• Korean Journal of Materials Research
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• v.24 no.5
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• pp.243-248
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• 2014

Silicon-carbon composite was prepared by the magnesiothermic reduction of mesoporous silica and subsequent impregnation with a carbon precursor. This was applied for use as an anode material for high-performance lithium-ion batteries. Well-ordered mesoporous silica(SBA-15) was employed as a starting material for the mesoporous silicon, and sucrose was used as a carbon source. It was found that complete removal of by-products ($Mg_2Si$ and $Mg_2SiO_4$) formed by side reactions of silica and magnesium during the magnesiothermic reduction, was a crucial factor for successful formation of mesoporous silicon. Successful formation of the silicon-carbon composite was well confirmed by appropriate characterization tools (e.g., $N_2$ adsorption-desorption, small-angle X-ray scattering, X-ray diffraction, and thermogravimetric analyses). A lithium-ion battery was fabricated using the prepared silicon-carbon composite as the anode, and lithium foil as the counter-electrode. Electrochemical analysis revealed that the silicon-carbon composite showed better cycling stability than graphite, when used as the anode in the lithium-ion battery. This improvement could be due to the fact that carbon efficiently suppressed the change in volume of the silicon material caused by the charge-discharge cycle. This indicates that silicon-carbon composite, prepared via the magnesiothermic reduction and impregnation methods, could be an efficient anode material for lithium ion batteries.

• Polymer(Korea)
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• v.36 no.1
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• pp.88-92
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• 2012

Long-term performance of polymer under constant sustained load has been the main research focus, which created a need for the accelerated test method providing proper lifetime assessment. Cycling fatigue loading is one of the accelerated test method and has been of great interest. Microstructure change of high density polyethylene under cyclic fatigue loading and creep was examined utilizing a tensile device specially designed for creep and fatigue test and also can be attachable to the X-ray diffractometer. In this way, the crystal morphology change of polyethylene under creep and cyclic fatigue load was successfully monitored and compared. Despite the marked differences in macroscopic deformation between the creep and cyclic fatigue tests, crystal morphology such as crystallinity, crystal size, and $d$-spacing was as nearly identical between the two test cases. Specimens pre-deformed to different strains, i.e., before yield point (BYP), at yield point (YP) and after yield point (AYP), however, showed markedly different changes in crystal morphology, especially between AYP and the other two specimens.

• Journal of Industrial and Engineering Chemistry
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• v.68
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• pp.161-167
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• 2018

In this study, transition metal coated carbon nanofibers (CNFs) were synthesized and applied as anode materials of Li secondary batteries. CNFs/Ni foam was immersed into 0.01 M transition metal solutions after growing CNFs on Ni foam via chemical vapor deposition (CVD) method. Transition metal coated CNFs/Ni foam was dried in an oven at $80^{\circ}C$. Morphologies, compositions, and crystal quality of CNFs-transition metal composites were characterized by scanning electron microscopy (SEM), Raman spectroscopy (Raman), and X-ray photoelectron spectroscopy (XPS), respectively. Electrochemical characteristics of CNFs-transition metal composites as anodes of Li secondary batteries were investigated using a three-electrode cell. Transition metal/CNFs/Ni foam was directly employed as a working electrode without any binder. Lithium foil was used as both counter and reference electrodes while 1 M $LiClO_4$ was employed as the electrolyte after it was dissolved in a mixture of propylene carbonate:ethylene carbonate (PC:EC) at 1:1 volume ratio. Galvanostatic charge/discharge cycling and cyclic voltammetry measurements were taken at room temperature using a battery tester. In particular, the capacity of the synthesized CNFs-Fe was improved compared to that of CNFs. After 30 cycles, the capacity of CNFs-Fe was increased by 78%. Among four transition metals of Fe, Cu, Co and Ni coated on carbon nanofibers, the retention rate of CNFs-Fe was the highest at 41%. The initial capacity of CNFs-Fe with 670 mAh/g was reduced to 275 mAh/g after 30 cycles.

• Journal of Powder Materials
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• v.26 no.1
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• pp.49-57
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• 2019

Layered $LiNi_{0.83}Co_{0.11}Mn_{0.06}O_2$ cathode materials single- and dual-doped by the rare-earth elements Ce and Nd are successfully fabricated by using a coprecipitation-assisted solid-phase method. For comparison purposes, non-doping pristine $LiNi_{0.83}Co_{0.11}Mn_{0.06}O_2$ cathode material is also prepared using the same method. The crystal structure, morphology, and electrochemical performances are characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) mapping, and electrochemical techniques. The XRD data demonstrates that all prepared samples maintain a typical ${\alpha}-NaFeO_2$-layered structure with the R-3m space group, and that the doped samples with Ce and/or Nd have lower cation mixing than that of pristine samples without doping. The results of SEM and EDS show that doped elements are uniformly distributed in all samples. The electrochemical performances of all doped samples are better than those of pristine samples without doping. In addition, the Ce/Nd dual-doped cathode material shows the best cycling performance and the least capacity loss. At a 10 C-rate, the electrodes of Ce/Nd dual-doped cathode material exhibit good capacity retention of 72.7, 58.5, and 45.2% after 100, 200, and 300 cycles, respectively, compared to those of pristine samples without doping (24.4, 11.1, and 8.0%).

• Journal of Powder Materials
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• v.28 no.6
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• pp.462-469
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• 2021

Tin/graphite composites are prepared as anode materials for Li-ion batteries using a dry ball-milling process. The main experimental variables in this work are the ball milling time (0-8 h) and composition ratio (tin:graphite=5:95, 15:85, and 30:70 w/w) of graphite and tin powder. For comparison, a tin/graphite composite is prepared using wet ball milling. The morphology and structure of the different tin/graphite composites are investigated using X-ray diffraction, Raman spectroscopy, energy-dispersive X-ray spectroscopy, and scanning and transmission electron microscopy. The electrochemical properties of the samples are also examined. The optimal dry ball milling time for the uniform mixing of graphite and tin is 6 h in a graphite-30wt.%Sn sample. The electrode prepared from the composite that is dry-ball-milled for 6 h exhibits the best cycle performance (discharge capacity after 50^th cycle: 308 mAh/g and capacity retention: 46%). The discharge capacity after the 50^th cycle is approximately 112 mAh/g, higher than that when the electrode is composed of only graphite (196 mAh/g after 50^th cycle). This result indicates that it is possible to manufacture a tin/graphite composite anode material that can effectively buffer the volume change that occurs during cycling, even using a simple dry ball-milling process.

• Korean Journal of Materials Research
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• v.31 no.12
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• pp.710-718
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• 2021

Recently, due to high theoretical capacitance and excellent ion diffusion rate caused by the 2D layered crystal structure, transition metal hydroxides (TMHs) have generated considerable attention as active materials in supercapacitors (or electrochemical capacitors). However, TMHs should be designed using morphological or structural modification if they are to be used as active materials in supercapacitors, because they have insulation properties that induce low charge transfer rate. This study aims to modify the morphological structure for high cycling stability and fast charge storage kinetics of TMHs through the use of nickel cobalt hydroxide [NiCo(OH)₂] decorated on nickel foam. Among the samples used, needle-like NiCo(OH)₂ decorated on nickel foam offers a high specific capacitance (1110.9 F/g at current density of 0.5 A/g) with good rate capability (1110.9 - 746.7 F/g at current densities of 0.5 - 10.0 A/g). Moreover, at a high current density (10.0 A/g), a remarkable capacitance (713.8 F/g) and capacitance retention of 95.6% after 5000 cycles are noted. These results are attributed to high charge storage sites of needle-like NiCo(OH)₂ and uniformly grown NiCo(OH)₂ on nickel foam surface.

• Journal of Electrochemical Science and Technology
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• v.12 no.2
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• pp.237-245
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• 2021

Atomic layer deposition (ALD) enhances the stability of cathode materials via surface modification. Previous studies have demonstrated that an Ni-rich cathode, such as LiNi_0.8Co_0.1Mn_0.1O₂, is a promising candidate owing to its high capacity, but is limited by poor cycle stability. In this study, to enhance the stability of the Ni-rich cathode, synthesized LiNi_0.8Co_0.1Mn_0.1O₂ was coated with Al₂O₃ using ALD. Thus, the surface-modified cathode exhibited enhanced stability by protecting the interface from Ni-O formation during the cycling process. The coated LiNi_0.8Co_0.1Mn_0.1O₂ exhibited a capacity of 176 mAh g^-1 at 1 C and retained up to 72% of the initial capacity after 100 cycles within a range of 2.8-4.3 V (vs Li/Li⁺. In contrast, pristine LiNi_0.8Co_0.1Mn_0.1O₂ presented only 58% of capacity retention after 100 cycles with an initial capacity of 173 mAh g^-1. Improved cyclability may be a result of the ALD coating, which physically protects the electrode by modifying the interface, and prevents degradation by resisting side reactions that result in capacity decay. The electrochemical impedance spectra and structural and morphological analysis performed using electron microscopy and X-ray techniques establish the surface enhancement resulting from the aforementioned strategy.

• Korean Journal of Materials Research
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• v.32 no.4
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• pp.210-215
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• 2022

Extensive research is being carried out on Ni-rich Li(Ni_xCo_yMn_1-x-y)O₂ (NCM) due to the growing demand for electric vehicles and reduced cost. In particular, Ni-rich Li(Ni_xCo_yMn_1-x-y-zAl_z)O₂ (NCMA) is attracting great attention as a promising candidate for the rapid development of Co-free but electrochemically more stable cathodes. Al, an inactive element in the structure, helps to improve structural stability and is also used as a doping element to improve cycle capability in Ni-rich NCM. In this study, NCMA was successfully synthesized with the desired composition by direct coprecipitation. Boron and tin were also used as dopants to improve the battery performance. Macro- and microstructures in the cathodes were examined by microscopy and X-ray diffraction. While Sn was not successfully doped into NCMA, boron could be doped into NCMA, leading to changes in its physicochemical properties. NCMA doped with boron revealed substantially improved electrochemical properties in terms of capacity retention and rate capability compared to the undoped NCMA.

• Korean Journal of Materials Research
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• v.32 no.5
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• pp.270-279
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• 2022

In this study, N/S co-doped carbon felt (N/S-CF) was prepared and characterized as an electrode material for electric double-layer capacitors (EDLCs). A commercial carbon felt (CF) was immersed in an aqueous solution of thiourea and then thermally treated at 800 ℃ under an inert atmosphere. The prepared N/S-CF showed a large specific surface area with hierarchical pore structures. The electrochemical performance of the N/S-CF-based electrode was evaluated using both 3-electrode and 2-electrode systems. In the 3-electrode system, the N/S-CF-based electrode showed a good specific capacitance of 177 F/g at 1 A/g and a good rate capability of 41% at 20 A/g. In the 2-electrode system (symmetric capacitor), the freestanding N/S-CF-based electrode showed a specific capacitance of 275 mF/cm² at 2 mA/cm², a rate capability of 62.5 % at 100 mA/cm², a specific power density of ~ 25,000 mW/cm² at an energy density of 23.9 mWh/cm², and a cycling stability of ~ 100 % at 100 mA/cm² after 20,000 cycles. These results indicate the N/S co-doped carbon felts can be a promising candidate as a new electrode material in a symmetric capacitor.

• Journal of the Korean institute of surface engineering
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• v.56 no.1
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• pp.104-114
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• 2023

Three dimensional (3D) porous structures consisting of Cu@CoO core-shell-type nano-dendrites were synthesized and tested as the anode materials in lithium secondary batteries. For this purpose, first, the 3D porous films comprising Cu@Co core-shell-type nano-dendrites with various thicknesses were fabricated through the electrochemical co-deposition of Cu and Co. Then the Co shells were selectively anodized to form Co hydroxides, which was finally dehydrated to get Cu@CoO nanodendrites. The resulting electrodes exhibited very high reversible specific capacity almost 1.4~2.4 times the theoretical capacity of commercial graphite, and excellent capacity retention (~90%@50^th cycle) as compared with those of the existing transition metal oxides. From the analysis of the cumulative irreversible capacity and morphology change during charge/discharge cycling, it proved that the excellent capacity retention was attributed to the unique structural feature of our core-shell structure where only the thin CoO shell participates in the lithium storage. In addition, our electrodes showed a superb rate performance (70.5%@10.8 C-rate), most likely due to the open porous structure of 3D films, large surface area thanks to the dendritic structure, and fast electron transport through Cu core network.