• Journal of Industrial and Engineering Chemistry
• /
• 제68권
• /
• pp.161-167
• /
• 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.

• 한국분말재료학회지
• /
• 제26권1호
• /
• pp.49-57
• /
• 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%).

• 한국분말재료학회지
• /
• 제28권6호
• /
• pp.462-469
• /
• 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.

• 한국재료학회지
• /
• 제31권12호
• /
• pp.710-718
• /
• 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
• /
• 제12권2호
• /
• pp.237-245
• /
• 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.

• 한국재료학회지
• /
• 제32권4호
• /
• pp.210-215
• /
• 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.

• 한국재료학회지
• /
• 제32권5호
• /
• pp.270-279
• /
• 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.

• 한국표면공학회지
• /
• 제56권1호
• /
• pp.104-114
• /
• 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.

• Journal of Electrochemical Science and Technology
• /
• 제14권1호
• /
• pp.85-95
• /
• 2023

In recent years, solid-state Li metal batteries (SSLBs) have attracted significant attention as the next-generation batteries with high energy and power densities. However, uncontrolled dendrite growth and the resulting pulverization of Li during repeated plating/stripping processes must be addressed for practical applications. Herein, we report a plastic-crystal-based polymer/ceramic composite solid electrolyte (PCCE) to resolve these issues. To fabricate the one-side ceramic-incorporated PCCE (CI-PCCE) film, a mixed precursor solution comprising plastic-crystal-based polymer (succinonitrile, SN) with garnet-structured ceramic (Li₇La₃Zr₂O₁₂, LLZO) particles was infused into a thin cellulose membrane, which was used as a mechanical framework, and subsequently solidified by using UV-irradiation. The CI-PCCE exhibited good flexibility and a high room-temperature ionic conductivity of over 10^-3 S cm^-1. The Li symmetric cell assembled with CI-PCCE provided enhanced durability against Li dendrite penetration through the solid electrolyte (SE) layer than those with LLZO-free PCCEs and exhibited long-term cycling stability (over 200 h) for Li plating/stripping. The enhanced Li⁺ transference number and lower interfacial resistance of CI-PCCE indicate that the ceramic-polymer composite layer in contact with the Li anode enabled the uniform distribution of Li⁺ flux at the interface between the Li metal and CI-PCCE, thereby promoting uniform Li plating/stripping. Consequently, the Li//LiFePO₄ (LFP) full cell constructed with CI-PCCE demonstrated superior rate capability (~120 mAh g^-1 at 2 C) and stable cycle performance (80% after 100 cycles) than those with ceramic-free PCCE.

• Restorative Dentistry and Endodontics
• /
• 제49권1호
• /
• pp.9.1-9.14
• /
• 2024

Objectives: This study aimed to evaluate the effect of pomegranate solution (Punica granatum) on eroded dentin through antioxidant action, shear bond strength (SBS) and interface morphology. Materials and Methods: The 10% pomegranate peel extract was prepared by the lyophilization method. Punicalagin polyphenol was confirmed by high-performance liquid chromatography. Antioxidant activity was evaluated by capturing the 2,2-diphenyl1-picrylhydrazyl (DPPH) radical. For the SBS, 48 dentin fragments were divided into sound or eroded, and subdivided according to the pretreatment (n = 12): water or P. granatum. The surfaces were restored with self-etch adhesive and a bulk-fill resin (Ecosite; DMG). The SBS was done immediately (24 hours) and after thermal cycling + water storage (12 months). For scanning electron microscopy, 48 dentin fragments (24 sound and 24 eroded) received the same treatments as for SBS (n = 6), and they were analyzed after 24 hours and 12 months. Results: The P. granatum had antioxidant action similar (p = 0.246) to the phenolic standard antioxidants. After 24 hours, eroded dentin had lower SBS than sound dentin (p < 0.001), regardless of the pretreatment. After 12 months, P. granatum maintained the SBS of sound dentin (13.46 ± 3.42 MPa) and eroded dentin (10.96 ± 1.90 MPa) statistically similar. The lowest values were found on eroded dentin treated with water (5.75 ± 1.65 MPa) (p < 0.001). P. granatum on eroded dentin caused peritubular demineralization and hybrid layer with resin tags. Conclusions: The pomegranate extract had antioxidant action and preserved the adhesive interface of the eroded dentin.