• Journal of the Korean Ceramic Society
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• v.51 no.5
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• pp.466-471
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• 2014

Hydrous zirconia particles were prepared from $ZrOCl_2$ aqueous solution using an electro-dialysis [ED] process. For the preparation of $(Zr,Y)(OH)_4$ precipitates, 3 mol% $YCl_3$ was added into $ZrOCl_2$ aqueous solution. During the hydrolysis of 0.5 mol/L $(Zr,Y)OCl_2$ solution at $90^{\circ}C$ a slurry solution was obtained. The ED process was used for the removal of chlorine from the slurry solution. Two kinds of slurry solution were sampled at the beginning and end of the ED process. The morphology of hydrous zirconia particles in the solution was observed using an inverted optical microscope and an FE-SEM. The hydrous zirconia particles were nano-crystalline, and easily coagulated with drying. Yttrium stabilized zirconia [YSZ] powder could be obtained by the calcination of $(Zr,Y)(OH)_4$ precipitates prepared from a $(Zr,Y)OCl_2$ solution by the ED process. The coagulated dry powders were shaped and sintered at $1500^{\circ}C$ for 2 h. The sintered body showed a dense microstructure with uniform grain morphology.

• 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.

• Korean Journal of Materials Research
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• v.23 no.10
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• pp.543-549
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• 2013

The purpose of this paper was to investigate the effect of a high-energy milling (HEM) process on the particle morphology and the correlation between a thermal treatment and tetragonal/monoclinic nanostructured zirconia powders obtained by a precipitation process. To eliminate chloride residue ions from hydrous zirconia, a modified washing method was used. It was found that the used washing method was effective in removing the chloride from the precipitated gel. In order to investigate the effect of a pre-milling process on the particle morphology of the precipitate, dried $Zr(OH)_4$ was milled using a HEM machine with distilled water. The particle size of the $Zr(OH)_4$ powder exposed to HEM reduced to 100~150 nm, whereas that of fresh $Zr(OH)_4$ powder without a pre-milling process had a large and irregular size of 100 nm~1.5 ${\mu}m$. Additionally, modified heat treatment process was proposed to achieve nano-sized zirconia having a pure monoclinic phase. It was evident that two-step calcining process was effective in perfectly eliminating the tetragonal phase, having a small average particle of ~100 nm with good uniformity compared to the sample calcined by a single-step process, showing a large average particle size of ~300 nm with an irregular particle shape and a broad particle size distribution. The modified method is considered to be a promising process for nano-sized zirconia having a fully monoclinic phase.