• Electrical & Electronic Materials
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• v.1 no.2
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• pp.162-167
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• 1988

본 논문에서는 Pb(Sn$_{1}$7/Mn$_{2}$7/Nb$_{4}$7/)O$_{3}$- Pb(Zr, Ti)O$_{3}$계에 La$_{2}$O$_{3}$를 첨가하여 그양에 따른 압전일 전기력 성질의 변화를 고찰하였다. La$_{2}$O$_{3}$ 첨가량의 증가에 따라 유전상수, 압전 d상수, 유전손실, 비저항 등은 증가하였으나 경시 변화량은 오히려 감소하였다.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2001.11a
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• pp.442-445
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• 2001

In this study, microstructural and dielectric properties of P $b_{0.83}$(L $a_{0.2}$C $e_{0.8}$)$_{0.08}$Ti $O_3$PCT ceramics as a function of Mn $O_2$ addition were investigated for 30MHz ceramic resonator application. Grain size was gradually increased according to the increase of Mn $O_2$ addition amount and showed the highest value of 1.502${\mu}{\textrm}{m}$ at the 0.9wt% Mn $O_2$. Moreover, density showed the highest value of 7.582 g/$\textrm{cm}^2$ at the 0.7wt% Mn $O_2$. All the composition ceramics, curie temperature was nearly constant around 33$0^{\circ}C$.EX>.>.>.

• Journal of the Korean Ceramic Society
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• v.25 no.4
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• pp.321-328
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• 1988

The sintering phenomena, electrical resistivity, dielectric and piezoelectric properties of lead titanate ceramics modified by the partial substitution of La for Pb and Mn for Ti, (Pb1-1.5xLax)(Ti1-yMny)O3 ceramics, have been investigated. In (Pb1-1.5xLax)(Ti1-yMny)O3 system, with increasing lanthanum content, the realtive bulk density increased, but the Curie point and tetragonality (c/a) decreased. The tetragonal-to-cubic phase transition boundary existed in the range of 0.20

• Proceedings of the Korea Association of Crystal Growth Conference
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• 1996.06b
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• pp.219-222
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• 1996

수열법은 밀폐용기중에서 10$0^{\circ}C$이상의 가열, 가압된 수용액이 반응에 관여하는 것으로써, 수정, CaCO3, AlPO4, GaPO4 등과 같은 단결정의 육성 뿐만 아니라 균일분산계로부터 균일한 결정성의 미립자 합성에도 폭넓게 이용되고 있다. 세라믹분말의 합성에 있어서, 이 방법은 특히 형상, 입자크기의 제어가 용이할 뿐만 아니라 고상법, 졸-겔법, 공침법에서와 같은 열처리, 분쇄과정이 필요없기 때문에 고순도의 초미립자를 얻을 수 있는 장점이 있다. 근년 미국, 일본에서는 수열법을 이용한 유전, 압전체 등 세라믹분말의 일부가 공업적인 규모로 대량 생산되고 있다. 그러나 이에 대한 국내 기술은 아직 초기단계에 이르고 있는 실정이다. 따라서 본 연구실에서는 수열법에 의한 단결정 육성 (예; 자수정, CaCO3, AlPO4, GaPO4, KTP, Emerald 등), 박막제조 (예; GaP, PbTiO3, BaTiO3 등), 정제 (고령토, 장석, 도석 등), 원석처리 (진주, 인공 emerald, 비취 등) 그리고 각종 세라믹분말의 합성 등과 같은 다양한 기반기술의 축적과 동시에 공업화에 대응한 수열장치를 위하여 반응용기의 대형화, 엄밀한 밀폐방식, 실용적인 수열조건 등을 개발해 오고 있다. 본 발표에서는 현재까지의 연구개발 내용 중에서 결정성 미립자에 관련한 세라믹분말의 합성에 대한 일부의 결과들을 보고한다. 일반적으로 수열장치는 전기로, 반응용기, 온도 및 압력제어계 등을 기본으로 하고 있으며 시판용의 대부분이 교반기가 부착된 수직형 (vertical type)이다. 이와 같은 방식에 있어서는 엄밀한 밀폐가 곤란, 반응온도의 한계성 (25$0^{\circ}C$ 이하), 증진율의 한계성 (소량생산) 등과 같은 점이 있기 때문에 본 연구실에서는 개폐식 전기로내에 엄밀한 밀폐가 가능한 수평식(horizontal type)의 반응용기를 채택한 뒤 이를 회전 또는 시이소(seesaw)식으로 움직일 수 있도록 하여 연속공정화, 온도구배의 자율조절 그리고 보다 저온에서도 인위적인 이온의 확산을 효율적으로 유도할 수 있도록 하였다. 이와 같은 방식은 기존의 방식과 비교하여 반응용기 내에 응집현상과 미반응물이 존재하지 않으며 또한 단분산으로 결정성 미립자를 대량적으로 얻을 수 있는 장점이 있었다. 다음은 이상과 같이 본 연구실에서 자체 개발한 수열장치를 이용하여 PbTiO3, (Pb,La)TiO3Mn, BaTiO3, ZnSiO4:Mn, CaWO4 등과 같은 세라믹분말에 대한 합성 실험의 결과이다. 압전성, 초전성이 우수한 PbTiO3 및 (Pb,La)TiO3:Mn 분말의 수열합성은 PbO, TiO2, La2O3 등의 분말을 출발원료로 하여 합성도도 25$0^{\circ}C$부근의 알카리성 용액중에서 결정성 PbTiO3 및 (Pb,La)TiO3:Mn 미립자를 단상으로 얻었으며 입자의 형상 및 크기는 합성온도와 수열용매의 종류에 의존하였다. 유전체로서 폭넓게 응용되고 있는 BaTiO3 분말은 Ba(OH)2.8H2O, TiO2와 같은 최적의 출발원료를 선택함으로써 15$0^{\circ}C$ 부근의 저온영역에서도 용이하게 합성할 수 있었다. 특히 본 연구에서는 수용성인 Ba(OH)2.8H2O를 사용함으로써 host-guest적인 반응을 유도시키는데 있어 물의 가장 실용적이고 효과적인 수열용매임도 알았다. ZnSiO4:Mn, CaWO4, MgWO4와 같은 형광체 분말은 공업적으로 고상반응 또는 습식법에 의해 얻어지고 있으나 이들 방법에 있어서는 분쇄공정으로 인한 형광특성의 저하와 같은 문제점이 있다. 따라서 본 연구에서는 수열법을 이용하여 이들 화합물의 합성을 시도하였으며 그 결과 합성온도 30$0^{\circ}C$ 부근의 알칼리성 용액중에서 수열적으로 얻어짐을 알았다. 여기서의 합성분말을 이용하여 실제 조명램프로 제조한 결과 녹색, 청색 발광용 형광체로서 우수한 형광특성을 나타내었다. 천연에서 소량 산출되고 있는 고가의 (Li,Al)MnO2(OH)2:Co 분말은 도자기의 전사지용 청색안료로써 이용되고 있다. 본 연구실에서는 LiOH.H2O, Al(OH)3, MnO2 등의 분말을 출발원료로 하고 24$0^{\circ}C$ 온도 부근 그리고 물을 수열용매로 하여 천연산에 필적하는 (Li,Al)MnO2(OH)2:Co 분말을 인공적으로 합성하였다.

• Journal of the Korean Ceramic Society
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• v.20 no.4
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• pp.315-323
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• 1983

Effect of NiO and $MnO_2$ addtivies on the dielectric piezoelectrics and polarization-reversal properties of $(Pb_{0.936} La_{0.064})$$(Zr_{0.60}Ti_{0.40})O_3$ ceramics have been investigated. The specimens were prepared by the mixed oxide techni-que and atmosphere sintering method. The room temperature X-ray diffraction studies show that perfect perovskite solution with tetragonal structure was obtained from PLZT and its additives. The dielectric constant and dissipation factor decreased with the addition of both NiO and $MnO_2$ The Curie of Curie temperature was not observed but they displayed broadened maxima. The planar coupling factor was improved by addition of NiO and also increased with increasing sintering time carried out at 105$0^{\circ}C$ Addition of $MnO_2$ yielded a markedly high mechanical quality factor. The space-charge field decreased with the addition of NiO but increased with the addition of $MnO_2$ The planar coupling factor and space-charge field showed same dependence on the additivies. The tetragonality Curie temperature and planar coupling factor of $(Pb_{0.936} La_{0.064})$$(Zr_{0.60}Ti_{0.40})O_3$ were higher than those of $(Pb_{0.936} La_{0.064})$$(Zr_{0.568}NU_{0.032}Ti_{0.40})_{0.984}O_3$ but the grain size lattic parameter dielectric constant dissipation factor mechanical quality factor and space-charge field of the former were lower than those of the latter.

• Journal of the Korean Ceramic Society
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• v.33 no.6
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• pp.672-678
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• 1996

The relationship between domain switching and acoustic emission (AE) during poling was investigated using the tetragonal ferroelectric ceramics with composition of (Pb,La)TiO3+0.01MnO2 The amount of AE generation during poling increased with increasing dc electric field and raising temperature. It was confirmed that the change of the amount of AE generation with poling condition resulted from the difference of the amount of 90$^{\circ}$ domain switching and total amount of AE generation for 10 minutes was approximately proportional to the amount of 90$^{\circ}$domain switching. The A generations of two specimens which have different tetragonality rations(c/s rations) 15 at% and 24at% La-doped were also investigated. The sample with c/a ratio of 1.012 where 90$^{\circ}$ domains are dominate had larger amount of AE generation and 90$^{\circ}$ domain switching compared with the sample with c/a ratio of 1.004 where 180$^{\circ}$ domains are dominant.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.7 no.3
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• pp.418-427
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• 1997

The effect of $La_2O_3$ as a dopant on the microstructure structure, crystal structure and electrical properties was studied. $0.05Pb(Sn_{0.5}Sb_{0.5})O_3＋0.11PbTiO_3＋0.84PbZroO_3＋0.4Wt%MnO_2$ (=0.05PSS ＋0.11PT＋0.84PZ+0.4wt%$MnO_2$) systems doped with 0, 0.1, 0.3, 0.5, 0.7, 1, 3, 5 mole% $La_2O_3$ were fabricated and investigated sintering density, crystal structure and micro-structure. The sintered 0.05PSS＋0.11PT＋0.84PZ+0.4wt%$MnO_2$ system doped with $La_2O_3$showed sintering density of the range of 7.683 g/㎤ of 0 mole% doping to 7.815 g/㎤ of 0 mole% doping. The average grain sizes in the range of 0 to 5 mole% $La_2O_3$were decreased from 9.0 $\mu\textrm{m}$ to 1.3 $\mu\textrm{m}$. X-ray diffraction investigation of sintered bodies showed that solid solutions were formed between 0.05PSS＋0.11PT＋0.84PZ+0.4wt%$MnO_2$ system and $La_2O_3$ in the range of 0 to 1 mole% but second phases were formed in case of 3, 5 mole%. Dielectric constants at 1 kHz were increased with 0 to 3 mlole% $La_2O_3$ before and after poling at the condition of 5 $KV_{DC}$/mm at $120^{\circ}C$ or $140^{\circ}C$ during 20 minutes. All Dielectric losses at 1 kHz were less than 1%, Curie temperatures were $208^{\circ}C$, $183^{\circ}C$, $152^{\circ}C$ and $127^{\circ}C$ at 0, 0.5, 1, 3 mole% $La_2O_3$ respectively. The values of $K_p$ were increased from 0 to 3 mole% $La_2O_3$ after poling at condition of 5 $KV_{DC}$mm at the condition of $120^{\circ}C$ or $140^{\circ}C$. The case of 0.7 mole% $La_2O_3$doped 0.05PSS＋0.11PT＋0.84PZ+0.4wt%$MnO_2$ system showed $K_p$ of 14.5% by poling at $140^{\circ}C$ during 20 minutes.

• Korean Journal of Optics and Photonics
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• v.7 no.2
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• pp.162-166
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• 1996

We report a fiber optic interferometric electric field sensor that utilizes electrostrictive ceramics-1%, 2%, 3%, La-doped 0.9MN/0.1PT, respectively-as the transducing elements. It is also experimentally observed that 3% La-doped PMN/PT among the three elements has the largest electrostrictive coefficient $M=3.87{\times}10^ {-16}(m/V)^2$ at 3.38 kHz and displays small hysteresis. The optical fiber sensor with the 3% La-doped PMN/PT exhibits minimum detectable field of 2.08(V/m)/ $\sqrt{Hz}$ and has a good linearity over the dynamic range 40 dB.

• Transactions on Electrical and Electronic Materials
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• v.3 no.3
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• pp.25-28
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• 2002

In this study, microstructural, dielectric and electrical properties of (Pb$\sub$0.83/) (La$\sub$0.2/Ce$\sub$0.8/)$\sub$0.08/TiO$_3$(PCT) ceramics as a function of MnO$_2$ addition and electrode size variation were investigated for 30 MHz high frequency ceramic resonator application. Grain size was gradually increased according to the increase of MnO$_2$ addition amount. Moreover, the density showed a constant value with increasing MnO$_2$ addition amount. Dielectric constant was decreased with increasing MnO$_2$ addition amount. Curie temperature of all the composition ceramics was nearly constant around 330$^{\circ}C$. The maximum D.R.of 50.5 dB and maximum Q$\sub$mt3/ of 1842 in the 3$\^$rd/ overtone vibration mode were appeared at the composition of 0.3wt% MnO$_2$, respectively.

• Analytical Science and Technology
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• v.10 no.6
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• pp.439-444
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• 1997

Twelve kinds (1set) standard materials of chemical ingredients of lead zirconate titanate[$Pb(ZrTi)O_3$] have been developed in order to determine fast and accurate measurement of X-ray fluorescence spectrometry. Especially, we used diluted(ahout sixteen times) filling compound($Li_2B_4O_7/LiBO_2=4/1$) to consider removal effect of matrix, storage convenience, and homogenous characteristics. As a result from the four different laboratories, we obtained extremly good agreement about the standard curve on twelve standard materials which containing eleven elements, PbO, $ZrO_2$, $TiO_2$, SrO, $WO_3$, $La_2O_3$, $Cr_2O_3$, MgO, $Nb_2O_5$, and $MnO_2$. The correlation factor of standard curve was over 0.998. However, ZnO has relatively low correlation factor, 0.977, because the concentration was 10ppm lower than other original materials. This analysis reveals that ZnO has shown the poor linearity as well as low fluorescence intensity. In present work, XRF standard materials are useful for determining a rapid and accurate results for major and minor elements concentration among PZT.