• Journal of Ceramic Processing Research
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• 제20권6호
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• pp.603-608
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• 2019

In this study, the multilayered thin films of (Ba,Sr)TiO3/K(Ta,Nb)O3 were fabricated by the sol-gel and spin coating methods, and their structural and electrical properties were investigated. The specimen showed polycrystalline X-ray diffraction (XRD) characteristics with a tetragonal structure. The average grain size and film thickness for one coating were about 30~40nm and 60nm, respectively. The phase transition temperature of specimen was lower than 10 ℃. The dielectric constant and loss at 20 ℃ of the specimen coated six times were 1,231 and 0.69, respectively. The rate of change in dielectric constant at an applied direct current (DC) voltage of the six times coated thin films was 17.3%/V. The electrocaloric effect was the highest around the temperature at which the remanent polarization rapidly changed. When an electric field of 660kV/cm was applied to the triply coated thin films, the highest electrocaloric property of 4.41 ℃ was observed.

• 한국재료학회지
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• 제22권1호
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• pp.35-41
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• 2012

Presently, the most promising family of lead-free piezoelectric ceramics is based on $K_{0.5}Na_{0.5}NbO_3$(KNN). Lithium, silver and antimony co-doped KNN ceramics show high piezoelectric properties at room temperature, but often suffer from abnormal grain growth. In the present work, the $(Ba_{0.85}Ca_{0.15})(Ti_{0.88}Zr_{0.12})O_3$ component, which has relaxor ferroelectric characteristics, was doped to suppress the abnormal grain growth. To investigate this effect, Lead-Free $0.95(K_{0.5}Na_{0.5})_{0.95}Li_{0.05}NbO_3-(0.05-x)AgSbO_3-x(Ba_{0.85}Ca_{0.15})(Ti_{0.88}Zr_{0.12})O_3$[KNLN-AS-xBCTZ] piezoelectric ceramics were synthesized by ball mill and nanosized-milling processes in lead-Free $0.95(K_{0.5}Na_{0.5})_{0.95}Li_{0.05}NbO_3-(0.05-x)AgSbO_3$ in order to suppress the abnormal grain growth. The nanosized milling process of calcined powders enhanced the sintering density. The phase structure, microstructure, and ferroelectric and piezoelectric properties of the KNLN-AS ceramics were systematically investigated. XRD patterns for the doped and undoped samples showed perovskite phase while tetragonality was increased with increasing BCZT content, which increase was closely related to the decrease of TO-T. Dense and uniform microstructures were observed for all of the doped BCZT ceramics. After the addition of BCTZ, the tetragonal-cubic and orthorhombic-tetragonal phase transitions shifted to lower temperatures compared to those for the pure KNNL-AS. A coexistence of the orthorhombic and tetragonal phases was hence formed in the ceramics with x = 0.02 mol at room temperature, leading to a significant enhancement of the piezoelectric properties. For the composition with x = 0.02 mol, the piezoelectric properties showed optimum values of: $d_{33}$ = 185 pC/N, $k_P$ = 41%, $T_C=325^{\circ}C$, $T_{O-T}=-4^{\circ}C$.

• 대한전자공학회논문지SD
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• 제37권4호
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• pp.7-14
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• 2000

Bi/sub 4/Ti/sub 3/O/sub 12/ (BIT) 박막을 acetate 계 precursor 를 이용한 sol-gel 법으로 제작한 후, 구조적 및 전기적 특성을 조사하여 NVFRAM (Won-Volatile Ferroelectric RAM)으로의 응용가능성을 조사하였다. DT-TG (Differential Thermal-Thermal Gravimetric) 분석으로 drying 온도와 annealing 온도가 각각 400℃ 와 650℃ 인 BIT 박막의 열처리조건을 확립하였다. Pt/Ta/Sio/sub 2//Si 기판 위에 제작된 BIT 박막은 완전한 orthorhombic perovskite상을 가지며, 입자크기가 약 100nm 이고 표면 거칠기는 약 70.2Å 으로 비교적 치밀한 형상을 나타내었다. 10㎑ 의 주파수에서 비유전률과 유전손실은 각각 176 과 0.038 이었으며, 100 ㎸/cm 의 전기장에서 누설전류밀도는 4.71㎂/㎠ 이었다. ±250㎸/㎝ 에서 이력곡선을 측정한 결과, 잔류분극 (Pr)과 항전계 (Ec)는 각각 5.92μC/㎠ 과 86.3㎸/㎝ 이었다. BIT 박막에 ±5V 의 사각펄스를 인가하여 피로특성을 측정한 결과, 잔류분극은 초기값 5.92μC/㎠ 에서 10/sup 9/회에서는 3.95μC/㎠ 로 약 33% 감소하였다.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2014년도 제46회 동계 정기학술대회 초록집
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• pp.183-183
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• 2014

Recently, multiferroic materials gain much attention due to their fascinating fundamental physical properties. These materials offer wide range of potential applications such as data storage, spintronic devices and sensors, where both electronic and magnetic polarizations can be coupled. Among single-phase multiferroic materials, $BiFeO_3$ is typical because of the room-temperature magnetoelectric coupling in view of long-range magnetic- and ferroelectric-ordering temperatures. However, $BiFeO_3$ is well known to have large leakage current and small spontaneous polarization due to the existence of oxygen vacancies and other defects. Furthermore the magnetic moment of pure $BiFeO_3$ is very weak owing to its antiferromagnetic nature. Recently, various attempts have been performed to improve the multiferroic properties of $BiFeO_3$ through the co-doping at the A and the B sites, by making use of the fact that the intrinsic polarization and magnetization are associated with the lone pair of $Bi^{3+}$ ions at the A sites and the partially-filled 3d orbitals of $Fe^{3+}$ ions at the B sites, respectively. In this study, $BiFeO_3$, $Bi_{0.9}Ho_{0.1}FeO_3$, $BiFe_{0.97}Ni_{0.03}O_3$ and $Bi_{0.9}Ho_{0.1}Fe_{0.97}Ni_{0.03}O_3$ bulk compounds were prepared by solid-state reaction and rapid sintering. High-purity $Bi_2O_3$, $Ho_2O_3$, $Fe_2O_3$ and $NiO_2$ powders with the stoichiometric proportions were mixed, and calcined at $500^{\circ}C$ for 24 h to produce the samples. The samples were immediately put into an oven, which was heated up to $800^{\circ}C$ and sintered in air for 1 h. The crystalline structure of samples was investigated at room temperature by using a Rigaku Miniflex powder diffractometer. The field-dependent and temperature-dependent magnetization measurements were performed with a vibrating-sample magnetometer and superconducting quantum-interference device.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제42회 동계 정기 학술대회 초록집
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• pp.250-250
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• 2012

Recently, multiferroic materials have attracted much attention due to their fascinating fundamental physical properties and potential technological applications in magnetic/ferroelectric data storage systems, quantum electromagnets, spintronics, and sensor devices. Among single-phase multiferroic materials, $BiFeO_3$, in particular, has received considerable attention because of its very interesting magnetoelectric properties for application to spintronics. Enhanced ferromagnetism was found by Fe-site ion substitution with magnetic ions. In this study, $BiFe_{1-x}Ni_xO_3$ (x=0 and 0.05) bulk ceramic compounds were prepared by solid-state reaction and rapid sintering. High-purity $Bi_2O_3$, $Fe_3O_4$ and NiO powders were mixed with the stoichiometric proportions, and calcined at $450^{\circ}C$ for 24 h to produce $BiFe_{1-x}Ni_xO_3$. Then, the samples were directly put into the oven, which was heated up to $800^{\circ}C$ and sintered in air for 20 min. The crystalline structure of samples was investigated at room temperature by using a Rigaku Miniflex powder diffractometer. The Raman measurements were carried out with a Raman spectrometer with 514.5-nm-excitation Ar+-laser source under air ambient condition on a focused area of $1-{\mu}m$ diameter. The field-dependent magnetization and the temperature-dependent magnetization measurements were performed with a vibrating-sample magnetometer. The x-ray diffraction study demonstrates the compressive stress due to Ni substitution at the Fe site. $BiFe_{0.95}Ni_{0.05}O_3$ exhibits the rhombohedral perovskite structure R3c, similar to $BiFeO_3$. The lattice constant of $BiFe_{0.95}Ni_{0.05}O_3$ is smaller than of $BiFeO_3$ because of the smaller ionic radius of Ni3+ than that of Fe3+. The field-dependent magnetization of $BiFe_{0.95}Ni_{0.05}O_3$ exhibits a clear hysteresis loop at 300 K. The magnetic properties of $BiFe_{0.95}Ni_{0.05}O_3$ were improved at room temperature because of the existence of structurally compressive stress.

• 한국결정성장학회지
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• 제15권3호
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• pp.124-127
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• 2005

[ $Ti:LiNbO_3$ ], 광도파로 제작을 위해 큐리온도$(T_c)$ 아래에서 백금박스 내에서 알곤 과 산소 분위기 내에서 열처리 과정 동안 기판 표면의 강유전 도메인 특성 변화를 관찰하였다. 열처리 된 $LiNbO_3$ 기판의 +Z면의 경우 전체적으로 약 $1.6{\mu}m$ 두께로 도메인 반전이 이루어 졌으며, 표면에서 etch hillock이 관찰되었다. $LiNbO_3$ 결정 표면의 Li 이온이 외부로 확산 되는 영향을 감소시킬 수 있는 환경에 있는 기판 면에서 하나의 도메인이 관찰되었으며, 이때 결정 표면에서의 식각특성, 결정성 및 양이온 분포변화에 관하여 X-선 회절, AFM 및 SIMS를 이용하여 분석하였다.

• 한국재료학회지
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• 제12권6호
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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.

• 마이크로전자및패키징학회지
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• 제20권4호
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• pp.25-30
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• 2013

Pb-free ferroelectric $(Na_{0.5}Bi_{0.5})TiO_3$ (NBT) thin films were prepared by a modified sol-gel process. Their structural, dielectric and pyroelectric properties were investigated as a function of the excess Na/Bi ratio and the annealing temperature. In the case of thin films containing no excess Na and Bi, only partial amounts of the perovskite NBT were crystallized, where the films consisted mainly of the pyrochlore phase of $Bi_2Ti_2O_7$ for annealing conditions of $600{\sim}800^{\circ}C$. With increasing excess Na/Bi ratio, the proportion of the perovskite phase effectively increased due to the compensation of the volatile Na and Bi components. For a Na/Bi ratio of 2.0, the thin film with single NBT perovskite phase was obtained within XRD detection limit after annealing at $700^{\circ}C$ for 10 min and it showed the excellent dielectric properties, ${\varepsilon}r$ of ~550 and tan ${\delta}$ of 0.03. While these properties were degraded for Na/Bi ratio of 2.5 despite the existence of pure perovskite phase. The NBT thin film with Na/Bi ratio of 2.0 are also promising candidates for applications requiring pyroelectric devices because it was found to have pyroelectric coefficients of $1.3{\sim}7nC/cm^2K$ in the temperature range of $30{\sim}100^{\circ}C$.

• 대한전기학회:학술대회논문집
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• 대한전기학회 1988년도 전기.전자공학 학술대회 논문집
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• pp.799-801
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• 1988

This paper was studied on the effects of Ca-La-Nb substitution and Zr/Ti ratio variation to Pb(Zr, Ti)$O_3$ system on structural, electrical, optical and sound level characteristics in order to develope the piezoelectric and electrooptic ceramic devices. Also the specimens were prepared by the two stage sintering technique. The molecular formular was X($CaO{\cdot}1/4La_{2}O_{3}{\cdot}1/4Nb_{2}O_{5}){\cdot}(1-X)Pb(Zr_{Y}Ti_{1-Y})O_{3}$(x=100X, y=100Y), and the variation of x was $6{\sim}12$, y was 60${\sim}$49 and second stage sintering time was 20${\sim}$40 hours. The experimental results obtained from this study are as follows : 1. The density was decreased, the grain size was increased according to increase of Ca-La-Nb substitution. 2. The crystal structure was rhombohedral in composition 6/60/40, and the crystal structure was tetragonal and cubic according to increase of Ca-La-Nb substitution. 3. The Ca substitution of PZT system enhanced the sintering property. The Pb site vacancy resulting from the substitution of La-Nb increased the dielectrical constant, the piezoelectric charge constant, the dielectric loss and decreased the coercive field. 4. The resistivity of PZT system which has the P type conduction mechanism increased according to substitution of La-Nb because of the substituent acting as donor. 5. The PZT ceramics varied from ferroelectric substance according to increase of Ca-La-Nb substituent. The coercive field and saturation remanent polarization decreased, and at last straight line according to increase of La-Nb substitution. 6. The amount of Ca-La-Nb substitution to improve the light transmittance of speciment was 10 mol%, the Zr/Ti ratio was 49/51, and the second stage sintering time was 40 hours. 7. According to Ca-La-Nb substitution, the specimens was to be transparent. The 7.5/51/49 specimen was suitable for transparent sound vibrator because it had 58% light transmittance (thick 0.2[mm], wave length 700[mm]) and 48% electromechanical coupling factor.

• 한국재료학회지
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• 제11권9호
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• pp.769-775
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• 2001

High quality PZT piezoelectric thin films were sputter- deposited on$ RuO_2$/$SiO_2$/Si substrates by using 2-step deposition method. As the first step, PZT seed layers were fabricated at a low temperature($475^{\circ}C$ ) to form a pure perovskite phase by reducing the volatility of Pb oxide. and then, as the second step, the PZT films were deposited at high temperatures ($530^{\circ}C$~$570^{\circ}C$) to reduce the defect density in the films. By this method, the pure perovskite phase was obtained at high deposition temperature range ($530^{\circ}C$~$570^{\circ}C$) and the superior electrical properties of PZT films were obtained on $RuO_2$substrate : 2Pr : 60$\mu$C/$\textrm{cm}^2$, $E_c: 60kV/cm, \;J_t: 10^{-6}A/cm^2\; at\; 250kV/cm$. The residual stress of PZT films fabricated by the 2-step deposition method was tensile and below 150MPa. It was attempted to control the residual stress in the PZT films by applying a negative bias to the substrate. As the amplitude of the substrate bias was increased, the residual tensile stress was slightly decreased, however, the ferroelectric properties of PZT films were degraded by ion bombardment.