• Title/Summary/Keyword: High-temperature XRD

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Fabrication and Post-Annealing Effects of Ferroelectric $Sr_xBi_yTa_2O_{9+\alpha}$(SBT) Thin Films by MOD Process (MOD법에 의한 강유전성 $Sr_xBi_yTa_2O_{9+\alpha}$(SBT) 박막의 제조 및 후열처리 효과에 관한 연구)

  • 정병직;신동석;윤희성;김병호
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.11 no.3
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    • pp.229-236
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    • 1998
  • Ferroelectric $Sr_xBi_yTa_2O_{9+\alpha}$/(0.7$\leqSr\leq1.0,\; 2.0\leqBi\leq2.6)$ solutions were prepared by MOD (Metalorganic Deposition) process. These solutions were made into thin films with thickness ranging from 1500~2000${\AA}$ by spin coating. The phase transformation of the SBT thin films by variation of annealing temperature and annealing time were observed using high temperature XRD and SEM. The crystallization and grain growth of SBT thin film were accomplished at $800^{\circ}C$ for 30 minutes after deposition of Pt top electrode by sputtering to prevent electrical breakdown. Ferroelectric properties of the SBT thin films were measured in the range of $\pm$3V\; and\; \pm5V$. The specimen with composition ratio of Sr/Bi/Ta (0.8/2.4/2.0) has the excellent ferroelectric properties ; $2P_r = 10.5,\; 13.2\muC/cm^2 \;at\; \pm3V\; and\; \pm5V$ respectively. Observing the post annealed Pt/SBT/Pt interface by SEM, it was found that Pt electrode sputtered on to the SBT thin film penetrated into the hollow on the SBT thin film, thus decreasing the effective insulation thickness. The effective insulation thickness recovered by post annealing, and this was confirmed by leakage current density measurement.

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Effect of Seed-layer on the Crystallization and Electric Properties of SBN60 Thin Films (SBN60 박막의 결정화 및 전기적 특성에 관한 씨앗층의 영향)

  • Jang, Jae-Hoon;Lee, Dong-Gun;Lee, Hee-Young;Jo, Sang-Hee
    • 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.

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Preparation and Characterization of Porous and Composite Nanoparticulate Films of CdS at the Air/Water Interface

  • Ji, Guanglei;Chen, Kuang-Cai;Yang, Yan-Gang;Xin, Guoqing;Lee, Yong-Ill;Liu, Hong-Guo
    • Bulletin of the Korean Chemical Society
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    • v.31 no.9
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    • pp.2547-2552
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    • 2010
  • CdS nano-particulate films were prepared at the air/water interface under Langmuir monolayers of arachidic acid (AA) via interfacial reaction between $Cd^{2+}$ ions in the subphase and $H_2S$ molecules in the gaseous phase. The films were made up of fine CdS nanoparticles with hexagonal Wurtzite crystal structure after reaction. It was revealed that the formation of CdS nano-particulate films depends largely on the experimental conditions. When the films were ripened at room temperature or an increased temperature ($60^{\circ}C$) for one day, numerous holes were appeared due to the dissolution of smaller nanoparticles and the growth of bigger nanoparticles with an improved crystallinity. When the films were ripened further, CdS rodlike nanoparticles with cubic zinc blende crystal structure appeared due to the re-nucleation and growth of CdS nanoparticles at the stacking faults and defect structures of the hexagonal CdS grains. These structures were characterized by transmission electron microscopy (TEM), high-resolution TEM (HRTEM), and X-ray diffraction (XRD). These results declare that CdS semiconductor nanoparticles formed at the air/water interface change their morphologies and crystal structures during the ripening process due to dissolution and recrystallization of the particles.

Synthesis of Sphene (CaSnSiO5)-Pink Pigments with CrCl3

  • Lee, Hyun-Soo;Lee, Byung-Ha
    • Journal of the Korean Ceramic Society
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    • v.46 no.4
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    • pp.405-412
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    • 2009
  • In high temperature ceramic glazes, a stable range of pink-red colors that produced $Cr_2O_3-SnO_2-CaO-SiO_2$ pigments were factored by Cassiterite($SnO_2$) and Malayaite($CaSnSiO_5$) by $Cr_2O_3$. The experiment examined the influence of $CrCl_3$, a Sn-Cr substitution added with a mineralizer ($H_3BO_3$), as a chromophore in pigments. The experiment also studied the effect of $H_3BO_3$ (2 wt%) when added to malayaite($CaSnSiO_5$) to see if the crystalline reaction will increase. $Cr_2O_3$ was also substituted with $CrCl_3$ in order to prove how much influence $CrCl_3$ had on the $H_3BO_3$. Malayaite and cassiterite were the basic compound materials and the experiment was conducted both with and without mineralizers (2 wt% of $H_3BO_3$). Each compound was synthesized at 800, 1000, 1200, 1300, 1400, $1500^{\circ}C$ for 2 h. Synthesized pigments were analyzed by XRD, FT-IR and UV-Vis. The temperature variation produced two crystal phases that showed the different engaging effects of Cr oxidation. $CrCl_3$ produced a better effect on the malayaite crystal phase, resulting in a more defined pigmentation of the pink-red coloration compared to $Cr_2O_3$.

Particle Size and Reaction Temperature Effects on the Hydrolysis Reaction of Zinc in TGA (Thermo Gravimetric Analyzer) (열 중량 분석기에서 zinc 입자 크기와 반응 온도에 따른 물 분해 특성 연구)

  • Ahn, Seung-Hyuck;Kang, Kyoung-Soo;Kim, Chang-Hee;Bae, Ki-Kwang;Kim, Young-Ho;Park, Chu-Sik
    • Transactions of the Korean hydrogen and new energy society
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    • v.19 no.4
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    • pp.305-312
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    • 2008
  • ZnO/Zn redox cycle is the one of the promising thermochemical cycles for hydrogen production via water splitting with high temperature heat source like a concentrated solar energy. This paper reports the particle size effect of Zinc on water splitting behavior. Water splitting reaction experiments were carried out at isothermal conditions of 350 and 400$^{\circ}C$ in TGA (Thermo Gravimetric Analyzer) using four commercial Zinc powders (nano, <10 ${\mu}m$, <150 ${\mu}m$ and $150{\sim}600\;{\mu}m$ particle sizes). Before the experiments, average particle size of Zinc powders was analyzed by PSA (Particle Size Analysis). After the experiments, XRD (X-Ray Diffraction) and SEM (Scanning Electron Microscope) analyses were conducted on the samples. The experimental results showed that particle size had a effect on the conversion of Zinc to ZnO. Zinc conversion was increased, as the particle size decreased. Especially, the nano size particles were aggregated and the particle's morphology changed on the surface during hydrolysis reaction.

Photoluminescence of Nanocrystalline CdS Thin Films Prepared by Chemical Bath Deposition

  • Park, Wug-Dong
    • Transactions on Electrical and Electronic Materials
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    • v.11 no.4
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    • pp.170-173
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    • 2010
  • Nanocrystalline cadmium sulfide (CdS) thin films were prepared using chemical bath deposition in a solution bath containing $CdSO_4$, $SC(NH_2)_2$, and $NH_4OH$. The CdS thin films were investigated using X-ray diffraction (XRD), photoluminescence (PL), and Fourier transform infrared spectroscopy (FTIR). The as-deposited CdS thin film prepared at $80^{\circ}C$ for 60 min had a cubic phase with homogeneous and small grains. In the PL spectrum of the 2,900 A-thick CdS thin film, the broad red band around 1.7 eV and the broad high-energy band around 2.7 eV are attributed to the S vacancy and the band-to-band transition, respectively. As the deposition time increases to over 90 min, the PL intensity from the band-to-band transition significantly increases. The temperature dependence of the PL intensity for the CdS thin films was studied from 16 to 300 K. The $E_A$ and $E_B$ activation energies are obtained by fitting the temperature dependence of the PL intensity. The $E_A$ and $E_B$ are caused by the deep trap and shallow surface traps, respectively. From the FTIR analysis of the CdS thin films, a broad absorption band of the OH stretching vibration in the range $3,000-3,600\;cm^{-1}$ and the peak of the CN stretching vibration at $2,000\;cm^{-1}$ were found.

Thermal Stability, Mechanical Properties and Magnetic Properties of Fe-based Amorphous Ribbons with the Addition of Mo and Nb

  • Han, Bo-Kyeong;Jo, Hye-In;Lee, Jin Kyu;Kim, Ki Buem;Yim, Haein
    • Journal of Magnetics
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    • v.18 no.4
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    • pp.395-399
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    • 2013
  • The metallic glass ribbons of $[(Fe_xCo_{1-x})_{0.75}B_{0.2}Si_{0.05}]_{96}Mo_4$ (x = 0, 0.3, 0.6, 0.9 at.%) and $[(Fe_xCo_{1-x})_{0.75}B_{0.2}Si_{0.05}]_{96}Nb_4$ (x = 0, 0.3, 0.6, 0.9 at.%) were obtained by melt spinning with 25-30 ${\mu}m$ thickness. The thermal stability, mechanical properties and magnetic properties of Fe-Co-B-Si based systems were investigated. The values of thermal stability were measured using differential scanning calorimetry (DSC), including glass transition temperature ($T_g$), crystallization temperature ($T_x$) and supercooled liquid region (${\Delta}T_x=T_x-T_g$). These amorphous ribbons were identified as fully amorphous, using X-ray diffraction (XRD). The mechanical properties of Febased samples were measured by nano-indentation. Magnetic properties of the amorphous ribbons were measured by a vibrating sample magnetometer (VSM). The amorphous ribbons of $[(Fe_xCo_{1-x})_{0.75}B_{0.2}Si_{0.05}]_{96}Mo_4$ (x = 0, 0.3, 0.6, 0.9 at.%) and $[(Fe_xCo_{1-x})_{0.75}B_{0.2}Si_{0.05}]_{96}Nb_4$ (x = 0, 0.3, 0.6, 0.9 at.%) exhibited soft magnetic properties with low coercive force ($H_c$) and high saturation magnetization (Ms).

A Study on Thermal Stability of Ga-doped ZnO Thin Films with a $TiO_2$ Barrier Layer

  • Park, On-Jeon;Song, Sang-Woo;Lee, Kyung-Ju;Roh, Ji-Hyung;Kim, Hwan-Sun;Moon, Byung-Moo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.434-436
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    • 2013
  • Ga-doped ZnO (GZO) was substitutes of the SnO2:F films on soda lime glass substrate in the photovoltaic devices such as CIGS, CdTe and DSSC due to good properties and low cost. However, it was reported that the electrical resistivity of GZO is unstable above $300^{\circ}C$ in air atmosphere. To improve thermal stability of GZO thin films at high temperature above $300^{\circ}C$ an $TiO_2$ thin film was deposited on the top of GZO thin films as a barrier layer by Pulsed Laser Deposition (PLD) method. $TiO_2$ thin films were deposited at various thicknesses from 25 nm to 100 nm. Subsequently, these films were annealed at temperature of $300^{\circ}C$, $400^{\circ}C$, $500^{\circ}C$ in air atmosphere for 20 min. The XRD measurement results showed all the films had a preferentially oriented ( 0 0 2 ) peak, and the intensity of ( 0 0 2 ) peak nearly did not change both GZO (300 nm) single layer and $TiO_2$ (50 nm)/GZO (300 nm) double layer. The resistivity of GZO (300 nm) single layer increased from $7.6{\times}10^{-4}{\Omega}m$ (RT) to $7.7{\times}10^{-2}{\Omega}m$ ($500^{\circ}C$). However, in the case of the $TiO_2$ (50 nm)/GZO (300 nm) double layer, resistivity showed small change from $7.9{\times}10^{-4}{\Omega}m$ (RT) to $5.2{\times}10^{-3}{\Omega}m$ ($500^{\circ}C$). Meanwhile, the average transmittance of all the films exceeded 80% in the visible spectrum, which suggests that these films will be suitable for photovoltaic devices.

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Effect of Heat Treatment on Interface Behavior in Ni-P/Cr Double Layer (열처리 시간에 따른 Ni-P/Cr 이중 도금 층의 계면 거동에 관한 연구)

  • Choi, Myung-Hee;Park, Young-Bae;Rhee, Byong-ho;Byon, Eungsun;Lee, Kyu Hwan
    • Journal of the Korean institute of surface engineering
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    • v.48 no.6
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    • pp.260-268
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    • 2015
  • The thermal barrier coating (TBC) for inner wall of liquid-fuel rocket combustor consists of NiCrAlY as bonding layer and $ZrO_2$ as a top layer. In most case, the plasma spray coating is used for TBC process and this process has inherent possibility of cracking due to large difference in thermal expansion coefficients among bonding layer, top layer and metal substrate. In this paper, we suggest crack-free TBC process by using a precise electrodeposition technique. Electrodeposited Ni-P/Cr double layer has similar thermal expansion coefficient to the Cu alloy substrate resulting in superior thermal barrier performance and high temperature oxidation resistance. We studied the effects of phosphorous concentrations (2.12 wt%, 6.97 wt%, and 10.53 wt%) on the annealing behavior ($750^{\circ}C$) of Ni-P samples and Cr double layered electrodeposits. Annealing temperature was simulated by combustion test condition. Also, we conducted SEM/EDS and XRD analysis for Ni-P/Cr samples. The results showed that the band layers between Ni-P and Cr are Ni and Cr, and has no formed with heat treatment. These band layers were solid solution of Cr and Ni which is formed by interdiffusion of both alloy elements. In addition, the P was not found in it. The thickness of band layer was increased with increasing annealing time. We expected that the band layer can improve the adhesion between Cr and Ni-P.

Characteristic Evaluation of the Fe-Al Alloy Preform Fabrication by Reactive Sintering Process for the Al Matrix Composites. (반응소결법으로 제조한 Al기 복합재용 Fe-Al합금 예비성형체의 특성평가)

  • Choi, Dap-Chon;Park, Sung-Hyuk;Joo, Hyung-Gon
    • Journal of Korea Foundry Society
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    • v.19 no.6
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    • pp.493-500
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    • 1999
  • Squeeze casting was used for fabricating a light metal base composite having high strength and wearresistance. Reactive sintering was used to prepare the preform of Squeeze casting. To utilize Fe-Al intermetallic compounds and SiC particle as a reinforcement, there needs to prepare Fe-Al mixed powder at 50, 60, 70at.%Al, and add SiC powder to the above mixture at 4, 7, 16, 24wt.%. The prepared mixture with SiC was reactive sintered in a tube furnace at $660^{\circ}C$ to get a porous hybrid preform of intermetallic compound and SiC. The preform prepared above was placed in a metal mold, preheated at $660^{\circ}C$ AC4C matrix was injected into the mold with the temperature of the melt at $610^{\circ}C$ After these processes, 66MPa was applied to the mold for 5 minute to finish the whole procedure. The maximum reaction temperature was increased with the increased Al amount, but decreased with the increased SiC amount. The density of the preform was decreased with SiC amount increase in the compacts due to swelling of the preform. An optical microscope was applied to observe the micro structure and the dispersion of the reinforcements. To analyze phases, We utilized XRD, EDS. Hardness test were chosen to get the information of mechanical properties. There were no significant changes in micro structure between the composite and preform. However, it was shown that uniform dispersion of the reinforcers and complete infiltration of the melt into the preform were achieved through the procedure of the squeeze casting. It was observed that the hardness of the composite is decreased with increased SiC amount, resulting from the volumetric expansion of the preform.

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