• Korean Journal of Materials Research
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• v.21 no.12
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• pp.703-707
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• 2011

The electrochromic properties of tungsten oxide films grown by RF sputtering were investigated. Among the sputter parameters, first the $Ar:O_2$ ratios were controlled with division into only an $O_2$ environment, 1:1 and 4:1. The structure of each film prepared by these conditions was studied by X-ray diffraction, X-ray photoelectron spectroscopy and Rutherford backscattering spectroscopy. The sputter-deposited tungsten oxide films had an amorphous structure regardless of the $Ar:O_2$ ratios. The chemical compositions, however, were different from each other. The stoichiometric structure and low-density film was obtained at higher $O_2$ contents. Electrochemical tests were performed by cyclic voltammetry and chronoamperometry at 0.05 M $H_2SO_4$ solutions. The current density and charge ratio was estimated during the continuous potential and pulse potential cycling at -0.5 V and 1.8 V, respectively. The film grown in a higher oxygen environment had a higher current density and a reversible charge reaction during intercalation and deintercalation. The in-situ transmittance tests were performed by He-Ne laser (633 nm). At higher oxygen contents, a big transmittance difference was observed but the response speed was too slow. This was likely caused by higher film resistivity. Furthermore, the effect of sputtering pressure was also investigated. The structure and surface morphology of each film was observed by X-ray diffraction and scanning electron microscopy. A rough surface was observed at higher sputtering pressure, and this affected the higher transmittance difference and coloration efficiency.

• Applied Chemistry for Engineering
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• v.9 no.5
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• pp.786-790
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• 1998

K-GIC of the new carbon electrode to improve performance of carbon negative electrode in lithium ion secondary battery was prepated and its electrical characteristics were studied. Form this study, intercalated K quantity was increased in order of $2>3>1mole/{\ell}$ of KCl solution. And, for KCl solution of 1mole, the mole ratio of carbon and potassium was 156~388 carbon/potassium. The proper condition of K-GIC preparation was KCl solution of $1mole/{\ell}$, reaction temperature of $700^{\circ}C$, reaction time of 1 hour. From this condition, the intercalation and deintercalation behavior of lithium was very excellent. Also the reversibility was excellent.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.8 no.3
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• pp.435-441
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• 1998

Li-SGICs as a anode of lithium ion battery were synthesized by high-pressure method as a function of the Li-contents. The characteristics of these prepared compounds were determined from the studies with X-ray diffraction method and differential scanning calorimeter (DSC) analysis. From the results of X-ray diffraction, it was found that the lower stage intercalation compounds were formed with increase of Li-contents. The mixed stages in these compounds were also observed. In the case of the $Li_{30;wt%}$-SGIC, the compounds in the stage 1 structure were formed predominantly, but the structure of only pure stage 1, due to the structural defect of synthetic graphite, was not observed. The enthalpy and entropy changes of the compounds could be obtained from the differential scanning calorimetric analysis results. From the results, it was found that exothermic and endothermic reactions of Li-SGICs are related to thermal stability of lithium between artificial graphite layers.

• Journal of the Korean Electrochemical Society
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• v.3 no.2
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• pp.85-89
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• 2000

For replacing Li metal at Lithium ion Battery(LIB) system, we used carbon powder material which prepared by Pyrolysis of Phenol resin as starting material. It became amorphous carbon by Pyrolysis through it's self condensation by thermal treatment. Amorphous carbon can be doped with Li intercalation and deintercalation because it has wide interlayer. However, it has a problem with structural destroy due to weak carbon-carbon bond. So, we used $ZnCl_2$ as the pore-forming agent. This inorganic salt was used together with the resin serves not only as the pore-forming agent to form open pores, which grow into a three-dimensional network structure in the cured material, but also as the microstructure-controlling agent to form a loose structure doped with bulky dopants. We used SEM in order to find to difference of structure, and can calculate the distance of interlayer by XRD analysis. CV test showed oxidation and reduction.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.8 no.4
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• pp.660-666
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• 1998

We discussed structure, energy state, characteristics of thermal stability, and electrochemical properties of Li-GFICs, Li-PCICs, and Li-AGICs during the intercalation process. According to X-ray diffraction patterns, we observed phase of stage 2 mainly from Li-GFICs, while stage 1 phase as well as stage 2 from Li-PCICs. For the structure of Li-AGICs, stage 1 phase was dominant, but it was not possible to obtain pure stage 1 compound probably due to structural characteristics of artificial graphite. We measured energy state of the compounds to stage stability, and revealed that Li-AGICs and Li-GFICs were in more stable state than Li-PCICs. Therefore, those two compounds could be excellent candidate for energy reserve material. From the study of thermal degradation, Li-GFICs showed strong exothermic reaction at around 300 and $400^{\circ}C$. In the study of thermal stability of Li-AGIC at various temperatures, we observed that lithium was not completely deintercalated and high stage was maintained even at high temperature. In the case of charge, discharge, and electrochemical studies, Li-GFICs showed the best results.

• KIEE International Transactions on Electrophysics and Applications
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• v.4C no.1
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• pp.21-25
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• 2004

From the gradual increasing state of charge (GISOC) observations, electrochemical behavior of multi-walled carbon nanotube│(lM LiP $F_{6}$ , EC,DEC,DME 3:5:5 volume ratio)│lithium cells was evaluated using the galvanostatic charge-discharge process. A MWCNT delivers a specific charge capacity of 1,300 mAh/g in a Li cell when cycled up to an end voltage of 0 V (vs. Li/L $i^{＋}$ )at a constant current rate every 10 hours. However, in the present study, the specific discharge capacity obtained is 338 mAh/g, thus amounting to a coulombic efficiency of only 26％. Further, when the MWCNT│Li cells were tested using the GISOC method, two distinguishable linear-fit ranges were observed due to the intercalation/deintercalation of lithium, which were found to have II $E_1$, IIC $s_1$ and II $E_2$of 27.3％, 372 mAh/g, and 25.5％, respectively. Q $c_1$, could be calculated from the data of IIE and IICs of each range by the modified equation "II $C_{sum}$= $\Sigma$( $Q_{C}$- $Q_{D}$)=(II $E_{1}$$^{-1}$ ) $Q_{Dl}$ ＋(II $E_2$$^{-1}$ -1) ( $Q_{D2}$- $Q_{Dl}$ ) ＋ IIC $s_1$= $Q_{Cl}$ - $Q_{Dl}$ ". Results of the GISOC method could be converted to the results of galvanostatic charge-discharge process, irrespective of the state of charge of the cell or battery.ery.y.y.

• Transactions of the Korean hydrogen and new energy society
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• v.16 no.2
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• pp.142-149
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• 2005

[ $LiNiO_2$ ] was mixed with $TiO_2$ or ZnO for the preparation of a cathode. The electrochemical properties of the cathode were investigated and the effects of the addition of $TiO_2$ or ZnO were discussed. The first discharge capacity decreased as the quantity of the added $TiO_2$ or ZnO increased. It is probably due to the decrease in the area of reaction interface according to the increase in the amount of the added oxide. When 2wt.% and 5wt.% of oxides are added, the discharge capacity increased as the number of cycles increased. It is considered that this results from the increase in the area of reaction interface because the oxide is detached from the $LiNiO_2$ with the increase in the number of cycles. The 1wt.% $TiO_2$ or ZnO-added $LiNiO_2$ had a larger first charge capacity than $LiNiO_2$. This is considered to result from the deintercalation of Li ions in the Ni sites along with the Li ions in the Li sites.

• Proceedings of the Korean Vacuum Society Conference
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• 2000.02a
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• pp.167-167
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• 2000

전지 재료의 충방전 과정 연구에는 X-선 분말회절(x-ray powder diffraction techniques)과 중성자회절을 많이 사용하였다. 하지만 이러한 분석기술은 long-range order의 구조에 관한 정보를 제공하는데 유용하지만 atomic scale의 구조에 관한 정보를 얻기에는 한계가 있다. Li 전지에서의 전기화학적 반응에서는 cathode 물질에 포함된 전이금속의 산화, 환원 반응에 의한 Li 이온의 intercalation (charge process)과 deintercalation (discharge process) 현상이 일어난다. 이러한 충방전 과정은 알려지지 않은 다양한 형태의 위상 변화를 동반하게 되는데 x-선 이나 중성자를 이용한 powder diffraction techniques 로는 단지 정성적인 결정학적 정보를 얻을 수 있다. 따라서 최근에 원자 단위의 local structure에 관한 정보와 electrochemical state에 관한 정보를 동시에 얻을 수 있는 X-ray Absorption Fine Structure (XAFS) 분석기술을 Li 전지분석에 활용하기 시작하였다. XAFS는 하나의 x-ray 흡수원자에 대해서 주변원자들의 원자구조에 관한 정보와 구성 원소의 electrochemical state에 관한 정보를 얻을 수 있는 분석방법이다. X-ray Induced Electron Emission Spectroscopy (XIEES)는 x-ray에 의해서 방출된 전자를 검출하여 스펙트럼을 얻는 기능을 함축적으로 나타낸 것으로, x-ray를 물질 표면에 조사하여 발생하는 광전자, Auger 전자, 이차전자 등을 전자검출기(Channel Electron Multiplier: CEM)로 검출하는 기능과, 시료를 투과한 x-ray와 시료에서 발생하는 형광 x-ray를 비례계수기로 검출하는 기능을 가지고 있다. 이러한 검출 능력을 바탕으로 EXAFS, XANES, Standing Wave Technique, Elemental Composition Analysis, DXRD, Total Reflection Technique 등을 이용하여 물질을 구성하고 있는 원소의 성분, 미세원자구조, 전자구조에 관한 정보를 얻을 수 있는 새로운 spectrometer이다. 본 연구에서는 자체 개발한 XIEES의 XAFS 기능을 이용하여 여러 가지 방법으로 제조한 LiMn2-xO4와 LiMnO2, MnO2에서 Mn K-absorption edge에 대한 chemical state 변화를 측정하였다. Absorption edge에서 chemical shift를 측정하기 위해서는 방사광 가속기 수준의 에너지 분해능(~0.3eV)이 필요하다. 이번 연구에서는 SiO2(3140) monochromator를 사용하고 여기에 맞는 적절한 parameter를 적용하여 x-ray 에너지 분해능을 포항방사광가속기 수준으로 개선하였다. XIEES에서 얻은 스펙트럼과 포항방사광가속기에서 얻은 스펙트럼을 비교하였다. Chemical shift가 일어나는 경향은 두 실험 결과가 잘 일치하였다.

• Journal of Powder Materials
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• v.25 no.1
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• pp.7-11
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• 2018

In this study, we synthesize tungsten oxide thin films by electrodeposition and characterize their electrochromic properties. Depending on the deposition modes, compact and porous tungsten oxide films are fabricated on a transparent indium tin oxide (ITO) substrate. The morphology and crystal structure of the electrodeposited tungsten oxide thin films are investigated by scanning electron microscopy (SEM) and X-ray diffraction (XRD). X-ray photoelectron spectroscopy is employed to verify the chemical composition and the oxidation state of the films. Compared to the compact tungsten oxides, the porous films show superior electrochemical activities with higher reversibility during electrochemical reactions. Furthermore, they exhibit very high color contrast (97.0%) and switching speed (3.1 and 3.2 s). The outstanding electrochromic performances of the porous tungsten oxide thin films are mainly attributed to the porous structure, which facilitates ion intercalation/deintercalation during electrochemical reactions.

• Journal of the Korean Electrochemical Society
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• v.1 no.1
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• pp.28-32
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• 1998

The electrochemical behavior of film and charge-discharge capacity of Li-ion cell in 1 M $LiPF_6/EC:DME$ (1 : 1, by volume ratio) electrolyte solution was studied using chronopotentiometry, cyclic voltammetry, chronoamperometry, and impedance spectroscopy. The first irreversible capacity was higher than the second irrversible capacity because of solvent decomposition. Especially, passivation film that is electron insulating and ionic conducting were formed on the MPCF by solvent decomposition during the first charge. The solvated Li is co-intercalated with solvent into MPCF electrode. Part of the MPCF is expoliated during co-intercalation of solvent-Li. The MPCF ends up nonuniformly covered by a relatively thick layer of exfoliated particles embedded in a matrix of product by solvent decomposition.