成型和热处理。采用本发明的方法可生产高技术标准的基于MgB2化合物的超导线和带，它们可在能源技术领域被用作超导体。

Description

基于化合物MgB2的超导线和带的生产方法
技术领域
本发明涉及一种基于化合物MgB2的超导线和带的生产方法。该线和带特别适合于在能源技术领域用作超导体。
背景技术
最近在二元合金MgB2中首次证实了具有Tc＝38K至40K的超导体(J.Nagamatsu，N.Nagakawa，T.Muranaka，Y.Zenitani和J。Akamitsu，自然410(2001)，63)。
在一项实验中，借助在石英安培瓶中，在Mg-粉的存在时通过对硼-线进行热处理所产生的Mg向硼-线中的扩散，也生产出了一种MgB2-线(Canfield等人，在致密MgB2线中的超导性，Publ.Cond-matHomepage vom 15.02.01：cond-mat/0102289)。该方法不适合工业技术类线材的生产。
另外的MgB2-线的生产方法，例如采用一种紧密的材料，由于MgB2太脆看来也不可能。
发明内容
本发明的任务是给出一种生产方法，采用该法可生产基于MgB2的，长的，具有高电流密度载荷的超导线和带。
该任务可通过按照本发明的生产方法加以解决。
本发明提供一种以“粉末-在-管-技术”生产超导线和带的方法，其包括如下步骤：提供一普通导电材料的外管；向所述外管加入以下材料以形成结合物；a)含有完全反应的MgB2化合物的粉状超导化合物或b)含有由Mg、B以及反应的MgB2化合物构成的粉状机械合金混合物的粉状超导化合物初产品；或基于Mg与B粉的混合物的粉状超导化合物初产品；对该结合物进行重新成型和热处理。
本发明是基于已知的“粉末-在-管-技术”，在此通过将一普通导电材料的外管和一含有超导体的粉末或该化合物的初产品的结合物进行重新成型和热处理，生产出超导线和带。
按照本发明该加工会提供一结合物，该结合物中的外管内含有一粉状的超导性的MgB2-化合物，或一粉状的超导性的MgB2-化合物初产品，这里作为机械合金粉末的仅部分地被反应为MgB2-化合物的粉状的初产品，或作为由所期望的MgB2-化合物的单组份组成的粉末混合物被送入到外管中。
优点是，在使用一完全反应的MgB2-化合物或MgB2-初产品时，在它的晶格中会嵌入Al、Ag、Cu、Au、Sc、Y、Dy、Gd、Hf、Ti、Zr、Ta、V、Nb、Cr、Mo、Mn、Os、Ru、C、Si、N和/或O。
也可使用一仅由Mg-粉和B-粉组成的单组份的粉末混合物。
也可以使用由Mg-粉和B-粉以及一种或多种由Al、Ag、Cu、Au、Sc、Y、Dy、Gd、Hf、Ti、Zr、Ta、V、Nb、Cr、Mo、Mn、Os和Ru金属粉组成的单组份的粉末混合物。
按照本发明最好使用粉末，该粉末应具有一窄的平均粒子大小d＜10μm的颗粒分布，或应使用这样的粉末，该粉末中颗粒大小之比为5-10。
外管可由Cu、Ag、Ta、Nb、Mo、W、Fe或Mg或它们的合金构成。
在使用Mg-外管时，最好是将其用一个其它的由Fe，Nb或Ta构成的外管套起来。
按照本发明，为在结合物重新成型范围内对外管软化和/或由MgB2-初产品形成超导MgB2-化合物和/或超导MgB2-化合物在紧密的结合物中烧结，将在带低氧分压或少量还原性添加物，如H2的惰性气体中进行一次或多次温度介于300℃和1100℃间的热处理。
对外管软化的热处理在温度介于300℃和1100℃间进行。
对由一仅部分地被反应为MgB2-化合物的机械合金粉末构成的粉状初产品形成超导MgB2-化合物的热处理将在温度介于300℃和700℃间进行。
对由所期望MgB2-化合物的单组份粉末混合物构成的MgB2-初产品形成超导MgB2-化合物的热处理将在温度介于400℃和1000℃间进行。
超导MgB2-化合物在紧密的结合物中的烧结将在温度介于500℃和1000℃间进行。
为了使结合物紧密化，可使用温度＞500℃和压力＞2巴的热等静压法(HIP-处理)。
采用本发明的方法可生产高技术标准的基于MgB2化合物的超导线和带，它们可在能源技术领域被用作超导体。
具体实施方式
下面借助实施例子更详细的阐明本发明的生产方法。
例1
纯度为98％的MgB2粉在240Mpa的压力下冷均质压缩成一直径为8mm的圆杆。该杆放入一一端封闭的，内径为10mm壁厚为1mm的钽管中。再将该和钽管套在一起的MgB2杆插入一一端封闭的，内径为11mm壁厚为1mm的铜管中，它们的开口端在真空下同样进行封闭。然后借助锤子，轧辊和平辊将该制成的物体变形为一0.45mm厚和5.7mm宽的Cu/Ta/MgB2条，并将其在一Ar气-环境下900℃温度热处理一小时。该带的一块样品被测出具有一临界温度为33K和当外界电场为1.5T和4.2K时临界电流密度为5.1KA/cm2，当在自身场和4.2K时临界电流密度为20KA/cm2。
例2
为生产一机械合金Mg-B-粉，将一纯度为99.8％的Mg-粉和纯度为99.9％的非结晶硼粉按照化合物MgB2的化学计量成分比例混合，于一钨碳(WC)碾磨容器中在极纯Ar气-环境下，使用WC－球作为碾磨体在行星球磨中碾磨20个小时。所得到的粉末如例1所述制成一Cu/Ta/MgB2条。将该条在700℃ Ar气-环境下热处理20分钟。该带的一块样品被测出具有一临界温度为34K和当在自身场和4.2K时临界电流密度为25KA/cm2。

Claims (15)

1.以“粉末-在-管-技术”生产超导线和带的方法，其包括如下步骤：
提供一普通导电材料的外管；
向所述外管中加入以下材料以形成结合物，
a)含有完全反应的MgB2化合物的粉状超导化合物，或
b)含有由Mg、B以及反应的MgB2化合物构成的粉状机械合金混合物的粉状超导化合物初产品；或基于Mg与B粉的混合物的粉状超导化合物初产品；
对该结合物进行重新成型和热处理。
2.按照权利要求1的方法，其特征是使用了一完全反应的MgB2-化合物或MgB2-初产品，在它的晶格中会嵌入Al、Ag、Cu、Au、Sc、Y、Dy、Gd、Hf、Ti、Zr、Ta、V、Nb、Cr、Mo、Mn、Os、Ru、C、Si、N和/或O。
3.按照权利要求1的方法，其特征是使用一由Mg-粉和B-粉组成的粉末混合物。
4.按照权利要求1的方法，其特征是使用一由Mg-粉和B-粉以及一种或多种由Al、Ag、Cu、Au、Sc、Y、Dy、Gd、Hf、Ti、Zr、Ta、V、Nb、Cr、Mo、Mn、Os和Ru金属粉组成的粉末混合物。
5.按照权利要求1的方法，其特征是所使用的粉末应具有平均粒子大小d＜10μm的颗粒分布。
6.按照权利要求1的方法，其特征是所使用的粉末应具有两种不同颗粒大小的颗粒带，该颗粒带中的不同颗粒大小之比5-10。
7.按照权利要求1的方法，其特征是所使用的外管由Cu、Ag、Ta、Nb、Mo、W、Fe或Mg或它们的合金构成。
8.按照权利要求1的方法，其特征是在使用Mg-外管时，将其用一个其它的外管套起来。
9.按照权利要求8的方法，其特征是所述外管由Fe、Nb或Ta构成。
10.按照权利要求1的方法，其特征是为在结合物重新成型范围内对外管软化和/或由MgB2-初产品形成超导MgB2-化合物和/或超导MgB2-化合物在紧密的结合物中烧结，将在带氧分压或还原性添加物的惰性气体中进行一次或多次温度介于300℃和1100℃间的热处理。
11.按照权利要求10的方法，其特征是所述还原性添加物为H2。
12.按照权利要求10的方法，其特征是对由一仅部分地被反应为MgB2-化合物的机械合金粉末构成的粉状初产品形成超导MgB2-化合物的热处理将在温度介于300℃和700℃间进行。
13.按照权利要求10的方法，其特征是对由MgB2-化合物的单组分粉末混合物构成的MgB2-初产品形成超导MgB2-化合物的热处理将在温度介于400℃和1000℃间进行。
14.按照权利要求10的方法，其特征是超导MgB2-化合物在紧密的结合物中的烧结将在温度介于500℃和1000℃间进行。
15.按照权利要求10的方法，其特征是使用热等静压处理使结合物紧密化，在温度＞500℃和压力＞2巴下进行。
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