• Journal of the Korean Crystal Growth and Crystal Technology
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• v.20 no.3
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• pp.141-146
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• 2010

$LiFePO_4$ doped with Cr showed improved electrochemical properties as a cathode material of lithium-ion batteries compared to the undoped. The improvement was thought that the doping would raise the electronic conductivity of the compounds. The electrical conductivity of $LiFe_{0.965}Cr_{0.03}B_{0.005}PO_4$ and $LiFe_{0.965}Cr_{0.03}Al_{0.005}PO_4$ powder was measured in the temperature range from 30 to $80^{\circ}C$. The doped powders were synthesized via mechanochemical milling and subsequent heat treatment at 675~$750^{\circ}C$ for 5~10h. The doping enhanced grain growth and electrical conductivity. The electrical conductivity of the $LiFe_{0.965}Cr_{0.03}Al_{0.005}PO_4$ powder at $30^{\circ}C$ was $1{\times}10^{-8}S/cm$, which was higher two orders of magnitude than that of the undoped.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.18 no.6
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• pp.248-252
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• 2008

To get a fine $LiFePO_4$ powder with high electrical conductivity, the influences of doping of aliovalent elements(Cr+B and Cr+Al) on electrical conductivity and of heat treatment conditions on particle size of the doped powders were studied. Two kinds of the doped powders $LiFe_{0.965}Cr_{0.03}B_{0.005}PO_4$ and $LiFe_{0.065}Cr_{0.03}Al_{0.005}PO_4$ were synthesized using mechanochemical milling and subsequent heat treatment at $675{\sim}750^{\circ}C$ for $5{\sim}10\;h$. The doping enhanced grain growth and electrical conductivity. The electrical conductivity at $30^{\circ}C$ was $1{\times}10^{-8}S/cm$ in the doped with Cr and Al, and $5{\times}10^{-10}S/cm$ in the undoped one.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.06a
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• pp.363-364
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• 2007

Phospho-olivine $LiFePO_4$ cathode materials were prepared by hydrothermal reaction at different temperatures. The structural performance of $LiFePO_4$ powders were characterized by X-ray diffraction (XRD). $LiFePO_4$/Li batteries were characterized electrochemically by charge/discharge experiments. The XRD results demonstrate that $LiFePO_4$ powder has an orthorhombic olivine-type structure with a space group of Pnmb. Among the synthesized cathode materials, $LiFePO_4$synthesized at $170^{\circ}C$ and subsequently annealed at $500^{\circ}C$ shows the best electrochemical properties. It shows initial discharge capacity of $167\;mAh\;g^{-1}$ (98% of the theoretical capacity) close to the theoretical capacity of $LiFePO_4$ ($170\;mAh\;g^{-1}$) at 0.1 C rate, which is ascribed to the enhanced degree of crystallinity, better phase purity, more spherical and more finely dispersed nanoparticles, crystallization and activation of small amount impurity.

• Journal of the Mineralogical Society of Korea
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• v.26 no.1
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• pp.35-44
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• 2013

Synthetic carbon-coated olivine-like structured lithium iron phosphate ($Li^+Fe^{2+}(PO_4)^{3-}/C$) powder composites were compressed up to 35.0 GPa in the symmetrical diamond anvil cell at room temperature. Bulk modulus of $LiFePO_4/C$ was determined to be $130.1{\pm}10.3$ GPa. New peak appears at the d-spacing of 3.386 ${\AA}$ above 18 GPa, and another new one at 2.854 ${\AA}$ around 35 GPa. The crystallographic symmetry of the sample (i.e. orthorhombic) is apparently retained up to 35 GPa as no clear evidence for the phase transition into spinel structure has been observed. The pressure-induced volume change in the M1 site ($Li^+O_6$) is more significant than those in M2($Fe^{2+}O_6$) and $PO_4$ tetrahedral sites.

• Journal of Electrochemical Science and Technology
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• v.11 no.3
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• pp.282-290
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• 2020

In this article, we report the effect of blended cathode materials on the performance of all-solid-state lithium-ion batteries (ASLBs) with oxide-based organic/inorganic hybrid electrolytes. LiFePO₄ material is good candidates as cathode material in PEO-based solid electrolytes because of their low operating potential of 3.4 V; however, LiFePO₄ suffers from low electric conductivity and low Li ion diffusion rate across the LiFePO₄/FePO₄ interface. Particularly, monoclinic Li₃V₂(PO₄)₃ (LVP) is a well-known high-power-density cathode material due to its rapid ionic diffusion properties. Therefore, the structure, cycling stability, and rate performance of the blended LiFePO₄/Li₃V₂(PO₄)₃ cathode material in ASLBs with oxidebased inorganic/organic-hybrid electrolytes are investigated by using powder X-ray diffraction analysis, field-emission scanning electron microscopy, Brunauer-Emmett-Teller sorption experiments, electrochemical impedance spectroscopy, and galvanostatic measurements.

• Clean Technology
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• v.30 no.1
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• pp.28-36
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• 2024

As demand for electric vehicles increases, the market for lithium-ion batteries is also rapidly increasing. The battery life of lithium-ion batteries is limited, so waste lithium-ion batteries are inevitably generated. Accordingly, lithium was selectively preleached from waste lithium iron phosphate (LiFePO₄, hereafter referred to as the LFP) cathode material powder among lithium ion batteries, and iron phosphate (FePO₄) powder was recovered. The recovered iron phosphate powder was mixed with alkaline sodium carbonate (Na₂CO₃) powder and heat treated to confirm its crystalline phase. The heat treatment temperature was set as a variable, and then the leaching rate and powder characteristics of each ingredient were compared after water leaching using Di-water. In this study, lithium showed a leaching rate of approximately 100%, and in the case of powder heat-treated at 800 ℃, phosphorus was leached by approximately 99%, and the leaching residue was confirmed to be a single crystal phase of Fe₂O₃. Therefore, in this study, lithium, phosphorus, and iron components were individually separated and recovered from waste LFP powder.

• Journal of the Korean Ceramic Society
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• v.43 no.2 s.285
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• pp.121-125
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• 2006

[ $LiFePO_4$ ] is one of the promising materials for cathode material of secondary lithium batteries due to its high energy density, low cost, environmental friendliness and safety. $LiFePO_4$ was synthesized by the solid-state reaction method at 500 - 800°C. The crystal structure of $LiFePO_4$ was analyzed by X-ray powder diffraction. The samples synthesized at 600 and $700^{\circ}C$ showed a single phase of a olivine structure. The particle sizes were increased and the specific surface areas were decreased with heating temperatures. The electrochemical performance was investigated by coin cell test. The discharge capacities at 0.1 C-rate were 118 mAh/g and 112 mAh/g at $600^{\circ}C,\;700^{\circ}C$, respectively. In an attempt to improve the electrical conductivity of cathode materials, $LiFePO_4/graphite$ composite was prepared with various graphite contents. The electrical conductivity and discharge capacity were increased with increasing the graphite contents in composite samples. The rate capabilities at high current densities were also improved.

• Bulletin of the Korean Chemical Society
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• v.30 no.8
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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.

• Journal of Hydrogen and New Energy
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• v.22 no.5
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• pp.728-734
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• 2011

$LiFePO_4$ is a promising cathode material for secondary lithium batteries due to its high energy density, low cost and safety. $LiFePO_4$ was synthesized by the citrate process under reductive, neutral, and oxidative, atmospheres and the crystal structure was analyzed by X-ray powder diffraction. The samples synthesized under $N_2$ and $H_2$ atmosphere showed a single phase of a olivine structure, where the samples synthesized under $O_2$ atmosphere exhibited second phase of $Fe2O_3$. All the samples synthesized at 400, 600 and $800^{\circ}C$ under $N_2$ atmosphere presented a single phase of olivine. Residual organic material was observed for the sample synthesized at $400^{\circ}C$. There was nearly no intensity difference between the samples synthesized at $600^{\circ}C$ and $800^{\circ}C$. The electrochemical characteristic of the $LiFePO_4$ synthesized at $600^{\circ}C$ in the $N_2$ atmosphere was analyzed. The result exhibited an high discharge capacity of 160 mAh/g at the first cycle, and 155-160 mAh/g after 45 cycles.

• Resources Recycling
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• v.31 no.4
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• pp.40-48
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• 2022

In waste lithium iron phosphate (LFP) batteries, the cathode material contains approximately 4% lithium. Recycling the constituent elements of batteries is important for resource circulation and for mitigating the environmental pollution. Li contained in the waste LFP cathode powder was selectively leached using persulfate-based oxidizing agents, such as sodium persulfate, potassium persulfate, and ammonium persulfate. Leaching efficiency and waste LFP powder properties were compared and analyzed. Pulp density was used as a variable during leaching, which was performed for 3 h under each condition. The leaching efficiency was calculated using the inductively coupled plasma (ICP) analysis of the leachate. All types of persulfate-based oxidizing agents used in this study showed a Li leaching efficiency over 92%. In particular, when leaching was performed using (NH₄)₂S₂O₈, the highest Li leaching percentage of 93.3% was observed, under the conditions of 50 g/L pulp density and an oxidizing agent concentration of 1.1 molar ratio.