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## Creator

[Akihiro Kikuchi](https://orcid.org/0000-0002-5044-7156), [Yasuo Iijima](https://orcid.org/0000-0002-9008-9429), [Hiroaki Kumakura](https://orcid.org/0000-0001-9070-4068), Masaru Yamamoto, Masatoshi Kawano, Masato Otsubo

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[Development of the Ultrafine MgB<sub>2</sub> Superconducting Wires and Flexible Cables](https://mdr.nims.go.jp/datasets/b1f98301-8672-4b5f-98b7-c04031b72b17)

## Fulltext

Microsoft Word - Manuscript ID_EUCAS23-2-MP-MW-10S_finalEUCAS23-2-MP-MW-10S   Template version 8.0c, 7 August 2017. IEEE will put copyright information in this area See http://www.ieee.org/publications_standards/publications/rights/index.html for more information. 1Development of the ultrafine MgB2 superconducting wires and flexible cables  Akihiro Kikuchi, Yasuo Iijima, Hiroaki Kumakura, Masaru Yamamoto, Masatoshi Kawano, and Masato Otsubo    Abstract— We successfully fabricated the ultrafine MgB2 mono-core superconducting wires through the general in-situ powder-in-tube process by using a starting mixture of commercial Mg and B powders without C doping.  In addi-tion, some bundled cables were fabricated by using ul-trafine MgB2 wires.  Those cables showed surprisingly flexible mechanical performance even after the heat treatment.  The critical current (Ic) decreased monoton-ically with decreasing the wire diameter, meanwhile, the critical current density was almost the same value with de-creasing the wire diameter down to 0.05 mm.  The Ic of the twisted cables was increased almost by the number of bundled wires.  This is a very promising result from a practical application point of view.  In addition, we recog-nized the Monel outer sheath was very effective in improv-ing the cold-die-drawability to forward the ultrafine diam-eter.  It was fabricated 4 km of long piece length without the wire breakage for the Monel sheathed mono-core wire 0.05 mm in diameter.  Furthermore, we challenged the limits of diameter reduction in the present drawing tech-nique, and eventually, the Monel sheathed MgB2 mono-core superconducting wire with 0.015 mm in diameter and 135 m in length was obtained.  This is currently the thin-nest MgB2 superconducting wire in the world. Index Terms—MgB2, wire, in-situ process, powder in tube pro-cess, die-drawing, fine diameter, twisted cable, flexibility I.  INTRODUCTION ACING global environmental problems, such as climate change, global warming, etc., we have to enable a sustain-able world as soon as possible.  Hydrogen is world-widely garnering attention as a crucial energy resource in achieving carbon neutrality [1].  If liquid hydrogen becomes familiar to our society, superconducting applications operating at 20 K may be able to contribute to saving energy.  MgB2 supercon-ducting wire is promising for practical conductor at 20 K be-cause it has a high Tc of 39 K [2], small superconducting ani- Manuscript receipt and acceptance dates will be inserted here. Acknowledg-ment of support is placed in this paragraph as well. Consult the IEEE Editorial Style Manual for examples. A part of this work is based on results obtained from a project, JPNP16006, commissioned by the New Energy and Industrial Tech-nology Development Organization (NEDO). (Corresponding author: Akihiro Kikuchi.) Akihiro Kikuchi, Yasuo Iijima and Hiroaki Kumakura are with the National Institute for Materials Science (NIMS), Tsukuba, Ibaraki 305-0028, Japan (e-mail: KIKUCHI.Akihiro@nims.go.jp). Masaru Yamamoto, Masatoshi Kawano and Masato Otsubo are with Japan Superconductivity Application Development Inc. (JSA), Chuo, Yamanashi 409-3842, Japan. Color versions of one or more of the figures in this paper are available online at http://ieeexplore.ieee.org. Digital Object Identifier will be inserted here upon acceptance. sotropy [3], no weak-link problem [4], lightweight, simple chemical composition, possibly to make round wires [5], [6], expect low production cost [7], etc.  The critical current in MgB2 superconducting materials depends on the connectivity between grains and the density of pinning centers [8], [9].  Although MgB2 multifilamentary wires are already being de-veloped and commercially available from several companies at present [10], [11].  However, in order to meet wide practical applications including AC use with liquid hydrogen, there re-main some issues, such as mechanical brittleness, stability, AC loss, etc. Recently, we are promoting R&D of ultrafine A15 type su-perconducting wires having a very small diameter much less than human hair.  In principle, the bending strain decreases with decreasing the wire diameter, therefore, we may expect that the brittle compound superconducting wire becomes flex-ible through the wire diameter reduction.  This is a big ad-vantage of applying the React and Wind method for magnet fabrication, and it would minimize the fabrication cost and improve the magnetic field quality.  So far, we successfully fabricated the jelly-rolled Nb3Al monofilament wires having 0.05 mm in outer diameter and over 400 m in length [12], [13] as well as the bronze processed Nb3Sn 19 filaments wires hav-ing 0.05 mm in outer diameter and over 7 km in length [14].   In this paper, we studied the limit of the diameter reduction of general in-situ powder-in-tube (PIT) processed MgB2 mono-core wires through the cold die-drawing technique.  The drawing of PIT wires up to very small diameters is not a trivial process and the critical current density of thin wires is usually reduced for diameters [15].  We also made the bundled cables using the obtained ultrafine MgB2 wires.  Their superconduct-ing properties, such as the critical temperature and the critical current were investigated. II. EXPERIMENTAL PROCEDURES A. In-Situ PIT(Powder-In-Tube) Process We made the precursor wires through the In-Situ PIT(Powder-In-Tube) process using commercial Mg powders (99.8% purity, under 45 m of particle size) and commercial amorphous B powders (99.0% purity, under 350 nm of particle size).  The outermost tubes 14.3 mm in outer diameter and 10 mm in inner diameter used the OFC (oxygen-free Cu) and Monel (Ni-based Cu alloy).  The pure Nb tube was inserted in the OFC or Monel for a diffusion barrier.  Mg and B powders were manually mixed with an atomic ratio of 1:2 in the groove F  2box in the Ar atmosphere, and the mixtures were filled in the Nb tube with applying a vibration.  It was no carbon doping in this study.  Both ends of the Nb tube were tightly stuffed with Cu caps and it has been avoided a remarkable oxidation of powder mixtures after taking it out into the open air.   B. Wire Drawing Eventually, the PIT precursor billet had an outer diameter of 14.3 mm and a length of about 200 mm.  Before the wire drawing, the billet diameter was reduced by using the swaging machine from 14.3 mm to about 5.0 mm.  Then, the wire drawing from 5.0 mm to 0.6 mm in diameters were performed by using general hard steel metal dies and a lubricant of a rapeseed oil.  It is used 4 meters draw-bench for drawing from 5.0 mm to 2.0 mm in diameter, and is used a horizontal single-head drawing machine for drawing from 2.0 mm to 0.6 mm in diameter.  An area reduction ratio between dies was consist-ently about 11 % and the drawing speed was approximately 5.0 m/min. No wire-breakages were happened down to 0.6 mm.  And the wire drawing from 0.6 mm to 0.05 mm in diam-eters was performed by using the wet typed continuously mul-tiple cold drawing machine with diamond dies.  The entrance angle for every die was 60 degrees. The approach angle was selected at an appropriate angle between 6 and 15 degrees. The die-bearing length was 30% of the inner hole diameter.  A general area reduction ratio between dies was 10-20 % and the drawing speed was 50-100 m/min.  A part of the 0.05 mm wire has been tried additionally to draw down to a much smaller outer diameter.  In addition, some ultrafine wires were used for fabricating 7 or 49 bundled primally twisted cables in one step. C. Superconducting Properties and Microstructures The resistivity critical temperature was measured by DC four probe method with appropriate constant current.  The dis-tance between the voltage taps and the current taps are 10 mm and 40 mm, respectively.  Measurement wire samples were set at an appropriate stable temperature position from the surface of liquid helium and a temperature was controlled by small coil heater with a ramping rate of 4.0 K/h.  The critical current in liquid helium (4.2 K) was also measured by DC four probe method under the applied magnetic field using 18T supercon-ducting magnet at National Institute for Materials Science.  The external magnetic fields were applied perpendicular to the wire/cable samples. Microstructures of the cross-section of the wire and cable samples were studied by using an optical microscope (Nikon, ECLIPSE-LV150) and a scanning electron microscope (Hita-chi, TM3030Plus).   III. EXPERIMENTAL RESULTS A. The OFC sheathed Wires and Cables Fig. 1 shows the enlarged SEM images of the transverse cross-section of the powder-filled core on the OFC sheathed MgB2 wires with different outer diameters, (a) 0.6 mm, (b) 0.4 mm, (c) 0.2 mm, and (d) 0.12 mm, respectively.  There is a large difference of two orders of magnitude in the particle size between Mg and amorphous B raw powders.  It was clearly observed that a crack in the coarse Mg particle as shown in Fig. 1 (a), and was also observed Mg particle size became small with a decrease in the wire diameter.  Thus, it was rec-ognized that coarse Mg powders surrounded by B fine pow-ders would be gradually grounded through a drawing process.  The wire breakage happened not frequently for the outer di-ameter from 0.6 mm to 0.12 mm, but that happened below 0.12 mm in outer diameter.  The maximum piece lengths of 1,115 m, 1,001 m, and 478 m were obtained for the MgB2 wires with 0.12 mm, 0.07 mm, and 0.05 mm in outer diameter.  The wire drawing speed from 0.6 mm to 0.05 mm was a con-stant which was 100 m/min.  Fig. 2 (a) is the optical micro-scope image of the transverse cross-section of the 7 strands bundled cable fabricated by using MgB2 wire 0.05 mm in di-ameter (to be shown as 7/0.05).  The twist pitch length is 5.0 mm and the cable diameter is 0.15 mm.  Fig. 2 (b) is that of Fig. 1.  The enlarged SEM images of the transverse cross-section of thepowder-filled core on the OFC sheathed MgB2 wires with different outerdiameters, (a) 0.6 mm, (b) 0.4 mm, (c) 0.2 mm, and (d) 0.12 mm, respectively. Fig. 2.  Optical microscope images of the transverse cross-section of (a) the0.05 mm and 7 strands MgB2 bundled cable (7/0.05) and (b) the 0.05 mm and49 strands MgB2 bundled cable (49/0.05).  The cable diameters are 0.15 mmand 0.41 mm, and twist pitch lengths are 5.0 mm and 8.0 mm, respectively.The twist direction of both cables is the same as S (clockwise) direction.   3the 47 strands bundled cable (to be shown as 49/0.05).  The twist pitch length is 8.0 mm and the cable diameter is 0.41 mm.  The twist direction of both cables is the same as S (clockwise) direction.  These cables show surprisingly flexible mechanical performance after heat treatment, although the central core of all wires of the cable is MgB2 which is a brittle compound. Fig. 3 is the voltage versus temperature curve of MgB2 mono-core wire 0.05 mm in diameter with the heat treatment at 650 oC for 30 min.  The critical temperature, Tc (on set) is about 36.5 K and Tc (off set) is about 36.2 K.  The supercon-ducting transition width is about 0.3 K, which would be a sharp transition.  In General, heat treatment of the in-situ MgB2 wire is performed at a rather lower temperature, such as around 650 oC, in order to reduce remarkable grain growth.  Therefore, those Tc values are somewhat lower than that of the MgB2 bulk sample (~39 K), because MgB2 crystal structure in the wire sample may slightly be disordering and off stoichi-ometry composition.  In addition, Tc value is more depressed by C doping because C contributes the lattice parameter changes [16].  Fig. 4 shows the transport critical current (Ic) at 4.2 K under the applied magnetic field (B) of MgB2 mono-core wire with different diameters, 0.5 mm, 0.2 mm, 0.12 mm, 0.07 mm, and 0.05 mm.  The Ic criterion was used as 1 V/cm.  Fig. 5 shows the critical current density (Jc) which was calcu-lated from the Ic as shown in Fig. 4 divided by the cross-sectional area of superconducting MgB2 core.  The Ic was de-creased monotonically with decreasing the wire diameter, but the Jc has kept the mostly same values for all wires.  This re-sult may suggest that remarkable sausaging did not happen even though the wire drawing was performed to 0.05 mm in diameter, which is much less than that of human hair.   Fig. 6 shows the comparison in the transport Ic -B curves of 0.05 mm single wire, 7/0.05 cable, and 47/0.05 cable.  The transport Ic was increased almost by the number of bundled wires.  This is very promising results for the practical application point of view because the current capacity could be increased easily by increasing the number of bundles. Fig. 4.  The critical current (Ic) at 4.2 K under the applied magnetic field(B) of MgB2 mono-core wire with different diameters, 0.5 mm, 0.2 mm, 0.12mm, 0.07 mm, and 0.05 mm. The Ic criterion was used as 1 V/cm.   Fig. 5.  The critical current density (Jc) at 4.2 K under the applied magneticfield (B) of MgB2 mono-core wire with different diameters, 0.5 mm, 0.2mm, 0.12 mm, 0.07 mm, and 0.05 mm.  The Jc was calculated from the Ic asshown in Fig. 4 divided by the cross-sectional area of MgB2 core.  Fig. 6.  The critical current (Ic) at 4.2 K under the applied magnetic field(B) of 0.05 mm single wire, 0.05 mm and 7 strands bundled cable (7/0.05)and 0.05 mm and 49 strands cable (49/0.05).  Fig. 3.  The voltage and temperature curve of MgB2 mono-core wire 0.05mm in diameter after the reaction at 650 oC for 30 min.  The voltage tapdistance is 10 mm and measurement current is 0.3 mA.   4B. The Monel sheathed Wire Monel, which is Ni-based Cu alloy, is known to show me-chanical performance both high strength and excellent plastic workability, and is already used as the sheath material for some of commercial MgB2 wires [10], [11].  For improving the wire drawability, the outermost sheath material switched from OFC to Monel in this study.  The wire breakage was ap-parently decreased and it was successfully obtained 4 km of long piece length for Monel sheathed MgB2 mono-core wire 0.05 mm in diameter.  The OFC sheathed wire 0.05 mm in di-ameter showed 720 MPa of tensile strength and 1.3 % of elon-gation at room temperature.  On the other hand, The Monel sheathed wire showed 1,450 MPa of tensile strength and 2.4 % elongation at room temperature at the same diameter.  Both values of the Monel sheathed wire are approximately two times larger than those of the OFC wire.  In addition, it was al-so obtained 3 km long piece length for the Monel sheathed wire 0.033 mm in diameter.  Furthermore, we tried to draw down a much thinner diameter and finally could fabricate the Monel sheathed MgB2 mono-core superconducting wire 0.015 mm in diameter and 135 m in length.  This is the thinnest MgB2 superconducting wire in the world at the moment.  The SEM image of the transverse cross-section of 0.015 mm MgB2 ultrafine wire is shown in Fig. 7.  The MgB2 superconducting core diameter is about 0.0055 mm.  After the heat treatment at 650 oC for 30 min, Tc is obtained about 35.5 K, which was slightly lower than that of the wire 0.05 mm in diameter.   IV. CONCLUSION We successfully fabricated the ultrafine MgB2 supercon-ducting wires with small diameters which is less than a human hair.  Those bundled cables show surprisingly flexible me-chanical performance even after the heat treatment.  In addi-tion, very low AC loss could be strongly expected because of maintaining a low hysteresis loss due to a small SC filament size and a low coupling loss by increasing the contact re-sistance between the bundled wire surfaces. Therefore, we would conclude that these ultrafine MgB2 wires and flexible cables in this study are promising for the React & Wind coils probably for AC application in liquid hydrogen. ACKNOWLEDGMENT A part of this work is based on results obtained from a pro-ject, JPNP14004, commissioned by the New Energy and In-dustrial Technology Development Organization (NEDO). We also deeply thank Dr. Shirabe Akita of CRIEPI and other members of the committee for this project for their strong support and useful discussion. REFERENCES [1] The Government of Japan.  KIZUNA Linking Japan and the World. “Harnessing Hydrogen to Realize a Carbon-Free Society.” [Online]. Available: https://www.japan.go.jp/kizuna/2021/09/hydrogen_carbon-free_society.html, Accessed on: Sep. 26, 2023. [2] J. Nagamatsu, N. Nakagawa, T. Muranaka, Y. Zenitani, and J. Akimitsu, “Superconductivity at 39 K in magnesium diboride,” Nature, vol. 410, 2001, p.p. 63-64. [3] M. Xu, H. Kitazawa, Y. Takano, J. Ye, K. Nishida, H. Abe, A. Matsushita, N. Tsujii, and G. Kido, “Anisotropy of superconductivity from MgB2 single crystals,” Appl. Phys. Lett., vol. 79, no. 17, 2001, p.p. 2779-2781. [4] S. B. Samanta, H. Narayan, A. Gupta, and A. V. Narlikar, “Grain boundaries as weak links: The case of MgB2 with reference to YNi2B2C,” Phys. Rev. B, vol. 65, 2002, Art. no. 092510. [5] B. A. Glowacki, M. Majoros, M. Vickers, J. E. Evetts, Y. Shi, and I. McDougall, “Superconductivity of powder-in-tube MgB2 wires,” Super-cond. Sci. Technol., vol. 14, 2001, p.p. 193-199. [6] W Goldacker, S. I. Schlachter, S. Zimmer, and H. Reiner, “High transport currents in mechanically reinforced MgB2 wires,” Supercond. Sci. Technol., vol. 14, 2001, p.p. 787-793. [7] A. Yamamoto, H. Tanaka, J. Shimoyama, H. Ogino, K. Kishio, and T. Matsushita, “Towards the Realization of Higher Connectivity in MgB2 Conductors: In-situ or Sintered Ex-situ?”, Jpn. J. Appl. Phys. vol. 51, 2012, Art. no. 010105. [8] D Gajda, A Morawski, A J Zaleski, M Akdoğan, H Yetiş, F Karaboğa, T Cetner, I Belenli, “Formation of High-Field Pinning Centers in Super-conducting MgB2 Wires by Using High Hot Isostatic Pressure Process”, J. Supercond. Nov. Magn. vol. 30, 2017, p.p. 3397-3402. [9] M. Tomsic, M. Rindfleisch, J. Yue, K. McFadden, J. Phillips, M. D. Sumption, M. Bhatia, S. Bohnenstiehl, and E. W. Collings, “Overview of MgB2 Superconductor Applications,” Int. J. Appl. Ceram. Technol., vol. 4, no. 3, 2007, p.p. 250-259. [10] Hyper Tech Research, Inc. “MgB2 Wire.” [Online]. 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Supercond., vol. 32, no. 4, Jun. 2022, Art. no. 6000104. [15] Y. Yamada, M. Kanazawa, T. Ohno, K. Tachikawa, K. Kajikawa, T. In-oue, I. Aoki, A. Matsumoto, and H. Kumakura, “PIT Processed Thin Wires Sheathed With Stainless Steel,” IEEE Trans. Appl. Supercond., vol. 22, no. 3, Jun. 2012, Art. no. 6200304. [16] S. Lee, T. Masui, A. Yamamoto, H. Uchiyama, and S. Tajima, “Crystal growth of C-doped MgB2 superconductors: accidental doping and inho-mogeneity”, Physica C, vol. 412–414, 2004, p.p. 31-35.   Fig. 7.  The SEM image of the transverse cross-section of MgB2 ultrafine wire 0.015 mm in diameter and 135 m in length. <<  /ASCII85EncodePages false  /AllowTransparency false  /AutoPositionEPSFiles true  /AutoRotatePages /None  /Binding /Left  /CalGrayProfile (Dot Gain 20%)  /CalRGBProfile (sRGB IEC61966-2.1)  /CalCMYKProfile (U.S. Web Coated \050SWOP\051 v2)  /sRGBProfile (sRGB IEC61966-2.1)  /CannotEmbedFontPolicy /Error  /CompatibilityLevel 1.4  /CompressObjects /Tags  /CompressPages true  /ConvertImagesToIndexed true  /PassThroughJPEGImages true  /CreateJobTicket false  /DefaultRenderingIntent /Default  /DetectBlends true  /DetectCurves 0.0000  /ColorConversionStrategy /CMYK  /DoThumbnails false  /EmbedAllFonts true  /EmbedOpenType false  /ParseICCProfilesInComments true  /EmbedJobOptions true  /DSCReportingLevel 0  /EmitDSCWarnings false  /EndPage -1  /ImageMemory 1048576  /LockDistillerParams false  /MaxSubsetPct 100  /Optimize true  /OPM 1  /ParseDSCComments true  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