• Journal of the Korean Ceramic Society
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• v.47 no.4
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• pp.343-352
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• 2010

A zirconia gel/polymer hybrid nanofiber was produced in a nonwoven fabric mode by electrospinning a sol derived from hydrolysis of zirconium butoxide with a polyvinyl butyral. Results indicated that the hydroxyl groups on the vinyl alcohol units in the backbone of the polymer were involved in the hydrolysis as well as grafting the hydrolyzed zirconium butoxide. In addition, use of acetic acid as a catalyst resulted in further hydrolysis and condensation in the sol, which led to the growth of -Zr-O-Zr- networks among the polymer chains. These networks gradually transformed into a crystalline zirconia structure upon heating. The as-spun fiber was smooth but partially wrinkled on the surface. The average fiber diameter was $690{\pm}110\;nm$. The fiber exhibited a strong but broad blue photoluminescence with its maximum intensity at a wavelength of ~410 nm at room temperature. When the fiber was heat-treated at $400^{\circ}C$, the fiber diameter shrunk to $250{\pm}60\;nm$. Nanocrystals which belonged to a tetragonal zirconia phase and were ~5 nm in size appeared. A strong white photoluminescence was observed in this fiber. This suggests that oxygen or carbon defects associated with the formation of the nanocrystals play a role in generating the photoluminescence. Further heating to $800^{\circ}C$ resulted in a monoclinic phase beginning to form In the heat-treated fibers, coloring occurred but varied depending on the heating temperature. Crystallization, coloring, and phase transition to the monoclinic structure influenced the photoluminescence. At $600^{\circ}C$, the fiber appeared to be fully crystallized to a tetragonal zirconia phase.

• Korean Chemical Engineering Research
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• v.53 no.5
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• pp.620-626
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• 2015

$Ho^{3+}$ doped $SrAl_2O_4$ upconversion phosphor powders were synthesized by spray pyrolysis, and the crystallographic properties and luminescence characteristics were examined by varying activator concentrations and heattreatment temperatures. The effect of organic additives on the crystal structure and luminescent properties was also investigated. $SrAl_2O_4:Ho^{3+}$ powders showed intensive green emission due to the $^5F_4/^5S_2{\rightarrow}^5I_8$ transition of $Ho^{3+}$. The optimal $Ho^{3+}$ concentration in order to achieve the highest luminescence was 0.1%. Over this concentration, emission intensities were largely diminished via a concentration quenching due to dipole-dipole interaction between activator ions. According to the dependence of emission intensity on the pumping power of a laser diode, it was clear that the upconversion of $SrAl_2O_4:Ho^{3+}$ occurred via the ground state absorption-excited state absorption processes involving two near-IR photons. Synthesized powders were monoclinic as a major phase, having some hexagonal phase. The increase of heat-treatment temperatures from $1000^{\circ}C$ to $1350^{\circ}C$ led to crystallinity enhancement of monoclinic phase, reducing hexagonal phase. The hexagonal phase, however, did not disappear even at $1350^{\circ}C$. When both citric acid (CA) and ethylene glycol (EG) were added to the spray solution, the resulting powders had pure monoclinic phase without forming hexagonal phase, and led to largely enhancement of crystallinity. Also, N,N-Dimethylformamide (DMF) addition to the spray solution containing both CA and EG made it possible to effectively reduce the surface area of $SrAl_2O_4:Ho^{3+}$ powders. Consequently, the $SrAl_2O_4:Ho^{3+}$ powders prepared by using the spray solution containing CA/EG/DMF mixture as the organic additives showed about 168% improved luminescence compared to the phosphor prepared without organic additives. It was concluded that both the increased crystallinity of high-purity monoclinic phase and the decrease of surface area were attributed to the large enhancement of upconversion luminescence.

• Journal of the Institute of Electronics Engineers of Korea TE
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• v.39 no.4
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• pp.341-349
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• 2002

Electrical, mechanical and sinterability properties of yttria-stabilized zirconia doped with 5.35wt% $Y_2$O$_3$(Y$_2$O$_3$- containing stabilized zirconia : YSZ) were studied as a function of $Al_2$O$_3$, CoO, Fe$_2$O$_3$ and MnO$_2$ addition. The ratio of monoclinic phase to tetragonal phase was changed by the addition of $Al_2$O$_3$, CoO, Fe$_2$O$_3$ and MnO$_2$ to 8.00 wt% and sintered density decreased with increasing $Al_2$O$_3$, CoO, Fe$_2$O$_3$ and MnO$_2$ addition. Fracture toughness increased with the increase of monoclinic to tetragonal phase ratio and was maximum at about 18%. When transition metals such as CoO, Fe$_2$O$_3$ or MnO$_2$ was added more than 1.5 wt%, the electrical conductivity of YSZ increased. But $Al_2$O$_3$ hardly affected the electrical conductivity of YSZ. The addition of $Al_2$O$_3$, CoO, Fe$_2$O$_3$ and MnO$_2$ into YSZ resulted in the more complex behavior of fracture toughness and hardness variation and the specimen with 1.5wt%-Fe$_2$O$_3$, 3.0wt%-Al$_2$O$_3$ and 1.5wt%-CoO showed the monoclinic to tetragonal phase ratio of 18% and the highest toughness of 10.8 MPa.m$^{1}$2/ and Vickers hardness of 1201 kgf/mm$^2$.

• Korean Journal of Materials Research
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• v.21 no.10
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• pp.563-567
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• 2011

We report the structural characterization of $Bi_xZn_{1-x}O$ thin films grown on c-plane sapphire substrates by plasma-assisted molecular beam epitaxy. By increasing the Bi flux during the growth process, $Bi_xZn_{1-x}O$ thin films with various Bi contents (x = 0~13.17 atomic %) were prepared. X-ray diffraction (XRD) measurements revealed the formation of Bi-oxide phase in (Bi)ZnO after increasing the Bi content. However, it was impossible to determine whether the formed Bi-oxide phase was the monoclinic structure ${\alpha}-Bi_2O_3$ or the tetragonal structure ${\beta}-Bi_2O_3$ by means of XRD ${\theta}-2{\theta}$ measurements, as the observed diffraction peaks of the $2{\theta}$ value at ~28 were very close to reflection of the (012) plane for the monoclinic structure ${\alpha}-Bi_2O_3$ at 28.064 and the reflection of the (201) plane for the tetragonal structure ${\beta}-Bi_2O_3$ at 27.946. By means of transmission electron microscopy (TEM) using a diffraction pattern analysis and a high-resolution lattice image, it was finally determined as the monoclinic structure ${\alpha}-Bi_2O_3$ phase. To investigate the distribution of the Bi and Bi-oxide phases in BiZnO films, elemental mapping using energy dispersive spectroscopy equipped with TEM was performed. Considering both the XRD and the elemental mapping results, it was concluded that hexagonal-structure wurtzite $Bi_xZn_{1-x}O$ thin films were grown at a low Bi content (x = ~2.37 atomic %) without the formation of ${\alpha}-Bi_2O_3$. However, the increased Bi content (x = 4.63~13.17 atomic %) resulted in the formation of the ${\alpha}-Bi_2O_3$ phase in the wurtzite (Bi)ZnO matrix.

• The Korean Journal of Ceramics
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• v.1 no.1
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• pp.35-39
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• 1995

Yttrium aluminum garnet(YAG) powders were synthesized by spray-drying of the hydroxides coprecipitated from a mixture of aqueous solutions of $Al(NO_3)_3.9H_2O \;and\; Y(NO_3)_3.6H_2O$ Phase formation in the powders during heat treatments and their sintering charactristics were investigated. In the powder obtained by washing the hydroxides before spray-drying, a metastable yttrium aluminum hexagonal (YAH) phase was first crystallized and then transformed into YAG as temperature was increased. The formation of YAH was attributed to a deviation in compositions of the particles from the starting composition of YAG. However, the powder prepared without washing step contained a stable yttrium aluminum monoclinic(YAM) phase in addition to YAG due to a large deviation from the starting composition. A powder compact of a single phase YAG was pressureless-sintered for 4 hrs at $1700^{\circ}C$ and the density was 93% of the theoretical density.

• Journal of the Korean Ceramic Society
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• v.39 no.5
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• pp.438-445
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• 2002

In this study, the glass frit of $PbO-TiO-2-SiO_2-BaO-ZnO-Al_2O-3-CaO-B_2O_3-Bi_2O_3-MgO$ system was manufactured. The glass was melted at $1,400{\circ}C$, quenched and attrition-milled. The glass frit powder was pressed and fired for 2h at the range of $750~1,000{\circ}C$. The crystallization of glass frit began at about $750{\circ}$ and at low temperature, the main crystal phases were hexagonal celsian($BaAl_2Si_2O_8$) and alumina. As the firing temperature increased, the crystal phases of monoclinic celsian, zinc aluminate, zinc silicate, calcium titanium silicate and titania appeared. And the increase of firing temperature led to transformation of hexagonal celsian to monoclinic. The only glass frit containing 15wt% PbO had the crystal phase of solid solution of $PbTiO_3-CaTiO_3$. At the frequency of 1 MHz, the dielectric constant of glass frit crystallized was in the range of 11~16 and the dielectric loss less than 0.020. But the glass frit containing 15wt% PbO had the dielectric constant of 17~26 and loss of 0.010~0.015 because of crystal phase of solid solution of $PbTiO_3-CaTiO_3$.

• Proceedings of the Korean Society of Tribologists and Lubrication Engineers Conference
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• 2000.11a
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• pp.298-303
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• 2000

The 3 mol% yttria stabilized zirconia (3-Y PSZ) powder was heat treated at 50 0$^{\circ}C$ to evaporate the polymer binder and stabilize the tetragonal phase. The wear experiments were carried out on a ring-on-plate type reciprocating wear tester at selected temperatures with in the range room temperature to 600$^{\circ}C$ The results show that the heat treatment of powder decreases the wear rate due to the reduction of microcracks and pores in coatings and the stabilization of the tetragonal phase. Powder heat treatment enhanced the quality of the coating layer by removing remnant gases during coating process and the powder heat treatment at which tetragonal phase is stable diminished phase ratio of monoclinic. These two effects improved wear resistance characters.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.12 no.3
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• pp.126-132
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• 2002

The nanocrystalline zirconia powder with anisotropic shapes was synthesized by hydrothermal treatment of the tetragonal zirconia prepared by aging the zirconium hydroxide precipitate, which was obtained from the reaction between $ZrOCl_2{\cdot}8H_2O$ and KOH solutions under the fixed pH of 13.5, at $100^{\circ}C$ for 24 h. With increasing the hydrothermal reaction temperature and time, the fraction of tetragonal phase with spherical zirconia decreased, whereas, relatively the fraction of monoclinic phase with spindle-like and rod shape zirconia increased. As increased concentration of the NaOH solution it promoted the particle size to become larger and the crystalline phase to transform tetragonal to monoclinic. However, the specific surface area at the early stage of the reaction increased and subsequently decreased because of grain growth in powder with longer reaction time.

• Electrical & Electronic Materials
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• v.16 no.9
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• pp.62.2-62
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• 2003

Material Characteristics of zirconium oxide thin films obtained by plasma enhanced chemical vapor deposition on p-type Si(100) substrates were investigated to explain their unable electrical properties. The films obtained without heating had polycrystalline nanograins that are mostly of a tetragonal phase under oxygen-deficient plasma conditions but transformed into a monoclinic phase with increasing $O_2$ addition in the plasma. Mostly amorphous bulk $ZrO_2$ with a relatively thicker and smoother interfacial layer was obtained from oxygen-rich plasmas, resulting in a decrease in both the overall dielectric constant and the leakage current density. the interfacial layer formed between the bulk $ZrO_2$ and Si substrate was analyzed to be zirconium silicate, which approached $SiO_2$ as its zirconium content decreased with the increasing gas phase $O_2$ content.

• Journal of the Korean Ceramic Society
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• v.29 no.5
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• pp.341-346
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• 1992

The effects of CaO addition on the low temperature degradation behavior of 2.5Y-TZP ceramics were investigated. Y2O3-CaO-ZrO2 ceramics were prepared from the commercial Y-TZP powder added within 1 mol% of CaO. Fully tetragonal phase could be obtained at each composition under sintering condition of 1500$^{\circ}C$ for 1 hour. As the amount of CaO increased, grain size was decreased. From the result of heat treatment at 200$^{\circ}C$, volume fraction of monoclinic phase formed on the surface of each specimen was decreased with higher CaO amount. Stability of tetragonal ZrO2 phase for low temperature heat treatment was increased by CaO addition without the degradation of mechanical properties.