• Korean Journal of Materials Research
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• v.20 no.3
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• pp.142-147
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• 2010

Nano-sized $BaNd_2Ti_5O_{14}$ powders were prepared by the spray pyrolysis process. Sucrose used as the organic additive enabled the formation of nano-sized $BaNd_2Ti_5O_{14}$ powders. The powders prepared from the spray solution without sucrose had a spherical shape, dense structure and micron size before and after calcination. However, the precursor powders prepared from the spray solution with sucrose had a large size, and hollow and porous morphology. The precursor powders had an amorphous crystal structure because of the short residence time of the powders inside the hot wall reactor. The complete decomposition of sucrose did not occur inside the hot wall reactor. Therefore, the precursor powders obtained from the spray solution with sucrose of 0.5M had a carbon content of 39.2wt.%. The powders obtained from the spray solution with sucrose of 0.5M had a slightly aggregated structure of nano-sized primary powders of $BaNd_2Ti_5O_{14}$ crystalline phase after calcination at $1000^{\circ}C$. The calcined powders turned into nano-sized $BaNd_2Ti_5O_{14}$ powders after milling. The mean size of the $BaNd_2Ti_5O_{14}$ powders was 125 nm.

• Journal of the Korean Society for Heat Treatment
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• v.4 no.1
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• pp.13-18
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• 1991

The formation of high $T_c$ phase is very sluggish and c parameter of unit cell of high $T_c$ phase is about $37{\AA}$. High $T_c$ oxide superconductor with a $T_c$ above 100 K has been successfully prepared by solid state reaction method in BiSrCaCuO system by Pb adding. The microstructure related to the formation of the high $T_c$ phase has been investigated. As compared with YBCO compound, the formation reaction of the high $T_c$ requires long time heat treatment. It is due to the transformation from the low $T_c$ phase to high $T_c$ phase. The sintering just below the melting point of the calcined powder mixture is effective on the formation of the high $T_c$ phase in Pb-added BiSrCaCuO system. The growth of the high $T_c$ superconducting phase has a thin plate shape, which is characterized by the c parameter of $37{\AA}$. The formation of the high $T_c$ phases is delayed by the excessive addition of Pb. The lattice parameter(c) of the unit cell (both the low and high $T_c$ phases) is increased with increase of Pb.

• Nuclear Engineering and Technology
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• v.54 no.3
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• pp.1062-1070
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• 2022

In the present communication, pure and stable α-Bismuth Oxide (Bi₂O₃) nanoparticles (NPs) were synthesized by low temperature solution combustion method using urea as a fuel and calcined at 500℃. The synthesized sample was characterized by using powder X-ray Diffraction (PXRD), Scanning Electron Microscopy (SEM), Energy dispersive X-ray analysis (EDAX), Transmission Electron Microscopy (TEM), Fourier Transform Infrared Spectroscopy (FTIR) and UV-Visible absorption spectroscopy. The PXRD pattern confirms the formation of mono-clinic, stable and low temperature phase α-Bi₂O₃. The direct optical energy band gap was estimated by using Wood and Tauc's relation which was found to be 2.81 eV. The characterized sample was studied for X-ray/gamma ray shielding properties in the energy range 0.081-1.332 MeV using NaI (Tl) detector and multi channel analyzer (MCA). The measured shielding parameters agrees well with the theory, whereas, slight deviation up to 20% is observed below 356 keV. This deviation is mainly due to the influence of atomic size of the target medium. Furthermore an accurate theory is necessary to explain the interaction of X-ray/gamma ray with the NPs.The present work opens new window to use this facile, economical, efficient, low temperature method to synthesize nanomaterials for X-ray/gamma ray shielding purpose.

• Nanomaterials
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• v.12 no.7
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• pp.1158-1168
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• 2022

Commercial lithium-ion batteries using liquid electrolytes are still a safety hazard due to their poor chemical stability and other severe problems, such as electrolyte leakage and low thermal stability. To mitigate these critical issues, solid electrolytes are introduced. However, solid electrolytes have low ionic conductivity and inferior power density. This study reports the optimization of the synthesis of sodium superionic conductor-type Li_1.5Al_0.3Si_0.2Ti_1.7P_2.8O₁₂ (LASTP) solid electrolyte. The as-prepared powder was calcined at 650 ℃, 700 ℃, 750 ℃, and 800 ℃ to optimize the synthesis conditions and yield high-quality LASTP powders. Later, LASTP was sintered at 950 ℃, 1000 ℃, 1050 ℃, and 1100 ℃ to study the dependence of the relative density and ionic conductivity on the sintering temperature. Morphological changes were analyzed using field-emission scanning electron microscopy (FE-SEM), and structural changes were characterized using X-ray diffraction (XRD). Further, the ionic conductivity was measured using electrochemical impedance spectroscopy (EIS). Sintering at 1050 ℃ resulted in a high relative density and the highest ionic conductivity (9.455 × 10^-4 S cm^-1). These findings corroborate with the activation energies that are calculated using the Arrhenius plot. Therefore, the as-synthesized superionic LASTP solid electrolytes can be used to design high-performance and safe all-solid-state batteries.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.16 no.5
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• pp.216-221
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• 2006

An investigation of the influence of $WO_3$ and $V_2O_5$ catalysts on the microstructure, phase formation and selective catalytic reduction (SCR) efficiency of the synthesized SCR powders has been carried out. A commercial anatase-$TiO_2$ was used as the catalysts support. For $WO_3(10wt%)/TiO_2$, the W loading to the $TiO_2$ support led to the lower in anatase to rutile transition temperature from $1200^{\circ}C$ of $TiO_2$ support to ${\sim}900^{\circ}C$. The transition temperature was also lowered to below $650^{\circ}C$ in the $V_2O_5$(5 and 10 wt%) added composition. The $WO_3(10wt%)/TiO_2$ SCR powder obtained at $450^{\circ}C$ showed near 100% of $NO_x$ conversion efficiency at $350{\sim}400^{\circ}C$ and for the powder prepared at $650^{\circ}C$ the same efficiency was achieved in wider temperature range $300{\sim}400^{\circ}C$. The highest $NO_x$ conversion efficiency of 100% was obtained in the $V_2O_5(5wt%)/TiO_2$ SCR composition calcined at $650^{\circ}C$ in the relatively wider temperature range $250{\sim}350^{\circ}C$, while the catalytic efficiency considerably decreased for the $V_2O_5(10wt%)/TiO_2$. The lowered conversion efficiency of $NO_x$ observed in the $V_2O_5(10wt%)/TiO_2$ composition calcined at $650^{\circ}C$ was considered to be correlated with the lowered surface area resulting from the increased crystallite growth by highly reactive vanadium loading.

• Journal of the Korean Ceramic Society
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• v.39 no.1
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• pp.68-73
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• 2002

The dielectric properties and synthesis of $LaAlO_3$ ceramics from mixtures of $La_2O_3-Al_2O_3$ (LAO) and $La_2O_3-Al(OH)_3$(LAH) via grinding process were investigated. The single phase $LaA1O_3$of LAO and LAH powders were formed at $1300^{\circ}C$ and $1000^{\circ}C$, respectively. A non-reacted $La_2O_3$ existing in calcined powder was changed to La(OH)$_3$by moisture in the air, and their samples were worse than those of the samples made from a $LaA1O_3$single phase powder. The densities of LAO samples sintered at 150$0^{\circ}C$ for 4 h and LAH samples sintered at $1400^{\circ}C$ for 4 h were 97.3% and 98.3% of theory density, respectively. Grains of LAH sample showed uniformity and their sizes were 0.75 ${\mu}{\textrm}{m}$, and LAO samples showed non-uniformity and their sizes were 4-5 ${\mu}{\textrm}{m}$. Dielectric constant of LAO and LAH samples were the same value (≒22), however dielectric loss of LAH sample (0.0003) were lower than that of LAO sample(0.001)due to grain size.

• Journal of the Korean Ceramic Society
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• v.39 no.11
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• pp.1074-1082
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• 2002

Nanocomposite PMN-PT-BT/Ag/MgO was prepared by sintering at $950{\circ}C$ with addition of $AgNO_3$ and MgO sol to the PMN-PT-BT powder sinterable at $1200{\circ}C$. The low-temperature-sinterable PMN-PT-BT/Ag powder prepared by the modified mixed oxide method was calcined at $600{\circ}C$ for 1h and surface modified with the MgO sol of 0-10 wt% and then subjected to consolidation at $850-950{\circ}C$ for 4h under a flowing oxygen. The nanocomposite PMN-PT-BT/Ag/MgO(0.5wt%) sintered at $950{\circ}C$ showed the microstructure with grains of $1-3{\mu}m$, the second phase of MgO of $0.1-0.3{\mu}m$ by SEM and Ag of << $1{\mu}m$ qualitatively by SIMS. It showed the sintered relative density of 99%, the room temperature dielectric constant of 17200, the dielectric loss of 2.1% and the specific resistivity of $5.46{\times}10^{12}{\Omega}{\cdot}cm$. But the PMN-PT-BT/Ag/MgO(0 wt%) nanocomposite sintered at $950{\circ}C$ showed a little better properties : the sintered relative density of 99.5%, the room temperature dielectric constant of 19500, the dielectric loss of 2.1% and the specific resistivity of $7.30{\times}10^{12}{\Omega}{\cdot}cm$.

• Korean Journal of Materials Research
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• v.22 no.7
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• pp.346-351
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• 2012

$Li_{1+x}Al_xTi_{2-x}(PO_4)_3$(LATP) is a promising solid electrolyte for all-solid-state Li ion batteries. In this study, LATP is prepared through a sol-gel method using relatively the inexpensive reagents $TiCl_4$. The thermal behavior, structural characteristics, fractured surface morphology, ion conductivity, and activation energy of the LATP sintered bodies are investigated by TG-DTA, X-ray diffraction, FE-SEM, and by an impedance method. A gelation powder was calcined at $500^{\circ}C$. A single crystalline phase of the $LiTi_2(PO_4)_3$(LTP) system was obtained at a calcination temperature above $650^{\circ}C$. The obtained powder was pelletized and sintered at $900^{\circ}C$ and $1000^{\circ}C$. The LTP sintered at $900{\sim}1000^{\circ}C$ for 6 h had a relatively low apparent density of 75~80%. The LATP(x = 0.3) pellet sintered at $900^{\circ}C$ for 6 h was denser than those sintered under other conditions and showed the highest ion conductivity of $4.50{\times}10^{-5}$ S/cm at room temperature. However, the ion conductivity of LATP (x = 0.3) sintered at $1000^{\circ}C$ decreased to $1.81{\times}10^{-5}$ S/cm, leading to Li volatilization and abnormal grain growth. For LATP sintered at $900^{\circ}C$ for 6 h, x = 0.3 shows the lowest activation energy of 0.42 eV in the temperature range of room temperature to $300^{\circ}C$.

• 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 the Korean Ceramic Society
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• v.41 no.12 s.271
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• pp.921-928
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• 2004

Calcium phosphate powders have been prepared by using $Ca(OH)_2\;and\;H_{3}PO_4$ solution under various conditions such as pH, calcination temperature, and reaction time. ${\beta}-TCP({\beta}-tricalcium phosphate)$and HAp(hydroxyapatite) were synthesized at pH=5.21 and pH > 7.62, respectively. From XRD results, $Ca(OH)_2\;and\;H_{3}PO_4$ solution reacted quickly to form HAp, which was structurally stable up to 16h. Calcination temperature having good crystallinity is revealed to be at $1200^{\circ}C$. SEM analysis showed that ${\beta}-TCP$ and HAp with needle type were synthesized at pH 5.21 and pH 7.62, respectively. However, at pH 9.16, tiny and homogeneous HAp having sphere was prepared and rearranged to show needle morphology. HAp synthesized at pH 9.16 was utilized as bonechina body and calcined. The sample was analyzed its crystallinity, water absorbtion, color, and shape to check physical properties.