• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.17 no.2
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• pp.127-137
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• 2019

Zr electrorefining is demonstrated herein using Zirlo tubes in a chloride-fluoride mixed molten salt in the presence of $AlF_3$. Cyclic voltammetry reveals a monotonic shift in the onset of metal reduction kinetics towards positive potential and an increase in intensity of the additional peaks associated with Zr-Al alloy formation with increasing $AlF_3$ concentration. Unlike the galvanostatic deposition mode, a radial plate-type Zr growth is evident at the top surface of the salt during Zr electrorefining at a constant potential of -1.2 V. The diameter of the plate-type Zr deposit gradually increases with increasing $AlF_3$ concentration. Scanning electron microscopy-energy-dispersive X-ray spectroscopy (SEM-EDX) and X-ray photoelectron spectroscopy (XPS) analyses for the plate-type Zr deposit show that trace amount of Al is incorporated as Zr-Al alloys with different chemical compositions between the top and bottom surface of the deposit. Addition of $AlF_3$ is effective in lowering the residual salt content in the deposit and in improving the current efficiency for Zr recovery.

• Korean Chemical Engineering Research
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• v.57 no.1
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• pp.133-141
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• 2019

High specific surface area zirconia with acid-basic property was synthesized by precipitation using reflux method or hydrothermal synthesis method using ammonium hydroxide solution as precipitant in the range of pH of Zr solution from 2 to 10. The prepared zirconia was characterized by the nitrogen adsorption, X-ray diffraction (XRD), isopropanol temperature programmed desorption (IPA-TPD), scanning electron microscopy and X-ray photoelectron spectroscopy, and the catalytic activity in the IPA decomposition reaction was correlated with the acid-basic properties. When using reflux method, high pH of Zr solution was required to obtain high fraction of tetragonal zirconia, and pure tetragonal zirconia was possible at pH 9 or higher. High pH was required to obtain high specific surface area zirconia, and the hydrous zirconia synthesized at pH 10 had high specific surface area zirconia of $260m^2g^{-1}$ even after calcination at $600^{\circ}C$. However, hydrothermal synthesis with high pressure under the same conditions resulted in very low specific surface area below $40m^2g^{-1}$ and monoclinic phase zirconia was synthesized. High pH of the solution was required to obtain high specific surface area tetragonal phase zirconia. In hydrothermal synthesis requiring high pressure, monoclinic zirconia was produced irrespective of the pH of the solution, and the specific surface area was relatively low. Zirconia with high specific surface area and tetragonal phase was predominantly acidic compared to basicity and only propylene, which was observed as selective dehydration reaction in IPA decomposition reaction, was produced.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.29 no.3
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• pp.83-90
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• 2019

In this paper, Mg-doped AlN epilayers for power semiconductor devices are grown by mixed-source hydride vapor phase epitaxy. Magnesium is used as p-type dopant material in the grown AlN epilayer. The AlN epilayers on the GaN-templated sapphire substrate and GaN-templated-patterned sapphire substrate (PSS), respectively, as the base substrates for device application, were selectively grown. The surface and the crystal structures of the AlN epilayers were investigated by field emission scanning electron microscopy (FE-SEM) and high-resolution-X-ray diffraction (HR-XRD). From the X-ray photoelectron spectroscopy (XPS) and Raman spectra results, the p-type AlN epilayers grown by using the mixed-source HVPE method could be applied to power devices.

• Applied Chemistry for Engineering
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• v.22 no.2
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• pp.167-172
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• 2011

In this work, the effect of surface treatment on mesoporous carbons (MCs) supports was investigated by analyzing surface functional groups. MCs were prepared by a conventional templating method using mesoporous silica (SBA-15) for using catalyst supports in direct methanol fuel cells (DMFCs). The MCs were treated with different phosphoric acid ($H_3PO_4$) concentrations i.e., 0, 1, 3, 4, and 5 M at 343 K for 6 h. And then Pt-Ru was deposited onto surface treated MCs (H-MCs) by chemical reduction method. The characteristics of Pt-Ru catalysts deposited onto H-MCs were determined by specific surface area and pore size analyzer, X-ray diffraction, X-ray photoelectron, transmission electron microscopy, and inductive coupled plasma-mass spectrometer. The electrochemical properties of Pt-Ru/H-MCs catalysts were also analyzed by cyclic voltammetry experiments. From the results of surface analysis, an oxygen functional group was introduced to the surface of carbon supports. From the results, the H4M-MCs carbon supports surface treated with 4 M $H_3PO_4$ led to uniform dispersion of Pt-Ru onto H4M-MCs, resulting in enhancing the electro-catalytic activity of Pt-Ru catalysts.

• Applied Chemistry for Engineering
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• v.22 no.6
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• pp.672-678
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• 2011

In this work, carbon fibers were electrolessly Ni-plated in order to investigate the effect of metal plating on the electromagnetic shielding effectiveness (EMI-SE) of Ni-coated carbon fibers-reinforced epoxy matrix composites. The surfaces of carbon fibers were characterized by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Electric resistance of the composites was tested using a 4-point-probe electric resistivity tester. The EMI-SE of the composites was evaluated by means of the reflection and adsorption methods. From the results, it was found that the EMI-SE of the composites enhanced with increasing Ni plating time and content. In high frequency region, the EMI-SE didn't show further increasing with high Ni content (Ni-CF 10 min) compared to the Ni-CF 5 min sample. In conclusion, Ni content on the carbon fibers can be a key factor to determine the EMI-SE of the composites, but there can be an optimized metal content at a specific electromagnetic frequency region in this system.

• Korean Journal of Metals and Materials
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• v.56 no.12
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• pp.885-892
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• 2018

Molybdenum disulfide ($MoS_2$) based electrocatalysts have been proposed as substitutes for platinum group metal (PGM) based electrocatalyst to hydrogen evolution reaction (HER) in water electrolysis. Here, we studied $MoS_2/CNFs$ hybrid catalyst prepared by electrospinning method with heat treatment for polymer electrolyte membrane(PEM) water electrolysis to improve the HER activity. The physicochemical and electrochemical properties such as average diameter, crystalline properties, electrocatalitic activity for HER of synthesized $MoS_2/CNFs$ were investigated by the Scanning Electron Microscope (SEM), X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Transmission Electron Microscopy (TEM), Raman Spectroscopy (Raman) and Linear Sweep Voltammetry (LSV). The as spun ATTM/PVP nanofibers were prepared by sol-gel and electrospinning method. Subsequently, the $MoS_2/CNFs$ was dereived from reduction heat treatment of ATTM at the ATTM/PVP nanofibers and carbonization heat treatment. Synthesized $MoS_2/CNFs$ electrocatalyst had an average diameter of $179{\pm}30nm$. We confirmed that the $MoS_2$ layers in $MoS_2/CNF$ electrocatalyst consist of 3~4 layers from the Raman results. In addition, We confirmed that the $MoS_2$ layers in $MoS_2/CNF$ catalyst consist of 7.47% octahedral 1T phase $MoS_2$, 63.77% trigonal prismatic 2H phase $MoS_2$ with 28.75% $MoO_3$ through the XRD, Raman and XPS results. It was shown that $MoS_2/CNFs$ had the overpotential of 0.278 V at $10mA/cm^2$ and tafel slope of 74.8 mV/dec in 0.5 M sulfuric acid ($H_2SO_4$) electrolyte.

• Korean Chemical Engineering Research
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• v.60 no.1
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• pp.159-168
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• 2022

Catalytic activity in ammonia decomposition reaction was studied on Mo-Al nitride obtained through temperature programmed nitridation of calcined Mo-Al mixed oxide prepared by varying the MoO₃ quantity in the range of 10-50 wt%. N₂ sorption analysis, X-ray diffraction analysis (XRD), X-ray photoelectron spectroscopy (XPS) and H₂-temperature programmed reduction (H₂-TPR), and transmission electron microscopy (TEM) to investigate the physicochemical properties of the prepared catalyst were performed. After calcination at 600 ℃, the XRD of Mo-Al oxide showed γ-Al₂O₃ and Al₂(MoO₄)₃ phases, and the nitride after nitridation showed an amorphous form. The specific surface area after nitridation by topotactic transformation of MoO₃ to nitride was increased due to the formation of Mo nitride, and the Mo nitride was observed to be supported on γ-Al₂O₃. As for the catalytic activity in the ammonia decomposition reaction, 40 wt% MoO₃ showed the best activity, and as the nitridation time increases, the activity increased, and thus the activation energy decreased.

• Clean Technology
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• v.28 no.3
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• pp.210-217
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• 2022

Boron(B) is a rare resource used for various purposes such as glass, semiconductor materials, gunpowder, rocket fuel, etc. However, Korea depends entirely on imports for boron. Considering the global boron reserves and its current production rate, boron will be depleted on earth in 50 years. Thus, a process including proper adsorbent materials recovering boron from seawater is demanded. This research proposed carbonized nanofibers prepared from electrospun PAN(polyacrylonitrile) mats as promising materials to adsorb boron in aqueous solution. First, the mechanism of boron adsorption on carbonized nanofibers was investigated by DFT(density functional method)-based molecular modeling and the calculated energetics demonstrated that the boron chemisorption on the nitrogen-doped graphene surface by a two-step dehydration is possible with viable activation energies. Then, the electrospun PAN mats were stabilized in air and then carbonized in an argon atmosphere before being immersed in the boric acid aqueous solution. Analytically, SEM(scanning electron microscopy) and Raman measurements were employed to confirm whether the electrospinning and carbonization of PAN mats proceeded successfully. Then, XPS(X-ray photoelectron spectroscopy) peak analysis showed whether the intended nitrogen-doped carbon nanofiber surface was formed and boron was properly adsorbed on nanofibers. Those results demonstrated that the carbonized nanofibers prepared from electrospun PAN mats could be feasible adsorbents for boron recovery in seawater.

• Applied Chemistry for Engineering
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• v.25 no.5
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• pp.455-462
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• 2014

This work investigated the hydrophobic coating of silicate yellow phosphor powder in the form of divalent europium-activated strontium orthosilicate ($Sr_2SiO_4:Eu^{2+}$) by using an atmospheric pressure dielectric barrier discharge (DBD) plasma with argon as a carrier and hexamethyldisiloxane (HMDSO), toluene and n-hexane as precursors. After the plasma treatment of the phosphor powder, the lattice structure of orthosilicate was not altered, as confirmed by an X-ray diffractometer. The coated phosphor powder was characterized by scanning electron microscopy, fluorescence spectrophotometry and contact angle analysis (CAA). The CAA of the phosphor powder coated with the HMDSO precursor revealed that the water contact angle increased from $21.3^{\circ}$ to $139.5^{\circ}$ (max. $148.7^{\circ}$) and the glycerol contact angle from $55^{\circ}$ to $143.5^{\circ}$ (max. $145.3^{\circ}$) as a result of the hydrophobic coating, which indicated that hydrophobic layers were successfully formed on the phosphor powder surfaces. Further surface characterizations were performed by Fourier transform infrared spectroscopy and X-ray photoelectron spectrometry, which also evidenced the formation of hydrophobic coating layers. The phosphor coated with HMDSO exhibited a photoluminescence (PL) enhancement, but the use of toluene or n-hexane somewhat decreased the PL intensity. The results of this work suggest that the DBD plasma may be a viable method for the preparation of hydrophobic coating layer on phosphor powder.