• Journal of the Korean Chemical Society
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• v.63 no.6
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• pp.453-458
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• 2019

Synthesis of ZnCo₂O₃ oxide is performed by sol-gel method via nitrate-citrate route. Powder X-ray diffraction (XRD) study shows monoclinic unit cell having lattice parameters: a = 5.721(1) Å, b = 8.073(2) Å, c = 5.670(1) Å, β = 93.221(8)°, space group P_2/m and Z = 4. Average crystallite sizes determined by Scherrer equation are the range ~14-32 nm, whereas SEM micrographs show nano-micro meter size particles formed in ZnCo₂O₃. Endothermic peak at ~798 K in the Differential scanning calorimetric (DSC) trace without weight loss could be due to structural transformation and the endothermic peak ~1143 K with weight loss is due to reversible loss of O₂ in air atmosphere. Energy Dispersive X-ray (EDX) analysis profile shows the presence of elements Zn, Co and O which indicates the purity of the sample. Magnetic measurements in the range of +12 kOe to -12 kOe at 10 K, 77 K, 120 K and at 300 K by PPMS-II Physical Property Measurement System (PPMS) shows hysteresis loops having very low values of the coercivity and retentivity which indicates the weakly ferromagnetic nature of the oxide. Observed X-band EPR isotropic lineshapes at 300 K and 77 K show positive g-shift at g_iso ~2.230 and g_iso ~2.217, respectively which is in agreement with the presence of paramagnetic site Co²⁺(3d⁷) in the oxide. DC conductivity value of 2.875 ×10^-8 S/cm indicates very weakly semiconducting nature of ZnCo₂O₃ at 300 K. DRS absorption bands ~357 nm, ~572 nm, ~619 nm and ~654 nm are due to the d-d transitions ⁴T_1g(⁴F)→²E_g(²G), ⁴T_1g(⁴F)→⁴T_1g(⁴P), ⁴T_1g(⁴F)→⁴A_2g(⁴F), ⁴T_1g(⁴F)→⁴T_2g(⁴F), respectively in octahedral ligand field around Co²⁺ ions. Direct band gap energy, E_g~ 1.5 eV in the oxide is obtained by extrapolating the linear part of the Tauc plot to the energy axis indicates fairly strong semiconducting nature of ZnCo₂O₃.

• Clean Technology
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• v.12 no.2
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• pp.53-61
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• 2006

A PGSS (Particles from Gas Saturated Solutions) process designed to generate nano-particles using supercritical fluids has been conducted for the fabrication of Poly(lactide-co-glycolide) (PLGA) microparticles that encapsulate a protein drug. It is demonstrated that the polymer and the dry powder of a protein can be mixed under supercritical carbon dioxide conditions and that the protein component retains its biological activity. In this experiment, the mixture of polymer which is plasticized and dry powder protein was sprayed to form solid polymer that encapsulate the protein. It is found that supercritical fluid process give fine tuning of particle size and particle size distribution by simple manipulations of the process parameters. Porous particles were formed with irregular shape. Protein encapsulated in the polymer was found to have enzymatic activity without significant loss of its initial value.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2009.06a
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• pp.113-114
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• 2009

Silicon carbide is one of the most attractive and promising wide band-gap semiconductor material with excellent physical properties and huge potential for electronic applications. Up to now, the most successful method for growth of large SiC crystals with high quality is the physical vapor transport (PVT) method [1, 2]. Since further reduction of defect densities in larger crystal are needed for the true implementation of SiC devices, many researchers are focusing to improve the quality of SiC single crystal through the process modifications for SiC bulk growth or new material implementations [3, 4]. It is well known that for getting high quality SiC crystal, source materials with high purity must be used in PVT method. Among various source materials in PVT method, a SiC powder is considered to take an important role because it would influence on crystal quality of SiC crystal as well as optimum temperature of single crystal growth, the growth rate and doping characteristics. In reality, the effect of powder on SiC crystal could definitely exhibit the complicated correlation. Therefore, the present research was focused to investigate the quality difference of SiC crystal grown by conventional PVT method with using various SiC powders. As shown in Fig. 1, we used three SiC powders with different particles size. The 6H-SiC crystals were grown by conventional PVT process and the SiC seeds and the high purity SiC source materials are placed on opposite side in a sealed graphite crucible which is surrounded by graphite insulation[5, 6]. The bulk SiC crystal was grown at $2300^{\circ}C$ of the growth temperature and 50mbar of an argon pressure. The axial thermal gradient across the SiC crystal during the growth is estimated in the range of $15\sim20^{\circ}C/cm$. The chemical etch in molten KOH maintained at $450^{\circ}C$ for 10 min was used for defect observation with a polarizing microscope in Nomarski mode. Electrical properties of bulk SiC materials were measured by Hall effect using van der Pauw geometry and a UV/VIS spectrophotometer. Fig. 2 shows optical photographs of SiC crystal ingot grown by PVT method and Table 1 shows electrical properties of SiC crystals. The electrical properties as well as crystal quality of SiC crystals were systematically investigated.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.25 no.5
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• pp.398-402
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• 2012

Synthesis of $Li_2MnSiO_4$ was attempted by the conventional solid-state reaction method, and the phase formation behavior according to the change of the calcination condition was investigated. When the mixture of the three source materials, $Li_2O$, MnO and $SiO_2$ powders, were used for calcination in air, it was difficult to develop the $Li_2MnSiO_4$ phase because the oxidation number of $Mn^{2+}$ could not be maintained. Therefore, two-step calcination was applied: $Li_2SiO_3$ was made from $Li_2O$ and $SiO_2$ at the first step, and $Li_2MnSiO_4$ was synthesized from $Li_2SiO_3$ and MnO at the second step. It was easy to make $Li_2MnSiO_3$ from $Li_2O$ and $SiO_2$. $Li_2MnSiO_4$ single phase was developed by the calcination at $900^{\circ}C$ for 24 hr in Ar atmosphere as the oxidation of $Mn^{2+}$ was prevented. However, the $Li_2MnSiO_4$ was ${\gamma}-Li_2MnSiO_4$, one of the polymorph of $Li_2MnSiO_4$, which could not be used as the cathode materials in Li-ion batteries. By applying the additional low temperature annealing at $400^{\circ}C$, the single phase ${\beta}-Li_2MnSiO_4$ powder was synthesized successfully through the phase transition from ${\gamma}$ to ${\beta}$ phase.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.23 no.5
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• pp.255-264
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• 2013

Cobalt aluminate ($CoAl_2O_4$) is a highly stable pigment with excellent resistance to light, weather, etc., which has resulted in widespread use as a ceramic pigment. Due to the unique optical characteristics, $CoAl_2O_4$ is generally used as a coloring agent to decorate porcelain products, glass, paints and plastics. Here, $CoAl_2O_4$ pigments were synthesized by polymerized complex method and solid state reaction. Then $CoAl_2O_4$ pigment were grinded using the attrition milling with 1 mm size zirconia ball for 3 hours. The attrition milling process was performed at the constant speed of 800 rpm and ball to powder weight ratio (BPR) was 100 : 1. The characteristics of synthesized pigment were analyzed by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), particle size analyser (PSA) and CIE $L^*a^*b^*$. The XRD patterns of $CoAl_2O_4$ show single phase spinel structure. The particle size of $CoAl_2O_4$ measured by FE-SEM, TEM and PSA analysis was in the range of 100~200 nm. The blue color of obtained $CoAl_2O_4$ pigments could be confirmed through CIE $L^*a^*b^*$ measurement.

• Journal of the Korean Ceramic Society
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• v.39 no.8
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• pp.789-794
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• 2002

In this study, nano-sized Si-C-N precursor powders were synthesized by Chemical Vapor Condensation Method(CVC) using TMS(Tetramethylsilane: $Si(CH_3)_4$), $NH_3$ and $H_2$ gases under the various reaction conditions of the reaction temperature, TMS/$NH_3$ ratio and TMS/$H_2$ ratio. XRD and FESEM were used to analysis the crystalline phase and the average particle size of the synthesized powders. It was found that the obtained powders under the considering conditions were all spherical amorphous powder with the particle size of 87∼130 nm. The particle size was decreased as the reaction temperature increased and TMS/$NH_3$ and TMS/$H_2$ ratio decreased. As the results of EA analysis, it was found that the synthesized powders had been formed the powders composed of Si, N, C and H. Through FT-IR results, it was found that the synthesized powders were Si-C-N precursor powders with Si-C, Si-N and C-N bonds.

• Journal of the Korean Ceramic Society
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• v.39 no.8
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• pp.783-788
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• 2002

In this study, nano-sized Si-C-N precursor powders were synthesized by Chemical Vapor Condensation Method(CVC) using TMS(Tetramethylsilane: Si($CH_3)_4$), $NH_3$ and $H_2$ gases under the various reaction conditions of the reaction temperature, TMS/$NH_3$ ratio and TMS/$H_2$ ratio. XRD and FESEM were used to analysis the crystalline phase and the average particle size of the synthesized powders. It was found that the obtained powders under the considering conditions were all spherical amorphous powder with the particle size of 87∼130 nm. The particle size was decreased as the reaction temperature increased and TMS/$NH_3$ and TMS/$H_2$ ratio decreased. As the results of EA analysis, it was found that the synthesized powders had been formed the powders composed of Si, N, C and H. Through FT-IR results, it was found that the synthesized powders were Si-C-N precursor powders with Si-C, Si-N and C-N bonds.

• Journal of the Korean Ceramic Society
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• v.45 no.12
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• pp.839-844
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• 2008

$TiO_2$ is an environment-friendly semiconducting material, and it has photocatalytic and hydrophilic effect. There are a lot of reports on the photocatalytic characteristics of $TiO_2$, such as organic pollutants resolving, anti-bacterial, and self-purification material. In this paper, $TiO_2$ micron-sized powders were deposited on the glass by room temperature powder spray in vacuum process, so called aerosol deposition (AD), and nano-grained $TiO_2$ photocatalytic thin films were fabricated. The thickness of the films were controlled by changing the number of deposition cycle. Morphologies and characteristics of the AD-$TiO_2$ thin films were examined by SEM, TEM, XRD, and UV-Visible Spectrophotometer. As the thickness of $TiO_2$ films increased, surface roughness increased. By this increment, the reaction area between film and pollutant was enlarged, resulting in better photocatalytic property.

• Korean Journal of Materials Research
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• v.22 no.11
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• pp.631-635
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• 2012

Nickel oxide was doped with a wide range of concentrations (mol%) of Aluminum (Al) by solvothermal synthesis; single-phased nano powder of nickel oxide was generated after calcination at$900^{\circ}C$. When the concentration of Al dopant was increased, the reduced intensity was confirmed through XRD analysis. Lattice parameters of the synthesized NiO powder were decreased after treatment of the dopant; parameters were increased when the concentration of Al was over the doping limit (5 mol% Al). The binding energy of $Ni^{2+}$ was chemically shifted to $Ni^{3+}$ by doping $Al^{3+}$ ion, as confirmed by the XPS analysis. The tilted structure of the synthesized NiO with 5 mol% Al dopant and the polycrystalline structure of the $Ni_{0.75}Al_{0.25}O$ were observed by HR-TEM analysis. The electrical conductivity of the newly synthesized NiO was highly improved by Al doping in the conductivity test. The electrical conductivity values of the commercial NiO and the synthesized NiO with 5 mol% Al dopant ($Ni_{0.95}Al_{0.05}O$) were 1,400 s/cm and 2,230 s/cm at $750^{\circ}C$, respectively. However, the electrical conductivity of the synthesized NiO with 10 mol% Al dopant ($Ni_{0.9}Al_{0.1}O$) decreased due to the scattering of free-electrons caused by the large number of impurity atoms; the electrical conductivity of $Ni_{0.9}Al_{0.1}O$ was 545 s/cm at $750^{\circ}C$.

• Resources Recycling
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• v.26 no.1
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• pp.22-29
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• 2017

When the ambient air pressure was $0.1kg/cm^2$, there were few spherically formed droplets, which showed very badly fragmented state. The average particle size of the particles constituting the droplet was about 40 nm. When the air pressure increased to $0.5kg/cm^2$, the ratio of the spherical droplet forms increased, but still showed a state of severe disruption. The average particle size of the particles was reduced to about 35 nm. As the air pressure increased to $3kg/cm^2$, the ratio of spherical droplet form significantly increased, the degree of fragmentation even further decreased and the average particle size decreased to 30 nm. When the air pressure increased from 0.1 to $1kg/cm^2$, the XRD peak intensity showed little change, but the specific surface area was decreased. As the air pressure increased to $3kg/cm^2$, the intensity of XRD peaks showed a little decrease, while the specific surface area increased.