• 한국해양공학회지
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• 제24권6호
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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.

• 대한전기학회:학술대회논문집
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• 대한전기학회 2001년도 하계학술대회 논문집 C
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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.

• 한국세라믹학회지
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• 제38권9호
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• pp.834-838
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• 2001

고체 전해질로 많이 사용되는 이트리아로 안정화된 입방정형(cubic) 지르코니아의 기계적 강도를 향상시키기 위하여, 단사형(monoclinic) 지르코니아(m-$ZrO_2$)를 원료로 지르코니아　 안정화시키는 이트리아와 지르코니아의 낮은 기계적 강도를 향상시켜 주기 위한 알루미나를 Yag($Y_3Al_5O_{13}$)졸의 형태로 첨가하여, 졸 형태로 첨가된 이트리아와 알루미나가 입방정 지르코니아 소결체의 기계적, 전기적 특성에 미치는 영향을 조사하였다. 17.8 wt% Yag(6.3mol% $Y_2O_3$)가 첨가된 경우 파괴인성은 3.62MPa${\cdot}m^{1/2}$, 파괴강도는 447MPa로 8mol%의 이트리아로 안정화된 지르코니아(TZ8Y)의 1.44MPa${\cdot}m^{1/2}$, 270MPa에 비하여 기계적 특성이 현저히 향상되었으나, 950$^{\circ}$C, 공기분위기에서의 전기전도도는 0.057${\Omega}^{-1}cm^{-1}$로 TZ8Y에 비해 반 정도로 낮아졌으며, 21.6wt% Yag(8.0mol% $Y_2O_3$)가 첨가된 경우에는 파괴인성은 2.93MPa${\cdot}m^{1/2}$, 파괴강도는 388MPa로 TZ8Y에 비하여 향상되었고, 전기전도도는 0.076${\Omega}^{-1}cm^{-1}$을 나타내었다.

• 한국세라믹학회지
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• 제32권1호
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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.

• 한국재료학회지
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• 제9권8호
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• pp.792-797
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• 1999

고체 산화물 연료전지의 전해질로 주로 사용되는 8mol.%$Y_2$$O_3$-$ZrO_2$는 전기 전도성은 우수하나 기계적 특성이 좋지 못하므로, 전기적 특성과 기계적 특성이 동시에 우수한 고체산화물 연료전지의 전해질의 개발이 요구되고 있다. 본 연구는 이러한 두 가지 요구조건을 충족시키기 위해서 수행되어졌다. 단위전지의 공기극 재료인 LSM(La(sub)0.75Sr(sub)0.25MnO$_3$) 기판과 Si wafer를 기판으로 기계적 성질이 우수한 3mol.%의 YSZ(3-YSZ)와 전기 전도성이 우수한 8mol.%의 YSZ(8-YSZ)를 각각 단층 및 다층 박막의 네 가지 형태로 전자빔 코팅에 의해 전해질 막을 제작하였다. 박막층의 분석결과, 결정조직은 증착된 3-YSZ 박막의 정방정 및 일부 단사정 구조, 8-YSZ 박막은 입방정 구조의 결정성이 나타났다. 단층막 보다 다층막이 낮은 내부 응력을 보였으며, 다층막이 기존의 8-YSZ 단층막의 열처리 전, 후와 비슷한 미세 경도 값을 보였다.

• 한국재료학회지
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• 제34권2호
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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.

• 한국전기전자재료학회논문지
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• 제30권9호
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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 $550^{\circ}C$.

• 한국세라믹학회지
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• 제33권6호
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• pp.637-644
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• 1996

$Zr(i-OC_3H_7)_4$로부터 가수분해법으로 Y-TZP 분말을 제조한 다음, 하소온도를 달리하여 정방정상의 상온 안정화와 25$0^{\circ}C$에서의 등온상전이 거동을 고찰하였다. 그 결과, 정방정상 지르코니아 입자의 상온 안정화 효과는 하소온도가 낮을 수록, 고용된 $Y_2O_3$의 양이 클 수록 증가하였다. 또한 25$0^{\circ}C$에서 aging 하면서 Y-TZP 분말의 등온상전이를 관찰한 결과, 입자크기 효과 및 고용효과에 의해 상온 안정화된 정방정상 지르코니아 입자에서는 aging 시 등온상전이가 일어나지 않고, 반면에 구속효과에 의하여 상온 안정화된 정방정상 입자에서는 등온상전이가 활발히 진행되었다. 등온상전이로 생성된 단사정상 입자의 내부에는 많은 쌍정과 미세균열들이 존재하였는데 이는 상전이시 변형에너지를 감소시키기 위한 것으로 사료되었다.

• 한국전기전자재료학회논문지
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• 제29권2호
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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.

• 공업화학
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• 제8권2호
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• pp.292-300
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• 1997

본 연구에서는 출발물질을 변화시켜 입방체의 PZT(Lead Zirconate Titanate) 분말을 수열합성법으로 제조하였으며 합성된 분말을 이용하여 소결특성을 조사하였다. 출발물질에 관계없이 입방체 형태를 갖는 PZT 결정분말이 형성되었으나 $Pb(NO_3)_2$, $Ti(OC_4H_9)_4$와 $Zr(OC_4H_9)_4$을 출발물질로 사용한 경우 다른 여러 출발물질을 사용한 경우보다 상대적으로 작은 입자가 생성되었다. 수열합성시 교반을 시키면서 합성한 경우 교반없이 반응시킨 경우에 비해 핵생성을 위한 수열 반응온도가 낮아졌으며 상대적으로 입경이 큰 입자들의 수가 늘어났다. Zr대Ti의 조성비를 변화시켜 수열합성한 반응물을 XRD 분석한 결과, 조성비가 40대60인 경우 정방정상이 주상(major phase)으로 형성되었으며 조성비가 60대40인 경우에는 주상의 결정형이 능면체정상으로 바뀌었다. 여러 조건에서 합성된 PZT 분말을 PbO 분위기에서 소결시키면서 소결온도 및 소결시간 변화에 따른 소결밀도의 변화를 분컥하였으며, $1150^{\circ}C$에서 2시간 소결시켰을 때 최적의 소결밀도, $7.6g/cm^3$을 갖는 소결체가 제조되었다.