• Journal of Powder Materials
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• v.15 no.5
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• pp.371-377
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• 2008

This paper deals with the phase analysis of $MgB_2$ bulk using spark plasma sintering process after ball milling. Mg and amorphous B powders were used as raw materials, and milled by planetary-mill for 9 hours at argon atmosphere. In order to confirm formation of $MgB_2$ phase, DTA and XRD were used. The milled powders were fabricated to $MgB_2$ bulk at the various temperatures by Spark Plasma Sintering. The fabricated $MgB_2$ bulk was evaluated with XRD, EDS, FE-SEM and PPMS. In the DTA result, reaction on formation of $MgB_2$ phase started at $340^{\circ}C$. This means that ball milling process improves reactivity on formation of $MgB_2$ phase. The $MgB_2$ MgO and FeB phases were characterized from XRD result. MgO and FeB were undesirable phases which affect formation of $MgB_2$ phase, and it's distribution could be confirmed from EDS mapping result. Spark Plasma Sintered sample for 5 min at $700^{\circ}C$ was relatively densified and it's density and transition temperature showing super conducting property were $1.87\;g/cm^3$ and 21K.

• Progress in Superconductivity
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• v.12 no.2
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• pp.88-92
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• 2011

[ $MgB_2$ ]superconducting sheets have been fabricated using powder roll compaction method. Sheet-type $MgB_2$ bulk samples were successfully fabricated using the pre-reacted $MgB_2$ powders. In this work, $MgB_2$ powders were compacted by two rotating rolls and squeezed out as a form of $MgB_2$ sheets of ~1 mm thickness. The rolling speed of 0.3-0.7 rpm and the gap distance of 0.3-0.8 mm between the two rollers were carefully controlled to get a full compaction of the powders into bulk $MgB_2$ sheets. The densities of $MgB_2$ sheets were 1.98-2.05 g/$cm^3$, which is 75.44-77.99 % of the theoretical value of 2.63 g/$cm^3$. And the density comparison was made compared to those of typical $MgB_2$ bulks from uni-axial pressing and $MgB_2$ wires from Powder-In-Tube processing.

• Progress in Superconductivity and Cryogenics
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• v.19 no.2
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• pp.19-24
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• 2017

Cryogenic milling which is a combined process of low-temperature treatment and mechanical milling was applied to fabricate high critical current density $(J_c)MgB_2$ bulk superconductors. Liquid nitrogen was used as a coolant, and no solvent or lubricant was used. Spherical Mg ($6-12{\mu}m$, 99.9 % purity) and plate-like B powder (${\sim}1{\mu}m$, 97 % purity) were milled simultaneously for various time periods (0, 2, 4, 6 h) at a rotating speed of 500 rpm using $ZrO_2$ balls. The (Mg+2B) powders milled were pressed into pellets and heat-treated at $700^{\circ}C$ for 1 h in flowing argon. The use of cryomilled powders as raw materials promoted the formation reaction of superconducting $MgB_2$, reduced the grain size of $MgB_2$, and suppressed the formation of impurity MgO. The superconducting critical temperature ($T_c$) of $MgB_2$ was not influenced as the milling time (t) increased up to 6 h. Meanwhile, the critical current density ($J_c$) of $MgB_2$ increased significantly when t increased to 4 h. When t increased further to 6 h, however, $J_c$ decreased. The $J_c$ enhancement of $MgB_2$ by cryogenic milling is attributed to the formation of the fine grain $MgB_2$ and a suppression of the MgO formation.

• Progress in Superconductivity
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• v.10 no.2
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• pp.79-86
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• 2009

We successfully fabricated C-doped ex-situ $MgB_2$ wires using two different methods such as mechanical alloying(MA) and combined process(CP) of in-situ and ex-situ. In the MA, the precursor powder was prepared with a mixture of $MgB_2$ and 1 at% C powders by planetary ball milling for 0-100 h. In the CP, on the other hand, C-doped $MgB_2$ powder was prepared with Mg, B, and C powders by in-situ process via compaction, sintering, and crushing. The powders prepared by two methods were loaded into Fe tube and then the assemblages were drawn by a conventional powder-in-tube technique. The MA treatment of C-added $MgB_2$ decreased the particles/grains size and resulted in C-doping into $MgB_2$ after sintering, improving the critical current density($J_c$) in high external magnetic field. For the C-doped $MgB_2$ wire by MA for 25 h, the $J_c$ was $4.1{\times}10^3A/cm^2$ at 5 K and 6.4 T, which was 5.9 times higher than that of pure and untreated $MgB_2$ wire. The CP also provided C-doping into $MgB_2$ and improved the $J_c$ in high magnetic field; the C-doped $MgB_2$ wire fabricated by CP exhibited a $J_c$ being 2.3 times higher than that of the ex-situ wire used commercial $MgB_2$ powder at 5 K and 6.0 T($2.7{\times}10^3A/cm^2\;vs.\;1.2{\times}10^3A/cm^2$).

• Progress in Superconductivity and Cryogenics
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• v.21 no.2
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• pp.40-44
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• 2019

In this study, the effects of the compaction method for (Mg+2B) powders on the apparent density and superconducting properties of $MgB_2$ bulk superconductor were investigated. The raw powders used in this study were nano-sized boron (B) and spherical magnesium (Mg). A batch of a powder mixture of (Mg+2B) was put in a steel mold and uniaxially pressed at 1 ton or 3 tons into pellets. Another batch of the powder mixture was uniaxially pressed at 1 ton and then pressed isostatically at $1800kg/cm^2$ in the water chamber. All pellets were heat-treated at $650^{\circ}C$ for 1 h in flowing argon gas for the formation of $MgB_2$. The apparent density of powder compacts pressed at 3 ton was higher than that at 1 ton. The cold isostatic pressing (CIP) in a water chamber allowed further increase of the apparent density of powder compacts, which influenced the pellet density of the final products ($MgB_2$). The compaction methods (uniaxial pressing and CIP) did not affect the formation of $MgB_2$ and superconducting critical temperature ($T_c$) of $MgB_2$, but affected the critical current density ($J_c$) of $MgB_2$ significantly. The sample with the high apparent density showed high $J_c$ at 5 K and 20 K at applied magnetic fields (0-5 T).

• Progress in Superconductivity and Cryogenics
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• v.25 no.3
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• pp.22-27
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• 2023

Magnetic properties of MgB₂ superconducting powder were investigated. M(H), the magnetic field H dependence of magnetization M, was measured and analyzed using a PPMS instrument. The MgB₂ superconducting powder showed high critical current density J_c > ~ 10⁷ A/cm² and clean limit superconducting properties. The equilibrium magnetization M_eq properties of MgB₂ powders exhibiting various superconducting properties were studied. We find that the equilibrium magnetization M_eq(H) properties of MgB₂ powders showing conventional BCS properties deviate from the predictions of the standard local-London theory at temperatures below T = 19 K and are in good agreement with the generalized nonlocal-London theory. Nonlocal-London analysis was used to determine and analyze the nonlocal parameters. The temperature dependence of the London penetration depth values λ(T) was studied.

• Korean Journal of Materials Research
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• v.24 no.9
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• pp.465-468
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• 2014

The crystallization effects of boron (B) powder on the phase, full width at half maximum (FWHM) values, and critical properties were investigated for in-situ reacted $MgB_2$ bulk superconductors. The semi-crystalline B powder was heat-treated at different temperatures of 1000, 1300 and $1500^{\circ}C$ for 5 hours in an Ar atmosphere. Then, using as-received and heat-treated B powders, the $MgB_2$ samples were prepared at $600^{\circ}C$ for 40 hours in an Ar atmosphere. As the heat-treatment temperature of the B powder increased, both the particle size of the B powder and crystalline phase increased. In the case of $MgB_2$ samples using B powders heat-treated at above $1300^{\circ}C$, unreacted magnesium (Mg) and B remained due to the improved crystallinity of the B powder. As the heat-treatment temperature of B powder increased, the critical current density of $MgB_2$ decreased continuously due to the reduction of grain boundary density and superconducting volume caused by unreacted Mg and B.

• Journal of the Korean Ceramic Society
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• v.34 no.11
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• pp.1165-1172
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• 1997

ZrB2 powders were prepared from a mixture of ZrO2, B2O3 and Mg by self-propagating high temperature synthesis method. The combustion product was successfully obtained from a mixture of ZrO2:B2O3:Mg=1:2:8.5 molar ratio. By-product, MgO was effectively removed by leaching with 1M HCl solution at 9$0^{\circ}C$ for over 5hours. After leaching, the Mg content was 0.86~1.42 wt%, and the mean particle size was 4.72${\mu}{\textrm}{m}$. The addition of 7.5 wt%(14Ni:1.0C) as a sintering aid greatly densified ZrB2 bodies compared with that of only Ni. The ZrB2 sintered bodies containing 7.5 wt%(14Ni:1.0C) was 94.3% of the theoretical density. In this case, ZrB2 existed as a major phase and had a bend strength of 300 MPa and a vickers hardness of 2000 kg/$\textrm{mm}^2$.

• Journal of Powder Materials
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• v.21 no.6
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• pp.460-466
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• 2014

Al-Si-SiC composite powders with intra-granular SiC particles were prepared by a gas atomization process. The composite powders were mixed with Al-Zn-Mg alloy powders as a function of weight percent. Those mixture powders were compacted with the pressure of 700 MPa and then sintered at the temperature of $565-585^{\circ}C$. T6 heat treatment was conducted to increase their mechanical properties by solid-solution precipitates. Each relative density according to the optimized sintering temperature of those powders were determined as 96% at $580^{\circ}C$ for Al-Zn-Mg powders (composition A), 97.9% at $575^{\circ}C$ for Al-Zn-Mg powders with 5 wt.% of Al-Si-SiC powders (composition B), and 98.2% at $570^{\circ}C$ for Al-Zn-Mg powders with 10 wt.% of Al-Si-SiC powders (composition C), respectively. Each hardness, tensile strength, and wear resistance test of those sintered samples was conducted. As the content of Al-Si-SiC powders increased, both hardness and tensile strength were decreased. However, wear resistance was increased by the increase of Al-Si-SiC powders. From these results, it was confirmed that Al-Si-SiC/Al-Zn-Mg composite could be highly densified by the sintering process, and thus the composite could have high wear resistance and tensile strength when the content of Al-Si-SiC composite powders were optimized.

• Progress in Superconductivity
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• v.10 no.1
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• pp.17-22
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• 2008

We have examined the effect of ball-milling on the superconducting properties of $MgB_2$ doped with C. The ball-milling of pre-reacted $MgB_2$ powder was carried out in dry or wet state using C or diethylenetriamine ($C_{4}H_{13}N_3$) as additives. The diethylenetriamine, whose chemical formula contains no oxygen, was chosen to avoid an excess oxidation during doping. The superconducting transition temperature (Tc) of the ball-milled or doped $MgB_2$ powders was only slightly smaller than that of undoped $MgB_2$. The critical current density (Jc) of the highly ball-milled $MgB_2$ was higher than that of C-doped $MgB_2$. The addition of diethylenetriamine was detrimental to Jc, although Tc was almost unchanged.