• Journal of the Korean Ceramic Society
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• v.49 no.5
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• pp.454-460
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• 2012

The nano-sized zirconia powders were synthesized in an impregnation method using pulp and $ZrOCl_2{\cdot}8H_2O$ as an initial material. The synthesized powders were characterized by XRD and FE-SEM. The particle size of the powder was controlled by preparation conditions, such as drying temperature and time. As a result of the various drying and calcination conditions, 30~50 nm sized homogeneous zirconia particles were obtained at $800^{\circ}C$ for 1 h. Crystallization and the rapid growth of particles were accelerated with increasing calcination temperature and time. Tetragonal phase generated below $800^{\circ}C$ were transferred to monoclinic phase with increasing calcination temperature and time. Moreover, above $800^{\circ}C$, heat treatment time had very large influence on the particle growth, and the change of drying condition also had large influence on the growth of a crystal.

• Korean Journal of Materials Research
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• v.24 no.7
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• pp.357-362
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• 2014

Thermal barrier coatings(TBCs) are being applied in many industrial fields such as thermal power generation, aviation and seasonal fields. $ZrO_2-Y_2O_3$(8%) thermal spray coating powders are commercially used as thermal-barrier coating materials to protect against oxidation and corrosion of heat-resistant alloys at elevated temperatures. Currently, $ZrO_2-Y_2O_3$(8%) thermal-spray powder is made using the industrial co-precipitation process, which is very complex and requires a lot of time. In this study, orthorhombic $ZrO_2$ and $Y_2O_3$ powders were fabricated by mechanical mixing, which is more economical than the co-precipitation process. A tetragonal, yttria-stabilized zirconia(YSZ) coating-layer was produced by plasma spraying, using orthorhombic $ZrO_2-Y_2O_3$(8%) powder. Our experimental results indicate that $ZrO_2-Y_2O_3$(8%) mixed powder can be used economically in industry because it is no longer necessary to make this powder by liquid and gas-phase methods.

• Journal of the Korean Ceramic Society
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• v.30 no.6
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• pp.485-491
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• 1993

Porous glass in the ZrO2.SiO2 system containning up to 30mol% zirconia were prepared by the sol-gel method from metal alkoxides and their pore characteristics with reaction parameters were investigated. The gels were made by hydrolyzing and condensation of the mixed metla alkoxides and were converted into the porous glass by heating up to $700^{\circ}C$. As a results, the mean pore radius became larger with increasing contents of HCl, H2O and hydrolysis temperature, and an alcohol with a large molecular weight for making the porous glass. In the case of 20ZrO2.80SiO2 porous glass with heated at $700^{\circ}C$, HCl and H2O content was 0.3mol and 4mol, the specific surface area was 284$m^2$/g, average mean pore radius was about 19.4$\AA$, porosity was 22.55% and pore characteristics depended on heating temperature.

• Journal of the Korean Ceramic Society
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• v.27 no.8
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• pp.955-964
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• 1990

A new process of emulsiion-spray pyrolysis for synthesizing ceramic powders was developed and the characteristics of Al2O3-20w/o ZrO2 composite powders prepared by this method were investigated. The composite powders synthesized in this study were spherical dense particles with 0.1~0.4${\mu}{\textrm}{m}$ of diameter. As found in powders derived by the emulsion-hot kerosene drying method, all zirconia in Al2O3-20w/o ZrO2 powders heat-treated at 120$0^{\circ}C$ was in the tetragonal form at room temperature. The relative density and the fracture toughness of composites sintered at 1$650^{\circ}C$ for 4hrs were 95% and 5.2MPa.m1/2, respectively.

• Proceedings of the Materials Research Society of Korea Conference
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• 2011.05a
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• pp.241.1-241.1
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• 2011

Numerous possible applications for $ZrO_2$ nanotubes exist such as for catalyst support structures, for sensing or for applications as a solid state electrolyte. Especially, because of a large specific surface area, high efficiency for solid oxide fuel cell (SOFC) application at low temperature can be expected for nanotublar structures in even small size. A zirconium precursor, Tetrakis (ethylmethylamino) zirconium, TEMAZr and $H_2O$ oxidant were used to deposit$ZrO_2$ thin films on an anodized aluminum oxide (AAO) templates having sub-100nm cylindrical pores by atomic layer deposition (ALD) in the temperature range of 150~250$^{\circ}C$. The crystalline structures of as-prepared and post-annealed $ZrO_2$ nanotubes were characterized by x-ray diffraction and high-resolution transmission electron microscopy. The as-prepared samples at $150^{\circ}C$ and $200^{\circ}C$ were showed amorphous, whereas a mixed phase of tetragonal, monoclinic and amorphous polymorph was observed at $250^{\circ}C$. In the bulk, zirconia remains monoclinic phase up to $1,175^{\circ}C$, however, $ZrO_2$ nanotubes were showed tetragonal phase upon post thermal treatments merely at $400^{\circ}C$. This trend may be indicative of high-curvature surfaces of nanotubes and thereby the presence of intrinsic compressive strain. The amount of amorphous structures in the mixed phase as well as as-grown $ZrO_2$ nanotubes were also gradually decreased by subsequent heat treatment.

• Korean Journal of Materials Research
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• v.26 no.2
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• pp.95-99
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• 2016

In this study, 5 um sized $ZrSiO_4$ was ground to 1.9 um, 0.3 um, and 0.1 um sized powders by wet high energy milling process, and the sintering characteristics were observed. Pure $ZrSiO_4$ itself can-not be sintered to these levels of theoretical density, but it was possible to sinter $ZrSiO_4$ powder of nano-scale size of, -0.1 um to the theoretical density and to lower the sintering temperature for full density. Also, the decomposition of $ZrSiO_4$ with a size in the micron range resulted in the formation of monoclinic $ZrO_2$; however, in the nano sized range, the decomposition resulted in the tetragonal phase of $ZrO_2$. So, it was possible to improve the sintering characteristics of nano-sized $ZrSiO_4$ powders.

• Korean Journal of Materials Research
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• v.20 no.10
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• pp.518-523
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• 2010

In this study, partially stabilized zirconia was synthesized using a chemical $Y_2O_3$ stabilizer and hydrothermal method. First, $YCl_3-6H_2O$ and $ZrCl_2O-8H_2O$ was dissolved in distilled water. Y-TZP (a $Y_2O_3$-doped toughened zirconia polycrystalline precursor) was also prepared by conventional co-precipitates in the presence of an excess amount of $NH_4OH$ solution under a fixed pH of 12. The Y-TZP precursors were filtered and repeatedly washed with distilled water to remove $Cl^-$ ions. $ZrO_2$-Xmol%$Y_2O_3$ powder was synthesized by a hydrothermal method using Teflon Vessels at $180^{\circ}C$ for 6 h of optimized condition. The powder added with the Xmol%- $Y_2O_3$ (X = 0,1,3,5 mol%) stabilizer of the $ZrO_2$ was synthesized. The crystal phase, particle size, and morphologies were analyzed. Rectangular specimens of $33mm{\times}8mm{\times}3$ mm for three-point bend tests were used in the mechanical properties evaluation. A teragonal phase was observed in the samples, which contains more than 3 mol% $Y_2O_3$. The $3Y-ZrO_2$ agglomerated particle size was measured at $7.01{\mu}m$. The agglomerated particle was clearly observed in the sample of 5 mol % $Y_2O_3-ZrO_2$, and and the agglomerated particle size was measured at 16.4 um. However, a 20 nm particle was specifically observed by FE-SEM in the sample of 3 mol% $Y_2O_3-ZrO_2$. The highest bending fracture strength was measured as 321.3 MPa in sample of 3 mol% $Y_2O_3-ZrO_2$.

• Journal of the Korean Ceramic Society
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• v.29 no.2
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• pp.119-126
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• 1992

3 mol% Y2O3-doped ZrO2 powders were prepared by hydrolysis with 0.1, 0.2, 0.3, 0.4, 0.5, 0.6 mol/ιH2O/ethanol into 0.1 mol/ι zirconium and yttrium alkoside/ethanol. Spherical monodispersed yttria-partially stabilized zirconia particles with an average diameter of about 0.5 ${\mu}{\textrm}{m}$ were prepared by hydrolysis with 0.2 mol/ιH2O/ethanol. The as-prepared powder was amorphous and with heating it transformed into cubic up to 80$0^{\circ}C$ and into tetragonal over 100$0^{\circ}C$. 3 mol% Y2O3-doped ZrO2 powders calcined over and up to 80$0^{\circ}C$ were a mixture of tetragonal and monoclinic and only tetragonal as determined by X-ray diffraction, respectively.

• Journal of the Korean Ceramic Society
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• v.34 no.2
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• pp.145-156
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• 1997

ZrO2 phase transformations depending on the type and amount of dopants and the sintering temperatures were studied for the 2 components (CaO-, Y2O3-, MgO-ZrO2) and the 3 components(MgO-ZrO2-Al2O3)ZrO2 powder by X-ray diffraction and Raman spectroscopy. In the CaO- and Y2O3-ZrO2 systems, as the CaO and Y2O3 contents increased to 6~15mol% and 3~15mol% respectively, we were not able to identify between tetragonal and cubic in the X-ray diffraction patterns. On the other hand, all Raman modes shifted to lower wavenumbers, decreasing in intensity and the number of bands, markedly. These phenomena were caused by tetragonallongrightarrowcubic phase transformation and interpreted by the breakdown of the wave vector selection rule(k=0) and the structural disorder associated with the formation of oxygen sublattice which was caused by the substitution between Zr4+ ion and Ca2+ or Y3+ ion in ZrO2 matrix. The monoclinic to cubic phase transformation occurred in 10mol% MgO-ZrO2 system. As the Al2O3 content increased from 0 to 20mol% in the MgO-ZrO2-Al2O3 systems, cubic phase transformed to monoclinic phase, this is because the MgO didn't play a role in a stabilizer because of the formation of the spinel(MgAl2O4) by the reaction between MgO and Al2O3, Also, the ZrO2 phase transformation was explained by the change of it's lattice parameters depending on the type and amount of dopants. Namely, as the amount of dopant increased to 10~13mol%, the axial ra-tio c/a came close to unity with increasing the lattice parameter a and decreasing the lattice parameter c. At that time, the tetragonallongrightarrowcubic phase transformation occurred.

• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.204.2-204.2
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• 2014

Among various metal oxides, ZrO2 is of particular interests and has received widespread attention thanks to its ideal mechanical and chemical stability. As a cheap metal, Ag nanoparticles are also widely used as catalysts in ethylene epoxidation and methanol oxidation. However, the nature of Ag-ZrO2 interfaces is still unknown. In this work, the growth, interfacial interaction and thermal stability of Ag nanoparticles on ZrO2(111) film surfaces were studied by low-energy electron diffraction (LEED), synchrotron radiation photoemission spectroscopy (SRPES), and X-ray photoelectron spectroscopy (XPS). The ZrO2(111) films were epitaxially grown on Pt(111). Three-dimensional (3D) growth model of Ag on the ZrO2(111) surface at 300 K was observed with a density of ${\sim}2.0{\times}1012particles/cm2$. The binding energy of Ag 3d shifts to low BE from very low to high Ag coverages by 0.5 eV. The Auger parameters shows the primary contribution to the Ag core level BE shift is final state effect, indicating a very weak interaction between Ag clusters and ZrO2(111) film. Thermal stability experiments demonstrate that Ag particles underwent serious sintering before they desorb from the zirconia film surface. In addition, large Ag particles have stronger ability of inhibiting sintering.