• Journal of the Korean Ceramic Society
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• v.24 no.3
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• pp.243-250
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• 1987

The effects aging on some properties and thermal-shock behavior of zirconia partially stabilized with 9 mol% MgO (9MZ) were studied. 9MZ specimens were aged over $1200^{\circ}$-$1400^{\circ}C$ for 12hours subsequently, after sintering at $1650^{\circ}C$ for 4 hours. Fracture strength(both before and after thermal-shock test), linear thermal expansion, monoclinic fraction and phase transition by XRD, density, galvanic potential and microstructure were measured. Quantitative chemical analysis around the grain-boundary of the specimen aged at $1350^{\circ}C$ was also conducted by EDX. The aging of 9MZ specimen causes a thermal decomposition of cubic-$ZrO^{2}$ into the formation metastable tetragonal-$ZrO^{2}$ and MgO. The former increases the residual strength after thermal-shock test and the latter improves the thermal-shock resistance due to thermal conduction through the continuous magnesia phase and the formation of monoclinic phase content in matrix were increased with decreasing the aging temperature from $1400^{\circ}C$ to $1200^{\circ}C$. Galvanic potential of the aged specimen exhibited a proper emf characteristic.

• Journal of the Korean Institute of Illuminating and Electrical Installation Engineers
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• v.24 no.4
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• pp.140-148
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• 2010

The effects of the addition of either monoclinic $ZrO_2(ZrO_2(m))$ or tetragonal $ZrO_2(ZrO_2(t))$ containing 5.35[wt%] $Y_2O_3$ on the physical properties and electrical conductivity of $Al_2O_3$ were investigated. The addition of $ZrO_2$(m) and $ZrO_2$(t) increased sintered density of $Al_2O_3$. The Vickers hardness also increased as addition of $ZrO_2$(t) increased going through a maximum at 20[wt%] and the hardness of the specimens was found to be dependent on the sintered density. The addition of $ZrO_2$(t) improved the hardness of $Al_2O_3-ZrO_2$ systems and the $ZrO_2$(m) addition showed the better effect on the thermal shock property of $Al_2O_3-ZrO_2$ systems than that of the $ZrO_2$(t) addition. Above 15[wt%] addition of $ZrO_2$(t), the electrical conductivity is gradually increased with increasing applied voltage but not effects by addition of $ZrO_2$(m).

• Journal of the Korean Vacuum Society
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• v.15 no.5
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• pp.534-540
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• 2006

Thin films of $V_2O_3$, $VO_2$, and $V_2O_5$ were obtained from a single precursor solution through post-annealing processes under different annealing conditions. As annealed in air, the deposited films became $V_2O_5$ with orthorhombic crystal structure, while they were $V_2O_3$ and $VO_2$ with rhombohedral and monoclinic crystal structure as annealed in vacuums with base pressure of $1{\times}10^{-6}$ Torr and with 10 mTorr $O_2$ pressure, respectively. Electrical and optical measurements indicated that the $V_2O_5$ and $VO_2$ films are semiconducting, while the $V_2O_3$ films are metallic at room temperature. Chromium doping in $VO_2$ resulted in a decrease of the resistivity and changed the conduction type from n-type to p-type. 10% Cr-doped $VO_2$ films were found to have orthorhombic crystal structure, which is different from that of the undoped $VO_2$. Spectral features in the optical absorption spectra of all the films were interpreted as the transitions involving O 2p and V 3d bands. The crystal-field splittings between $t_{2g}$ and $e_g$ states of the V 3d bands are estimated to be about 1.5 and 1.0 eV for $V_2O_5$ and $VO_2$, respectively.

• Korean Chemical Engineering Research
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• v.46 no.3
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• pp.550-554
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• 2008

The synthesis of dimethyl carbonate (DMC) from methanol and supercritical carbon dioxide over $K_2CO_3/ZrO_2$ catalysts have been studied. The catalysts were prepared by impregnating $ZrO_2$ with an aqueous $K_2CO_3$ solution. The optimum calcination temperature to disperse K species on the $ZrO_2$ surface was found to be 673 K. Monoclinic $ZrO_2$ was not active, as itself, for the DMC production. However, when the $K_2CO_3$ was impregnated on the $ZrO_2$, the catalytic performance was improved. Besides the catalyst, $CH_3I$ was used as a promoter. The $CH_3I$ promoter as well as the $K_2CO_3/ZrO_2$ catalyst was found to take an important role to improve the production of DMC. The optimum quantities for the catalyst and the promoter were estimated. The effect of the catalyst and the promoter for the DMC synthesis from methanol and supercritical carbon dioxide was investigated and the reaction mechanism was proposed.

• 전자공학회논문지 IE
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• v.49 no.2
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• pp.1-8
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• 2012

The effects of the addition of either monoclinic $ZrO_2(pure)$ or tetragonal $ZrO_2$ containing 5.35wt% $Y_2O_3(Y-TZP)$ on the mechanical properties and thermal shock resistance of $Al_2O_3$ ceramics were investigated. The addition of $ZrO_2$(m) and Y-TZP increased sintered density of $Al_2O_3$. The Vickers hardness also increased as the volume fraction of Y-TZP increased going through a maximum at 20wt%. The hardness of the specimens was found to be dependent on the sintered density. The higher volume fraction of either $ZrO_2(m)$ or Y-TZP resulted in the higher fracture toughness of the composite was. This result may be taken as evidence that toughening of $Al_2O_3$ can be achieved by not only the transformation toughening but microcrack toughening of $ZrO_2$. The thermal shock property for $Al_2O_3-ZrO_2$ composites was improved by increasing the volume fraction of monoclinic $ZrO_2(pure)$. The grain size increased as the volume fraction of $ZrO_2$ did.

• Analytical Science and Technology
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• v.13 no.2
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• pp.173-178
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• 2000

A new open-chain ligand containing two phenol groups, 1, 14-Bis (2-hydroxybenzyl)-2, 6, 9, 12-tetraazatetradecane(bsated) was synthesized as its tetrahydrochloride salt and characterized by elemental analysis, mass, infrared and NMR. Its proton dissociation constants ($logK^n{_H}$) and stability constants ($logK_{ML}$) toward $Co^{2+}$, $Ni^{2+}$, $Cu^{2+}$ and $Zn^{2+}$ were determined at $25^{\circ}C$ and 0.10M($KNO_3$) ionic strength in aqueous solution by potentiometry. The X-ray structure of its copper (II) complex [Cu(bsated)]$(ClO_4)_2$ was reported: Monoclinic space group $P2_1/n$, $a=17.856(4){\AA}$, $b=17.709(1){\AA}$, $c=8.539(2){\AA}$, $V=2700(2){\AA}$ with Z=4. Electrochemical studies of [Cu(bsated)]$(ClO_4)_2$ complex in dimethyl sulfoxide (DMSO) solution containing tetrabutylammonium perchlorate (supporting electrolyte) were carried out by cyclic voltammograms (CV) and normal pulse voltammetry (NPV).

• Korean Journal of Materials Research
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• v.9 no.9
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• pp.943-947
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• 1999

The crystal structure and the microwave dielectric properties of $La(Mg_{1/2}Ti_{1/2})O_3$ ceramics have been investigated. $La(Mg_{1/2}Ti_{1/2})O_3$ has the 1:1 ordered monoclinic structure with the lattice parameters of $a = 5.5467(3){\AA}, b = 5.5616(3){\AA}, c = 7.8426(5) {\AA} and \beta = 89.9589 (2)^{\circ}$ The spacegroup of LMT is $P2_1/n$. Monoclinic LMT has the in­phase and anti-phase tilting of octahedra with the $a^_a^_c^_$ tilting system. Anti-parallel shift of A-site cations was also found in LMT. The relative density of the specimens sintered above $1600^{\circ}C$ was ranged between 95 % and 96 % of the theoretical density and the dielectric constant of specimens was about 28. The highest $Q\timesf$ achieved in this investigation was 63,100 for the specimen sintered at $1630^{\circ}C$ for 5 hr. Temperature coefficient of resonance frequency ranged from $>-74 ppm/^{\circ}C ~ -79 ppm/^{\circ}C$.

• Korean Journal of Materials Research
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• v.22 no.5
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• pp.220-226
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• 2012

Pure zirconia and $x$ mol% calcia partially stabilized zirconia ($x$ = 1.5, 3, and 8) nanopowders were synthesized by hydrothermal method with various reaction temperatures for 24 hrs. The precipitated precursor of pure zirconia and $x$ mol% calcia doped zirconia was prepared by adding $NH_4OH$ to starting solutions; resulting sample was then put into an autoclave reactor. The optimal experimental conditions, such as reaction temperatures and times and amounts of stabilizer CaO, were carefully studied. The synthesized $ZrO_2$ and $x$ mol% CaO-$ZrO_2$ ($x$ = 1.5, 3, and 8) powders were characterized by XRD, SEM, TG-DTA, and Raman spectroscopy. When the hydrothermal temperature was as low as $160^{\circ}C$, pure $ZrO_2$ and $x$ mol% CaO-$ZrO_2$ ($x$ = 1.5 and 3) powders were identified as a mixture of monoclinic and tetragonal phases. However, a stable tetragonal phase of zirconia was observed in the 8 mol% calcia doped zirconia nanopowder at hydrothermal temperature above $160^{\circ}C$. To observe the phase transition, the 3 mol% CaO-$ZrO_2$ and 8 mol% CaO-$ZrO_2$ nanopowders were heat treated from 600 to $1000^{\circ}C$ for 2h. The 3 mol% CaO-$ZrO_2$ heat treated at above $1000^{\circ}C$ was found to undergo a complete phase transition from mixture phase to monoclinic phase. However, the 8 mol% calcia doped zirconia appeared in the stable tetragonal phase after heat treatment. The result of this study therefore should be considered as the preparation of 8 mol% CaO-$ZrO_2$ nanopowders via the hydrothermal method.

• Korean Chemical Engineering Research
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• v.40 no.6
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• pp.741-745
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• 2002

Yttria-stabilized zirconia(YSZ) nanopowders were prepared by sol-gel method using zirconium-n-butoxide(ZNB) and yttrium nitrate as precursors. In addition, the effect of water content added during the hydrolysis reaction of ZNB was investigated on the phase composition and pore structure of the product powders. The phase composition of YSZ nanopowders with calcination temperatures showed the same trend, irrespective of $H_2O$ amounts added during the hydrolysis reaction of ZNB. All powders dried at $100^{\circ}C$ were amorphous and transformed to cubic phase at $400^{\circ}C$, which converted to tetragonal phase at $1,000^{\circ}C$. Monoclinic phase also appeared at $1,000^{\circ}C$. The powders showed the mixture of tetragonal and monoclinic phases from $1,000^{\circ}C$ to $1,400^{\circ}C$. The pore size distributions of the dried powders prepared with small amounts of water(less than or equal to $H_2O/ZNB=20$) showed mesopores, while those prepared with large amounts of water(greater than or equal to $H_2O/ZNB=50$) exhibited micropores.

• Bulletin of the Korean Chemical Society
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• v.33 no.1
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• pp.48-54
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• 2012

The $[Fe_4S_4]^{2+}$ clusters with 2-, 3-, and 4-pyridinemethanethiolate (S2-Pic, S3-Pic, and S4-Pic, respectively) terminal ligands have been synthesized from the ligand substitution reaction of the $(^nBu_4N)_2[Fe_4S_4Cl_4]$ (I) cluster. The new $(^nBu_4N)_2[Fe_4S_4(SR)_4]$ (R = 2-Pic; II, 3-Pic; III, 4-Pic; IV) clusters were characterized by FTIR and UV-Vis spectroscopy. Cluster II was crystallized in the monoclinic space group C2/c with a = 24.530 (5) $\AA$, b = 24.636(4) $\AA$, c = 21.762(4) $\AA$, ${\beta}=103.253(3)^{\circ}$, and Z = 8. The X-ray structure of II showed two unique 2:2 site-differentiated $[Fe_4S_4]^{2+}$ clusters due to the bidentate-mode coordination by 2-pyridinemethanethiolate ligands. Cluster III was crystallized in the same monoclinic space group C2/c with a = 26.0740(18) $\AA$, b = 23.3195(16) $\AA$, c = 22.3720(15) $\AA$, ${\beta}=100.467(2)^{\circ}$, and Z = 8. The 3-pyridinemethanethiolate ligand of III was coordinated to the $[Fe_4S_4]^{2+}$ core as a terminal mode. Cluster IV with 4-pyridinemethanethiolate ligands was found to have a similar structure to the cluster III. Fully reversible $[Fe_4S_4]^{2+}/[Fe_4S_4]^+$ redox waves were observed from all three clusters by cyclic voltammetry measurement. The electrochemical potentials for the $[Fe_4S_4]^{2+}/[Fe_4S_4]^+$ transition decreased in the order of II, III and IV, and the reduction potential changes by the ligands were explained based on the structural differences among the complexes. The complex III was reacted with sulfonium salt of $[PhMeSCH_2-p-C_6H_4CN](BF_4)$ in MeCN to test possible radical-involving reaction as a functional model of the [$Fe_4S_4$]-SAM (S-adenosylmethionine) cofactor. However, the isolated reaction products of 3-pyridinemethanethiolate-p-cyanobenzylsulfide and thioanisole suggested that the reaction followed an ionic mechanism and the products formed from the terminal ligand attack to the sulfonium.