• Journal of the Korean Ceramic Society
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• v.50 no.5
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• pp.333-340
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• 2013

To fabricate spherical lithium titanate ($Li_2TiO_3$) pebbles which are used for a breeder material in fusion reactor, titanium oxide ($TiO_2$) granules were used as a starting material. The granules were pre-sintered, and then aqueous lithium nitrate solution infiltrated into the granules at vacuum condition. The granules were crystallized to $Li_2TiO_3$ after sintering under the control of process parameters. In this study, the concentration of lithium in the solution, as well as the number of penetration times and sintering temperature affected the final crystallite phase and the microstructure of the pebbles. In particular, the sphericity and size of the pebbles were effectively controlled by a technical rolling process. The useful spherical $Li_2TiO_3$ pebbles which have 10~20% porosity and 60~120 N compressive strength were obtained through the sintering at $1000{\sim}1100^{\circ}C$ in the multi-times infiltration process with 50 wt% solution. The physical properties of pebbles such as density, porosity and strength, can be controlled by a selection of $TiO_2$ powders and control of processing parameters. It can be thought that the lithium penetration method is a useful method for the fabrication of mass product of spherical $Li_2TiO_3$ pebbles.

• Applied Science and Convergence Technology
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• v.23 no.2
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• pp.72-82
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• 2014

Lithium-ion batteries (LIBs) have become popular electrochemical devices. Due to the unique advantages of LIBs in terms of high operating voltage, high energy density, low self-discharge, and absence of memory effects, their application range, which was primarily restricted to portable electronic devices, is now being extended to high-power applications, such as electric vehicles (EVs) and hybrid electrical vehicles (HEVs). Among various anode materials, $Li_4Ti_5O_{12}$ (LTO) is believed to be a promising anode material for high-power LIBs due to its advantages of high working potential and outstanding cyclic stability. However, the rate performance of LTO is limited by its intrinsically low electronic conductivity and poor $Li^+$ ion diffusion coefficient. This review highlights the recent progress in improving the rate performance of LTO through doping, compositing, and nanostructuring strategies.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.11a
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• pp.510-510
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• 2007

Titanate nanotube(TNT)는 높은 비표면적과 우수한 물리화학적 특성을 가지고 있어 광촉매, 수소 저장재료, 태양전지용 전극재료 등에 적용되고 있다. 또한, 티타네이트 나노튜브는 전자 이동이 원활한 구조적 특징을 가지고 있어 리듐 이차전지용 호스트 재료로서 많은 연구가 진행 중이다. 이에 본 연구에서는 저온균일침전법으로 제조한 루틸상 $TiO_2$ 분말에 Lithium chloride를 1~10wt%를 동시에 첨가한 후 10M의 sodium hydroxide 수용액 내에서 수열합성하여 리튬이 도핑된 티타네이트 나노튜브를 제조하였다. 제조된 분말의 입자형상 및 크기는 전자주사 현미경을 이용하여 관찰하였으며, X-선 회절분석을 이용하여 리튬 첨가에 따른 결정상 변화를 관찰하였다. 또한 리튬이 도핑된 티타네이트 나노튜브의 전기화학적 특성 평가를 위해 양극 활물질 : 도전제 : 바인더를 75 : 20 : 5의 비율로 혼합한 후 coin cell을 제조하였고, potentiostat를 이용하여 용량 측정 및 cycle 특성을 실시하였다. 수열 합성법에 의해 형성된 입자는 직경 10nm, 길이 수 ${\mu}m$로 관찰되었으며, X-선 회절 시험 결과 LiO와 같은 이차상은 발견되지 않았다. 측정된 coin cell의 용량은 240mAh/g을 나타내었으나, 싸이클 특성이 빠르게 저하됨을 확인할 수 있었다.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.279-279
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• 2010

한국형 헬륨 냉각 고체형 증식(Helium Cooled Solid Breeder : HCSB) 시험 블랑켓(Test Blanket Module : TBM)은 삼중수소 증식을 위해서 $Li_2TiO_3$ 및 $Li_4SiO_4$ 페블을 고려하고 있으며, 중성자 반사 재료로는 SiC가 코팅된 흑연 페블을 사용할 예정이다. $Li_2TiO_3$ 및 $Li_4SiO_4$ 페블을 제조하기 위해서는 먼저 각각의 분말 제조가 선행되어야 한다. $Li_2TiO_3$ 분말을 합성하기 위해서는 먼저 Lithium 금속염과 Isopropoxide를 용매 및 폴리머 캐리어로서의 두 가지 기능을 하는 에틸렌글리콜에 첨가한 후 가열하여 완전히 용해시킨 후 혼합 용액을 건조시켜 겔형의 전구체를 제조한다. 이를 하소한 후 결정화시켜 Titanate 분말을 얻는데 이때의 건조, 하소 및 결정화 온도의 조건에 따른 분말의 크기 및 특성이 각각 다르다. 즉 하소 온도가 $600^{\circ}C$ 미만이면 열분해된 폴리머로부터 잔유 탄소가 남게 되고, $700^{\circ}C$를 초과하면 결정화가 시작된다. 이렇게 얻어진 Titanate분말은 지르코니아 볼을 이용하여 약 24 시간 동안 볼 밀링 과정을 통해 입도분포가 좁은 미세한 Titanate 분말로 만들었다. $Li_2TiO_3$ 페블은 위의 과정에서 얻어진 미세분말에 바인더를 이용하여 페블화 시킨 후 $1200^{\circ}C$의 전기로에서 최종 소결한 것이다. 중성자 반사 재료인 흑연페블은 강도가 약하기 때문에 표면에 SiC를 수 ${\mu}m$ 코팅해서 사용할 예정이다. 선행실험으로 건식법을 이용하여 SiC 코팅을 실시했으며, 그 결과를 소개할 것이다.

• Journal of the Korean Electrochemical Society
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• v.9 no.1
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• pp.1-5
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• 2006

Lithium titanium oxide $(Li_4Ti_5O_{12})$ with spinel-framework structures as anode material for lithium-ion battery was prepared by sol-gel and high energy ball milling (HEBH) method. According to the X-ray diffraction (XRD), Particle Size Analyses(PSA) and scanning electron microscopy (SEM) analysis, uniformly distributed $Li_4Ti_5O_{12}$ particles with grain sizes of 100 nm were observed. Half cells, consisting of $Li_4Ti_5O_{12}$ as working electrode and lithium foil as both counter and reference electrodes showed the high performance of high rate discharge capacity and 173 mAh/g at 0.2C in the range of $1.0\sim2.5 V$. Furthermore, the crystalline structure of $Li_4Ti_5O_{12}$ didn't transform during the lithium intercalation and deintercalation process.

• Journal of Powder Materials
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• v.22 no.5
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• pp.315-320
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• 2015

The present work reports a systematic study of using carboxymethylated cellulose (CMC) as water-borne binder to produce $Li_4Ti_5O_{12}$-based anodes for manufacture of high rate performance lithium ion batteries. When the LTO-to-CB-to-CMC mass ratio is carefully optimized to be 8:1:0.57, the special capacity of the resulting electrodes is $144mAh{\cdot}g^{-1}$ at 10 C and their capacity retention was 97.7% after 1000 cycles at 1 C and 98.5% after 500 cycles at 5 C, respectively. This rate performance is comparable or even better than that of the electrolytes produced using conventional, organic, polyvinylidene fluoride binder.

• Bulletin of the Korean Chemical Society
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• v.33 no.12
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• pp.4059-4062
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• 2012

The effect of a conductive agent on the structural and electrochemical properties of $Li_4Ti_5O_{12}$(LTO) spinel was investigated through neutron diffraction during Li intercalation and electrochemical measurements. The charging process of LTO is known as transformation of the white $(Li_3)_{8a}[LiTi_5]_{16d}O_{12}$ into a dark-colored $(Li_{3-X})_{8a}[Li_{X+Y}]_{16c}[LiTi_5]_{16d}O_{12}$ by incorporating the inserted Li into octahedral 16c sites, and the Li in tetrahedral 8a sites shifted to 16c sites. The occupancy of the tetrahedral 8a site varied with the existence of carbon in the electrode. Without carbon, the lattice parameter and cell volume of LTO decreased more notably than in the carbon-containing LTO electrode during Li insertion process. These phenomena might be attributed that the Li occupancy of the tetrahedral 8a of the LTO electrode without carbon was less than that of the carbon-containing LTO electrode.

• Journal of the Korean Ceramic Society
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• v.41 no.8
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• pp.593-598
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• 2004

To make the all-solid-state lithium thin film battery having less than 1 fm in thickness, LiCoO$_2$ thin films were deposited on Pt/TiO$_2$/SiO$_2$/Si substrate as a function of Li/Co mole ratio and the deposition temperature by Pulsed Laser Deposition (PLD). Especially, LiCoO$_2$ thin films deposited at 50$0^{\circ}C$ with target of Li/Co=1.2 mole ratio show an initial discharge capacity of 53 $\mu$Ah/cm$^2$-$\mu$m and capacity retention of 67.6％. The microstructural and electrochemical properies of (Li, La)TiO3 thin films grown on LiCoO$_2$Pt/TiO$_2$/SiO$_2$/Si structures by Pulsed Laser Deposition (PLD) were investigated at various deposition temperatures. The thin films grown at 10$0^{\circ}C$ show an initial discharge capacity of approximately 51 $\mu$Ah/cm$^2$-$\mu$m and moreover show excellent discharge capacity retention of 90％ after 100 cycles. An amorphous (Li, La)TiO$_3$ solid electrolyte is possible for application to solid electrolyte for all-solid-state lithium thin film battery below 1 $\mu$m.

• Journal of the Korean Chemical Society
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• v.49 no.6
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• pp.560-566
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• 2005

Sintered ceramic samples of pure and some copper doped layered sodium lithium tri-titanate ($Na_{1.9}Li_{0.1}Ti_{3-X}Cu_XO_{7-X}$) materials with different dopant molar percentages (0.0$Cu^{2+}$ at $Ti^{4+}$ sites in the lattice is proposed in this paper. Furthermore, three distinct regions have been identified in log(${\sigma}_{d.c.}T$) versus 1000/T plots. The lowest temperature region is attributed to electronic hopping conduction(polaron) for all copper doped derivatives and ionic conduction for lithium substituted $Na_2Ti_3O_7$.The mechanism of conduction in the intermediate region is associated interlayer ionic conduction and in the highest temperature region is associated modified interlayer ionic conduction.

• Journal of Electrical Engineering and Technology
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• v.10 no.3
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• pp.1102-1106
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• 2015

A hybrid supercapacitor (HS) is an energy storage device used to enhance the low weight energy density (Wh/kg) of a supercapacitor. On the other hand, a sudden decrease in capacity has been pointed out as a reliability problem after many charge/discharge cycles. The reliability problem of a HS affects the early aging process. In this study, the capacity performance of a HS was observed after charge/discharge. For detailed analysis of the initial charge/discharge cycles, the charge and discharge curve was measured at a low current density. In addition, a solid electrolyte interphase (SEI) layer was confirmed after the charge/discharge. A HC composed of a lithium titanate (LTO) anode and active carbon cathode was used. The charge/discharge efficiency of the first cycle was lower than the late cycles and the charge/discharge rate was also lower. This behavior was induced by SEI layer formation, which consumed Li ions in the LTO lattice. The formation of a SEI layer after the charge/discharge cycles was confirmed using a range of analysis techniques.