• Bulletin of the Korean Chemical Society
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• 제30권8호
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• pp.1719-1723
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• 2009

The LiFeP$O_4$ powder was synthesized by using the solid state reaction method with Fe($C_2O_4){\cdot}2H_2O,\;(NH_4)_2HPO_4,\;Li_2CO_3$, and chitosan as a carbon precursor material for a cathode of a lithium-ion battery. The chitosan added LiFePO4 powder was calcined at 350 ${^{\circ}C}$ for 5 hours and then 800 ${^{\circ}C}$ for 12 hours for the calcination. Then we calcined again at 800 ${^{\circ}C}$ for 12 hours. We characterized the synthesized compounds via the crystallinity, the valence states of iron ions, and their shapes using TGA, XRD, SEM, TEM, and XPS. We found that the synthesized powders were carbon-coated using TEM images and the iron ion is substituted from 3+ to 2+ through XPS measurements. We observed voltage characteristics and initial charge-discharge characteristics according to the C rate in LiFeP$O_4$ batteries. The obtained initial specific capacity of the chitosan added LiFeP$O_4$ powder is 110 mAh/g, which is much larger than that of LiFeP$O_4$ only powder.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제42회 동계 정기 학술대회 초록집
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• pp.100-101
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• 2012

The plasma damage free and room temperature processedthin film deposition technology is essential for realization of various next generation organic microelectronic devices such as flexible AMOLED display, flexible OLED lighting, and organic photovoltaic cells because characteristics of fragile organic materials in the plasma process and low glass transition temperatures (Tg) of polymer substrate. In case of directly deposition of metal oxide thin films (including transparent conductive oxide (TCO) and amorphous oxide semiconductor (AOS)) on the organic layers, plasma damages against to the organic materials is fatal. This damage is believed to be originated mainly from high energy energetic particles during the sputtering process such as negative oxygen ions, reflected neutrals by reflection of plasma background gas at the target surface, sputtered atoms, bulk plasma ions, and secondary electrons. To solve this problem, we developed the NBAS (Neutral Beam Assisted Sputtering) process as a plasma damage free and room temperature processed sputtering technology. As a result, electro-optical properties of NBAS processed ITO thin film showed resistivity of $4.0{\times}10^{-4}{\Omega}{\cdot}m$ and high transmittance (>90% at 550 nm) with nano- crystalline structure at room temperature process. Furthermore, in the experiment result of directly deposition of TCO top anode on the inverted structure OLED cell, it is verified that NBAS TCO deposition process does not damages to the underlying organic layers. In case of deposition of transparent conductive oxide (TCO) thin film on the plastic polymer substrate, the room temperature processed sputtering coating of high quality TCO thin film is required. During the sputtering process with higher density plasma, the energetic particles contribute self supplying of activation & crystallization energy without any additional heating and post-annealing and forminga high quality TCO thin film. However, negative oxygen ions which generated from sputteringtarget surface by electron attachment are accelerated to high energy by induced cathode self-bias. Thus the high energy negative oxygen ions can lead to critical physical bombardment damages to forming oxide thin film and this effect does not recover in room temperature process without post thermal annealing. To salve the inherent limitation of plasma sputtering, we have been developed the Magnetic Field Shielded Sputtering (MFSS) process as the high quality oxide thin film deposition process at room temperature. The MFSS process is effectively eliminate or suppress the negative oxygen ions bombardment damage by the plasma limiter which composed permanent magnet array. As a result, electro-optical properties of MFSS processed ITO thin film (resistivity $3.9{\times}10^{-4}{\Omega}{\cdot}cm$, transmittance 95% at 550 nm) have approachedthose of a high temperature DC magnetron sputtering (DMS) ITO thin film were. Also, AOS (a-IGZO) TFTs fabricated by MFSS process without higher temperature post annealing showed very comparable electrical performance with those by DMS process with $400^{\circ}C$ post annealing. They are important to note that the bombardment of a negative oxygen ion which is accelerated by dc self-bias during rf sputtering could degrade the electrical performance of ITO electrodes and a-IGZO TFTs. Finally, we found that reduction of damage from the high energy negative oxygen ions bombardment drives improvement of crystalline structure in the ITO thin film and suppression of the sub-gab states in a-IGZO semiconductor thin film. For realization of organic flexible electronic devices based on plastic substrates, gas barrier coatings are required to prevent the permeation of water and oxygen because organic materials are highly susceptible to water and oxygen. In particular, high efficiency flexible AMOLEDs needs an extremely low water vapor transition rate (WVTR) of $1{\times}10^{-6}gm^{-2}day^{-1}$. The key factor in high quality inorganic gas barrier formation for achieving the very low WVTR required (under ${\sim}10^{-6}gm^{-2}day^{-1}$) is the suppression of nano-sized defect sites and gas diffusion pathways among the grain boundaries. For formation of high quality single inorganic gas barrier layer, we developed high density nano-structured Al2O3 single gas barrier layer usinga NBAS process. The NBAS process can continuously change crystalline structures from an amorphous phase to a nano- crystalline phase with various grain sizes in a single inorganic thin film. As a result, the water vapor transmission rates (WVTR) of the NBAS processed $Al_2O_3$ gas barrier film have improved order of magnitude compared with that of conventional $Al_2O_3$ layers made by the RF magnetron sputteringprocess under the same sputtering conditions; the WVTR of the NBAS processed $Al_2O_3$ gas barrier film was about $5{\times}10^{-6}g/m^2/day$ by just single layer.

• 전기화학회지
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• 제15권2호
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• pp.101-108
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• 2012

본 연구에서는 탄소를 첨가하여 $Li_3V_2(PO_4){_3}$의 낮은 전기전도도를 개선시켜서 고율 방전특성, 충 방전 사이클 특성을 향상시키는 것을 목적으로 하고 있다. 탄소 첨가제로는 글루코스와 CNT (carbon nano tube)를 사용하였으며, 탄소의 첨가 여부와 탄소 원료의 종류에 따라 합성된 $Li_3V_2(PO_4){_3}$의 구조적 그리고 전기화학적 특성에 대해 연구를 하였다. $Li_3V_2(PO_4){_3}$와 $Li_3V_2(PO_4){_3}$/C의 $Li_3V_2(PO_4){_3}$/CNT의 합성방법으로는 고상법을 이용하였다. 합성된 물질을 수소환원방법을 통하여 600, 700, 800, $900^{\circ}C$에서 소성해주었다. 합성된 물질로 양극 집전판을 제작하여 상대전극을 리튬메탈로 한 Coin 2032 cell을 만들어 전기화학적 특성분석을 진행하였다. 전지테스트는 정전류법을 이용하여 3.0~4.8 V까지 충 방전 실험을 하였다.

• 한국수소및신에너지학회논문집
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• 제25권4호
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• pp.436-442
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• 2014

$LaCoO_3$ powders synthesized by Pechini process were pulverized by planetary ball-milling to decrease particle size and characterized as a catalyst in alkaline solution for oxygen reduction and evolution reaction (ORR & OER). The changes of physical properties, such as particle size distribution, surface area and electric conductivity, were analyzed as a function of ball-milling time. Also, the variations of the crystal structure and surface morphology of ball-milled powders were examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The electrochemically catalytic activities of the intrinsic $LaCoO_3$ powders decreased with increasing ball-milling time, but their electrochemical performance as an electrode improved by the increase of the surface area of the powder.

• Journal of the Korean Physical Society
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• 제73권12호
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• pp.1863-1866
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• 2018

The sodium-iron phosphate maricite-$NaFe_{0.9}Mn_{0.1}PO_4$ was synthesized using the ball mill method. The crystal structure and magnetic properties of the prepared materials were studied using X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and $M{\ddot{o}}ssbauer$ spectroscopy. Structural refinement of maricite-$NaFe_{0.9}Mn_{0.1}PO_4$ was analyzed using the FullProf program. From the XRD patterns, the crystal structure of maricite-$NaFe_{0.9}Mn_{0.1}PO_4$ was found to be orthorhombic with the space group Pmnb. The lattice parameters of maricite-$NaFe_{0.9}Mn_{0.1}PO_4$ are as follows: $a_0=6.866{\AA}$, $b_0=8.988{\AA}$, $c_0=5.047{\AA}$, and $V=311.544{\AA}^3$. Maricite-$NaFePO_4$ has an edge-sharing structure that consists of $FeO_6$ octahedral. Under an applied field of 100 Oe, the temperature dependences of zero-field-cooled (ZFC) and field-cooled (FC) curves were measured from 4.2 to 295 K. $M{\ddot{o}}ssbauer$ spectra were also recorded at various temperatures ranging from 4.2 to 295 K. We thus confirmed that the $N{\acute{e}}el$ temperature of $NaFe_{0.9}Mn_{0.1}PO_4$ ($T_N=14K$) was lower than that of maricite-$NaFePO_4$ ($T_N=15K$).

• 한국전기전자재료학회논문지
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• 제25권5호
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• pp.398-402
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• 2012

Synthesis of $Li_2MnSiO_4$ was attempted by the conventional solid-state reaction method, and the phase formation behavior according to the change of the calcination condition was investigated. When the mixture of the three source materials, $Li_2O$, MnO and $SiO_2$ powders, were used for calcination in air, it was difficult to develop the $Li_2MnSiO_4$ phase because the oxidation number of $Mn^{2+}$ could not be maintained. Therefore, two-step calcination was applied: $Li_2SiO_3$ was made from $Li_2O$ and $SiO_2$ at the first step, and $Li_2MnSiO_4$ was synthesized from $Li_2SiO_3$ and MnO at the second step. It was easy to make $Li_2MnSiO_3$ from $Li_2O$ and $SiO_2$. $Li_2MnSiO_4$ single phase was developed by the calcination at $900^{\circ}C$ for 24 hr in Ar atmosphere as the oxidation of $Mn^{2+}$ was prevented. However, the $Li_2MnSiO_4$ was ${\gamma}-Li_2MnSiO_4$, one of the polymorph of $Li_2MnSiO_4$, which could not be used as the cathode materials in Li-ion batteries. By applying the additional low temperature annealing at $400^{\circ}C$, the single phase ${\beta}-Li_2MnSiO_4$ powder was synthesized successfully through the phase transition from ${\gamma}$ to ${\beta}$ phase.