• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.24 no.5
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• pp.392-397
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• 2011

The effect of various post-annealing temperature to sputtered Pb(Zr,Ti)$O_3$ (PZT) thin films was investigated. The crystallization process, surface morphology and the electrical characteristics strongly depends on the rapid thermal annealing (RTA). In radio frequency (RF) sputtering methods, there were many papers mostly forcing on the crystal forming and the surface variations with different elements distribution (Pb, Ti, Zr, O) on the surface of the PZT layer. In this experiment, the post-annealing treatment promoted the Pb volatilization in PZT thin film and affected the Ti diffused throughout the Pt layer into the PZT layer. Second ion mass spectroscopy (SIMS) analysis was employed to show that the Pb element in the PZT layer was decreased at the same time the Ti element mass was slight decreased than Pb with increasing RTA temperature. That result prove the content of Pb affect the PZT thin film property.

• Journal of the Microelectronics and Packaging Society
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• v.24 no.4
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• pp.85-90
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• 2017

The $TiCl_4$ as a blocking material is adsorbed in the mesoporous $TiO_2$ electron transfer layer(ETL) of the Perovskite solar cell to prevent the direct contact between the FTO electrode and the photoactive layer(AL), and facilitate the movement of the electrons between $TiO_2:TiCl_4$ ETL and Perovskite AL to improve the photoelectric conversion efficiency(PCE). The structure of the perovskite solar cell is FTO/$TiO_2:TiCl_4$/Perovskite($CH_3NH_3PbI_3$)/spiro-OMeTAD/Ag. It was investigated that the dipping time of the $TiO_2$ into $TiCl_4$ aqueous solution affects on the photoelectric characteristics of the device. By the dipping for 30 minutes, the PCE of the perovskite solar cell with the $TiO_2:TiCl_4$ ETL was the highest 10.46%, which is 27% higher than the cell with $TiO_2$ ETL. From SEM, EDS, and XRD characterization on the $TiO_2:TiCl_4$ ETL and the perovskite AL, it was measured that the decrease of the porosity of the $TiO_2$ layer, the detection of the Cl component by the $TiCl_4$ adsorption, the cube-type morphology of perovskite AL, and shift of the $PbI_2$ peak of the perovskite AL. From these results, it was confirmed that the $TiO_2:TiCl_4$ ETL and the perovskite AL were formed.

• Journal of the Korean Ceramic Society
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• v.23 no.3
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• pp.15-20
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• 1986

Formation of powders and electromechanical coupling factor of $Pb(Mn_{1/3} Sb_{2/3})_{0.08} Ti_{0.495}Zr_{0.425}O_3$ by hydro-thermal synthesis are described. The hydrothermal reactions each were accomplished at 12$0^{\circ}C$~25$0^{\circ}C$ for 5hours and sintering was accomplished at 1, .20$0^{\circ}C$ for 1hours. The PZT powders by hydrothermal synthesis were formed above 16$0^{\circ}C$ and the forms were cubic types. The ratio of grain size of sintered sample to powder was slowly decreased with the rising of hydrothermal reactino temperature but decreased rapidly above 22$0^{\circ}C$ Sintering density was decreased with the rising of hydrothermal reaction temperature above 16$0^{\circ}C$ but dielectric constant was increased. Electromechanical coupling factor $K_P$ was almost constant at 16$0^{\circ}C$~24$0^{\circ}C$ range and the value of $K_P$ was about 0.43-0.45.

• The Transactions of the Korean Institute of Electrical Engineers
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• v.44 no.11
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• pp.1488-1493
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• 1995

In this study, the structural, electrical and dielectric properties were investigated in (P $b_{0.76}$ $Ca_{0.24}$)[( $Co_{1}$2/ $W_{1}$2/)$_{0.04}$ $Ti_{0.96}$) $O_{3}$ system ceramics which were manufactured with the addition of Mn $O_{2}$. According to the increment of Mn $O_{2}$ addition, tetragonality was decreased. The specimen added with 1.5 mol% Mn $O_{2}$ and sintered at 1150.deg. C showed the highest density of 7.06[g/c $m^{3}$]. The variations of grain xize as a function of Mn $O_{2}$ addition were negligibly small. But grain was grown until 7.88[.mu.m] with increasing sintering temperature. Electromechamical coupling factor planar mode $K_{p}$ was decreased to a small value of $K_{p}$ = 0 in all the specimens added with Mn $O_{2}$ and sintered at 1150.deg. C & 1200.deg. C.& 1200.deg. C.

• The Transactions of the Korean Institute of Electrical Engineers
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• v.44 no.4
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• pp.479-482
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• 1995

In this study, to improve sintering condition, anisotropic properties ( $k_{t}$/ $k_{p}$) of electromechanical coupling coefficient and piezoelectric constant $d_{h}$ and $g_{h}$, Mn $O_{2}$ impurity was added to the (P $b_{0.76}$C $a_{0.24}$)[( $Co_{1}$2/ $W_{1}$2/)$_{0.04}$ $Ti_{0.96}$] $O_{3}$ ceramics for application to hydrophone devices. Electromechanical coupling coefficients of the specimen with 1.5 [mol%] Mn $O_{2}$ sintered at 1150.deg. C were $k_{t}$=49% and $k_{p}$ = O, which exibited the highest value in piezoelectric anisotropic properties (kt/kp). Without relations with sintering temperature, the highest value of hydrostatic piezoelectric constant $d_{h}$ & $g_{h}$ were shown at the specimen with 1.5 [mol%] Mn $O_{2}$. Accordingly, the best addition amount of Mn $O_{2}$ was 1.5 [mol%] and proper sintering temperature was 1150.deg. C. Hydrostatic piezoelectric constant values of $d_{h}$=64.52[10$^{-12}$ C/N], $g_{h}$=35.92[10$^{-3}$ Vm/N] in the above condition were effectiely extended for hydrophone applications.pplications.ons.

• Electrical & Electronic Materials
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• v.6 no.6
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• pp.573-581
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• 1993

0.10Pb(Sb$_{1}$2/Sn$_{1}$2/)O$_{3}$-0.25PbTiO$_{3}$-0.65PbZrO$_{3}$ 세라믹을 소결온도 및 시간을 각각 1200-1250[.deg.C]에서 2, 4, 6시간으로 변화시켜 제작하였으며 시편의 소결조건 및 MnO$_{2}$(0~0.30mol%)첨가량에 따른 잡음특성을 관찰하였다. 초전계수 및 전압감도는 1250[.deg.C]에서 2시간 소결시킨 시편에서 각각 3.49x$10^{-8}$[C/$cm^{2}$K], 147[V/W]의 최대값을 나타내었다. 초전형 적외선 검출기의 잡음특성에 있어 증폭기의 전류잡음 .DELTA.V$_{i}$가 총 잡음전압에 대해 지배적인 경향을 나타내었으며 MnO$_{2}$가 0.24[mol%] 첨가된 1250[.deg.C]에서 2시간 소결시킨 시편에서 가장 양호한 pop-corn잡음특성을 나타내었다.다.

• 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 Institute of Electrical and Electronic Material Engineers
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• v.18 no.6
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• pp.550-553
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• 2005

[ $Pb(Zr_{0.2}Ti_{0.8})O_3$ ] powders, prepared by the sol-gel method, were mixed with an organic vehicle and the PZT thick films were fabricated by the screen-printing techniques on Pt/alumina substrates. The structural and dielectric properties were examined as a function of sintering temperature. The particle size distribution of the powder is bimodal with the mean particle size of about $1.2\;{\mu}m$. The average grain size of the PZT thick films sintered above $1000^{\circ}C$ was about $3.1\;{\mu}m$ and the thickness of the specimens was approximately $41\;{\mu}m$. The relative dielectric constant and dielectric loss of the thick films sintered at $1050^{\circ}C$ were 337 and $1.24\%$, respectively.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.32 no.1
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• pp.20-24
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• 2019

Ferroelectric material properties are strongly governed by domain structures and their evolution processes, but the evolution processes of complex domain patterns during a macroscopic electrical poling process are still elusive. In the present work, domain-evolution processes in a PZT ceramic near the morphotropic phase-boundary composition were studied during a step-wise electrical poling using piezoresponse force microscopy (PFM). Electron backscatter diffraction was used with the PFM data to identify the grain boundaries in the region of interest. In response to an externally the applied electric field, growth and retreat of non-$180^{\circ}$ domain boundaries wasere observed. The results indicate that ferroelectric polarization-switching nucleates and evolves in concordance with the pattern of the pre-existing domains.

• Journal of Sensor Science and Technology
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• v.19 no.3
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• pp.202-208
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• 2010

This study examined the dependency of crystalline orientation and electric properties of sol-gel PZT film on hydrolysis, a $PbTiO_3$ seed layer and a concentration of sol-gel solution. The PZT thin films were prepared by using 2-Methoxyethanol-based sol-gel method and spin-coating on Pt/Ti/$SiO_2$/Si substrates. The 1-${\mu}m$-thick PZT films were coated and then fired in a furnace by direct insert method. The highly (111) oriented PZT film of pure perovskite structure could be obtained. We could control the degree of orientation by various parameters such as hydrolysis, a $PbTiO_3$ seed layer and a concentration of sol-gel solution. The highest measured remanent polarization, dielectric constant and piezoelectric coefficient are $24.16\;{\mu}C/cm^2$, 2808, and 159 pC/N, respectively.