• Journal of the Korean Crystal Growth and Crystal Technology
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• v.28 no.5
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• pp.211-216
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• 2018

The recovery of rare earth elements (REE) including La, Nd and Ce from spent batteries is important issues to reuse scarce resources. Herein, we present a simple recovery process to obtain lanthanum oxide ($La_2O_3$) from spent Ni-MH batteries, and demonstrate the conversion mechanism from $NaLa(SO_4)_2{\cdot}H_2O$ to $La_2O_3$. This strategy requires the initial preparation of $NaLa(SO_4)_2{\cdot}H_2O$ and subsequent metathesis reaction with $Na_2CO_3$ at $70^{\circ}C$. This metathesis reaction resulted in the crystalline lanthanum carbonate hydrate ($La_2(CO_3)_3{\cdot}xH_2O$) powder with plate-like morphology. On the basis of TGA result, the $La_2(CO_3)_3{\cdot}xH_2O$ powder was calcined in air at three different temperatures, that is, $300^{\circ}C$, $500^{\circ}C$, and $1000^{\circ}C$. As the calcination temperature increased, the morphology of powder was changed; prism-like ($NaLa(SO_4)_2{\cdot}H_2O$) ${\rightarrow}$ platelike ($La_2(CO_3)_3{\cdot}xH_2O$) ${\rightarrow}$ aggregated irregular shape ($La_2O_3$). Futhermore, XRD results indicated that the crystalline $La_2O_3$ could be synthesized after the metathesis reaction with $Na_2CO_3$, followed by heat-treatment at $1000^{\circ}C$, along with a change of crystallographic structures; $NaLa(SO_4)_2{\cdot}H_2O$ ${\rightarrow}$ $La_2(CO_3)_3{\cdot}xH_2O$ ${\rightarrow}$ $La_2O_3$.

• Journal of Powder Materials
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• v.22 no.1
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• pp.52-59
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• 2015

As well-known wrought stainless steel, sintered stainless steel (STS) has excellent high-temperature anti-corrosion even at high temperature of $800^{\circ}C$, and exhibits good corrosion resistance in air. However, when temperature increases above $900^{\circ}C$, the corrosion resistance of STS begins to deteriorate and dramatically decreases. In this study, the effects of phase and composition of STS on high-temperature corrosion resistances are investigated for STS 316L, STS 304 and STS 434L above $800^{\circ}C$. The morphology of the oxide layers are observed. The oxides phase and composition are identified using X-ray diffractometer and energy dispersive spectroscopy. The results demonstrate that the best corrosion resistance of STS could be improved to that of 434L. The poor corrosion resistance of the austenitic stainless steels is due to the fact that $NiFe_2O_4$ oxides forming poor adhesion between the matrix and oxide film increase the oxidation susceptibility of the material at high temperature.

• Nuclear Engineering and Technology
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• v.50 no.3
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• pp.470-477
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• 2018

With a highly functional methyl vinyl silicone rubber (VMQ) matrix and filler materials of $B_4C$, PbO, and benzophenone (BP) and through powder surface modification, silicone rubber mixing, and vulcanized molding, a flexible radiation shielding and resistant composite was prepared in the study. The dispersion property of the powder in the matrix filler was improved by powder surface modification. BP was added into the matrix to enhance the radiation resistance performance of the composites. After irradiation, the tensile strength, elongation, and tear strength of the composites decreased, while the Shore hardness of the composites and the crosslinking density of the VMQ matrix increased. Moreover, the composites with BP showed better mechanical properties and smaller crosslinking density than those without BP after irradiation. The initial degradation temperatures of the composites containing BP before and after irradiation were $323.6^{\circ}C$ and $335.3^{\circ}C$, respectively. The transmission of neutrons for a 2-mm thick sample was only 0.12 for an Am-Be neutron source. The transmission of ${\gamma}$-rays with energies of 0.662, 1.173, and 1.332 MeV for 2-cm thick samples were 0.7, 0.782, and 0.795, respectively.

• Journal of the Korean Chemical Society
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• v.32 no.1
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• pp.3-8
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• 1988

Nonstoichiometric solid solutions of the $Sr_{1+x}Dy_{1-x}FeO_{4-y}$ system (x = 0. 00, 0. 25, 0. 50, 0. 75 and 1. 00) with layered $K-2NiF_4$ type structure were prepared at 1200$^{\circ}$C under atmospheric pressure. X-ray powder diffraction spectra show that the crystallographic phases of the samples are tetragonal within the x range. Nonstoichiometric chemical formulas have been determined by Mohr salt analysis and it shows that the amount of $Fe^{4+}$ ion or ${\tau}$ value increases with increasing x. Electrical conductivities of the samples which were measured in the temperature range of $-100{\sim}200^{\circ}$C under atmospheric air pressure are varied within the semiconductivity range of $l0^{-8}{\sim}10^{-2}(ohm^{-1}{\cdot}cm^{-1}$) and the activation energies are also varied from 0.02 to 0.08 eV. Mixed valency state of $Fe^{3+}$ and $Fe^{4+}$ in the sample of $Sr_{1.00}Dy_{1.00}FeO_{4.04}$ was identified again by Mossbauer spectrum at 200K.

• Journal of the Korean Chemical Society
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• v.37 no.11
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• pp.923-928
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• 1993

The series of solid solutions in the $Sr_{1+x}Ho_{1-x}FeO_{4-y}$ (x = 0.00, 0.25, 0.50, 0.75 and 1.00) systems with $K_2NiF_4$ type structure have been prepared at 1550$^{\circ}$C under an atmospheric air pressure. The X-ray powder diffraction spectra of these samples assign that the crystallographic phases are tetragonal system over the whole x range. The lattice volume was increased with increasing the substitution amount of the $Sr^{2+}$ ion. The mole ratio of the $Fe^{4+}$ ion to total iron ions or ${\tau}$ value has been determined by Mohr salt titration of the sample and then the y value was calculated from x and ${\tau}$ values. The ${\tau}$ and y values have been increased with x values. The nonstoichiometric chemical formula are formulated from the general formula of $Sr_{1+x}Ho_{1-x}Fe^3_{1-}\;^+_{\tau}Fe_{\tau}^{4+}O_{4-y}$ replaced by x,${\tau}$ and y values. Mossbauer spectra show the mixed valence state and coordination state of $Fe^{3+}\;and\;Fe^{4+}$ ions. It is found out that the magnetic property of the samples is paramagnetic at room temperature. Electrical conductivity varied within the semiconductivity range of 1.0 to 1 ${\times}\;10^{-9}{\Omega}^{-1}cm^{-1}$. Activation energy of the electrical conductivity was decreased with the $\tau$ value. The conduction mechanism should be explained by the hopping model of the conduction electrons between the valence states of $Fe^{3+}\;and\;Fe^{4+}$ ions.

• Journal of the Korean Ceramic Society
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• v.41 no.6
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• pp.456-463
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• 2004

To enhance the performance of anode-supported SOFC, single cell fabrication procedure was changed for better and resulting power generating characteristics of single cell were investigated. Liquid condensation process was employed for the granulation of NiO/YSZ powder mixture and the produced powder granules were compacted into anode green substrate by uni-axial pressing. YSZ electrolyte was printed on green substrate via screen-printing method and co-fired at 1400$^{\circ}C$ for 3 h. LSM/YSZ composite cathode of which the composition and heat treatment condition was adjusted to minimize the polarization#resistance with AC-impedance spectroscopy, was screen printed. The final single cell size from this multi-step procedure was 5${\times}$5 $\textrm{cm}^2$ and 10${\times}$10 $\textrm{cm}^2$. The maximum power densities of 5${\times}$5 and 10${\times}$10 single cells were about 0.45 W/$\textrm{cm}^2$ and 0.22 W/$\textrm{cm}^2$ at 800$^{\circ}C$, which are two times superior than those from single cells fabricated by the conventional process in previous our work.

• Journal of the Mineralogical Society of Korea
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• v.9 no.2
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• pp.102-112
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• 1996

The precious serpentine, referring to a rare and highly valuable gem variety of serpentine group minerals, is found to occur in serpentinite from Booyo Gren Jade Mine which is located in Oesan-myun, Booyo-gun of Chungchungnam-do. Geommological properties of the precious serpentine have been investigated by use of polarizing microscope, specific gravity balance, refractometer, hardness pencils, X-ray diffractometer, XRF, ICP-MS analyser, and infrared absorption spectroscope.The precious serpentine from Booyo is colored deep green with oily luster and semi-transparent. It is highly tough and Mohs's scale of hardness is measured to be 5-6. Specific gravity is determined to be 2.67, and a single refractive index ND=1.56 is observed by a spot method, using sodium light source. X-ray powder diffraction data is represented by the reflection lines at 7.40(100), 4.64(25), 3.68(68), 2.757(69), 2.530(49), 2.549(32), and 1.710(21${\AA}$), which compares very well with that of antigorite of serpentine group minerals. The major chemical compositions of the precious serpentine group minerals. The major chemical compositions of the precious serpentine are SiO2 42.49%, MgO 39.08%, Fe2O3 3.85%, and H2O 11.87%. Besides, trace elements such as Cr(2188), Ni(1110ppm), Co(58ppm), and Ta (108ppm) are relatively spectrum shows peaks at 3670, 1190, 1070, 980 and 610cm-1. Strong absorption at 3670cm-1 is due to OH stretching, and 1190, 1070 and 980cm-1 due to SiO stretching. The absorption 610cm-1 is formed by alteration of pre-existing ultramafic rock, namely peridotite, with an introduction of fluid with very little content of CO2, under 400$^{\circ}C$ environment. Magnetite inclusions, finely disseminated in the precious serpentine, may be a result of Fe precipitation, during serpentinization of olivine-bearing country rock.

• Composites Research
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• v.28 no.4
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• pp.155-161
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• 2015

A composite structure was fabricated with embedded impact detection capabilities for applications in Structural Health Monitoring (SHM). By embedding sensor functionality in the composite, the structure can successfully perform impact localization in real time. Smart resin, composed of $Pb(Ni_{1/3}Nb_{2/3})O_3-Pb(Zr,\;Ti)O_2$ (PNN-PZT) powder and epoxy resin with 1:30 wt%, was used instead of conventional epoxy resin in order to activate the sensor function in the composite structure. The embedded impact sensor in the composite was fabricated using Hand Lay-up and Vacuum Assisted Resin Transfer Molding(VARTM) methods to inject the smart resin into the glass-fiber fabric. The electrodes were fabricated using silver paste on both the upper and bottom sides of the specimen, then poling treatment was conducted to activate the sensor function using a high voltage amplifier at 4 kV/mm for 30 min at room temperature. The composite's piezoelectric sensitivity was measured to be 35.13 mV/N by comparing the impact force signals from an impact hammer with the corresponding output voltage from the sensor. Because impact sensor functionality was successfully embedded in the composite structure, various applications of this technique in the SHM industry are anticipated. In particular, impact localization on large-scale composite structures with complex geometries is feasible using this composite embedded impact sensor.

• Resources Recycling
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• v.28 no.5
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• pp.60-67
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• 2019

A valuable metal recovery from waste resources such as spent rechargeable secondary batteries is of critical issues because of a sharp increase in the amount of waste resources. In this context, it is necessary to research not only recycling waste lithium-ion batteries (LIBs), but also reusing valuable metals (e.g., Li, Co, Ni, Mn etc.) recovered from waste LIBs. In particular, the lithium hydroxide ($LiOH{\cdot}xH_2O$), which is of precursors that can be prepared by the recovery of Li in waste LIBs, can be reused as a catalyst, a carbon dioxide absorbent, and again as a precursor for cathode materials of LIB. However, most studies of recycling the waste LIBs have been focused on the preparation of lithium carbonate with a recovery of Li. Herein, we show the preparation of high purity lithium hydroxide powder along with the precipitation process, and the systematic study to find an optimum condition is also carried out. The lithium carbonate, which is recovered from waste LIBs, was used as starting materials for synthesis of lithium hydroxide. The optimum precipitation conditions for the preparation of LiOH were found as follows: based on stirring, reaction temperature $90^{\circ}C$, reaction time 3 hr, precursor ratio 1:1. To synthesize uniform and high purity lithium hydroxide, 2-step precipitation process was additionally performed, and consequently, high purity $LiOH{\cdot}xH_2O$ powder was obtained.

• Resources Recycling
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• v.30 no.6
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• pp.43-52
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• 2021

In this study, the optimal nitration process for selective lithium leaching from powder of a spent battery cell (LiNi_xCo_yMn_zO₂, LiCoO₂) was studied using Taguchi method. The nitration process is a method of selective lithium leaching that involves converting non-lithium nitric compounds into oxides via nitric acid leaching and roasting. The influence of pretreatment temperature, nitric acid concentration, amount of nitric acid, and roasting temperature were evaluated. The signal-to-noise ratio and analysis of variance of the results were determined using L₁₆(4⁴) orthogonal arrays. The findings indicated that the roasting temperature followed by the nitric acid concentration, pretreatment temperature, and amount of nitric acid used had the greatest impact on the lithium leaching ratio. Following detailed experiments, the optimal conditions were found to be 10 h of pretreatment at 700℃ with 2 ml/g of 10 M nitric acid leaching followed by 10 h of roasting at 275℃. Under these conditions, the overall recovery of lithium exceeded 80%. X-ray diffraction (XRD) analysis of the leaching residue in deionized water after roasting of lithium nitrate and other nitrate compounds was performed. This was done to determine the cause of rapid decrease in lithium leaching rate above a roasting temperature of 400℃. The results confirmed that lithium manganese oxide was formed from lithium nitrate and manganese nitrate at these temperatures, and that it did not leach in deionized water. XRD analysis was also used to confirm the recovery of pure LiNO₃ from the solution that was leached during the nitration process. This was carried out by evaporating and concentrating the leached solution through solid-liquid separation.