• Korean Chemical Engineering Research
• /
• v.57 no.1
• /
• pp.133-141
• /
• 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.

• Proceedings of the Materials Research Society of Korea Conference
• /
• 1994.11a
• /
• pp.138-139
• /
• 1994

• Proceedings of the Korean Ceranic Society Conference
• /
• 2003.10a
• /
• pp.48.2-48
• /
• 2003

• Journal of Powder Materials
• /
• v.8 no.2
• /
• pp.98-103
• /
• 2001

Metallic tin powder with diameter less than 50 nm was synthesized by inert gas condensation method and subsequently oxidized to tin oxide ($SnO_2$) along the two heat-treatment routes. The $SnO_2$ powder of single phase with a tetragonal structure was obtained by the heat-treatment route with intermediate annealing step-wise oxidation, whereas the $SnO_2$ powder with mixture of orthorhombic and tetragonal phases was obtained by the heat-treatment route without intermediate annealing (direct oxidation). $SnO_2$ gas sensors fabricated from the nano-phase $SnO_2$ powders were investigated by structural observations as well as measurement of electrical resistance. The $SnO_2$ gas sensors fabricated from the mixed-phase powder exhibited much lower sensitivity against $H_2$ gas than those fabricated from the powder of tetragonal phase. Reduced sensitivity of gas sensors with the new orthorhombic phase was attributed to detrimental effects of phase boundaries between orthorhombic and tetragonal phases and many twin boundaries on the charge mobility.

• Journal of the Korean Ceramic Society
• /
• v.40 no.6
• /
• pp.513-518
• /
• 2003

La/sub 2/3-x/Li/sub 3x/□/sub 1/3-2x/TiO₃ compounds with x=0.13 and 0.12 were prepared by slow cooling (x=0.13) and rapid quenching (x=0.12) into the liquid nitrogen after sintering at 1350℃ for 6 h. Their crystal structure has been determined by Rietveld refinement of both the powder neutron and X-ray diffraction data. From neutron diffraction data, we found that the main phase was not tetragonal (P4/mmm), but trigonal (R3cH). The refinement of neutron diffraction for the slow cooled samples were in a good agreement with a new model; a mixture of trigonal (R3cH, 45.7 wt％), tetragonal (p4/mmm, 37.0 wt％), and Li/sub 0.57/Ti/sub 0.86/O₂(pbnm, 17.2 wt%), but the quenched sample was found not to contain tetragonal (p4/mmm). X-ray diffraction data couldn't be well fitted because of the Poor scattering factor of lithium ions and the similar reflection patterns among trigonal (R3cH), tetragonal (p4/mmm), and cubic (Pm3m). We also knew that one transport bottlenecks is destroyed by one La vacancy in the case of trigonal (R3cH).

• Journal of the Korean Ceramic Society
• /
• v.27 no.2
• /
• pp.233-243
• /
• 1990

For theinvestigation of MgO addition effect on 12Ce-TZP ceramics, MgO-CeO2-ZrO2 ceramics was fabricated using commercial powders under sintering condition of 130$0^{\circ}C$-1$600^{\circ}C$ for 2hr. Fully tetragonal phase could be obtained by proper heat treatment and MgO addition amount. Minor cubic phase was appeared in relatively high MgO content composition at each sintering temperature. As alloying amount of MgO increased, tetragonal stability increased and grain size decreased. Grain size dependence on MgO content was verified by SEM observation of fractured surface. Surface bloating was observed from the 2 m/o to 6m/o in the temperature range of 150$0^{\circ}C$ to 1$600^{\circ}C$. In spite of very porous microstructure owing to surface bloating, 100% TZP could be maintained in 2.0m/o MgO composition by heat treatment of 150$0^{\circ}C$. This result indicated that MgO was more powerful stabilizer than CeO2. Mechanical proprties of MgO-CeO2-ZrO2 ceramics were consistent with the stability observation of tetragonal phase very well.

• Journal of the Korean Ceramic Society
• /
• v.45 no.3
• /
• pp.139-141
• /
• 2008

The piezoelectric properties of tetragonal 0.88Pb$(Zn_{1/3}Nb_{2/3)O_3-0.12PbTiO_3$ single crystals are characterized along the <111> direction, which composed the engineering domain configuration in the tetragonal phase. The <111>-oriented crystal possessed smaller $d_{33}$ values compared to the crystal along the <001> spontaneous polarization direction. Based on phenomenological theory, it is shown that the engineering domain configuration does not enhance the piezoelectric constant in tetragonal 0.88Pb$(Zn_{1/3}Nb_{2/3)O_3-0.12PbTiO_3$ single crystals. In addition, the electrostrictive coefficients of $Q_{12}=-0.03706m^4/C^2,\;Q_{11}=0.10765m^4/C^2,\;and\;Q_{44}=0.02020m^4/C^2$ of tetragonal 0.88PZN-0.12PT single crystals were calculated.

• Korean Journal of Materials Research
• /
• v.19 no.8
• /
• pp.412-416
• /
• 2009

In this study, 3 mol% yttria-tetragonal zirconia polycrystal (3Y-TZP) nanoparticles were synthesized by the glycothermal method under various reaction temperatures and times. The co-precipitated precursor of 3Y-TZP was prepared by adding $NH_4OH$ to starting solutions, and then the mixtures were placed in an autoclave reactor. Tetragonal yttria-doped zirconia nanoparticles were afforded through a glycothermal reaction at a temperature as low as $220^{\circ}C$, using co-precipitated gels of $ZrCl_4$ and $YCl_3{\cdot}6H_2O$ as precursors and 1,4-butanediol as the solvent. The synthesized 3Y-TZP particles were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and Raman spectroscopy. The 3Y-TZP particles have a stable tetragonal phase only at glycothermal temperatures above $200^{\circ}C$. To investigate phase transition, the 3Y-TZP particles were heat treated from 400 to $1400^{\circ}C$ for 2 h. Raman analysis indicated that, after heat treatment, the tetragonal phase of the 3Y-TZP particles remained stable. The results of this study, therefore, suggest that 3Y-TZP powders can be prepared by the glycothermal method.

• The Korean Journal of Ceramics
• /
• v.4 no.4
• /
• pp.297-303
• /
• 1998

The effect of aliovalent dopants, $ Nb_2O_5$ and MnO, on the phase stability of 12 mol% ceria partially-stabilized zirconia (Ce-TZP) polycrystals was studied. Both dopants (MnO and $ Nb_2O_5$) significantly increased the stability of the tetragonal zirconia phase (Mb temperature lower than liquid nitrogen temperature). The enhancement of the stability of the tetragonal phase in Ce-TZP doped with 1 mol% of Mno(Ce-TZP/MnO) andCe-TZP doped with 1 mol% of $ Nb_2O_5$(Ce-TZP/$ Nb_2O_5$) were explained by the significant reduction of the driving force, -${\Delta}$Gchem, for the tetragonal-to-mono-clinic phase transformation caused by the addition of MnO and $ Nb_2O_5$. The enhanced stability of the tetragonal phase in the Ce-TZP and Al2O3 composite (Ce-TZP/$Al_2O_3$) is believed to be caused by smaller grain size, moderate reduction in the chemical driving force and increase in the strain energy barrier to the transformation. Mechanical properties of the Ce-TZP and the Ce-TZP/$Al_2O_3$ with (i) the same grain size and (ii) the same Mb temperature were examined by measuring stress-strain behavior in 3 point bending. The Ce-TZP/$Al_2O_3$ composite doped with 1.3w% MnO (Ce-TZP/$Al_2O_3$/MnO), which had the same grain size as the Ce-TZP and De-TZP/$Al_2O_3$ showed more transformation plasticity than either the Ce-TZP or the Ce-TZP/$Al_2O_3$ composite. The Ce-TZP wihch had the same Mb temperature as that of the Ce-TZP/$Al_2O_3$/MnO did not show any transformation plasticity.

• Korean Journal of Materials Research
• /
• v.2 no.5
• /
• pp.320-329
• /
• 1992

In 2Y-TZP powders calcined at temperature range of 80$0^{\circ}C$0 to 150$0^{\circ}C$, the effect of stabilization and the transformability of tetragonal phase on the tetragonal to monoclinic transformation have been investigated. The transformability of tetragonal phase in calcined powders shows maximum at the calcination temperature of 130$0^{\circ}C$. This result is explained by a combined effect of the increase of particle size and of constrained force among the particles with increasing the calcination temperature. The amount of transformed monoclinic phase with calcination temperature after quenching in liquid nitrogen, stress induction and isothermal aging at 25$0^{\circ}C$is also explained by the transformability of tetragonal phase determined by the sum of particle size effect and constraint effect.