• Korean Journal of Materials Research
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• v.23 no.11
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• pp.655-660
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• 2013

Photoelectrochemical cells have been used in photolysis of water to generate hydrogen as a clean energy source. A high efficiency electrode for photoelectrochemical cell systems was realized using a ZnO hierarchical nanostructure. A ZnO nanofiber mat structure was fabricated by electrospinning of Zn solution on the substrate, followed by oxidation; on this substrate, hydrothermal synthesis of ZnO nanorods on the ZnO nanofibers was carried out to form a ZnO hierarchical structure. The thickness of the nanofiber mat and the thermal annealing temperature were determined as the parameters for optimization. The morphology of the structures was examined by field-emission scanning electron microscopy, transmission electron microscopy, and X-ray diffraction. The performance of the ZnO nanofiber mat and the potential of the ZnO hierarchical structures as photoelectrochemical cell electrodes were evaluated by measurement of the photoelectron conversion efficiencies under UV light. The highest photoconversion efficiency observed was 63 % with a ZnO hierarchical structure annealed at $400^{\circ}C$ in air. The morphology and the crystalline quality of the electrode materials greatly influenced the electrode performance. Therefore, the combination of the two fabrication methods, electrospinning and hydrothermal synthesis, was successfully applied to fabricate a high performance photoelectrochemical cell electrode.

• Korean Journal of Materials Research
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• v.23 no.10
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• pp.592-598
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• 2013

Graphene oxide powders prepared by two different drying processes, freeze drying and spray drying, were studied to compare the effect of the drying method on the physical properties of graphene oxide powder. The graphene oxide dispersion was prepared from graphite by chemical delamination with the aid of sulfuric acid and permanganic acid, and the dispersion was further washed and re-dispersed in a mixed solvent of water and isopropyl alcohol. A freeze drying method can feasibly minimize damage to the sample, but it requires a long process time. In contrast, spray drying is able to remove a solvent in a relatively short time, though this process requires exposure to a high temperature for a rapid evaporation of the solvent. The powders prepared by freeze drying and spray drying were characterized and compared by Raman spectroscopy, X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, and by an elemental analysis. The graphene oxide powders showed similar chemical compositions; however, the morphologies of the powders differed in that the graphene oxide prepared by spray drying had a winkled morphology and a higher apparent density compared to the powder prepared by freeze drying. The graphene oxide powders were reduced at $900^{\circ}C$ in an atmosphere of $N_2$. The effect of the drying process on the properties of the reduced graphene oxide was examined by SEM, TEM and Raman spectroscopy.

• Korean Journal of Materials Research
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• v.24 no.1
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• pp.60-65
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• 2014

Fe-based amorphous coatings were fabricated on a soda-lime glass substrate by the vacuum kinetic spray method. The effect of the gas flow rate, which determines particle velocity, on the deposition behavior of the particle and microstructure of the resultant films was investigated. The as-fabricated microstructure of the film was studied by field emission scanning electron microscopy (FE-SEM) and high resolution transmission electron microscopy (HR-TEM). Although the activation energy for transformation from the amorphous phase to crystalline phase was lowered by severe plastic deformation and particle fracturing under a high strain rate, the crystalline phases could not be found in the coating layer. Incompletely fractured and small fragments 100~300 nm in size, which are smaller than initial feedstock material, were found on the coating surface and inside of the coating. Also, some pores and voids occurred between particle-particle interfaces. In the case of brittle Fe-based amorphous alloy, particles fail in fragmentation fracture mode through initiation and propagation of the numerous small cracks rather than shear fracture mode under compressive stress. It could be deduced that amorphous alloy underwent particle fracturing in a vacuum kinetic spray process. Also, it is considered that surface energy caused by the formation of new surfaces and friction energy contributed to the bonding of fragments.

• Korean Journal of Materials Research
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• v.24 no.1
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• pp.37-42
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• 2014

Well-distributed ruthenium (Ru) nanoparticles decorated on porous carbon nanofibers (CNFs) were synthesized using an electrospinning method and a reduction method for use in high-performance elctrochemical capacitors. The formation mechanisms including structural, morphological, and chemical bonding properties are demonstrated by means of field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). To investigate the optimum amount of the Ru nanoparticles decorated on the porous CNFs, we controlled three different weight ratios (0 wt%, 20 wt%, and 40 wt%) of the Ru nanoparticles on the porous CNFs. For the case of 20 wt% Ru nanoparticles decorated on the porous CNFs, TEM results indicate that the Ru nanoparticles with ~2-4 nm size are uniformly distributed on the porous CNFs. In addition, 40 wt% Ru nanoparticles decorated on the porous CNFs exhibit agglomerated Ru nanoparticles, which causes low performance of electrodes in electrochemical capacitors. Thus, proper distribution of 20 wt% Ru nanoparticles decorated on the porous CNFs presents superior specific capacitance (~280.5 F/g at 10 mV/s) as compared to the 40 wt% Ru nanoparticles decorated on the porous CNFs and the only porous CNFs. This enhancement can be attributed to the synergistic effects of well-distributed Ru nanoparticles and porous CNF supports having high surface area.

• Journal of Environmental Science International
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• v.27 no.7
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• pp.611-620
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• 2018

In this study, a metal-organic framework (MOF) material $NH_2$-MIL-101(Fe) was synthesized using the solvothermal method, and characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), UV-visible spectrophotometry, field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), and surface area measurements. The XRD pattern of the synthesized $NH_2$-MIL-101(Fe) was similar to the previously reported patterns of MIL-101 type materials, which indicated the successful synthesis of $NH_2$-MIL-101(Fe). The FT-IR spectrum showed the molecular structure and functional groups of the synthesized $NH_2$-MIL-101(Fe). The UV-visible absorbance spectrum indicated that the synthesized material could be activated as a photocatalyst under visible light irradiation. FE-SEM and TEM images showed the formation of hexagonal microspindle structures in the synthesized $NH_2$-MIL-101(Fe). Furthermore, the EDS spectrum indicated that the synthesized material consisted of Fe, N, O, and C elements. The synthesized $NH_2$-MIL-101(Fe) was then employed as an adsorbent and photocatalyst for the removal of Indigo carmine and Rhodamine B from aqueous solutions. The initial 30 min of adsorption for Indigo carmine and Rhodamine B without light irradiation achieved removal efficiencies of 83.6% and 70.7%, respectively. The removal efficiencies thereafter gradually increased with visible light irradiation for 180 min, and the overall removal efficiencies for Indigo carmine and Rhodamine B were 94.2% and 83.5%, respectively. These results indicate that the synthesized MOF material can be effectively applied as an adsorbent and photocatalyst for the removal of dyes.

• Journal of Sensor Science and Technology
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• v.29 no.3
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• pp.156-161
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• 2020

In this study, hierarchical mesoporous CuO spheres, ZnO flowers, and heterojunction CuO/ZnO nanostructures were fabricated via a facile hydrothermal method. The as-prepared materials were characterized in detail using various analytical methods such as powder X-ray diffraction, micro Raman spectroscopy, X-ray photoelectron spectroscopy, field-emission scanning electron microscopy, and transmission electron microscopy. The obtained results are consistent with each other. The H₂S-sensing characteristics of the sensors fabricated based on the CuO spheres, ZnO flowers, and CuO/ZnO heterojunction were investigated at different temperatures and gas concentrations. The sensor based on ZnO flowers showed a maximum response of ~141 at 225 ℃. The sensor based on CuO spheres exhibited a maximum response of 218 at 175 ℃, whereas the sensor based on the CuO/ZnO nano-heterostructure composite showed a maximum response of 344 at 150 ℃. The detection limit (DL) of the sensor based on the CuO/ZnO heterojunction was ~120 ppb at 150 ℃. The CuO/ZnO sensor showed the maximum response to H₂S compared with other interfering gases such as ethanol, methanol, and CO, indicating its high selectivity.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.277-277
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• 2010

The capacity of the carbonaceous materials reached ca. $350\;mAhg^{-1}$ which is close to theorestical value of the carbon intercalation composition $LiC_6$, resulting in a relatively low volumetric Li capacity. Notwithstanding the capacities of carbon, it will not adjust well to the need so future devices. Silicon shows the highest gravimetric capacities (up to $4000\;mAhg^{-1}$ for $Li_{21}Si_5$). Although Si is the most promising of the next generation anodes, it undergoes a large volume change during lithium insertion and extraction. It results in pulverization of the Si and loss of electrical contact between the Si and the current collector during the lithiation and delithiation. Thus, its capacity fades rapidly during cycling. We focused on electrode materials in the multiphase form which were composed of two metal compounds to reduce the volume change in material design. A combination of electrochemically amorphous active material in an inert matrix (Si-M) has been investigated for use as negative electrode materials in lithium ion batteries. The matrix composited of Si-M alloys system that; active material (Si)-inactive material (M) with Li; M is a transition metal that does not alloy with Li with Li such as Ti, V or Mo. We fabricated and tested a broad range of Si-M compositions. The electrodes were sputter-deposited on rough Cu foil. Electrochemical, structural, and compositional characterization was performed using various techniques. The structure of Si-M alloys was investigated using X-ray Diffractometer (XRD) and transmission electron microscopy (TEM). Surface morphologies of the electrodes are observed using a field emission scanning electron microscopy (FESEM). The electrochemical properties of the electrodes are studied using the cycling test and electrochemical impedance spectroscopy (EIS). It is found that the capacity is strongly dependent on Si content and cycle retention is also changed according to M contents. It may be beneficial to find materials with high capacity, low irreversible capacity and that do not pulverize, and that combine Si-M to improve capacity retention.

• Korean Journal of Materials Research
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• v.25 no.3
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• pp.125-131
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• 2015

Fluorine-doped $SnO_2$ (FTO) thin film/Ag nanowire (NW) double layers were fabricated by means of spin coating and ultrasonic spray pyrolysis. To investigate the optimum thickness of the FTO thin films when used as protection layer for Ag NWs, the deposition time of the ultrasonic spray pyrolysis process was varied at 0, 1, 3, 5, or 10 min. The structural, chemical, morphological, electrical, and optical properties of the double layers were examined using X-ray diffraction, X-ray photoelectron spectroscopy, field-emission scanning electron microscopy, transmission electron microscopy, the Hall effect measurement system, and UV-Vis spectrophotometry. Although pure Ag NWs formed isolated droplet-shaped Ag particles at an annealing temperature of $300^{\circ}C$, Ag NWs covered by FTO thin films maintained their high-aspect-ratio morphology. As the deposition time of the FTO thin films increased, the electrical and optical properties of the double layers degraded gradually. Therefore, the double layer fabricated with FTO thin films deposited for 1 min exhibited superb sheet resistance (${\sim}14.9{\Omega}/{\Box}$), high optical transmittance (~88.6 %), the best FOM (${\sim}19.9{\times}10^{-3}{\Omega}^{-1}$), and excellent thermal stability at an annealing temperature of $300^{\circ}C$ owing to the good morphology maintenance of the Ag NWs covered by FTO thin films.

• Korean Journal of Materials Research
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• v.29 no.8
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• pp.491-496
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• 2019

In this study, we prepare pure $WO_3$ inverse opal(IO) film with a thickness of approximately $3{\mu}m$ by electrodeposition, and an ultra-thin $TiO_2$ layer having a thickness of 2 nm is deposited on $WO_3$ IO film by atomic layer deposition. Both sets of photoelectrochemical properties are evaluated after developing dye-sensitized solar cells(DSSCs). In addition, morphological, crystalline and optical properties of the developed films are evaluated through field-emission scanning electron microscopy(FE-SEM), High-resolution transmission electron microscopy(HR-TEM), X-ray diffraction(XRD) and UV/visible/infrared spectrophotometry. In particular, pure $WO_3$ IO based DSSCs show low $V_{OC}$, $J_{SC}$ and fill factor of 0.25 V, $0.89mA/cm^2$ and 18.9 %, achieving an efficiency of 0.04 %, whereas the $TiO_2/WO_3$ IO based DSSCs exhibit $V_{OC}$, $J_{SC}$ and fill factor of 0.57 V, $1.18mA/cm^2$ and 50.1 %, revealing an overall conversion efficiency of 0.34 %, probably attributable to the high dye adsorption and suppressed charge recombination reaction.

• Korean Journal of Materials Research
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• v.23 no.2
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• pp.143-148
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• 2013

Well-distributed $SnO_2$-Sn-$Ag_3Sn$ nanoparticles embedded in carbon nanofibers were fabricated using a co-electrospinning method, which is set up with two coaxial capillaries. Their formation mechanisms were successfully demonstrated. The structural, morphological, and chemical compositional properties were investigated by field-emission scanning electron spectroscopy (FESEM), bright-field transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). In particular, to obtain well-distributed $SnO_2$ and Sn and $Ag_3Sn$ nanoparticles in carbon nanofibers, the relative molar ratios of the Ag precursor to the Sn precursor including 7 wt% polyacrylonitrile (PAN) were controlled at 0.1, 0.2, and 0.3. The FESEM, bright-field TEM, XRD, and XPS results show that the nanoparticles consisting of $SnO_2$-Sn-$Ag_3Sn$ phases were in the range of ~4 nm-6 nm for sample A, ~5 nm-15 nm for sample B, ~9 nm-22 nm for sample C. In particular, for sample A, the nanoparticles were uniformly grown in the carbon nanofibers. Furthermore, when the amount of the Ag precursor and the Sn precursor was increased, the inorganic nanofibers consisting of the $SnO_2$-Sn-$Ag_3Sn$ nanoparticles were formed due to the decreased amount of the carbon nanofibers. Thus, well-distributed nanoparticles embedded in the carbon nanofibers were successfully synthesized at the optimum molar ratio (0.1) of the Ag precursor to the Sn precursor after calcination of $800^{\circ}C$.