• 한국신재생에너지학회:학술대회논문집
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• 2011.11a
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• pp.137.2-137.2
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• 2011

Poly (sodium 4-styrenesulfonate) (PSS) is ionomer based on polystyrene that is electrical conductivity and isoviscosity. LiFePO4 has been a promising electrode material however its poor conductivity limits practical application. To enhance the electronic conductivity of LiFePO4, in this study we prepared LiFePO4- PSS composite by the hydrothermal method. LiFePO4 was heated at $170^{\circ}C$ for 12h and then different wt% PSS (0%, 2.91%, 4.75%, 7.36%, 10%) are added to LiFePO4 and milled at 300rpm for 10h. And then the obtained powders were subsequently heated at $500^{\circ}C$ for 1h under argon flow. The cathode electrode were made from mixtures of LiFePO4-PSS: SP-270- PVDF in a weighting ratio 75%: 25%:5%. The electrochemical properties of LiFePO4- PSS/Li batteries were analyzed by cyclic voltammetry and charge/discharge tests. LiFePO4-C/Li battery with 4.75 wt% PSS displays discharge capacity of 128 mAh g-1 at room temperature that is considerably higher than pure LiFePO4/Li battery ( 113.48 mAhg-1).

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.06a
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• pp.303-303
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• 2008

$LiMn_2O_4$는 출력특성이 좋고 가격이 저렴하지만 전해액 중에서 $Mn^{2+}$이 용출되어 나오는 것과 반복적인 충방전시 구조가 파괴되는 단점이 있어 이것을 보완하고자 $FePO_4\cdot2H_2O$를 $LiMn_2O_4$의 표면에 코팅하였다, $LiMn_2O_4$를 모재로, $FePO_4\cdot2H_2O$를 코팅재로 사용하여 $FePO_4\cdot2H_2O$의 코팅량 변화와, 열처리 온도변화에 따른 물성 변화를살펴보았다, LiOH 와 $MnO_2$의 혼합물을 $1000^{\circ}C$ 에서 소성하여 $LiMn_2O_4$를 합성하고, Fe$(NO_3)_3$ 수용액과 $NH_4H_2PO_4$ 수용액을 혼합하여 $FePO_4\cdot2H_2O$를 제조하였다, $LiMn_2O_4$에 $FePO_4\cdot2H_2O$를 1wt%, 2wt%, 3wt% 비율로 ball milling 을 통해 코팅한 후, 온도를 변화시키면서 열처리 하였다. 코팅한 물질을 XRD를 통해 구조를 분석하고 SEM을 이용하여 형상을 관찰하였다. 또한 고온에서의 $Mn^{2+}$의 용출량을 ICP로 측정하고 half-cell을 만들어 충방전 test를 통해 충방전 특성을 조사하였다. 아울러, 코팅량과 열처리 온도 등 합성변수들이 소재특성 및 전기화학적 특성에 미치는 영향을 조사하였다.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.33 no.5
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• pp.167-173
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• 2023

Li₃V₂(PO₄)₃ and Li₃V₂(PO₄)₃/C composite with single phase monoclinic structure for the cathode materials are successfully synthesized by direct co-precipitation method using N₂H₄·H₂O as the reducing agent and alginic acid as the carbon source, and their electrochemical properties were compared. The particles with approximately 1~2 ㎛ size and the uniform spherical-like morphology of the narrow particle size distribution were obtained. In addition, the residual carbon can also improve the electrical conductivity. The Li₃V₂(PO₄)₃/C composite has improved initial specific discharge capacity and excellent cycle characteristics to maintain capacity stably than Li₃V₂(PO₄)₃. The results indicate that the reducing agent and carbon composite can affect the good crystallinity and electrochemical performance of the cathode materials.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2010.06a
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• pp.248-248
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• 2010

리튬이온 2차전지의 대체 양극 후보 물질인 $LiFePO_4$를 합성하기 위하여 출발원료로 $Li_2CO_3$, $Fe_2O_3$, $NH_4H_2PO_4$를 사용하여 볼밀 방법으로 혼합 분쇄한 후 열처리를 실시하였다. 합성 시에 3가 Fe를 2가로 환원시키기 위하여 $C_{12}H_{22}O_{11}$(흑설탕)을 출발원료와 함께 5 ~ 12 wt%로 나눠서 첨가하였다. 합성 후 XRD로 결정구조의 양질성을 확인하였고. FE-SEM으로 나노미터 크기의 구형 입자를 관찰하였다. XRF를 이용하여 3 ~ 10 wt%의 탄소 잔량을 확인하였다. 전기화학적 특성을 충 방전시험기로 평가한 결과, 8wt%의 탄소원을 첨가한 $LiFePO_4$에서 가장 좋은 수명 특성을 얻었고, 최대 145 mAh/g의 방전용량을 얻었다.

• Korean Journal of Materials Research
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• v.21 no.11
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• pp.587-591
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• 2011

The effect of the precipitator (NaOH, $NH_4OH$) and the amount of the precipitator (150, 200, 250, 300 ml) on the formation of $Fe_3(PO_4)_2$, which is the precursor used for cathode material $LiFePO_4$ in Li-ion rechargeable batteries was investigated by the co-precipitation method. A pure precursor of olivine $LiFePO_4$ was successfully prepared with coprecipitation from an aqueous solution containing trivalent iron ions. The acid solution was prepared by mixing 150 ml $FeSO_4$(1M) and 100 ml $H_3PO_4$(1M). The concentration of the NaOH and $NH_4OH$ solution was 1 M. The reaction temperature (25$^{\circ}C$) and reaction time (30 min) were fixed. Nitrogen gas (500 ml/min) was flowed during the reaction to prevent oxidation of $Fe^{2+}$. Single phase $Fe_3(PO_4)_2$ was formed when 150, 200, 250 and 300 ml NaOH solutions were added and 150, 200 ml $NH_4OH$ solutions were added. However, $Fe_3(PO_4)_2$ and $NH_4FePO_4$ were formed when 250 and 300 ml $NH_4OH$ was added. The morphology of the $Fe_3(PO_4)_2$ changed according to the pH. Plate-like lenticular shaped $Fe_3(PO_4)_2$ formed in the acidic solution below pH 5 and plate-like rhombus shaped $Fe_3(PO_4)_2$ formed around pH 9. For the $NH_4OH$, the pH value after 30 min reaction was higher with the same amount of additions of NaOH and $NH_4OH$. It is believed that the formation mechanism of $Fe_3(PO_4)_2$ is quite different between NaOH and $NH_4OH$. Further investigation on this mechanism is needed. The prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and the pH value was measured by pH-Meter.

• Korean Journal of Materials Research
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• v.29 no.9
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• pp.519-524
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• 2019

Spherical $Li_3V_2(PO_4)_3$ (LVP) and carbon-coated LVP with a monoclinic phase for the cathode materials are synthesized by a hydrothermal method using $N_2H_4$ as the reducing agent and saccharose as the carbon source. The results show that single phase monoclinic LVP without impurity phases such as $LiV(P_2O_7)$, $Li(VO)(PO_4)$ and $Li_3(PO_4)$ can be obtained after calcination at $800^{\circ}C$ for 4 h. SEM and TEM images show that the particle sizes are $0.5{\sim}2{\mu}m$ and the thickness of the amorphous carbon layer is approximately 3~4 nm. CV curves for the test cell are recorded in the potential ranges of 3.0~4.3 V and 3.0~4.8 V at a scan rate of $0.01mV\;s^{-1}$ and at room temperature. At potentials between 3.0 and 4.8 V, the third $Li^+$ ions from the carbon-coated LVP can be completely extracted, at voltages close to 4.51 V. The carbon-coated LVP exhibits an initial specific discharge capacity of $118mAh\;g^{-1}$ in the voltage region of 3.0 to 4.3 V at a current rate of 0.2 C. The results indicate that the reducing agent and carbon source can affect the crystal structure and electrochemical properties of the cathode materials.

• Korean Journal of Materials Research
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• v.19 no.4
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• pp.220-223
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• 2009

Lithium dihydrogen phosphate ($LiH_2PO_4$) powder was purchased from Aldrich Chemical Co. From the scanning electron microscope (SEM) observation, these polycrystals have dimensions in the range of $25-250{\mu}m$. The electrical conductivity was measured at a measuring frequency of 1 kHz on heating polycrystalline lithium dihydrogen phosphate ($LiH_2PO_4$) from room temperature to 493 K. Two anomalies appeared at 451 K ($T_{p1}$) and 469 K ($T_{p2}$). The electrical conductivity reached the magnitude of the superprotonic phases: $3{\times}10^{-2}{\Omega}^{-1}cm^{-1}$ at 451 K ($T_{p1}$) and $1.2{\times}10{\Omega}^{-1}cm^{-1}$ at 469 K ($T_{p2}$). It is uncertain whether the superprotonic phase transformations are due to polymorphic transitions in the bulk, surface transitions, or chemical reactions (thermal decomposition) at the surface. Considering several previous thermal studies (differential scanning calorimetry and thermogravimetry), our experimental results seem to be related to the last case: chemical reactions (thermal decomposition) at the surface with the progressive solid-state polymerization.

• Bulletin of the Korean Chemical Society
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• v.32 no.2
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• pp.536-540
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• 2011

This study reports the origin of the electrochemical improvement of $LiFePO_4$ when synthesized by wet milling using acetone without conventional carbon coating. The wet milled $LiFePO_4$ delivers 149 $mAhg^{-1}$ at 0.1 C, which is comparable to carbon coated $LiFePO_4$ and approximately 74% higher than that of dry milled $LiFePO_4$, suggesting that the wet milling process can increase the capacity in addition to conventional carbon coating methods. UV spectroscopy, elemental microanalysis, and evolved gas analysis are used to find the root cause of the capacity improvement during the mechanochemical reaction in acetone. The analytical results show that the improvement is attributed to the conductive residual carbon on the surface of the wet milled $LiFePO_4$ particles, which is produced by the reaction of $FeC_2O_4{\cdot}2H_2O$ with acetone during wet milling through oxygen deficiency in the precursor.

• Journal of Electrochemical Science and Technology
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• v.9 no.2
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• pp.85-92
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• 2018

Olivine structure of $LiFePO_4$ (LFP) is one of the most commonly used materials in aqueous rechargeable lithium batteries (ARLBs), and can store and release charge through the insertion/de-insertion of $Li^+$ between LFP and FP. We have fabricated LFP and LFP/FP electrodes on titanium paper and studied their electrochemical properties in 2 M $Li_2SO_4$. The LFP/FP electrode was determined to be a suitable electrode for electo-ostmotic pump (EOP) in terms of efficiency in water and 0.5 mM $Li_2SO_4$ solution. Experiments to determine the effect of cations and anions on the performance of EOP using LFP/FP electrode have shown that $Li^+$ is the best cation and that the anion does not significantly affect the performance of the EOP. As the concentration of $Li_2SO_4$ solution was increased, the current increased. The flow rate peaked at $4.8{\mu}L/30s$ in 1.0 mM $Li_2SO_4$ solution and then decreased. When the EOP was tested continuously in 1.0 mM $Li_2SO_4$ solution, the EOP transported approximately 35 mL of fluid while maintaining a stable flow rate and current for 144 h.

• Journal of Electrochemical Science and Technology
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• v.2 no.2
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• pp.103-109
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• 2011

Nanocrystalline $LiFePO_4$ powders were prepared at 660-$670^{\circ}C$ in an Ar atmosphere using two different synthetic routes, solid-state and sol-gel. Both materials showed well-developed XRD patterns without any impurity peaks. Particles composed in the range of 200-300 nm from the solid-state method, and 50-100 nm from the sol-gel method, were confirmed through scanning electron microscopy and dynamic light scattering. The $LiFePO_4$ obtained by the sol-gel method offered a high discharge capacity (153 mAh/g) and stable discharge behavior, even at elevated temperatures (50 and $60^{\circ}C$), whereas poor electrochemical performance was observed from the solid-state method. Rate capability studies for sol gel-derived $LiFePO_4$ ranged from 0.2 to 30 C, which revealed excellent retention over 70 cycles with a 99.9% capacity.