• Journal of the Korean Chemical Society
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• v.57 no.1
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• pp.12-19
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• 2013

The single-crystal structure of fully dehydrated partially $Li^+$-exchanged zeolite Y, ${\mid}Li_{50}Na_{25}{\mid}[Si_{117}Al_{75}O_{384}]$-FAU, was determined by single-crystal synchrotron X-ray diffraction techniques in the cubic space group $Fd\bar{3}m$ at 100(1) K. Ion exchange was accomplished by flowing stream of 0.1 M aqueous $LiNO_3$ for 2 days at 293 K, followed by vacuum dehydration at 623 K and $1{\times}10^{-6}$ Torr for 2 days. The structure was refined using all intensities to the final error indices (using only the 801 reflections with ($F_o$ > $4{\sigma}(F_o)$) $R_1/R_2=0.043/0.140$. The 50 $Li^+$ ions per unit cell are found at three different crystallographic sites. The 19 $Li^+$ ions occupy at site I' in the sodalite cavity: the $Li^+$ ions are recessed 0.30 ${\AA}$ into the sodalite cavity from their 3-oxygens plane (Li-O = 1.926(5) ${\AA}$ and $O-Li-O=117.7(3)^{\circ}$). The 20 $Li^+$ ions are found at site II in the supercage, being recessed 0.23 ${\AA}$ into the supercage (Li-O = 2.038(5) ${\AA}$ and $O-Li-O=118.7(3)^{\circ}$). Site III' positions are occupied by 11 $Li^+$ ions: these $Li^+$ ions bind strongly to one oxygen atom (Li-O = 2.00(8) ${\AA}$). About 25 $Na^+$ ions per unit cell are found at four different crystallographic sites: 4 $Na^+$ ions are at site I, 5 at site I', 12 at site II, and the remaining 4 at site III'.

• Corrosion Science and Technology
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• v.21 no.6
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• pp.445-453
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• 2022

SiO_x was prepared from a mixture of Si and SiO₂ via high-energy ball milling as a negative electrode material for Li-ion batteries. The molar ratio of Si to SiO₂ as precursors and the milling time were varied to identify the synthetic condition that could exhibit desirable anode performances. With an appropriate milling time, the material showed a unique microstructure in which amorphous Si nanoparticles were intimately embedded within the SiO₂ matrix. The interface between the Si and SiO₂ was composed of silicon suboxides with Si oxidation states from 0 to +4 as proven by X-ray photoelectron spectroscopy and electrochemical analysis. With the addition of a conductive carbon (Super P carbon black) as a coating material, the SiO_x/C manifested superior specific capacity to a commercial SiO_x/C composite without compromising its cycle-life performance. The simple mechanochemical method described in this study will shed light on cost-effective synthesis of high-capacity silicon oxides as promising anode materials.

• Bulletin of the Korean Chemical Society
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• v.33 no.10
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• pp.3303-3310
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• 2012

Two single crystals of fully dehydrated partially $Li^+$-exchanged zeolite X were prepared by the exchange of Na-X, $Na_{92}Si_{100}Al_{92}O_{384}$ (Si/Al = 1.09), with $Li^+$ using aqueous 0.1 M $LiNO_3$ at 293 (crystal 1) and 333 K(crystal 2), followed by vacuum dehydration at 623 K and $1{\times}10^{-6}$ Torr for 2 days. Their structures were determined by single-crystal synchrotron X-ray diffraction techniques in the cubic space group $Fd{\overline{3}}$ at 100(1) K. Their structures were refined using all intensities to the final error indices (using the 1281 and 883 reflections for which ($F_o$ > $4{\sigma}(F_o)$) $R_1/R_2$ = 0.075/0.244 and 0.074/0.223 for crystals 1 and 2, respectively. Their compositions are seen to be ${\mid}Li_{86}Na_6{\mid}[Si_{100}Al_{92}O_{384}]$-FAU and ${\mid}Li_{87}Na_5{\mid}[Si_{100}Al_{92}O_{384}]$-FAU, respectively. In crystal 1, 17 $Li^+$ ions per unit cell are at site I', 15 another site I', 30 at site II, and the remaining 16 at site III; 2 $Na^+$ ions are at site II and the remaining 4 at site III'. In crystal 2, 32 and 30 $Li^+$ ions per unit cell fill sites I' and II, respectively, and the remaining 25 at site III'; 2 and 3 $Na^+$ ions are found at sites II and III', respectively. The extent of $Li^+$ exchange increases slightly with increasing ion exchange temperature from 93% to 95%.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.17 no.12
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• pp.1283-1288
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• 2004

Metal-ferroelectric-insulator-semiconductor(WFIS) capacitors using rapid thermal annealed LiNbO$_3$/AlN/Si(100) structure were fabricated and demonstrated nonvolatile memory operations. The capacitors on highly doped Si wafer showed hysteresis behavior like a butterfly shape due to the ferroelectric nature of the LiNbO$_3$ films. The typical dielectric constant value of LiNbO$_3$ film in the MFIS device was about 27, The gate leakage current density of the MFIS capacitor was 10$^{-9}$ A/cm$^2$ order at the electric field of 500 kV/cm. The typical measured remnant polarization(2P$_{r}$) and coercive filed(Ec) values were about 1.2 $\mu$C/cm$^2$ and 120 kV/cm, respectively The ferroelectric capacitors showed no polarization degradation up to 10$^{11}$ switching cycles when subjected to symmetric bipolar voltage pulses of 1 MHz. The switching charges degraded only by 10 % of their initial values after 4 days at room temperature.e.

• Journal of the Korean Ceramic Society
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• v.31 no.6
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• pp.660-670
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• 1994

Transparent, crack-free dried gel monoliths with a composition of LiZr1.5Si2P2O12.5 have been synthesized by the low temperature polymerization of the Sol-Gel technique using metal alkoxides as starting materials. After initial reaction (20~40 min), each metal alkoxide closely paralleled each other during the hydrolysis reactions. The safe drying conditions of gels with no creaks the control of the shrinkage rate. The gels converted into the glass by heat treatment at 75$0^{\circ}C$. FTIR data indicated that the gels were phase separated into silicarich and phosphate-rich regions with the lithium. XRD results showed the formation of crystalline LiH2PO4. The gels dried at 15$0^{\circ}C$ or fired at 75$0^{\circ}C$ contained the residual water. The high ionic conductivity at room temperature for these gels was attributed to the motion of protons.

• Journal of the Korean Ceramic Society
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• v.48 no.4
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• pp.269-277
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• 2011

Glass-ceramics based on lithium disilicate($Li_2Si_2O_5$) are prepared by heat-treatment of glasses in a system of $SiO_2-Li_2O-K_2O-Al_2O_3$ with different compositions. The crystallization heat-treatment was conducted at the temperature range of $700{\sim}900^{\circ}C$ and samples were analyzed by XRD and SEM. Mechanical properties were determined by a Vicker's hardness and 4 point bending strength. When $SiO_2/Li_2O$ ratio increased, cristobalite and tridymite crystals showed more predominate than lithium disilicate crystals. Increase in $Al_2O_3$ contents in the glass suppressed crystallzation of lithium disilicate crystals. Increase in ZnO, $B_2O_3$ contents in the glass decreased crystallization temperature of lithium disilicate crystals, and increased mechanical properties because of the reduction of the lithium disilicate crystal size.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.28 no.6
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• pp.229-234
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• 2018

The glass-ceramic of $Li_2O-Al_2O_3-SiO_2$ system was synthesized by using $ZrO_2$, $ZrSiO_4$, $ZrOCl_2$ and $Zr(SO_4)_2$, which is a raw material of Zr serving as a nucleation agent. It was confirmed that Avrami parameter of these four glasses is over 3 for bulk crystallization. The glass synthesized by $ZrOCl_2$, and $Zr(SO_4)_2$ showed high melting quality during the melting process. It is also observed that the Zr component is uniformly distributed in the glass. Various characterizations was evaluated, including composition analysis and bending strength.

• Journal of the Korean institute of surface engineering
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• v.25 no.5
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• pp.215-221
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• 1992

This research is aimed at developing(110) preferred TiS2 cathode films and glass typed solid electro-lytes which have high ionic migrations and low electron conductivities for thin secondary solid batteries. To obtain preferred oriented TiS2 thin films on a substrate by CVD method using TiCl4 and H2S gases three factors of heating temperature, inner pressure of furnace and TiCl4/H2S gas mole fraction were ex-amined systematically. To obtain solid films of Li2O-B2O3-SiO2 electrolytes by r.f. sputtering for thin proto-type batteries of Li/Li2O-B2O3-SiO2TiS2, sputtering conditions were examined. TiS2 cathode films showed columnar structure, namely c axis oriented parallely. At low pressure of reaction chamber and low heating temperature, surface of smooth TiS2 films couldd be obtained. Ionic conductivity of Li2O-B2O3-SiO2 films manufactured by r.f. magnetron sputtering were 3$\times$10-7$\Omega$-1cm-1 and electron conductivities were 10-11$\Omega$-1cm-1. Open cell voltage of thin lithium batteries were 2.32V with a designed prototype cell.

• Applied Chemistry for Engineering
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• v.27 no.4
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• pp.444-448
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• 2016

Hollow silicon/carbon (H-Si/C) composites as anode materials for lithium ion batteries were investigated to overcome the large volume expansion. H-Si/C composites were prepared as follows; hollow $SiO_2\;(H-SiO_2)$ was prepared by adding $NaBH_4$ to $SiO_2$ synthesized using $st{\ddot{o}}ber$ method followed by magnesiothermic reduction and carbonization of phenolic resin. The H-Si/C composites were analyzed by XRD, SEM, BET and EDX. To improve the capacity and cycle performance, the electrochemical characteristics of H-Si/C composites synthesized with various $NaBH_4$ contents were investigated by charge/discharge, cycle, cyclic voltammetry and impedance tests. The coin cell using H-Si/C composite ($SiO_2:NaBH_4=1:1$ in weight) in the electrolyte of $LiPF_6$ dissolved in organic solvents (EC : DMC : EMC = 1 : 1 : 1 vol%) has better capacity (1459 mAh/g) than those of other composition coin cells. It is found that the coin cell ($SiO_2:NaBH_4=1:1$ in weight) has an excellent capacity retention from 2nd cycle to 40th cycle.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 1999.11a
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• pp.25-28
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• 1999

Metal ferroelectric semiconductor Field Effect- Transistors(MFSFET) with various gate electrodes, that are aluminum, platinum and poly -Si, using LiNbO$_3$/Si(100) structures were fabricated and the properties of the FETs have been discussed. The drain current of the state of FET with Pt electrode was more than 3 orders of magnitude larger than the state current at the same gate voltage of 1.5 V, 7.rich means the memory operation of the MFSFET. A write voltage as low as about $\pm$4 V, which is applicable to low power integrated circuits, was used for polarization reversal. The retention properties of the FET using Al electrode were quite good up to about 10$^3$s and using Pt electrode remained almost the same value of its initial value over 2 days at room temperature.