• Korean Chemical Engineering Research
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• v.51 no.2
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• pp.208-213
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• 2013

Zirconium hydroxide was synthesized by varying the aging time of the zirconyl chloride octahydrate at $100^{\circ}C$ in aqueous solution and the resulting hydroxides were calcined at $700^{\circ}C$ for 6 h to obtain the crystalline $ZrO_2$. The materials used in this study were characterized by differential thermal analysis (DTA), X-ray diffraction (XRD), $N_2$-sorption, transmission electron microscopy (TEM), $NH_3$ temperature-programmed desorption ($NH_3$-TPD), $CO_2$-TPD and iso-propanol TPD analyses to correlate with catalytic activity for the dehydration of iso-propanol. The pure tetragonal $ZrO_2$ phase was obtained after 24 h aging of zirconium hydroxide and successive calcination at $700^{\circ}C$. The increase of aging time showed the production of smaller particle size $ZrO_2$ resulting that the higher specific surface area and total pore volume. $NH_3$-TPD results revealed that the relative acidity of the catalysts increased along with the increase of aging time. On the other hand, the results of $CO_2$-TPD showed the reverse trend of $NH_3$-TPD results. The best catalytic activity for the dehydration of iso-propanol to propylene was shown over $ZrO_2$ catalyst aged for 168 h which had the highest $S_{BET}$ ($178\;m^2\;g^{-1}$). The catalytic activity could be correlated with high surface area, relative acidity and easy desorption of iso-propanol.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.30 no.5
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• pp.200-207
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• 2020

MoSi₂, (Mo_1/2W_1/2)Si₂, and WSi₂ powders were synthesized by self-propagating high-temperature synthesis (SHS) method. The synthesized powders were heat-treated at 500, 1,000, 1,200, 1,300, 1,400, 1,500 and 1,600℃ in ambient atmosphere. Oxidation of Mo-W silicide powder was found at low temperature of 500℃. XRD structure analysis and DTA/TG data showed that MoO₃ was formed with 500℃ heat treatment for 1 hour, and that it was α-cristobalite phase that was formed with 1200℃ heat treatment, not α-quartz phase which is commonly found and stable at room temperature. Existence of W accelerated decomposition at both low and high temperature. Fully sintered MoSi₂ and (Mo_1/2W_1/2)Si₂ specimen did not show decomposition or weight loss by oxidation, with 1 hour heat treatment at either low or high temperature. Notably, it was difficult to sinter WSi₂ because of oxidation reaction at low temperature.

• 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.

• Journal of the Korean Applied Science and Technology
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• v.34 no.1
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• pp.50-57
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• 2017

Zinc oxide is, one of metal oxide semiconductor, harmless to human and environment-friendly. It has excellent chemical and thermal stability properties. Wurtzite-zinc oxide is a large band gap energy of 3.37 eV and high exciton binding energy of 60 meV. It can be applied to various fields, such as solar cells, degradation of the dye waste, the gas sensor. The photocatalytic activity of zinc oxide is varied according to the particle shape and change of crystallinity. Therefore, It is very important to specify the additives and the experimental variables. In this study, the zinc oxide were synthesized by using a microwave assisted hydrothermal synthesis. The precursor was used as the zinc nitrate, the pH value was controlled as 11 by NaOH. Surfactants are the ethanolamine, cetyltrimethylammonium bromide, sodium dodecyl sulfate, sorbitan monooleate was added by changing the concentration. The composite particles had the shape of a star-like, curcular cone, seed shape, flake-sphere. Physical and chemical properties of the obtained zinc oxide was characterized using x-ray diffractometer, field emission scanning electron microscopy, thermogravimetric analysis and optical properties was characterized using UV-visible spectroscopy, photoluminescence and raman spectroscopy.

• Journal of the Korea Concrete Institute
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• v.29 no.4
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• pp.399-406
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• 2017

CaO-based by-product, which consist of CaO, $SO_3$, $Al_2O_3$ and so on, has being used to raw materials of CaO compound. When It was applied to recycling water of remicon, concrete performance can be enhanced because hydration reaction of powder material is accelerated. In this study, activated-sludge, which was putted desulfurization gypsum of CaO-based in recycling water, was manufactured to verify effect of them, and then they was investigated by characteristics of cement matrix and mortar. As a results, they indicated reduction of setting time and high soundness in cement matrix, and acceleration of hydration reaction can be verified by XRD analysis. Also, it can be maintained good workability if water content by usage of desulfurization gypsum, which used for production of activated-sludge, was adjusted. In addition, it can be verified strength development by activated-sludge although cement content by usage of desulfurization gypsum was reduced.

• Progress in Superconductivity and Cryogenics
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• v.19 no.1
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• pp.36-41
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• 2017

The effects of $MgB_4$ addition on the superconducting properties and the microstructure of in situ processed $MgB_2$ bulk superconductors were studied. $MgB_4$ powder of 1-20 wt.% was mixed with (Mg + 2B) powder and then pressed into pellets. The pellets of (Mg + 2B + $xMgB_4$) were heat-treated at $650^{\circ}C$ for 1 h in flowing argon. The powder X-ray diffraction (XRD) analysis for the heat-treated samples showed that the major formed phase in all samples was $MgB_2$ and the minor phases were $MgB_4$ and MgO. The full width at half maximum (FWHM) values showed that the grain size of $MgB_2$ decreased as the amount of $MgB_4$ addition increased. $MgB_4$ particles included in a $MgB_2$ matrix is considered to suppress the grain growth of $MgB_2$. The onset temperatures ($T_{c,onset}$) of $MgB_2$ with $MgB_4$ addition (0-10 wt.%) was between 37-38 K. The 20 wt.% $MgB_4$ addition slightly reduced the $T_{c,onset}$ of $MgB_2$ to 36.5 K. This result indicates that $MgB_4$ addition did not influence the superconducting transition temperature ($T_c$) of $MgB_2$ significantly. On the other hand, the small additions of 1-5 wt.% $MgB_4$ increased the critical current density ($J_c$) of $MgB_2$. The $J_c$ enhancement by $MgB_4$ addition is attributed not only to the grain size refinement but also to the possible flux pinning of $MgB_4$ particles dispersed in a $MgB_2$ matrix.

• Applied Chemistry for Engineering
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• v.10 no.5
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• pp.772-777
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• 1999

$Y_2Ba_1Cu_1O_5(Y211)$ powders were prepared by pyrophoric synthesis method and by solid state reaction method using $Y_2O_3(99.9%)$, $BaCO_3(99.9%)$, and CuO(99.9%) powders in both of these processes. The phase formation and reaction kinetics of $Y_2Ba_1Cu_1O_5$ powders have been studied using X-ray diffraction analysis(XRD) of samples at various heat treatment temperatures and reaction time. The reaction characterization suggested that the phase formation rate is mainly controlled by the particle size of Y211 powders. The activation energy(${\Delta}E_a$) of Y211 phase formation in this pyrophoric synthesis method was found to be 136.42 kJ/mol compared with 149.46 kJ/mol for that of solid state reaction method. These results data showed that the pyrophoric synthesis method is kineticaly more efficient than the solid state reaction method in this $Y_2Ba_1Cu_1O_5$ system.

• The Journal of Korean Academy of Prosthodontics
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• v.43 no.3
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• pp.363-378
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• 2005

Statement of problem. Hydroxyapatite(HA) coated titanium surfaces have not yet showed the reliable osseointegration in various conditions. Purpose. This study was aimed to investigate microstructures, chemical composition, and surface roughness of the surface coated by the hydrothermal method and to evaluate the effect of hydrothermal coating on the cell attachment, as well as cell proliferation. Material and Methods. Commercially pure(c.p.) titanium discs were used as substrates. The HA coating on c.p. titanium discs by hydrothermal method was performed in 0.12M HCl solution mixed with HA(group I) and 0.1M NaOH solution mixed with HA(group II). GroupⅠ was heated at 180 $^{\circ}C$ for 24, 48, and 72 hours. GroupⅡ was heated at 180 $^{\circ}C$ for 12, 24, and 36 hours. And the treated surfaces were evaluated by Scanning electron microscopy(SEM), Energy dispersive X-ray spectroscopy(EDS), X-ray photoelectron spectroscopy(XPS), X-ray diffraction method(XRD), Confocal laser scanning microscopy(CLSM). And SEM of fibroblast and 3-(4,5- dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide(MTT) assay were used for cellular responses of the treated surfaces. Results. The color of surface changed in both groups after the hydrothermal process. SEM images showed that coating pattern was homogeneous in group II, while inhomogeneous in group I. H72 had rosette-like precipitates. The crystalline structure grew gradually in group II, according to extending treatment period. The long needle-like crystals were prominent in N36. Calcium(Ca) and phosphorus(P) were not detected in H24 and H48 in EDS. In all specimens of group II and H72, Ca was found. Ca and P were identified in all treated groups through the analysis of XPS, but they were amorphous. Surface roughness did not increase in both groups after hydrothermal treatment. The values of surface roughness were not significantly different between groups I and II. According to the SEM images of fibroblasts, cell attachments were oriented and spread well in both treated groups, while they were not in the control group. However, no substantial amount of difference was found between groups I and II. Conclusions. In this study during the hydrothermal process procedure, coating characteristics, including the HA precipitates, crystal growth, and crystalline phases, were more satisfactory in NaOH treated group than in HCl treated group. Still, the biological responses of the modified surface by this method were not fully understood for the two tested groups did not differ significantly. Therefore, more continuous research on the relationship between the surface features and cellular responses seems to be in need.

• The Transactions of The Korean Institute of Electrical Engineers
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• v.56 no.9
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• pp.1602-1608
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• 2007

The composites were fabricated, respectively, using 61[vol.%] SiC-39[vol.%] $TiB_2$ and using 61[vol.%] SiC-39[vol.%] $ZrB_2$ powders with the liquid forming additives of 12[wt%] $Al_2O_3+Y_2O_3$ by hot pressing annealing at $1650[^{\circ}C]$ for 4 hours. Reactions between SiC and transition metal $TiB_2$, $ZrB_2$ were not observed in this microstructure. The result of phase analysis of composites by XRD revealed SiC(6H, 3C), $TiB_2$, $ZrB_2$ and $YAG(Al_5Y_3O_{12})$ crystal phase on the Liquid-Phase-Sintered(LPS) $SiC-TiB_2$, and $SiC-ZrB_2$ composite. $\beta\rightarrow\alpha-SiC$ phase transformation was occurred on the $SiC-TiB_2$ and $SiC-ZrB_2$ composite. The relative density, the flexural strength and Young's modulus showed the highest value of 98.57[%], 249.42[MPa] and 91.64[GPa] in $SiC-ZrB_2$ composite at room temperature respectively. The electrical resistivity showed the lowest value of $7.96{\times}10^{-4}[\Omega{\cdot}cm]$ for $SiC-ZrB_2$ composite at $25[^{\circ}C]$. The electrical resistivity of the $SiC-TiB_2$ and $SiC-ZrB_2$ composite was all positive temperature coefficient resistance (PTCR) in the temperature ranges from $25[^{\circ}C]$ to $700[^{\circ}C]$. The resistance temperature coefficient of composite showed the lowest value of $1.319\times10^{-3}/[^{\circ}C]$ for $SiC-ZrB_2$ composite in the temperature ranges from $100[^{\circ}C]$ to $300[^{\circ}C]$ Compositional design and optimization of processing parameters are key factors for controlling and improving the properties of SiC-based electroconductive ceramic composites.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.3 no.1
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• pp.57-65
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• 2005

This study suggested a new method for the solidification of molten salt waste generated from the electro-metallurgical process in the spent fuel treatment. Using binary material system, sodium silicate and phosphoric acid, metal chlorides were converted into metal phosphate in the micro-reaction module formed by SiO$_{2} particles. The volatile element in the reaction module would little vaporized below 1100$^{circ}$C After the gel product was mixed with borosilicate glass powder and thermally treated at 1000$^{circ}$C, li exists as Li$_{3}$PO$_4$ separated from glass phase and, Cs and Sr would be incorporated into an amorphous phase from XRD analysis. In case of the addition of ZrCl$_{4}$ to the binary system, the gel products were transformed into NZP structure considered as an prospective ceramic waste form after heat-treatment above 700 $^{circ}$C. From these results, the gel-route pretreatment can be considered as an effective approach to the solidincation of molten salt waste by the confirmed process or waste form and this also would be an alternative method on the ANL method using zeolites in USA by the confirmation of its chemical durability as an future work.