Development of Magnesium Diboride Superconducting Wires through Hot Working with Different Initial Filling Density
Corresponding email: ahyuwono@eng.ui.ac.id
Published at : 07 Dec 2023
Volume : IJtech
Vol 14, No 7 (2023)
DOI : https://doi.org/10.14716/ijtech.v14i7.6695
Herbirowo, S., Yuwono, A.H., Sofyan, N., Imaduddin, A., Pramono, A.W., Supriyadi, S., Mohamed, J.J., 2023. Development of Magnesium Diboride Superconducting Wires through Hot Working with Different Initial Filling Density. International Journal of Technology. Volume 14(7), pp. 1570-1577
| Satrio Herbirowo | 1. Department of Metallurgical and Materials Engineering, Faculty of Engineering, Universitas Indonesia, Depok 16424, West Java, Indonesia, 2. Research Center for Advanced Materials, National Research |
| Akhmad Herman Yuwono | 1. Department of Metallurgical and Materials Engineering, Faculty of Engineering, Universitas Indonesia, Depok 16424, West Java, Indonesia, 2.Advanced Materials Research Center (AMRC), Faculty of Engi |
| Nofrijon Sofyan | 1. Department of Metallurgical and Materials Engineering, Faculty of Engineering, Universitas Indonesia, Depok 16424, West Java, Indonesia, 2. Advanced Materials Research Center (AMRC), Faculty of Eng |
| Agung Imaduddin | Research Center for Advanced Materials, National Research and Innovation Agency (BRIN) Building 440, PUSPIPTEK, South Tangerang 15314, Banten, Indonesia |
| Andika Widya Pramono | Research Center for Advanced Materials, National Research and Innovation Agency (BRIN) Building 440, PUSPIPTEK, South Tangerang 15314, Banten, Indonesia |
| Sugeng Supriyadi | Department of Mechanical Engineering, Faculty of Engineering, Universitas Indonesia, Depok 16424, West Java, Indonesia |
| Julie Juliewatty Mohamed | Faculty of Bioengineering and Technology, Universiti Malaysia Kelantan, 17700 Jeli, Kelantan, Malaysia |
This study aimed to investigate the use of the hot
working in a sealed tube method for the production of Magnesium Diboride (MgB2)
wires from a powder state. The wires were synthesized using different initial
filling densities of 60%, 80%, and 100%. The Magnesium and Boron powder was
ground using agate mortar into a stoichiometric mixture by weight of Mg:B=1:2
and then packed into a stainless steel (SUS316L) tube. Subsequently, the pack
was sintered for two hours at 800°C in an air atmosphere and continuously
rolled to form a wire. XRD and SEM analyses were then conducted to observe the
phase development of the sample produced. The diffraction pattern and
microstructure observation results showed that MgB2 phase was
successfully created using economically advantageous raw materials of
crystalline Mg and amorphous B with 60% filling density. The size of the
crystallites and superconducting phase was shown to experience a significant
increase. The R-T cryogenic magnet assessed the sample of critical temperature,
and MgB2 produced using full amorphous boron had a transition
temperature of 39 K.
Critical temperature; Filling density; Hot working; MgB2 Superconductors; Wire
Magnesium diboride, MgB2, is a novel high critical
temperature superconductor with a critical temperature of 39 K, initially
introduced in the early twenty-first century (Nagamatsu et al., 2001). The versatility of MgB2 also extends to its production in various
forms and shapes, including bulk (Arvapalli et al., 2021; Zhang et al., 2020; Zheng et al., 2019),
thin films, tapes, and wires (Balog et al., 2018;
Grivel, 2018b; Herbirowo
et
al., 2018; Kovác et al., 2011; Vinod et al., 2009). Consequently, this material has
found promising applications in various electronic devices due to its excellent
electrical contact between grains and cost-effectiveness. Several studies have
shown that its superconductivity has a
The
powder-in-tube (PIT) technique was used to create MgB2 monofilament
wire (Lubis et al., 2018; Glowacki et al.,
2001). The feedstocks used included magnesium powder (Sigma Aldrich, 98%
purity) and amorphous low-cost boron powder (Luoyang China, 95% purity).
Furthermore, the SUS316L tube with an outer diameter and inner diameter of 6
and 4 mm, respectively were used as a container for MgB2 powder with
a ratio Mg:B = 1:2. The powders were then mixed and ground in an agate mortar
for 30 minutes in an environment of air. The SUS316L stainless steel rod (4 mm
in diameter) was used to seal the stainless-steel tube container after it had
been filled with the mixture. The SUS316L tubes in wire product manufacturing
offered the advantage of enhanced corrosion resistance and durability, ensuring
a longer lifespan and reduced maintenance requirements for the final product (Widyianto, Baskoro and Kiswanto, 2022; Anwar et al.,
2021). The coarse-grained SUS 304 had a higher surface roughness ratio
compared to the coarse-grained SUS 316. The fine-grained SUS 304 and the
fine-grained SUS 316 had comparable inhomogeneous grain strengths (Abdul et al., 2021). Hot rolling was used
to create 3 mm square rods, introducing a novel method that enabled the
formation of the desired rod geometry but also effectively mitigated strain
hardening, thereby streamlining the overall manufacturing process. Hot working
in superconducting wire manufacturing was crucial for achieving densification,
consolidating the powder, refining the grain structure, improving mechanical
properties, and shaping the wire into the desired form. A wire specimen was
sintered for one hour at 1073 K in a muffle furnace. The hot rolling process in
this study showed that the wire that was still hot from the furnace was taken
out directly to be rolled by the rolling machine. X-ray diffraction (Smartlab
Rigaku) was used to determine the phase of materials. The Field Emission Scanning
Electron Microscope - EDX (JEOL JIB 4610F) was used to examine the specimen's
morphology, porosity, and elemental composition. The four-point probes method
and Oxford Instrument Teslatron PT's cryogenic magnet apparatus were used to
measure temperature dependence resistivity. Furthermore, the device was used to
measure resistivity at temperatures between 8 and 200 K for the samples.
X-ray diffraction was used to identify MgB2 wire that had been sintered at 800°C and then hot rolled. The wire was cut transversely to obtain MgB2 from inside the wire for XRD measurement. Figure 1 depicted the metallography preparation of the SUS316L tube wire, followed by the diffraction pattern of MgB2 powder. The pattern showed that MgB2 phase was one of the main phases, which increased from 98.2% to 98.5% and contained other elements, with a small quantity of Fe impurities. This proved that the SUS316L sheath was in contact with the diffraction process. According to Varghese et al., unreacted Fe and SS in MBFe and MBSS provided a greater volume percentage of MgB2 core, superior current density characteristics, and flux pinning behavior. This showed that Fe and SS were better sheath materials for the manufacture of MgB2 wire and tape (Varghese et al., 2007).
Figure
1 The
diffraction pattern and difference plot of MgB2 wire with 100% and
60% initial filling density
The largest current density was obtained when filling density was increased from 50% to 60% of the theoretical mass density of Mg+B in a previous study (Akdogan et al., 2015). However, the filling mass density had a significant impact on the temperature of production. Based on these results, the ideal filling density for powder was less than 100%. To prevent the porosity or size reduction of MgB2 wire, MgB2 formation problem must be addressed during sintering.
Figure 2 showed the W-H plot of MgB2 superconducting wire with various variations of powder filling, namely 100% and 60%. Analysis of the Williamson-Hall method for this computational analysis gave an increase in crystallite size from 85.6 nm to 159.9 nm, with a slight decrease in the amount of crystallite strain. This showed that slightly higher oxide formation tended to increase the crystallinity of the wire towards the ceramic material (Herbirowo et al., 2023). MgB2 wire specimen for morphological analysis is presented in Figures 3 and 4. Furthermore, the results showed that the porosity decreased from 6.3% to 5.4%, as shown in Figure 4. Based on Figure 3, it was easy to detect the location of the SUS316L tube and MgB2 phase boundaries. The results showed that the SUS316L did not react with Mg and B precursors. The cross-section line scan with EDX shown in Figure 3 also showed the presence of oxide in the material. Compared to XRD results, which did not show any oxide phase, it was estimated that the oxygen element in the EDS results was due to the oxidation process occurring on the surface of MgB2 sample.
Figure 3 EDX line scan on cross-sectional MgB2 wire of 60% filling density with a magnification of 20 times
Figure 4 The microstructure
of the SUS316L/MgB2 wire sintered at 1073K for 1 hour through hot
rolling with (a) 100% (b) 80%, and (c) 60% filling density under a
magnification of 5.000 times on the left (Secondary Image) and right (porosity
analysis) sides
Table 1 The objective of MgB2
synthesis was to create a material with a microstructure, phase, and composition
with the highest levels of superconductivity. The electrical resistivity's
temperature dependency was one of the most important properties to be assessed.
Furthermore, all synthesized MgB2-based samples had their
resistivity evaluated using a cryogenic magnet setup and the four-point probe
(FPP) method. The electrical resistivity of the SUS316L/MgB2
monofilament wire was shown as a function of temperature in Figure 5. The
results showed that the resistance value of the SUS316L/MgB2 wire
sample with 60% filling density was initially 2.00x10-4 ohm at 200 K
and decreased continuously until 8 K to 1.50x10-4 ohm, before
dropping at Tconset of 39K.
Figure 5 Resistivity measurement (left) and normalized resistivity (right) of the SUS316L/MgB2 wire specimen with different initial filling densities without an applied magnetic field
In
conclusion, MgB2 wires were fabricated successfully, leveraging the
economic benefits of using raw materials from crystalline Mg and amorphous B,
with a 60% initial filling density. Furthermore, the size of the crystallites
and superconducting phase greatly increased in this study. The R-T cryogenic
magnet assessed the specimen of critical temperature, and the results showed
that MgB2 specimen created using crystalline magnesium and fully
amorphous boron had a transition temperature of 39 K.
The
authors are grateful for the financial support from Universitas Indonesia
offered by the Research Grant of International Publication Indexed for Final
Project Student 2022 (PUTI Pascasarjana 2022) with contract number:
NKB-301/UN2.RST/HKP.05.000/2022. The authors are also grateful to the Research
Center for Advanced Materials BRIN (ELSA-BRIN), which provided characterization
for the study facilities.
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