• 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.

• Journal of Ocean Engineering and Technology
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• v.24 no.6
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• pp.81-85
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• 2010

The effects of co-doping with complex dopants of softeners, $La^{+3}$ and/or $Nb^{+5}$, and a hardener, $Fe^{+3}$, on the microstructural and piezoelectric properties of PZT ceramics with a composition of a rhombohedral-tetragonal morphotropic phase boundary, $PbZr_{0.53}Ti_{0.47}O_3$, were investigated. Unlike single-element doping, the complex doping of both the softener and hardener ions led to various compensation effects for the piezoelectric properties of the PZT ceramics. For 0.5 wt.% $La_2O_3$ softener and/or 0.5 wt.% $Nb_2O_5$ doped compositions, there were apparent hardener doping (compensation) effects for an addition of over 1.0 wt.% $Fe_2O_3$. For the $La_2O_3$ and/or $Nb_2O_5$ doped composition, the co-dopant $Fe_2O_3$ addition led to lower kp and $\varepsilon$r, and increased $Q_m$ values. The prepared PZT ceramics modified with complex soft dopants, $La^{+3}$ and $Nb^+$, as well as a hard dopant, $Fe^{+3}$, showed that the piezoelectric properties were stable with the compositional variations, which made it possible to establish piezoelectric performances with higher reliability and reproducibility. The most improved piezoelectric properties of enhanced $Q_m$ with $\varepsilon_r$ remaining higher $k_p$, were obtained in the PZT composition complexly doped with $La^{+3}$ and $Fe^{+3}$. From the results obtained in this study, the properties of compositionally modified PZT ceramics can also be tailored over a wider range by changing the dopant compositions to meet the specific requirements for underwater or other applications.

• Proceedings of the KIEE Conference
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• 2001.07c
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• pp.1439-1441
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• 2001

In this paper, the piezoelectric and dielectric properties as a function of x and r in $yPbZr_xTi_{1-x}O_3-(1-y)Pb(Mn_{1/3}Nb_{2/3})O_3$ piezoelectric ceramics is investigated. As a results, when y is 0.95 and x is 0.505, electromechanical coupling factor($k_p$), permittivity(${{\varepsilon}_{33}}^T/{\varepsilon}_0$), piezoelectric strain constant($d_{33}$) and mechanical quality factor($Q_m$) are 58[%], 1520, 272 [pC/N] and 1550, respectively. From XRD analysis, when x is 0.505, it is MPB which present rhombohedral and tetragonal phase in same quantity. Also, From SEM observation. when sintering temperature is 1150[$^{\circ}C$], grain size is about 2 [${\mu}m$]. As y decreases, piezoelectric and dielectric properties and curie temperature decreases, but mechanical quality factor and sintering temperature increases.

• Journal of the Korean Ceramic Society
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• v.38 no.9
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• pp.834-838
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• 2001

Attempts were made to improve mechanical properties of zirconia-based electrolyte by preparing yttria-stabilized cubic zirconia/alumina composite. It was performed by precipitating Yag precursor in aqueous m-zirconia slurry. The powder was separated and then followed by heat treatment with expecting yttria to react with m-$ZrO_2$ to give yttria stabilized zirconia and alumina to be dispersed homogeneously. When 17.8wt% Yag(6.3mol% $Y_2O_3$) was used, fracture toughness and strength were substantially improved from 1.44MPa${\cdot}m^{1/2}$ and 270Mpa for YZ8Y to 3.62MPa${\cdot}m^{1/2}$ and 447MPa respectively, but electrical conductivity at $^{\circ}$C in air was decreased from 0.126 to 0.057${\Omega}^{-1}cm^{-1}$. It seemed due to the presence of small amount of tetragonal zirconia. But when 21.58wt% Yag(8.0mol% $Y_2O_3$) was added, fracture toughness of 2.93MPa${\cdot}m^{1/2}$ and flexural strength of 388MPa were obtained with electrical conductivity of ${\Omega}^{-1}cm^{-1}$.

• Journal of the Korean Ceramic Society
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• v.32 no.1
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• pp.95-105
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• 1995

Ceria(CeO2) stabilized zirconia(CeSZ) sol was synthesized with zirconium n-butoxide Zr(OC4H9)4 and cerium nitrate hexahydrate Ce(NO3)3.6H2O as precursors and ethylacetoacetate(EAcAc) as a chelating agent under atmosphere. CeSZ films were deposited on AISI 304 stainless steel using the prepared polymeric sol by dipcoating and the coating characteristics were investigated by XRD, ellipsometry, scratch test and SEM. The CeSZ film began to crystallize from amorphous to tetragonal phase at 40$0^{\circ}C$ and it was not converted into monoclinic phase up to 100$0^{\circ}C$ by the addition of 16mol% CeO2 as a stabilizer which could suppress phase transformation of zirconia. The CeSZ films were prepared by varying the EAcAc contents and the cncentration of CeSZ sol and measured the thickness and refractive index. From these results, it was found that the EAcAc contents and concentration of CeSZ coating sol evidently affect the densification of CeSZ film. The CeSZ film coated with 0.4M CeSZ sol and heat-treated at $600^{\circ}C$ for 10min had thickness of 50nm and 17% porosity. The CeSZ film on 304 stainless steel effectively acted as a protective layer against oxidation up to 80$0^{\circ}C$ and had superior corrosion resistance in 25% H2SO4 solution for 4.5 hrs.

• Korean Journal of Materials Research
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• v.9 no.8
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• pp.792-797
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• 1999

The 8mol.%Y$_2$$O_3$-$ZrO_2$mainly employed as an electrolyte of solid oxide fuel cells(SOFCs) shows excellent electrical properties but has a weakness in the mechanical properties. Since the electrolyte of SOFCs requires both good electrical and mechanical properties, this study was conducted to meet both requirements. The electrolyte thin films were produced on the LSM(cathode material) substrate of a cell and Si wafer. Four electrolyte film types of single layer and the multiple layer, consisting of 3-YSZ(3mol.%$Y_2$$O_3$) with excellent mechanical properties and 8-YSZ with the excellent electric conduction, were produced by electron beam coating technology. Ther crystal structure and the mechanical properties were also analysed. As the results of the study, the 3-YSZ thin film turned out to be in the tetragonal, partially monoclinic phase, while the 8-YSZ thin film showed the cubic phase. The residual stress in the multiple layer was lower than that of the single layer. The microhardness of the multiple layer was similar to that of the existing 8-YSZ single layer both before and after annealing treatment.

• Korean Journal of Materials Research
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• v.34 no.2
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• pp.116-124
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• 2024

In this study, we investigated the microstructure and piezoelectric properties of 0.96(K_0.456Na_0.536)Nb_0.95Sb_0.05-0.04Bi_0.5(Na_0.82K_0.18)_0.5ZrO₃ (KNNS-BNKZ) ceramics based on one-step and two-step sintering processes. One-step sintering led to significant abnormal grain (AG) growth at temperatures above 1,085 ℃. With increasing sintering temperature, piezoelectric and dielectric properties were enhanced, resulting in a high d₃₃ = 506 pC/N for one-step specimen sintered at 1,100 ℃ (one-step 1,100 ℃ specimen). However, for one-step 1,115 ℃ specimen, a slight decrease in d₃₃ was observed, emphasizing the importance of a high tetragonal (T) phase fraction for superior piezoelectric properties. Achieving a relative density above 84 % for samples sintered by the one-step sintering process was challenging. Conversely, two-step sintering significantly improved the relative density of KNNS-BNKZ ceramics up to 96 %, attributed to the control of AG nucleation in the first step and grain growth rate control in the second step. The quantity of AG nucleation was affected by the duration of the first step, determining the final microstructure. Despite having a lower T phase fraction than that of the one-step 1,100 ℃ specimen, the two-step specimen exhibited higher piezoelectric coefficients (d₃₃ = 574 pC/N and k_p = 0.5) than those of the one-step 1,100 ℃ specimen due to its higher relative density. Performance evaluation of magnetoelectric composite devices composed of one-step and two-step specimens showed that despite having a higher g₃₃, the magnetoelectric composite with the one-step 1,100 ℃ specimen exhibited the lowest magnetoelectric voltage coefficient, due to its lowest k_p. This study highlights the essential role of phase fraction and relative density in enhancing the performance of piezoelectric materials and devices, showcasing the effectiveness of the two-step sintering process for controlling the microstructure of ceramic materials containing volatile elements.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.30 no.9
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• pp.541-545
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• 2017

$Pb(Zr_{0.52}Ti_{0.48})O_3$ (PZT) films with a thickness of $5{\sim}10{\mu}m$ at the morphotropic phase boundary were fabricated by aerosol-deposition (AD), and their phase evolution and electrical properties were investigated. The microstructure of the AD PZT films revealed nanosized grains with a low crystallinity and a dense structure at room temperature. The AD PZT films showed a mixture of tetragonal and rhombohedral phases. The post-annealing temperature was varied to study the phase transition behavior. The crystallinity of the AD PZT films was enhanced by annealing at 450, 550, and $650^{\circ}C$ for 2 h. At $650^{\circ}C$, the tetragonal and rhombohedral phases reacted to form a bridge phase between the two phases. The polarization-electric field hysteresis loops of the AD PZT film annealed at $650^{\circ}C$ exhibited a smaller cohesive field and a lower slim hysteresis than the films annealed at 450 and $550^{\circ}C$.

• Journal of the Korean Ceramic Society
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• v.33 no.6
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• pp.637-644
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• 1996

Phase stability and isothermal phase transformation during gaging at 25$0^{\circ}C$ were investigated in yttria stabilized zirconia powders prepared from hydrolysis of zirconium isopropoxide. The stability of tetragonal phase at room temperature in zirconia powder was decreased with calcination temperature but increased with the addition of yttria content. During aging at 25$0^{\circ}C$ in humid atmosphere isothermal phase transformation occurred in tetragonal zirconia powder stabilized by constraint effect not by alloying effect and grain size effect. Many twins and microcrackings were found in transformed monomlinic zirconia particles.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.29 no.2
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• pp.90-94
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• 2016

In this work, [$Pb(Mg_{1/2}W_{1/2})_{0.03}(Ni_{1/3}Nb_{2/3})_x(Zr_{0.5}Ti_{0.5})_{0.97-x}O_3-BiFeO_3$] (x=0.02 to 0.12) composition ceramics were fabricated by the conventional soild state reaction method and their microstructure and piezoelectric properties were investigated according to PNN substitution. The addition of small amount of $BiFeO_3$, $Li_2CO_3$, and $CaCO_3$ were used in order to decrease the sintering temperature of the ceramics. The XRD (x-ray diffraction patterns) of all ceramics exhibited a perovskite structure. The sinterability of PMW-PNN-PZT-BF ceramics was remarkably improved using liquid phase sintering of $CaCO_3$, $Li_2CO_3$. However, it was identified from of the X-ray diffraction patterns that the secondary phase formed in grain boundaries decreased the piezoelectric properties. According to the substitution of PNN, the crystal structure of ceramics is transformed gradually from a tetragonal to rhombohedral phase. The x=0.10 mol PNN-substituted PMW-PNN-PZT-BF ceramics sintered at $920^{\circ}C$ showed the optimum values of piezoelectric constant($d_{33}$), piezoelectric figure of merit($d_{33{\cdot}}g_{33}$), planar piezoelectric coupling coefficient($k_p$) and density : $d_{33}=566$ [pC/N], $g_{33}=29.28[10^{-3}mV/N]$, $d_{33{\cdot}}g_{33}=16.57[pm^2/N]$, $k_p=0.61$, density=7.82 [$g/cm^3$], suitable for duplex ultrasonic sensor application.