US20050245400A1 - Superconducting material and method of synthesis - Google Patents

Superconducting material and method of synthesis Download PDF

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US20050245400A1
US20050245400A1 US10/518,948 US51894805A US2005245400A1 US 20050245400 A1 US20050245400 A1 US 20050245400A1 US 51894805 A US51894805 A US 51894805A US 2005245400 A1 US2005245400 A1 US 2005245400A1
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accordance
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mgb
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Shi Dou
Hau Liu
Alexey Pan
Sihai Zhou
Mihail Ionescu
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University of Wollongong
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Definitions

  • the present invention relates to a superconducting compound and to a method of synthesising a superconducting compound, and, particularly, but not exclusively, a superconducting compound based on magnesium diboride and a method of synthesis thereof.
  • MgB 2 exhibits the superconducting characteristics and physics of BCS-type LTS (low-temperature superconductor) materials, as evidenced for example by a significant isotope effect [ 2 ]; however, its critical temperature (T c ) is more than twice those of the presently used superconductors Nb 3 Sn and Nb 3 Al, and more than four times that of the present LTS workhorse, NbTi.
  • MgB 2 lies in its simple crystal structure, high critical temperature T c , high critical current density (J c ), and large coherence length (hence transparency of grain boundaries to current flow). These properties of MgB 2 offer the promise of important large-scale and electronic device applications.
  • High J c at a level of 10 5 A/cm 2 to 10 6 A/cm 2 at 20 K to 30 K for MgB 2 wires have been reported by several groups [ 3 - 8 ].
  • J c drops rapidly with increasing magnetic field.
  • J c decreased more than 90% of its zero field value at 3 T within this temperature range due to the poor pinning ability of this material.
  • the present invention provides a superconducting material of formula MgB x Si y C z where X is a number in the range between 0 to 2, Y is a number in the range between 0 to 1 and Z is a number in the range 0 to 1, and where the sum of X, Y and Z is greater than or equal to 2.
  • X 1 to 2
  • Y 0.05 to 0.5
  • Z 0.05 to 0.5.
  • X 1.2 to 1.8
  • Y 0.1 to 0.3
  • Z 0.1 to 0.3.
  • the factors of critical current density, irreversibility field and flux pinning properties of MgB 2 are significantly improved by chemical doping with SiC, potentially paving the way for MgB 2 to replace the current market leaders NbTi and Ag/Bi2223.
  • a superconducting material in accordance with the present invention may preferably be made into superconducting bulk, wires, thin films and various articles and devices for any superconducting application.
  • the present invention provides a superconductor incorporating the superconducting material of the first aspect of the invention.
  • the present invention provides a method of synthesising the superconducting material of the first aspect of the present invention, comprising the step of utilising starting materials Mg, B, Si and C.
  • starting materials Mg, B, Si and C Preferably, these are in powder form.
  • the powders consist of nanoparticles.
  • the present invention provides a method of synthesizing the superconducting material of the first aspect of the invention comprising the steps of utilising starting materials Mg, B and SiC. Preferably, these are in powder form. Preferably, the powders consist of nanoparticles.
  • the present invention provides a method of synthesising a superconducting material in accordance with the first aspect of the invention comprising the step of utilising starting materials MgB 2 and SiC or Si and C. Preferably, these are in powder form. Preferably the powders consist of nanoparticles.
  • the present invention provides a method of producing a superconducting material, comprising the step of adding silicon carbide to a superconducting material.
  • the silicon carbide is added by way of addition.
  • the silicon carbide is added by way of substitution.
  • the silicon carbide may be added both by substitution and addition to the superconducting material.
  • the present invention comprises a superconducting material including a silicon carbide codopant.
  • the present invention provides a method of manufacturing a material capable of functioning as a superconductor, comprising the steps of,
  • the present invention provides a method of manufacturing a material capable of operating as a superconductor, comprising the steps of,
  • the mixture is heated to a temperature in the range from 650° to 2000° C. More preferably, the temperature is in the range 750°-900° C.
  • the elements are provided in a powder form.
  • the powders consist of nanoparticles.
  • the powders are groove-rolled into a tube manufactured from a material of one or more of the group comprising iron (Fe), copper (Cu), nickel (Ni) and stainless steel tube prior to heating the mixture.
  • the method comprises the further step of cooling the resultant material to the temperature of liquid nitrogen, to render the material capable of superconducting.
  • the present invention provides a superconducting material of the formula of formula MgB x Ti y C z where X is a number in the range between 0 to 2, Y is a number in the range between 0 to 1 and Z is a number in the range 0 to 1, where the sum of X, Y and Z is greater than or equal to 2, and X is greater than 0.
  • FIG. 2 is an image of X-ray diffraction patterns for the undoped and SiC-doped samples of a superconducting material in accordance with an embodiment of the present invention.
  • FIG. 3 is a graph depicting the lattice parameters ‘a’ and ‘c’ Plotted as a function of the SiC content x of a superconducting material in accordance with an embodiment of the present invention.
  • FIG. 7 a and 7 b are a transmission electron microscope (TEM) images depicting the high density dislocations within the grains and
  • FIG. 7 c is an energy dispersive x-ray (EDX) analysis map showing the incorporation of C and Si into the grains of MgB 2 .
  • TEM transmission electron microscope
  • EDX energy dispersive x-ray
  • the superconducting composition and the processes for synthesis of the materials of the present invention can significantly enhance J c and flux pinning.
  • the results which are described hereinbelow demonstrate that the claimed formula can be used for fabrication of superconductors for high-field applications, as chemical doping is a readily achievable and economically viable route to introduce effective flux pinning.
  • the magnetization of samples was measured over a temperature range of 5 to 30 K using Magnetic Property Measurement System (MPMS) and a Physical Property Measurement System (PPMS, Quantum Design) in a time-varying magnetic field of sweep rate 50 Oe/s and amplitude 5 T and 9 T, respectively.
  • MPMS Magnetic Property Measurement System
  • PPMS Physical Property Measurement System
  • a magnetic J c can be derived from this measurement.
  • FIG. 1 depicts the transition temperature (T c ) and transition width ⁇ T c for the doped and undoped samples determined by AC susceptibility measurements.
  • the T c onset for the undoped sample (38.6 K) is the same as reported by a number of groups.
  • FIG. 2 depicts x-ray diffraction patterns for SiC doped and undoped samples of an MgB 2 superconductor.
  • the lattice parameters, a and c of the hexagonal AlB 2 -type structure of MgB 2 were calculated using these peak shifts as shown in FIG. 3 .
  • the MgB 4 , MgO and MgB 4 O 7 peaks increased significantly with increasing SiC.
  • the continuous decrease of ‘a’ with increasing SiC doping level indicates that B was substituted by C and Si.
  • C substitution for B reached saturation at 7 at % of B [ 19 ] while the co-doping of Si and C for B raised the saturation level.
  • the sample consists of a major phase with MgB 2 structure and minority phases: MgB 4 , MgBO and MgO.
  • the axis reached a plateau at a C content of 7 at % of B where the variation of the axis is 0.016 A.
  • co-doping of Si and C into MgB 2 substantially reduced the variation of axis due to the counterbalance effect of Si and C. This also explains why the T c drops very slow with increasing SiC dopant.
  • FIG. 5 shows the J c (H) curves for doped and undoped samples at temperatures of 5 K (graph a) and 10 K (graph b). These results show the following striking features.
  • the J c (H) curves for undoped samples shows a crossover with those for all the doped sample at higher fields.
  • SiC doping at x values of greater than 0.22 caused a reduction of J c at low fields, it is important to note that the J c for all doped samples drops with increasing field much more slowly than for the undoped sample.
  • J c curves for doped samples with x values of 0.22 and 0.33 show an exponential relationship with the applied magnetic field up to the measurement field limit, while the J c curve for the undoped sample shows a rapid downward bend.
  • FIG. 6 A further comparison is shown in FIG. 6 , where the results of transport current measurements are shown for one of the most optimal SiC-doping levels and the best MgB 2 samples found in the literature. As can be seen, there is a striking difference between the two curves.
  • the SiC-doped sample is measured at a temperature of 5K, whereas the other samples are measured at a temperature of 4.2K. In other words, the actual enhancement induced by SiC-doping is even larger than the best MgB 2 samples found in the literature.
  • SiC doping has no densification effect, as evidenced by the fact that the density of doped samples is 1.2G/cm 2 , independent of doping level. This is understandable because SiC has a very high melting point and would not act as a sintering aid at temperatures in the range of 800° C. to 950° C.
  • SiC doping takes place in the form of substitution and/or addition while in the prior art [ 14 - 16 ] the element doping is in the form of additives, which are not incorporated into the lattice structure.
  • Doping MgB 2 with Ti and Zr showed an improvement of J c in self field and 4K [ 12 ].
  • H irr 4 T at 20K
  • Doping MgB 2 using Y 2 O 3 nanoparticles showed an improvement of irreversibility field (H irr ) at 4.2K, but H irr for the doped samples is not as good as the undoped ones at 20K [ 13 ].
  • Cimerle et al. found that doping with a small amount of Li, Al and Si showed some increase in J c , but there is no improvement in H irr [ 14 ]. It is evident that the additive pinning is more effective at low temperatures while the additives at the grain boundaries decouple the grains at high temperatures.
  • the first is intrinsic pinning due to substitution and impurity pinning (or a combination thereof).
  • the high fraction of substitution by both Si and C can result in lattice defects, which are capable of acting as effective pinning sites which are intrinsic in nature and independent of temperature.
  • the high content of MgO and other impurity phases in the SiC doped samples could also be potential pinning centers, consistent with the results obtained from a thin film with strong pinning where the ratio of Mg;B:O reached 1.0:0.9:07 [ 11 ].
  • the applicant has attempted to dope fine particle MgO into MgB 2 . However, the results did not show any improvement in J c .
  • the manner in which the impurities are introduced may be critical.
  • the nanoparticles When SiC reacts with liquid Mg and amorphous B at the sintering temperatures, the nanoparticles may act as nucleation sites to form MgB 2 and other phases. Some nanoparticles may be included within the grains as inclusions. Thus, the reaction induced products are highly dispersed in the bulk matrix.
  • the density of-the samples is only about 1.2 g/cm 3 .
  • the J c values for both the doped and undoped samples are far from optimum.
  • MgB 2 conductors From the study of effect of the purity of the precursor materials, it is noted that even 95% pure B degraded the J c appreciably. Therefore, it is necessary to use high purity B (98% or above). The cost for B increases significantly with increasing purity.
  • the main cost for making MgB 2 conductors will be the high purity B. Since C and Si are abundant, inexpensive and readily available materials, then if a portion of B can be replaced by co-doping with C and Si or SiC, the overall cost for making MgB 2 conductors will preferably be reduced. Furthermore, the SiC doping has already shown a significant benefit in enhancing flux pinning. It is evident that it is advantageous for MgB 2 conductors to be made using a formula of MgB x Si y C z where x+y+z ⁇ 2, instead of pure MgB 2 .
  • the magnetization of 1.0 ⁇ 1.0 ⁇ 0.8 mm 3 samples was measured over a temperature range of 5 to 30 K-using a Physical Property Measurement System (PPMS, Quantum Design) in a time-varying magnetic field of sweep rate 50 Oe/s and amplitude 9 T.
  • Polycrystalline samples of MgB 2 ⁇ x C x were prepared through a reaction in-situ method.
  • the powders were pressed into pellets of 10 mm in diameter and 3 mm in thickness using a hydraulic press.
  • the pellets were sealed in Fe tubes, then heat treated at 770° C. for 30 min in flowing high purity Ar. This was followed by a furnace cooling to room temperature.
  • the enhancement by C-doping is similar to that of Si-doping but not as strong as for nano-SiC doped MgB2.
  • X-ray diffraction results indicate that C reacted with Mg to form nano-size Mg 2 C 3 and MgB 2 C 2 particles.
  • Nano-particle inclusions and substitution both observed by transmission electron microscopy, are proposed to be responsible for the enhancement of flux pinning in high fields.
  • Polycrystalline samples of MgB 2 ⁇ x Si x were prepared through a reaction in-situ method.
  • the powders were pressed into pellets of 10 mm in diameter and 3 mm in thickness using a hydraulic press.
  • the pellets were sealed in Fe tubes, then heat treated at 800-900° C. for 30 min in flowing high purity Ar. This was followed by a furnace cooling to room temperature.
  • An un-doped sample was also made under the same conditions for use as a reference sample.

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WO2007071163A1 (fr) * 2005-12-23 2007-06-28 Institute Of Electrical Engineering, Chinese Academy Of Science Bande ou cable supraconducteur a base de mgb2 et de carbone et son procede de fabrication
US20080017279A1 (en) * 2006-07-24 2008-01-24 Venkataramani Venkat Subramani Wires made of doped magnesium diboride powders and methods for making the same
US20080236869A1 (en) * 2007-03-30 2008-10-02 General Electric Company Low resistivity joints for joining wires and methods for making the same
US7494688B2 (en) 2006-07-24 2009-02-24 General Electric Company Methods for making doped magnesium diboride powders
US20090258787A1 (en) * 2008-03-30 2009-10-15 Hills, Inc. Superconducting Wires and Cables and Methods for Producing Superconducting Wires and Cables
US20120094841A1 (en) * 2010-06-10 2012-04-19 Korea Institute Of Machinery And Materials METHOD OF PREPARING MgB2 SUPERCONDUCTING WIRE AND THE MgB2 SUPERCONDUCTING WIRE PREPARED THEREBY
US9887029B2 (en) 2012-08-29 2018-02-06 Hitachi, Ltd. Conductive cooling-type persistent current switch, MRI apparatus and NMR apparatus
US11387017B2 (en) 2017-03-03 2022-07-12 Hitachi, Ltd. Method of producing superconductor

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DE102006017435B4 (de) 2006-04-07 2008-04-17 Leibniz-Institut Für Festkörper- Und Werkstoffforschung Dresden E.V. Pulver für die Herstellung von MgB2-Supraleitern und Verfahren zur Herstellung dieser Pulver
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US8470743B2 (en) 2010-12-31 2013-06-25 Carlton Anthony Taft Composite superconductor
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WO2007071163A1 (fr) * 2005-12-23 2007-06-28 Institute Of Electrical Engineering, Chinese Academy Of Science Bande ou cable supraconducteur a base de mgb2 et de carbone et son procede de fabrication
US20080017279A1 (en) * 2006-07-24 2008-01-24 Venkataramani Venkat Subramani Wires made of doped magnesium diboride powders and methods for making the same
US7494688B2 (en) 2006-07-24 2009-02-24 General Electric Company Methods for making doped magnesium diboride powders
US20080236869A1 (en) * 2007-03-30 2008-10-02 General Electric Company Low resistivity joints for joining wires and methods for making the same
US9287485B2 (en) 2007-03-30 2016-03-15 General Electric Company Methods for making low resistivity joints
US20090258787A1 (en) * 2008-03-30 2009-10-15 Hills, Inc. Superconducting Wires and Cables and Methods for Producing Superconducting Wires and Cables
US20120094841A1 (en) * 2010-06-10 2012-04-19 Korea Institute Of Machinery And Materials METHOD OF PREPARING MgB2 SUPERCONDUCTING WIRE AND THE MgB2 SUPERCONDUCTING WIRE PREPARED THEREBY
US8709979B2 (en) * 2010-06-10 2014-04-29 Korea Institute Of Machinery And Materials Method of preparing MgB2 superconducting wire and the MgB2 superconducting wire prepared thereby
US9887029B2 (en) 2012-08-29 2018-02-06 Hitachi, Ltd. Conductive cooling-type persistent current switch, MRI apparatus and NMR apparatus
US11387017B2 (en) 2017-03-03 2022-07-12 Hitachi, Ltd. Method of producing superconductor

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