• Journal of the Korean Crystal Growth and Crystal Technology
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• v.6 no.2
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• pp.121-128
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• 1996

The optimum conditons were experimentally established for the powder synthesis and sintering of the feed-rods for $LiNbO_3$ crystal growth by a floating zone method. At the lower synthesis temperatures(700, $ 800^{\circ}C$) the minor amounts of $Li_2CO_3$ and $Nb_2O_5$ were present in the synthesized $LiNbO_3$ powder and at the higher temperature the particle size increased which is not favorable for the sintering process for the feed-rods. $LiNbO_3$ powder synthesized at $950^{\circ}C$ for 12 hours was found to be the best because it contains only the$LiNbO_3$ phase with the small particle size and uniform particle size distribution. As the sintering temperature and the soaking time increase, the sintered feed-rods exhibited the higher sintered density and grain growth phenomena. The $LiNbO_3$ feed rods sintering at $1100^{\circ}C$ for 2 hours were found to have the best microstructure for the precursor feed-rods of the floating zone crystal growth because of their higher density, small grain size and uniform particle size distribution. As the sintering temperature and the soaking time increase, the sintered feed-rods exhibited the higher sintered density and grain growth phenomena. The $LiNbO_3$ feed rods sintering at $1100^{\circ}C$ for 2 hours were found to have the best microstructure for the precursor feed-rods of the floating zone crystal growth because of their density, small grain size and uniform grain size distribution.

• Journal of Powder Materials
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• v.21 no.3
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• pp.185-190
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• 2014

$FeS_2$ has been widely used for cathode materials in thermal battery because of its high stability and current capability at high operation temperature. Salts such as a LiCl-KCl were added as a binder for improving electrical performance and formability of $FeS_2$ cathode powder. In this study, the effects of the addition of $Li_2O$ in LiCl-KCl binder on the formability of $FeS_2$ powder compact were investigated. With the increasing amount of $Li_2O$ addition to LiCl-KCl binder salts, the strength of the pressed compacts increased considerably when the powder mixture were pre-heat-treated above $350^{\circ}C$. The heat-treatment resulted in promoting the coating coverage of $FeS_2$ particles by the salts as $Li_2O$ was added. The observed coating as $Li_2O$ addition might be attributed to the enhanced wettability of the salt rather than its reduced melting temperature. The high strength of compacts by the $Li_2O$ addition and pre-heat-treatment could improve the formability of $FeS_2$ raw materials.

• Proceedings of the Materials Research Society of Korea Conference
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• 2010.05a
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• pp.37.2-37.2
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• 2010

Recently $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ has been consistently examined and investigated by scientists because of its high lithium storage capacity, which exceeds beyond the conventional theoretical capacity based on conventional chemical concepts. Consequently, $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ is considered as one of the most promising cathode candidates for next generation in Li rechargeable batteries. Yet the mechanism and the origin of the overcapacity have not been clarified. Previously, many authors have demonstrated simultaneous oxygen evolution during the first delithiation. However, it may only explain the high capacity of the first charge process, and not of the subsequent cycles. In this work, we report a clarified interpretation of the structural evolution of $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$, which is the key element in understanding its anomalously high capacity. We identify how the structural evolution of $Li_{1.2}Ni_{0.2}Mn_{0.6}O_2$ occurs upon the electrochemical cycling through careful study of electrochemical profiles, ex-situ X-ray diffraction (XRD), HR-TEM, Raman spectroscopy, and first principles calculation. Moreover, we successfully separated the structural change at subsequent cycles (mainly cation rearrangement) from the first charge process (mainly oxygen evolution with Li extraction) by intentionally synthesizing sample with large particle size. Consequently, the intermediate states of structural evolution could be well resolved. All observations made through various tools lead to the result that spinel-like cation arrangement and lithium environment are created and embedded in layered framework during repeated electrochemical cycling.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.25 no.6
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• pp.435-438
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• 2012

As lead-free piezoelectric materials, $Ag_2O$ doped $0.95(K_{0.5}Na_{0.5})NbO_3-0.05LiNbO_3+x$ mol% (where x = 0, 0.5, 1, 1.5, 2, 2.5 and 3, respectively) ceramics were fabricated by a conventional sintering process. The doping effects on the microstructure and electrical properties of the $0.95(K_{0.5}Na_{0.5})NbO_3-0.05LiNbO_3$ ceramics were systematically investigated. When the 3 mol % $Ag_2O$ doped $0.95(K_{0.5}Na_{0.5})NbO_3-0.05LiNbO_3$ samples were sintered at $1,080^{\circ}C$ for 5 hrs in air, these ceramics showed excellent values of density=4.20 $g/cm^3$, piezoelectric constant ($d_{33}$)=174 pC/N and phase transition temperature$(T_c)=421.6^{\circ}C$, respectively.

• Journal of the Korean Electrochemical Society
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• v.14 no.1
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• pp.16-21
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• 2011

$Li_4Sn_xTi_{5-x}O_{12}$ was manufactured by high energy ball milling (HEBM) and used as an anode material for lithium ion battery. Various amount of $SnO_2$was added to $Li_4Ti_5O_{12}$ and heated at different temperatures. The purpose of this research was to see the effect of $SnO_2$ addition into $Li_4Ti_5O_{12}$. Manufactured samples were analyzed by TGA, XRD, SEM, PSA. Battery cycler was used to test the charge/discharge properties of active materials. Heat treatment temperature of $800^{\circ}C$ was needed to make a stable structure of $Li_4Sn_xTi_{5-x}O_{12}$ and the particle size distribution was $0.2{\sim}0.6\;{\mu}m$. Charge/discharge process was repeated for 50 cycles at room temperature. The initial capacity was 168mAh/g and the voltage plateau was observed at 1.55V(Li/$Li^+$).

• Korean Journal of Materials Research
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• v.11 no.8
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• pp.671-678
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• 2001

All solid-state thin film micro supercapacitor, which consists of $RuO_2$/LiPON/$RuO_2$ multi layer structure, was fabricated on Pt/Ti/Si substrate using a $RuO_2$ electrode. Bottom $RuO_2$ electrode was grown by dc reactive sputtering system with increasing $O_2/[Ar+O_2]$ ratio at room temperature, and a LiPON electrolyte film was subsequently deposited on the bottom $RuO_2$ electrode at pure nitrogen ambient by rf reactive sputtering system. Room temperature charge-discharge measurements based on a symmetric $RuO_2$/LiPON/$RuO_2$ structure clearly demonstrates the cyclibility dependence on the microstructure of the $RuO_2$ electrode. Using both glancing angle x-ray diffraction (GXRD) and transmission electron microscopy (TEM) analysis, it was found that the microstructure of the $RuO_2$ electrode was dependent on the oxygen flow ratio. In addition, x- ray photoelectron spectroscopy(XPS) examination shows that the Ru-O binding energy is affected by increasing oxygen flow ratio. Furthermore, TEM and AES depth profile analysis after cycling demonstrates that the interface layer formed by interfacial reaction between LiPON and $RuO_2$ act as a main factor in the degradation of the cyclibility of the thin film micro-supercapacitor.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.24 no.3
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• pp.94-98
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• 2014

$LiCoO_2$ thin film has received diverse attention as cathodes material of thin-film micro-batteries. In this study, $LiCoO_2$ thin films were synthesized on Au substrates by sol-gel spin coating method and an annealing process. Their structures were studied using X-ray diffraction and Raman Spectroscopy. The particle morphologies of these thin films were observed by Scaning electron microscope. From the results of X-ray diffractometry and Raman Spectroscopy analyses, it was found that as-grown films had the structure of spinel (LT-$LiCoO_2$) and layered-Rock-salt (HT-$LiCoO_2$) at $550^{\circ}C$ and $750^{\circ}C$ respectively. The annealed films at $650^{\circ}C$ were presumed to be the mixed state of these two types. Throlugh the scanning electron microscope, It was estimated that the particle size in as-grown films at $750^{\circ}C$, were larger crystilline particle than in those at the other lower temperature and well distributed in the film.

• Resources Recycling
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• v.16 no.6
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• pp.10-19
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• 2007

The mechanical process followed by hydrometallurgical treatment has been developed in order to recover cobalt and lithium from spent lithium ion battery. In the previous study, a citrate precursor combustion process to prepare cathodic active materials from the leaching solution was elucidated. Resynthesis of electrode materials should be more valuable in spent battery recycling. Conventional slurry mixing of $LiCoO_2$ and carbon cannot make uniform distribution, and therefore the cathode cannot reach the theoretical charge-discharge capacity and is easily degraded during the charge-discharge cycling. In this study, ultra-fine $LiCoO_2$ powders has been prepared by modification of the combustion process and fabricated the enhanced cathode by modification of mixing method of $LiCoO_2$ and carbon added.

• Journal of the Korean Electrochemical Society
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• v.8 no.4
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• pp.172-176
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• 2005

Recently, many researches on the high-voltage 5 V class cathode material have focused on $LiNi_{0.5}Mn_{1.5}O_4$, where $Mn^{3+}$ in the existing $LiMn_2O_4 (Li[Mn^{3+}][Mn^{4+}]O_4)$ is replaced by $Ni^{2+}(Li[Ni^{2+}]_{0.5}[Mn^{4+}]_{1.5}O_4)$ in order to utilize $Ni^{2+}/Ni^{4+}$ redox reaction in the 5V region. The partial substitution of Mn in $LiMn_2O_4$ for other transition metal element, $LiM_yMn_{1-y}O_4$(M=Cr, Al, Ni, Fe, Co, Cu, Ga etc) is known as a good solution to overcome the problems associated with $LiMn_2O_4$ like the gradual capacity fading. In this study, we synthesized $LiNi_{0.5}Mn_{1.5}O_4$ through a mechanochemical process and investigated its morphological, crystallographic and electrochemical characteristics. The results showed that 4 V peaks had been found in the cyclic volammograms of the synthesized powders due to the existence of $Mn^{3+}$ from the incomplete substitution of $Ni^{2+}$ for $Mn^{3+}$ implying that the mechanochemical activation alone was not good enough to synthesize an exact stoichiometric compound of $LiNi_{0.5}Mn_{1.5}O_4$. The synthetic condition of mechanochemical process, such as type of starting materials, ball-mill and calcination condition was optimized for the best electrochemical performance.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2005.11a
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• pp.336-337
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• 2005

This study shows the effect of addition of $LiCoO_2$, with different milling time ranging from 0, 30, 200 hours, to the activated carbon electrode. Test cells consisting of activated carbon (100-X%) and $LiCoO_2$ (X%)were made (where X=10, 20, and 40). Test cells with varying concentrations of $LiCoO_2$ which differ in the milling time showed improved specific capacity compare with the cells fabricated using activated carbon alone. The enhanced capacity may be caused due to the addition of $LiCoO_2$ powders at varying concentration. An improved ESR value obtained may be caused by the smaller particle size of $LiCoO_2$. It was concluded that finer the particle size higher will be the efficiency.