• 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.

• Journal of the Korean Ceramic Society
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• v.27 no.6
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• pp.707-712
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• 1990

The basic zirconium sulfate was prepared from ZrOCl2.8H2O and H2SO4 in the 9$0^{\circ}C$ aqueous solution. The pH and amount of unreacted zirconium in the solution that reacton had completed was 0.2 and 10%. As the pH was increased to 1.4 by NH4OH theresulting precipitates were the mixtures of the basic zirconium sulfate and the zirconium hydroxide although the precipitates were recovered completely. The thermal decomposition behavior of this sample has been examined by thermal analysis(TG-DTA), X-ray diffraction study, infrared spectroscopy and sulfur analysis. As a result, it was found that the precipitates have perfectly been decomposed at 85$0^{\circ}C$ accompanying to the release of a molecule of water below 25$0^{\circ}C$ and 85% sulfate at about $600^{\circ}C$. The thermally decomlposed products were initially amorphous phase, which were become metastable tetragonal phase with increment of temperature and finally transformed to the stable monoclinic phase at 100$0^{\circ}C$.

• Proceedings of the KIEE Conference
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• 1991.07a
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• pp.213-216
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• 1991

In this study, PZT powder was synthesized by coprecipitation method us ing $Pb(NO_3)2$, $ZrOCl_2{\cdot}8H_2O$ and $TiCl_4$ as starting raw materials. Homogeneous and fine-grained PZT powder was obtained by the coprecipitation method. PZT powder was characterized by DTA, SEM and XRD analysis. The XRD peaks were observed at $600(^{\circ}C)$ and over.

• Journal of Powder Materials
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• v.9 no.5
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• pp.336-340
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• 2002

The $\alpha$-zirconium phosphate particles as fine as 20 nm were fabricated through solution technique using $ZrOCl_2{\cdot}8H_2O$ and $H_3PO_4$ as precursors. Stability of $\alpha$-Zirconium phosphate could be ensured by adding excess phosphoric acid to a stoichiometric composition Instead of using reflux route that resulted in coarsening of particles due to an inevitably long aging. The excess phosphorous incorporated in the crystal could be successfully eliminated afterwards through careful washing. Moreover, heavily agglomerated particles are observed before washing, but fairly dispersed state is found out after washing treatment. Thus, it is found that dispersed state as well as phase stability is ensured through proper washing treatment.

• Proceedings of the KIEE Conference
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• 1990.07a
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• pp.265-268
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• 1990

In this study, PZT powder prepared by the wet direct process was synthesized. As starting materials, $TiCl_4$. $ZrOCl_2{\cdot}8H_2O$ and PbO were used. Uniformly shape and fine-grained PZT powder was obtained by the wet-direct process and PZT powder was characterized by XRD, DTA analysis. The X-ray diffraotion peaks from the PZT powder were observed at 700($^{\circ}C$) or over.

• Applied Chemistry for Engineering
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• v.32 no.6
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• pp.621-626
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• 2021

A sequential design of experiments was used to optimize MOF-801 synthesis process. For the initial screening, a general 2^k factorial design was selected followed by the central composition design, one of the response surface methods. A 2³ factorial design based on the molar ratio of fumaric acid, dimethylformamide (DMF), and formic acid was performed to select the more suitable response variable for the design of experimental method among the crystallinity and BET specific surface area of MOF-801. After performing 8 synthesis experiments designed by MINITAB 19 software, the characteristic analysis was performed using XRD analysis and nitrogen adsorption method. The crystallinity with R² = 0.999 was found to be more suitable for the experimental method than that of BET specific surface area. Based on analysis of variance (ANOVA), it was confirmed that the molar ratio of fumaric acid and formic acid was a major factor in determining the crystallinity of MOF-801. Through the response optimization and contour plot of two factors, the optimal molar ratio of ZrOCl₂·8H₂O : fumaric acid : DMF : formic acid was 1 : 1 : 39 : 35. In order to optimize the synthesis process, the central composition design on synthesis time and temperature was performed under the identical molar ratio of precursors. The results derived through the designed 9 synthesis experiments were calculated using the quadratic model equation. Thus, the maximum crystallinity of MOF-801 predicted under the synthesis time and temperature of 7.8 h and 123 ℃, respectively.

• Korean Journal of Materials Research
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• v.14 no.4
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• pp.293-299
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• 2004

Transition metal ions doped $TiO_2$ nanostructured powders were prepared with simply heating aqueous $TiOCl_2$ solutions, contained various metal ions (Ni, Al, Fe, Zr, and Nb) of 1.47 mol% added as metal-chlorides, at $100^{\circ}C$ for 4 hrs by homogeneous precipitation process under suppressing conditions of water vaporization. The characterizations for prepared $TiO_2$ powders were carried out to observe doping of metal ions, their concentrations and microstructures using XRD, UV-VIS (DRS), XPS, SEM, TEM and ICP. Also, photo-oxidative abilities were evaluated by decomposition of 4-chlorophenol (4CP) under ultraviolet light irradiations. No secondary oxide phases were formed in all the $VTiO_2$ powders, showing doping with various transition metal ions. When adding ions ($Ni^{2+}$ or$ Al^{3+ }$ and $Zr^{4+}$ ) having valance states or ionic radii greatly different from those of $Ti^{4+}$ , the $TiO_2$ powders of mixed anatase and rutile phases were formed, whereas in the case of additions of $^Fe{3+ }$ and $Nb^{ 5+}$ as well as no addition of metal ion the powders with pure rutile phase alone were formed. Among the prepared $TiO_2$ powders, Ni$^{2+}$ doped $TiO_2$ powders, containing a small amount of anatase phase, showed excellent photo-oxidative ability in 4CP decomposition because of relative decreases in electron-hole recombination and poisoning of $TiO_2$ surface during the photoreaction.n.

• Journal of the Korean Ceramic Society
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• v.39 no.3
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• pp.308-314
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• 2002

The nanocrystalline zirconia powder was synthesized from the zirconium hydroxide precipitate by hydrothermal process with the reaction temperature range 100∼250$^{\circ}$C, reaction time 1∼48 hours and additive concentration 1, 5 N NaOH solutions. The lower hydrothermal treatment temperature, the inner spherical tetragonal zirconia was synthesized. The fraction of monoclinic phase zirconia with rod shape increased with increasing the hydrothermal treatment temperature. As the concentration of the NaOH solution increases, the synthesized particle in breadth and length increased; breadth and length ratio decreased. In the case of the low concentration of NaOH solution, however, the particle length became relatively larger than its breadth resulting in the rod-shaped particles with bigger aspect ratio.

• Korean Journal of Materials Research
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• v.17 no.1
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• pp.18-24
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• 2007

Mullite-PSZ composite was prepared by sol-gel method using $Al(sec-OC_4H_9)_3,\;Si(OC_2H_5)_4,\;ZrOCl_2\;8H_2O\;and\;Y_2O_3$. The sinterability ana mechanical properties of powder compacts sintered at $1,650^{\circ}C$ for 4 hrs were investigated for various PSZ contents. In result Al-Si spinel formed at $980^{\circ}C$ from amorphous dried gel, and zirconia as well as mullite crystal formed above $1,200^{\circ}C$. The sintered body was densified to $97{\sim}98%$ except the specimen containing 25vol% PSZ which showed the relative density of about 95% obtained by sintering at $1,650^{\circ}C$ for 4 h. The flexural strength of the sintered body was a maximum value of 290 MPa in 20 vol% PSZ, which was also considerably larger than the value of 200 MPa without PSZ. The value of the fracture toughness increased linearly with increase of PSZ content and showed a maximum value of $4.3MPam^{1/2}$ in 25 vol% PSZ, Namely this value was remarkably larger than the $value(2.6MPam^{1/2})$ of pure mullite without PSZ.

• Journal of the Korean Ceramic Society
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• v.53 no.5
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• pp.529-534
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• 2016

Nanocrystalline powder of zirconia stabilized with 8 mol% yttria (YSZ) has been synthesized through oxalate process using $ZrOCl_2{\cdot}8H_2O$ and $Y(NO_3)_3{\cdot}6H_2O$ as starting materials. Understanding of the characteristic changes of YSZ powder as a function of processing conditions is crucial in developing dense and porous microstructures required for fuel cell applications. In this research, microstructure change, surface area, particle shape and particle size were measured as a function of different processing conditions such as calcination temperature, stirring speed and concentration of starting materials. The resultant crystallite sizes were calculated by XRD-LB (X-Ray Diffraction Line-Broadening) method, BET method, and morphology of the crystal was observed in TEM and FE-SEM. The TEM examination showed that the powder synthesized with 0.7 M of YSZ concentration had a spherical morphology with sizes ranging from 20 to 40 nm. However, the powder was gradually aggregated above 1.0 M of YSZ concentration with the aggregation being intensified as the YSZ concentration was increased.