• Journal of the Korean Crystal Growth and Crystal Technology
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• v.19 no.2
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• pp.70-74
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• 2009

Effect of the processing variables on the formation of $Pb(Sc_{1/2}Nb_{1/2})O_3$(hereafter PSN) thin layers prepared on Pt(111)/Ti/$SiO_2$/Si substrates using the sol-gel and the spin coating method has been studied. After each deposition, the coated films were heated at $370^{\circ}C$ for 5 min. Then they were finally sintered at temperature range of $600{\sim}700^{\circ}C$ by RTA(rapid thermal annealing). The final multilayered films showed a (111) preferred orientation. On a while, the layer-by-layer crystallization of multilayered amorphous thin films without the intermediate heating exhibited a (100) preferred orientation. In case of heat treatment in the tube furnace with the heating rate of $4^{\circ}C/min$, (100) and (111) oriented thin layers were formed simultaneously. The microstructure of the deposited films were dense and crack-free with thickness of 300nm, irrespective of the processing variables.

• Journal of the Institute of Electronics Engineers of Korea SD
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• v.39 no.3
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• pp.1-8
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• 2002

In order to study electric properties of (Pb$\_$0.9/La$\_$0.1/)Ti$\_$0.975/O$_3$(PLT (10)) films with varying excess lead concentration (7.5, 10, 12.5, 15 ㏖% excess lead), the PLT films were deposited by sol-gel process. DTA analyses reveal that the crystallization temperature of the precursor powers decreased with increasing amount of excess lead. XRD patterns of PLT reveal pure perovskite structure and the preferred orientation increased with increasing Pb content in the films. With increasing amount of excess P$\_$b/, the relative permittivity ($\xi$$\_$r/) increased and leakage current density at 100 ㎸/cm transformed 4.01$\times$10$\^$-5/, 2.42$\times$10$\^$-6/, 1.27$\times$10$\^$-6/, 1.56$\times$10$\^$-6/A/㎠ respectively. In the results of hysteresis loops measured at 166 kV/cm, the remanent polarization (P$\_$r/) and the coercive field (E$\_$c) are 6.36$\mu$C/cm and 58.7 ㎸/cm, respectively (at 12.5 ㏖% excess P$\_$b/) With increasing amount of excess Pb, the remanent polarization for PLT thin film degraded to about 44%, 27%, 15%, 16% of the initial value after 10$\^$9/ cycles./TEX>) With increasing amount of excess Pb, the remanent polarization for PLT thin film degraded to about 44%, 27%, 15%, 16% of the initial value after $10^{9}$ cycles.

• Proceedings of the Materials Research Society of Korea Conference
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• 2003.03a
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• pp.200-200
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• 2003

고체산화물 연료전지(SOFC)에서 사용되는 연결재의 주 기능은 각 단위 셀의 연료극과 다음 셀의 공기극을 전기적으로 연결하여, 공기와 사용연료의 분리역할을 하기 위하여 사용된다. SOFC용 연결재는 다른 구성요소 소재보다, 높은 전자 전도성, 낮은 이온전도성, 우수한 기계 적강도가 요구되며, SOFC는 고온에서 작동되기 때문에, 상온에서 작동온도까지 다른 요소 소재들과 유사한 열팽창계수와 물리, 화학적으로 안정성이 요구된다. 현재 연결재 제조기술은 EVD, CVD, plasma spraying, tape casting 등 다양하게 연구되고 있으며, 본 연구는 세라믹 연결재 증착방법 중 저렴한 비용으로 대량 생산이 용이한 습식법(dip coaling)을 적용하여, 연료극 지지체식 flat-tube형 고체산화물 연료전지의 지지체를 위해 세라믹 연결재를 제조하고, 그 특성을 연구하였다. 세라믹 연결재로써 선정한 합성조성은 LaCr $O_3$에 Ca이 치환 고용된 L $a_{0.6}$C $a_{0.41}$Cr $O_3$으로 pechini법으로 합성하였다. 합성된 조성은 100$0^{\circ}C$에서 5시간 하소후 가속 Ball Milling하여 0.5$\mu\textrm{m}$의 평균입자크기를 얻을 수 있었다. XRD 상분석결과 perovskite상 (L $a_{1-x}$ Ca/x/Cr $O_3$)과 CaCr $O_4$를 얻을 수 있었다. slurry를 제조하여 막의 밀착성을 증진시키기 위해 sand blasting시킨 flat tube지지체에 진공펌프를 이용하여 소재내부와 외부의 압력차로 dip coating한 후, 140$0^{\circ}C$로 소결 하였다. coating 결과 박리현상은 없었으나, 표면과 단면의 SEM분석결과 다소 porous한 박막층이 형성되었으며, Ca이온이 지지체로 permeation되는 현상이 발생하였다. 이와 같은 결과로부터 보다 치밀한 박막생성을 위해, slurry 제조조건을 변화시켰으며, Ca이온의 migration을 막기 위해 barrier layer를 이용하였다 완전 소결된 지지체는 가스투과도와 전기전도도측정을 통하여 특성을 평가하였다.였다.다.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2001.07a
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• pp.170-173
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• 2001

Thin films of phase-pure perovskite (P $b_{0.72}$L $a_{0.28}$) $Ti_{0.93}$ $O_3$(PLT) were deposited in-situ onto Pt/Ti/ $SiO_2$/Si substrates by pulsed laser deposition. We have systematically investigated the variation of grain sizes depending on the process condition. Both in-situ annealing and ex-situ annealing treatments have been compared depending on the annealing time. Two-step process to grow (P $b_{0.72}$L $a_{0.28}$) $Ti_{0.93}$ $O_3$(PLT) films was adopted and verified to be useful to enlarge the grain size of the film and to enhance the leakage current characteristics. The grain sizes of PLT thin films were successfully controlled 260 to 350 nm by changing process parameters. Electrical properties including dielectric constant, ferroelectric characteristics, crystallization and leakage current of PLT thin films were shown to be strongly inf1uenced by grain size. Also PLT thin films on p-type(100) Si substrate will be fabricated by pulsed laser deposition technique using a Nd:YAG laser with different wavelengths of 355, 532 and 1064 nm. Effect of the variation of laser wavelength on dielectric properties will be discussed. Microstructural and electrical properties of the film were investigated by C-V measurement leakage current measurement and SEM.ent and SEM.

• Electrical & Electronic Materials
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• v.9 no.3
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• pp.251-258
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• 1996

Sol-Gel derived ferroelectric Pb(Z $r_{0.52}$ $Ti_{0.48}$) $O_{3}$ thin films have been fabricated on Pt/Ti/ $SiO_{2}$/Si substrate. Two kinds of fast annealing methods, F-I (six times of intermediate and final annealing) and F-II(one final annealing after six times of intermediate annealing) were used for preparation of multi-coated PZT thin films. As the annealing temperature was increased, high capacitance could be obtained, for instance, 2700.angs.-thick PZT thin film annealed at 680.deg. C had a capacitance value of approximately 20nF at 1kHz. In addition, it is found that the dielectric constant is a function of the perovskite phase fraction. In case of F-I method, PZT thin film had a remanent polarization(Pr) of 8-15.mu.C/c $m^{2}$ and a coercive field( $E_{c}$) of 35-44kV/cm according to annealing temperature, whereas PZT film fabricated by F-II method had as high as 24-25.mu.C/c $m^{2}$ and 48-59kV/cm, respectively. As a result of measuring Curie temperature, PZT thin film had a range of 460-480.deg. C by F-I method and more or less higher range of 525-530.deg. C by F-II method, which implied that different microstructures could cause the different Curie temperature. Through I-V measurement, leakage current of PZT thin film fabricated by F-I and F-II methods was 64nA/c $m^{2}$ and 2.2.mu.A/c $m^{2}$ in the electric field of 100kV/cm, respectively.y.y.y.

• Korean Journal of Materials Research
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• v.12 no.6
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• pp.464-469
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• 2002

$SrBi_2Nb_2O_9(SBN)$ thin films were grown on Pt/Ti/Si and p-type Si(100) substrates by rf-magnetron co-sputtering method using two ceramic targets, $SrNb_2O_6\; and \;Bi_2O_3$. The structural and electrical characteristics have been investigated to confirm the possibility of the SBN thin films for the applications to destructive and nondestructive read out ferroelectric random access memory(FRAM). For the optimum growth condition X-ray diffraction patterns showed that SBN films had well crystallized Bi-layered perovskite structure after $700^{\circ}C$ heat-treatment in furnace. From this specimen we got remnant polarization $(2P_r)$ of about 6 uC/$\textrm{cm}^2$ and coercive voltage $(V_c)$ of about 1.5 V at an applied voltage of 5 V. The leakage current density was $7.6{\times}10^{-7}$/A/$\textrm{cm}^2$ at an applied voltage of 5V. And for the NDRO-FRAM application, properties of SBN films on Si substrate has been investigated. From transmission electron microscopy (TEM) analysis, we found the furnace treated sample had a native oxide about 2 times thicker than the RTA treated sample and this thick native oxide layer had a bad effect on C-V characteristics of SBN/Si thin film. After $650^{\circ}C$ RTA process, we got the improved memory window of 1.3 V at an applied voltage of 5 V.

• Korean Journal of Materials Research
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• v.13 no.5
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• pp.317-322
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• 2003

Bismuth layered structure ferroelectric thin films, $Bi_4$$Ti_3$$O_{12}$ / (BTO) and Nb-doped BTO (BTN) were prepared on the Pt(111)/Ti/$SiO_2$/Si(100) substrates by a sol-gel route. We investigated the Nb-doping effect on the grain orientation and ferroelectric properties. $Nb^{5＋}$ ion substitution for $Ti^{4＋}$ ion in perovskite layers of BTO decreased the degree of c-axis orientation and increased the remanent polarization (2Pr). The fatigue resistance of Nb-doped BTO thin film was shown to be superior to that of BTO, and the leakage current of Nb-doped BTO thin film was decreased about 1 order of magnitude compared with BTO. The improvement of ferroelectric properties with $Nb^{5＋}$ doping in BTO could be attributed to the changes in space charge densities and grain orientation in the thin film.

• Korean Journal of Materials Research
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• v.14 no.10
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• pp.701-706
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• 2004

Bismuth layered structure ferroelectric thin films, La-substituted $Bi_{4}Ti_{3}O_{12}$ ($Bi_{1-x}La_{x}Ti_{3}O_{12}$, x=0.75, BLT) were prepared on the $Pt(111)/Ti/SiO_2/Si(100)$ substrates by a sol-gel spin coating process. The thin films were annealed in various conditions, i.e., oxygen, nitrogen and vacuum atmospheres for various annealing time. We investigated the annealing condition effects on the grain orientation and ferroelectric properties. The measured XRD patterns revealed that the BLT thin films showed only $Bi_{4}Ti_{3}O_{12}$-type phase with random orientation. $La^{3+}$ ion substitution for $Bi^{3+}$ ion in perovskite layers of $Bi_{4}Ti_{3}O_{12}$ decreased the degree of c-axis orientation and increased the remanent polarization ($2P_{r}$). The remanent polarization ($2P_{r}$) and the coercive field ($2E_{c}$) of the BLT thin film annealed at $650^{\circ}C$ for 5 min in oxygen atmosphere were $87{\mu}C/cm^2$ and 182 kV/cm, respectively, at an applied electric field of 240 kV/cm. For all of the BLT thin films annealed in various conditions, the fatigue resistance was shown. The improvement of ferroelectric properties with La substitution in $Bi_{4}Ti_{3}O_{12}$ could be attributed to the changes in space charge densities and grain orientation in the thin film.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2003.07b
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• pp.723-727
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• 2003

[ $Sr_xBa_{1-x}Nb_2O_6$ ] (SBN, $0.25{\leq}x{\leq}0.75$) ceramic is a ferroelectric material with tetragonal tungsten bronze (TTB) type structure, which has a high pyroelectric coefficient and a nonlinear electro-optic coefficient value. In spite of its advantages, SBN has not been investigated well compared to other ferroelectric materials with perovskite structure. In this study, SBN thin film was manufactured by ion beam sputtering technique using the prepared SBN target in $Ar/O_2$ atmosphere. SBN30 thin film of $1000{\AA}$ was pre-deposited as a seed layer on $Pt(100)/TiO_2/SiO_2/Si$ substrate followed by SBN60 deposition up to $3000{\AA}$ in thickness. As-deposited SBN60/SBN30 layer was heat-treated at different temperatures of 650, 700, 750, and $800^{\circ}C$ in air, respectively The crystallinity and orientation behavior as well as electric properties of SBN60/SBN30 multi-layer were examined. The deposited layer was uniform and the orientation was shown primarily along (001) plane from XRD pattern. There was no difference in the crystal structure with heat-treatment temperature, but the electric properties depended on the heating temperature and was the best at $750^{\circ}C$. In electric properties of Pt/SBN60/SBN30/Pt thin film capacitor prepared, the remnant polarization (2Pr) value was $15{\mu}C/cm^2$, the coercive field (Ec) 75 kV/cm, and the dielectric constant 1075, respectively.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2010.06a
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• pp.24-24
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• 2010

대형구조물의 구조안정성 진단, 로봇과 같은 지능기계의 제어, 환경오염을 감지하기 위한 센서의 중요성은 날로 증대되고 있다. 이러한 센서의 감도와 성능을 높이기 위해서 소형화, 다기능화, 집적화가 요구되고 있는데, 고성능 센서소자들의 집적화를 위해서 기존에 적용된 벌크형태의 재료들을 박막화하여 다층적층 및 소형화할 필요가 있다. 집적화 센서의 구현에 있어서 전극박막은 센서의 특성을 좌우하는 중요한 역할을 한다. 일반적으로 금속박막이 전극으로 사용되고 있으나 열적 불안정성 및 박리현상의 문제점을 지니고 있다. 따라서 이를 해결하기 위해 전도성산화막을 전극으로 적용하고자하는 연구가 요구되고 있다. 전도성산화막을 전극으로 적용하면 센서소자의 성능이 개선되는 경향이 있다. $Sr_2FeMoO_6$(SFMO) 산화물은 자기장을 인가했을 때 저항이 감소하는 CMR(colossal magnetoresistance) 물질이며 상온비저항이 낮은 것으로 알려져 있다. 이중 페롭스카이트 (double perovskite) 구조를 갖는 $Sr_2FeMoO_6$ 박막은 센서소자의 전극으로 적용 가능할 것으로 생각되어 박막을 제조하고자 하였으며 미세구조와 전기전도 특성을 조사하였다. 박막제조를 위해서는 RF 스퍼터법을 사용하였다. 스퍼터를 위한 타겟은 고상반응법으로 분말타겟을 제조하였다. Ar/$O_2$ 가스 유랑변화, 압력변화, 기판 온도변화가 박막의 상형성 등 박막특성에 미치는 영향을 조사하였다. 기판으로는 $SiO_2$(100nm)/Si 기판을 사용하였다. 증착직후에는 비정질막이 얻어졌으며 SFMO 상을 만들기 위해서는 후열처리가 필요하였는데, 환원성 가스 분위기 [$H_2$(5%)/Ar] 에서 열처리 조건을 최적화하여 이중 페롭스카이트 구조의 단일상 박막을 제조할 수 있었다. SFMO 단일상 박막은 증착시에나 후열처리 시 산소의 억제가 중요함을 알 수 있었다.