CN102498528B - 铁系超导电线材及其制造方法 - Google Patents
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 193
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 97
- 238000004519 manufacturing process Methods 0.000 title claims description 11
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- 229910018219 SeTe Inorganic materials 0.000 description 6
- FESBVLZDDCQLFY-UHFFFAOYSA-N sete Chemical compound [Te]=[Se] FESBVLZDDCQLFY-UHFFFAOYSA-N 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 4
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Abstract
本发明提供一种铁系超导电线材,其在主要由铁形成的筒状体的内部生成将形成筒状体的铁作为化学成分元素之一的铁系超导电体。
Description
技术领域
本发明涉及使用了以铁为主要成分的铁系超导电体的铁系超导电线材及其制造方法。
背景技术
2008年初发现铁系超导电体(非专利文献1)。以该发现为契机,在类似化合物中陆续发现超导电体,期待铁系超导电体成为新的高温超导电体的矿脉。
另外,铁系超导电体的临界电流密度及临界磁场高,应用性上也有高的期待。本发明者们开发了其中具有最简单构造的FeSe、FeTe、FeSe1-xTex(0<x<1)、FeTe1-xSx(0<x<1)等(例如非专利文献2-3)。另外,已知Fe和硫属化合物的摩尔比中Fe若干过量。这些铁系超导电体由于毒性比较弱、构造简单等,因此认为适于应用化。
非专利文献1:J.Am.Chem.Soc.,130,3296(2008)
非专利文献2:Appl.Phys.Lett.,94,012503(2009)
非专利文献3:Appl.Phys.Lett.,93,152505(2008)
发明内容
发明要解决的问题
本发明的课题在于,实现这样的铁系超导电体的实用性的开发,提供使用了FeSe、FeTe、FeSe1-xTex(0<x<1)、FeTe1-xSx(0<x<1)等铁系超导电物质的铁系超导电线材及其制造方法。
用于解决问题的手段
为了实现所述课题,本发明的铁系超导电线材的特征在于,在主要由铁形成的筒状体的内部生成将形成筒状体的铁作为化学成分元素之一的铁系超导电体。
该铁系超导电线材中,优选筒状体为超导电线材的覆盖物。
另外,该铁系超导电线材中,优选铁系超导电体的化学组成为FeSe、FeTe、FeSe1-xTex(0<x<1)或FeTe1-xSx(0<x<1)中的任一种。
另外,该铁系超导电线材中,也可以将多条铁系超导电线材一体化而形成多芯线。
本发明提供一种铁系超导电线材的制造方法,其特征在于,向主要由铁形成的筒状体的内部装填铁以外的构成铁系超导电体的化学成分元素即原料物质后,进行机械加工,进行线材化,在100-1000℃下进行1分钟-500小时的加热处理,使形成筒状体的铁和装填于筒状体的内部的原料物质发生反应,生成铁系超导电体,得到铁系超导电线材。
发明效果
根据本发明的铁系超导电线材及其制造方法,通过使用主要由铁形成的筒状体,并向其内部装填构成铁系超导电体的其它的原料物质,能够简单地制作铁系超导电线材,铁系超导电线材的超导电特性稳定地显现。
附图说明
图1是表示实施例中(a)轧制后、(b)加热处理后的线材的照片;
图2是表示实施例中制作的FeSe1-xTex(0<x<1)超导电线材的电流-电压特性的图;
图3是拍摄实施例中制作的FeSe1-xTex(0<x<1)超导电线材的剖面的光学显微镜照片;
图4是实施例中制作的FeSe1-xTex(0<x<1)超导电线材的扫描电子显微镜像;
图5是表示实施例中制作的FeSe1-xTex(0<x<1)超导电线材的剖面的面映像结果的照片。
具体实施方式
本发明的铁系超导电线材中,使用主要由铁形成的筒状体,通过形成该筒状体的铁和向筒状体的内部装填且构成铁系超导电体的铁以外的化学成分元素即原料物质生成铁系超导电体。即,在主要由铁形成的筒状体的内部生成将形成筒状体的铁作为化学成分元素之一的铁系超导电体。
筒状体为了助于铁系超导电体的生成而主要由铁形成,只要不阻碍铁系超导电体的生成,则筒状体可以含有铁以外的添加物、不可避免的杂质。例如允许Hexagonal相、Pyrite相、银、氧化铁、铋等的添加。
本发明的铁系超导电线材中铁系超导电体作为其化学组成,主要示例目前为止开发的FeSe、FeTe、FeSe1-xTex(0<x<1)、FeTe1-xSx(0<x<1)等,但只要可线材化,则化学组成就没有特别限制。
另一方面,构成铁系超导电体的化学成分元素的组成比可以适当变更。例如FeSe1-xTex(0<x<1)、FeTe1-xSx(0<x<1)中的Se和Te的比率、Te和S的比率等在0<x<1的范围内可以适当变更。
主要由铁形成的筒状体也可以起到作为超导电线材的覆盖物的功能及作用。
装填于筒状体的铁以外的元素原料中可以使用Se、Te、或S的单体或混合体、或SeTe等的预先合成的化合物。
本发明的铁系超导电线材的制造方法在下面示例。
1)向主要由铁形成的筒状体的内部装填构成铁系超导电体的铁以外的化学成分元素即原料物质。
2)进行轧制等机械性的加工,进行线材化。
3)在100-1000℃下进行1分钟-500小时的加热处理生成铁系超导电体。
在筒状体的内部装填的原料物质使用预先合成的SeTe及TeS的情况下,对抑制热处理时的Se及S的蒸发有效。
另外,加热处理通过在惰性气氛中的密闭状态下进行而能够有效地抑制Se及S的扩散。
另外,由于导入钉扎中心,因此可以在不阻碍超导电特性的程度下向装填于筒状体内部的SeTe等铁以外的原料物质中配合添加物,例如Hexagonal相、Pyrite相、银、氧化铁、铋等。
本发明通过在利用通电试验观察铁系超导电线材的临界电流上初步成功而完成,可在今后的铁系超导电体的线材化上赋予强大的技术性的方针。例如,可实现将铁系超导电线材的多数条一体化而形成多芯线的多芯铁系超导电线材。
线材的试制使用Powder-in-Tube法进行。使用外径6mm、内径3.5mm的铁制管作为覆盖物,在其内部装填Se或预先合成的SeTe,并将铁制管的两端密封。然后,使用槽辊轧制至外径为2mm,进而使用平辊轧制成宽度4-5mm、厚度0.55mm左右。将得到的线材切断成4cm左右,并将该短尺寸的线材在氩气气氛中(等同于环境压)封入石英管中。而且,在表1表示的条件下进行加热处理。加热温度为450-550℃。加热时间若包含升温时间则为3-4小时。加热处理后,通过通电试验进行电压-电流测定,估计临界电流(Ic)。
图1(a)是表示向铁制管(覆盖物)的内部装填SeTe粉末并进行轧制的烧成前的线材的照片,图1(b)是表示在氩气气氛中加热处理的烧成后的线材的照片。
另外,用于铁以外的原料物质的SeTe为将Se和Te按1∶1摩尔比计量,将其真空封入石英管的内部后在500℃下烧成8小时,由此合成,之后粉碎而成的物质。
另外,Se及Te中使用下面的物质。
Se为高纯度化学公司制造的Se粉末,纯度99.9%以上,平均粒径为75μm。
Te为高纯度化学公司制的Te粉末,纯度99.9%,平均粒径为150μm。
【表1】
如图2中所示的试样1及试样2所示,对在表1所示的实验No.1及No.2的条件下烧成并制作的FeSe1-xTex(0<x<1)线材(试样1与实验No.1对应,试样2与实验No.2对应),至某一定电流为止确认零电阻状态,将阈值设为0.1μV成功地估计临界电流。实现铁系超导电线材。
研磨线材的剖面,通过光学显微镜及SEM(Scanning ElectronMicroscope)进行剖面的观察,另外,使用EDX(Energy Dispersive X-rayspectroscopy)进行元素的面映像。
图3是拍摄将在表1所示的实验No.1的条件下制作的线材埋入树脂中并进行了研磨后的线材的剖面的光学显微镜照片。图4是在表1所示的实验No.1的条件下制作的线材的剖面的扫描电子显微镜图像。图5是在表1所示的实验No.1的条件下制作的线材的剖面的利用EDX(EnergyDispersive X-ray spectroscopy)的面映像。使用Fe-Kα线、Se-Lα线、及Te-Lα线进行分析。确认在铁覆盖物的内部生成化学组成FeSe1-xTex(0<x<1)即铁系超导电体。
在与表1所示的实验No.1及实验No.2一样的条件下能够制作化学组成为FeSe、FeTe1-xSx(0<x<1)的铁系超导电线材。FeTe1-xSx(0<x<1)超导电线材的制作中,使Te与S预先反应并合成,将变更其组成比的Te1-xSx用于铁以外的原料物质。根据FeSe、FeSe1-xTex(0<x<1)及FeTe1-xSx(0<x<1)的多结晶体的研究了解可以进行固溶系的合成。例如,将Te与S以1∶1的摩尔比混合并真空封入石英玻璃管内后,在400℃下烧成1/2天(半天),由此得到全量反应的TeS。
另外,为了调整组成比而向铁制管(覆盖物)内部同时装填该TeS和Te,在进行线材化后,进行450-600℃的加热处理,得到铁系超导电体的化学组成为FeTe1-xSx(0<x<1)的铁系超导电线材。关于全部铁系超导电线材也观测到临界电流。
另外,本发明的铁系超导电线材及其制造方法不限于上述实施例是不言而喻的。
产业上的可利用性
根据本发明的铁系超导电线材及其制造方法能够简单地制作使用了FeSe、FeTe、FeSe1-xTex(0<x<1)、FeTe1-xSx(0<x<1)等的铁系超导电物质的铁系超导电线材。希望铁系超导电体的实用化,期待其应用及开发。
Claims (3)
1.一种铁系超导电线材,其特征在于,
向主要由铁形成的筒状覆盖体的内部装填Se、Te或S单质或者2种以上的混合物或它们的化合物即原料物质,该原料物质与形成筒状覆盖体的铁反应而生成了铁系超导电体,
所述铁系超导电体的化学组成为FeSe、FeTe、FeSe1-xTex或FeTe1-xSx中的任一种,其中0<x<1。
2.一种多芯铁系超导电线材,其特征在于,
将权利要求1所述的铁系超导电线材的多条一体化而形成为多芯线。
3.一种铁系超导电线材的制造方法,其特征在于,
向主要由铁形成的筒状覆盖体的内部装填铁以外的构成铁系超导电体的化学成分元素即原料物质后,进行机械加工,进行线材化,在100-1000℃下进行1分钟-500小时的加热处理,使形成筒状覆盖体的铁和装填于筒状覆盖体的内部的原料物质发生反应,生成铁系超导电体,得到铁系超导电线材,
所述铁系超导电体的化学组成为FeSe、FeTe、FeSe1-xTex或FeTe1-xSx中的任一种,其中,0<x<1。
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JP5626991B2 (ja) * | 2011-01-18 | 2014-11-19 | 独立行政法人物質・材料研究機構 | 固相反応で合成したFeTe1−xSx化合物の超電導化方法 |
RU2522591C2 (ru) * | 2012-07-13 | 2014-07-20 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Способ синтеза монокристаллических селенидов железа |
CN110061367B (zh) * | 2019-04-23 | 2020-08-11 | 中国科学院电工研究所 | 一种铁基超导接头及其制备方法 |
CN112010270B (zh) * | 2019-05-31 | 2022-07-15 | 中国科学院物理研究所 | FeBi(Te,Se)多晶超导材料及其制备方法和应用 |
CN110867283B (zh) * | 2019-11-29 | 2020-11-24 | 西北有色金属研究院 | 一种FeSe基超导线材的制备方法 |
CN113345640B (zh) * | 2021-06-03 | 2022-08-02 | 西北有色金属研究院 | 一种Fe(Se,Te)超导线材的制备方法 |
CN114242333B (zh) * | 2021-12-23 | 2023-03-14 | 上海交通大学 | 一种铁硒碲硫超导靶材及其制备方法与应用 |
WO2023146540A1 (en) * | 2022-01-30 | 2023-08-03 | Fermi Research Alliance, Llc | Bi-layer barrier assembly for iron-based superconductor and associated methods |
CN114566326A (zh) * | 2022-03-29 | 2022-05-31 | 中国科学院电工研究所 | 一种通过挤压成形获得复合包套铁基超导线带材的方法 |
CN114822991B (zh) * | 2022-05-26 | 2023-01-31 | 西北有色金属研究院 | 一种Fe(Se,Te)超导线材的制备方法 |
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CN1865457A (zh) * | 2006-06-13 | 2006-11-22 | 中国科学院电工研究所 | 一种铁基二硼化镁超导线带材的热处理方法 |
CN1933036A (zh) * | 2005-09-13 | 2007-03-21 | 中国科学院电工研究所 | 一种MgB2超导材料及其制备方法 |
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US20030036482A1 (en) * | 2001-07-05 | 2003-02-20 | American Superconductor Corporation | Processing of magnesium-boride superconductors |
JP4476800B2 (ja) * | 2004-12-28 | 2010-06-09 | 株式会社神戸製鋼所 | Nb3Sn超電導線材の製造方法 |
CN101271747B (zh) * | 2008-05-07 | 2013-05-01 | 中国科学院电工研究所 | 一种铁基化合物超导线材、带材及其制备方法 |
JP5376499B2 (ja) * | 2008-11-04 | 2013-12-25 | 独立行政法人物質・材料研究機構 | 鉄系超電導物質 |
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CN1865457A (zh) * | 2006-06-13 | 2006-11-22 | 中国科学院电工研究所 | 一种铁基二硼化镁超导线带材的热处理方法 |
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Superconductivity in S-substituted FeTe;YOSHIKAZU MIZUGUCHI ET AL.;《APPLIED PHYSICS LETTERS》;20090131;第94卷;012503-1 - 012503-3 * |
YOSHIKAZU MIZUGUCHI ET AL..Superconductivity at 27 K in tetragonal FeSe under high pressure.《APPLIED PHYSICS LETTERS》.2008,第93卷152505-1 - 152505-3. |
YOSHIKAZU MIZUGUCHI ET AL..Superconductivity in S-substituted FeTe.《APPLIED PHYSICS LETTERS》.2009,第94卷012503-1 - 012503-3. |
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EP2447958B1 (en) | 2017-09-20 |
US8871684B2 (en) | 2014-10-28 |
US20120135869A1 (en) | 2012-05-31 |
EP2447958A4 (en) | 2015-04-15 |
JP5626658B2 (ja) | 2014-11-19 |
WO2010140593A1 (ja) | 2010-12-09 |
JPWO2010140593A1 (ja) | 2012-11-22 |
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