• Journal of Conservation Science
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• v.35 no.2
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• pp.145-152
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• 2019

The metal-manufacturing method and smelting temperature of ancient metal-production processes have been studied by analyzing the principal elements and microstructures of slag. However, the microstructure of slag varies according to the solidification cooling rate and types and relative amounts of various oxides contained within the smelting materials. Hence, there is a need for accurate analysis methods that allow slag to be distinguished by more than its composition or microstructure. In this study, the microstructures of slag discharged as a result of smelting iron sands collected from Pohang and Gyeongju, as well as the slag excavated from the Ungyo site in Wanju, were analyzed by using metalloscopy, scanning election microscopy-energy dispersine X-ray spectroscopy(SEM-EDS) and wavelength dispersive X-ray fluorenscence(WD-XRF). Furthermore, the microcrystals were accurately characterized by performing Raman micro-spectroscopy, which is a technique that can be used to identify the microcrystals of slags. SEM-EDS analysis of Pohang slag indicated that its white polygonal crystals could be Magnetite; however, Raman micro-spectroscopy revealed that these crystals were actually $ulv{\ddot{o}}spinel$. Raman micro-spectroscopy and SEM-EDS were also used to verify that the coarse white dendritic structures observed in the Gyeongju-slag were $W{\ddot{u}}stites$. Additionally, the Wanju slag was observed to have a glassy matrix, which was confirmed by Raman micro-spectroscopy to be Augite. Thus, we have demonstrated that Raman micro-spectroscopy can accurately identify slag microcrystals, which are otherwise difficult to distinguish as solely based on their chemical composition and crystal morphology. Therefore, we conclude that it has excellent potential as a slag analysis technique.

• Korean Journal of Metals and Materials
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• v.46 no.3
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• pp.174-181
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• 2008

The stability of the cathode materials for Li secondary battery is an important factor for its cyclability. The present paper focuses on the structural stability of $LiNi_{0.5}Mn_{1.5}O_4$ during lithiation/delithiation of Li ions and compared to that of $LiMn_{2}O_4$. $LiMn_{2}O_4$ and $LiNi_{0.5}Mn_{1.5}O_4$ powders are synthesized using a solgel method and their structural and electrochemical properties are investigated by XRD, SEM, and charge-discharge tests. $Li_xMn_2O_4$ and $Li_xNi_{0.5}Mn_{1.5}O_4$(x = 0.9,0.5,0.1) specimens are obtained after charge/discharge tests by controlling the cut-off voltage for XRD and TEM investigation. The charge-discharge tests shows that initial capacity of $LiNi_{0.5}Mn_{1.5}O_4$ is 125 mAh/g and that of LiMn2O4 is around 100 mAh/g. The capacity of $LiNi_{0.5}Mn_{1.5}O_4$ is maintained 95% of its initial capacity whereas the capacity of $LiMn_{2}O_4$ is maintained 65% of its initial capacity.

• Journal of Electrochemical Science and Technology
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• v.12 no.1
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• pp.112-125
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• 2021

The new emerging "High entropy materials" attract the attention of the scientific society because of their simpler structure and spectacular applications in many fields. A novel nanocrystalline high entropy (Be,Mg,Ca,Sr,Zn,Ni)3O4 oxide has been successfully synthesized through mechanochemical treatment followed by sintering and air quenching. The present research work focuses on the possibility of single-phase formation in the aforementioned high entropy oxide despite the great difference in the atomic sizes of reactant alkaline earth and 3d transition metal oxides. Structural properties of (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide were explored by confirmation of its single-phase Fd-3m spinel structure by x-ray diffraction (XRD). Further, nanocrystalline nature and morphology were analyzed by scanning electron microscopy (SEM). Among thermal properties, thermogravimetric analysis (TGA) revealed that the (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide is thermally stable up to a temperature of 1200℃. Whereas phase evolution in (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide before and after sintering was analyzed through differential scanning calorimetry (DSC). Electrochemical studies of (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide consists of a comparison of thermodynamic and kinetic parameters of water and hydrazine hydrate oxidation. Values of activation energy for water oxidation (9.31 kJ mol-1) and hydrazine hydrate oxidation (13.93 kJ mol-1) reveal that (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide is catalytically more active towards water oxidation as compared to that of hydrazine hydrate oxidation. Electrochemical impedance spectroscopy is also performed to get insight into the kinetics of both types of reactions.

• Journal of Powder Materials
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• v.28 no.2
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• pp.110-119
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• 2021

In this study, the high-temperature oxidation properties of austenitic 316L stainless steel manufactured by laser powder bed fusion (LPBF) is investigated and compared with conventional 316L manufactured by hot rolling (HR). The initial microstructure of LPBF-SS316L exhibits a molten pool ~100 ㎛ in size and grains grown along the building direction. Isotropic grains (~35 ㎛) are detected in the HR-SS316L. In high-temperature oxidation tests performed at 700℃ and 900℃, LPBF-SS316L demonstrates slightly superior high-temperature oxidation resistance compared to HR-SS316L. After the initial oxidation at 700℃, shown as an increase in weight, almost no further oxidation is observed for both materials. At 900℃, the oxidation weight displays a parabolic trend and both materials exhibit similar behavior. However, at 1100℃, LPBF-SS316L oxidizes in a parabolic manner, but HR-SS316L shows a breakaway oxidation behavior. The oxide layers of LPBF-SS316L and HR-SS316L are mainly composed of Cr₂O₃, Fe-based oxides, and spinel phases. In LPBF-SS316L, a uniform Cr depletion region is observed, whereas a Cr depletion region appears at the grain boundary in HR-SS316L. It is evident from the results that the microstructure and the high-temperature oxidation characteristics and behavior are related.

• Journal of Powder Materials
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• v.28 no.6
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• pp.470-477
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• 2021

Energy storage systems should address issues such as power fluctuations and rapid charge-discharge; to meet this requirement, CoFe₂O₄ (CFO) spinel nanoparticles with a suitable electrical conductivity and various redox states are synthesized and used as electrode materials for supercapacitors. In particular, CFO electrodes combined with carbon nanofibers (CNFs) can provide long-term cycling stability by fabricating binder-free three-dimensional electrodes. In this study, CFO-decorated CNFs are prepared by electrospinning and a low-cost hydrothermal method. The effects of heat treatment, such as the activation of CNFs (ACNFs) and calcination of CFO-decorated CNFs (C-CFO/ACNFs), are investigated. The C-CFO/ACNF electrode exhibits a high specific capacitance of 142.9 F/g at a scan rate of 5 mV/s and superior rate capability of 77.6% capacitance retention at a high scan rate of 500 mV/s. This electrode also achieves the lowest charge transfer resistance of 0.0063 Ω and excellent cycling stability (93.5% retention after 5,000 cycles) because of the improved ion conductivity by pathway formation and structural stability. The results of our work are expected to open a new route for manufacturing hybrid capacitor electrodes containing the C-CFO/ACNF electrode that can be easily prepared with a low-cost and simple process with enhanced electrochemical performance.

• Journal of the Korean institute of surface engineering
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• v.55 no.1
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• pp.32-37
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• 2022

In a carbon-zero social atmospher, research is underway to reduce the use of fossil fuels. Interest in cleaner energy sources and their storage system is growing, and among them, research on effective energy storage is being actively conducted. Energy storage system(ESS) can be divided into secondary batteries, fuel cells, and capacitors, and the superiority of energy density of secondary batteries has a dominent influence on the ESS market. However, as problems with secondary batteries, charge/discharge speed, safety, and deterioration of electrodes are being highlighted. In this study, an electrode for supercapacitor with superior charge/discharge speed and specific capacitance is manufactured. The manufactured spinel nickel cobalt electrodes had specific capacitances of 1018.8 F/g, 690.8 F/g, and 475.1 F/g at 1 A/g in 1 M KOH electrolyte, and shows a performance retention rate of 77.48%, 63.30%, and 58.16% after 2000cycles at 7 A/g.

• Nuclear Engineering and Technology
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• v.54 no.6
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• pp.1972-1981
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• 2022

A typical ferritic/martensitic (F/M) steel sheet was subjected to pulsed laser surface remelting (LSR) and corrosion test in lead-bismuth eutectic (LBE) at 550 ℃. There present two modification zones with distinct microstructures in the LSRed specimen: (1) remelted zone (RZ) consisting of both bulk δ-ferrite grains and martensitic plates and (2) heat-affected zone (HAZ) below the RZ, mainly composed of martensitic plates and high-density precipitates. Martensitic transformation occurs in both the RZ and the HAZ with the Kurdjumov-Sachs and Nishiyama-Wassermann orientation relationships followed concurrently, resulting in scattered orientations and specific misorientation characteristics. Hardnesses of the RZ and the HAZ are 364 ± 7 HV and 451 ± 15 HV, respectively, considerably higher than that of the matrix (267 ± 3 HV). In oxygen-saturated and oxygen-depleted LBE, thicknesses of oxide layers developed on both the as-received and the LSRed specimens increase with prolonging corrosion time (oxide layers always thinner under the oxygen-depleted condition). The corrosion resistance of the LSRed F/M steel in oxygen-saturated LBE is improved, which can be attributed to the grain-refinement accelerated formation of dense Fe-Cr spinel. In oxygen-depleted LBE, the growth of oxide layers is very low with both types of specimens showing similar corrosion resistance.

• Corrosion Science and Technology
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• v.21 no.6
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• pp.466-475
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• 2022

Surface oxides and intergranular (IG) oxidation phenomena in Alloy 600 depending on hydrogen concentration were characterized to obtain clear insight into the primary water stress corrosion cracking (PWSCC) behavior upon exposure to pressurized water reactor primary water. When hydrogen concentration was between 5 and 30 cm³ H₂/kg H₂O, NiFe₂O₄ and NiO type oxides were found on the surface. NiO type oxides were found inside the oxidized grain boundary when hydrogen concentration was 5 cm³ H₂/kg H₂O. However, only NiFe₂O₄ spinel on the surface and Ni enrichment were observed when hydrogen concentration was 30 cm³ H₂/kg H₂O. These results indicate that the oxidation/reduction reaction of Ni in Alloy 600 depending on hydrogen concentration can considerably affect surface oxidation behavior. It appears that the formation of NiO type oxides in a Ni oxidation state and Ni enrichment in a Ni reduction (or metallic) state are common in primary water. It is believed that the above different oxidation/reduction reactions of Ni in Alloy 600 depending on hydrogen concentration can also significantly affect the resistance to PWSCC of Alloy 600.

• Journal of Electrochemical Science and Technology
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• v.13 no.2
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• pp.177-185
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• 2022

Electrochemical properties of LiMn₂O₄ cathode were investigated in three types of Zn-containing electrolytes: lithium-zinc sulfate electrolyte (1M ZnSO₄ / 2M Li₂SO₄), zinc sulfate electrolyte (2MZnSO₄) and lithium-zinc-manganese sulfate electrolyte (1MZnSO₄ / 2MLi₂SO₄ / 0.1MMnSO₄). Cyclic voltammetry measurements demonstrated that LiMn₂O₄ is electrochemically inactive in pure ZnSO₄ electrolyte after initial oxidation. The effect of manganese (II) additive in the zinc-manganese sulfate electrolyte on the electrochemical performance was analyzed. The initial capacity of LiMn₂O₄ is higher in presence of MnSO₄ (140 mAh g^-1 in 1 M ZnSO₄ / 2 M Li₂SO₄ / 0.1 M MnSO₄ and 120 mAh g^-1 in 1 M ZnSO₄ / 2MLi₂SO₄). The capacity increase can be explained by the electrodeposition of MnO_x layer on the electrode surface. Structural characterization of postmortem electrodes with use of XRD and EDX analysis confirmed that partially formed in pure ZnSO₄ electrolyte Zn-containing phase leads to fast capacity fading which is probably related to blocked electroactive sites.

• Nuclear Engineering and Technology
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• v.55 no.5
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• pp.1519-1526
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• 2023

For the first time Aluminium-BariumeZinc oxide nanocomposite (ZABONC) was synthesized by solution combustion method where calcination was carried out at low temperatures (600℃) to study the electromagnetic (EM) (X/γ) radiation shielding properties. Further for characterization purpose standard techniques like PXRD, SEM, UV-VISIBLE, FTIR were used to find phase purity, functional groups, surface morphology, and to do structural analysis and energy band gap determination. The PXRD pattern shows (hkl) planes corresponding to spinel cubic phase of ZnAl₂O4, cubic Ba(NO₃)₂, α and γ phase of Al₂O₃ which clearly confirms the formation of complex nano composite. From SEM histogram mean size of nano particles was calculated and is in the order of 17 nm. Wood and Tauc's relation direct energy band gap calculation gives energy gap of 2.9 eV. In addition, EM (X/γ) shielding properties were measured and compared with the theoretical ones using standard procedures (NaI (Tl) detector and multi channel analyzer MCA). For energy above 356 keV the measured shielding parameters agree well with the theory, while below this value slight deviation is observed, due to the influence of atomic/crystallite size of the ZABONC. Hence synthesized ZABONC can be used as a shielding material in EM (X/γ) radiation shielding.