• Title/Summary/Keyword: High-temperature XRD

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Phase Transition and Formatio of $TiSi_2$ Codeposited on Atomicaily Clean Si(111) (초청정 Si기판에 동시 증착된 $TiSi_2$ 의 상전이 및 형성)

  • Gang, Eung-Yeol;Jo, Yun-Seong;Park, Jong-Wan;Jeon, Hyeong-Tak;Nemaniah, R.J.
    • Korean Journal of Materials Research
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    • v.4 no.1
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    • pp.107-112
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    • 1994
  • The phase transition and the surface and interface morphologies of $TiSi_2$ formed on atomically clean Si substrates are investigated. 200$\AA$ Ti and 400$\AA$ Si films on Si(ll1) have been codeposited at elevated temperatures (400~$800^{\circ}C$) in ultrahigh vacuum. The phase transition of TiSiL is characterized with using XRD. The results distinguish the formation of the C49 and C54 crystalline titanium silicides. The surface and interface morphologies of titanium silicides have been examined with SEM and TEM. A relatively smootb surface is observed for the C49 phase while a rough surface and interface are observed for C54 phase. The islanding of the C54 phase becomes severe at high temperature ($800^{\circ}C$). Islands of TiSiL have been observed at temperatures above $700^{\circ}C$ but no islands are observed at temperatures below $600^{\circ}C$. For films deposited at $400^{\circ}C$ and 500%. weak XRD peaks corresponding to TiSi were observed and TEM micrographs exhibited small crystalline regions of titanium silicide at the interface.

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GaN Epitaxy with PA-MBE on HF Cleaned Cobalt-silicide Buffer Layer (HF 크리닝 처리한 코발트실리사이드 버퍼층 위에 PA-MBE로 성장시킨 GaN의 에피택시)

  • Ha, Jun-Seok;Chang, Ji-Ho;Song, Oh-Sung
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.11 no.2
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    • pp.409-413
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    • 2010
  • We fabricated 10 nm-thick cobalt silicide($CoSi_2$) as a buffer layer on a p-type Si(100) substrate to investigate the possibility of GaN epitaxial growth on $CoSi_2/Si(100)$ substrates. We deposited 500 nm-GaN on the cobalt silicide buffer layer at low temperature with a PA-MBE (plasma assisted-molecular beam epitaxy) after the $CoSi_2/Si$ substrates were cleaned by HF solution. An optical microscopy, AFM, TEM, and HR-XRD (high resolution X-ray diffractometer) were employed to determine the GaN epitaxy. For the GaN samples without HF cleaning, they showed no GaN epitaxial growth. For the GaN samples with HF cleaning, they showed $4\;{\mu}m$-thick GaN epitaxial growth due to surface etching of the silicide layers. Through XRD $\omega$-scan of GaN <0002> direction, we confirmed the cyrstallinity of GaN epitaxy is $2.7^{\circ}$ which is comparable with that of sapphire substrate. Our result implied that $CoSi_2/Si(100)$ substrate would be a good buffer and substrate for GaN epitaxial growth.

Characteristics of Converter Slag Aggregates Reformed by $SiO_2$ added Reduction ($SiO_2$를 첨가하여 환원개질한 전로슬랙의 골재특성)

  • ;T. R. Meadowcroft
    • Resources Recycling
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    • v.9 no.1
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    • pp.52-62
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    • 2000
  • In order to maximize the recycling of converter slag to the more valuable fields, such as high quality aggregates for construction, cement industry and flux for ion making. It will be very important to control the compositions and properties of converter slag to suit the purpose of utilizastion. In this study, converter slag (STELCO, CANADA) was mixed with 5%~30% $SiO_2$and 7% carbon, and then reduced at $1650^{\circ}C$. After the reduction was completed, the reformed slags were cooled to room temperature in the furnace. All of the slags were then characterized using SEM-EDX, XRD and chemical analysis. Also the compressive strengths and densities of the reformed slags were measured to compare with natural aggregates. XRD analysis shows that th phases of reformed slags are changed from bredigite+merwinite mixed phases of 10% $SiO_2$added reduction to akermanite phases of 20% and 30% $SiO_2$ added reduction. But the SEM-EDX analysis revealed that the phase distribution of the reformed slags was changed very sensitively and complicately depends on the change of slag compositions. And also the properties of reformed slags are changed very much depend on the phase distribution. About one third of Cadmium and on fifth of Vanadium are remained in reduction reformed converter slag. Another heavy metal elements such as cobalt, zinc, lead are removed up to more than 90-95% of original slag. The compressive strength and density of 25% $SiO_2$ added and reformed slag is very near to natural granite. This is superior more than 10% to Thyssen's $SiO_2$ added and oxidized converter slag aggregates.

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Synthesis of Novel (Be,Mg,Ca,Sr,Zn,Ni)3O4 High Entropy Oxide with Characterization of Structural and Functional Properties and Electrochemical Applications

  • Arshad, Javeria;Janjua, Naveed Kausar;Raza, Rizwan
    • Journal of Electrochemical Science and Technology
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    • v.12 no.1
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    • pp.112-125
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    • 2021
  • The new emerging "High entropy materials" attract the attention of the scientific society because of their simpler structure and spectacular applications in many fields. A novel nanocrystalline high entropy (Be,Mg,Ca,Sr,Zn,Ni)3O4 oxide has been successfully synthesized through mechanochemical treatment followed by sintering and air quenching. The present research work focuses on the possibility of single-phase formation in the aforementioned high entropy oxide despite the great difference in the atomic sizes of reactant alkaline earth and 3d transition metal oxides. Structural properties of (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide were explored by confirmation of its single-phase Fd-3m spinel structure by x-ray diffraction (XRD). Further, nanocrystalline nature and morphology were analyzed by scanning electron microscopy (SEM). Among thermal properties, thermogravimetric analysis (TGA) revealed that the (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide is thermally stable up to a temperature of 1200℃. Whereas phase evolution in (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide before and after sintering was analyzed through differential scanning calorimetry (DSC). Electrochemical studies of (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide consists of a comparison of thermodynamic and kinetic parameters of water and hydrazine hydrate oxidation. Values of activation energy for water oxidation (9.31 kJ mol-1) and hydrazine hydrate oxidation (13.93 kJ mol-1) reveal that (Be,Mg,Ca,Sr,Zn,Ni)3O4 high entropy oxide is catalytically more active towards water oxidation as compared to that of hydrazine hydrate oxidation. Electrochemical impedance spectroscopy is also performed to get insight into the kinetics of both types of reactions.

Fabrication of $Gd_2O_3:Eu^{3+}$ Nano Phosphor and Optical Characteristics for High Resolution Radiation Imaging (고해상도 방사선 영상을 위한 $Gd_2O_3:Eu^{3+}$ 나노 형광체 제조 및 광학적 특성)

  • Kim, So-Yeong;Kang, Sang-Sik;Park, Ji-Koon;Cha, Byung-Youl;Choe, Chi-Won;Lee, Hyung-Won;Nam, Sang-Hee
    • Journal of Biomedical Engineering Research
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    • v.28 no.1
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    • pp.148-152
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    • 2007
  • In this paper, we have synthesized $Gd_2O_3:Eu^{3+}$ nano phosphor particle using a low temperature solution-combustion method. We have investigated the structure and the luminescent characteristic as the sintering temperature and europium concentration. From XRD(X-ray diffraction) and SEM(scanning electron microscope) results, we have verified that the phosphor particle was fabricated a spherical shape with $30{\sim}40nm$ particle size. From the photoluminescence results, the strong peak exhibits at 611 um and the luminescent intensity depends on europium concentration. $Gd_2O_3:Eu$ fine phosphor particle has shown excellent luminescent efficiency at 5 wt% of europium concentration. The phosphors calcinated at $500^{\circ}C$ have possessed the x-ray peaks corresponding to the cubic phase of $Gd_2O_3$. As calcinations temperature increased to $700^{\circ}C$, the new monoclinic phase has identified except cubic patterns. From the luminescent decay time measurements, mean lifetimes were $2.3{\sim}2.6ms$ relatively higher than conventional bulk phosphors. These results indicate that $Gd_2O_3:Eu$ nano phosphor is possible for the operation at the low x-ray dose, therefore, the application as medical imaging detector.

Crystallization Behavior and Electrical Properties of BNN Thin Films by IBSD Process

  • Lou, Jun-Hui;Jang, Jae-Hoon;Lee, Hee-Young;Cho, Sang-Hee
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2004.07b
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    • pp.960-964
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    • 2004
  • [ $Ba_2NaNb_5O_{15}$ ](BNN) thin films have been prepared by the ion beam sputter deposition (IBSD) method on Pt coated Si substrate at temperature as low as $600^{\circ}C$ XRD, SEM were used to investigate the crystallization and microstructure of the films. It was found that the films were crack-free and uniform in microstructure. The electric properties of thin films were carried out by observation of D-E hysteresis loop, dielectric constant and leakage current. It was found the deposition rate strongly influenced the phase formation of the films, where the phase of $BaNb_2O_6$ was always formed when the deposition rate was high. However, the single phase (tungsten bronze structure ) BNN thin film was obtained with the deposition rate as low as $22{\AA}/min$. The remanent polarization Pr and dielectric constant are about 1-2 ${\mu}C/cm^2$ and $100\sim200$, respectively. It was also founded the electric properties of thin films were influenced by the deposition rate. The Pr and dielectric constant of films increased with the decrease of deposition rate. The effects of annealing temperature and annealing time to the crystallization behavior of films were studied. The crystallization of thin film started at about $600^{\circ}C$. The adequate crystallization was gotten at the temperature of $650^{\circ}C$ when the annealing time is 0.5 hour or at the temperature of $600^{\circ}C$ when the annealing time is long as 6 hours.

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Synthesis and Characterization of Fe Doped TiO2 Nanoparticles by a Sol-Gel and Hydrothermal Process

  • Kim, Hyun-Ju;Jeong, Kwang-Jin;Bae, Dong-Sik
    • Korean Journal of Materials Research
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    • v.22 no.5
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    • pp.249-252
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    • 2012
  • Fe doped $TiO_2$ nanoparticles were prepared under high temperature and pressure conditions by mixture of metal nitrate solution and $TiO_2$ sol. Fe doped $TiO_2$ particles were reacted in the temperature range of 170 to $200^{\circ}C$ for 6 h. The microstructure and phase of the synthesized Fe doped $TiO_2$ nanoparticles were studied by SEM (FE-SEM), TEM, and XRD. Thermal properties of the synthesized Fe doped $TiO_2$ nanoparticles were studied by TG-DTA analysis. TEM and X-ray diffraction pattern shows that the synthesized Fe doped $TiO_2$ nanoparticles were crystalline. The average size and distribution of the synthesized Fe doped $TiO_2$ nanoparticles were about 10 nm and narrow, respectively. The average size of the synthesized Fe doped $TiO_2$ nanoparticles increased as the reaction temperature increased. The overall reduction in weight of Fe doped $TiO_2$ nanoparticles was about 16% up to ${\sim}700^{\circ}C$; water of crystallization was dehydrated at $271^{\circ}C$. The transition of Fe doped $TiO_2$ nanoparticle phase from anatase to rutile occurred at almost $561^{\circ}C$. The amount of rutile phase of the synthesized Fe doped $TiO_2$ nanoparticles increased with decreasing Fe concentration. The effects of synthesis parameters, such as the concentration of the starting solution and the reaction temperature, are discussed.

Synthesis and Characterization of BaTiO3 Powder by Solid State Method (고상반응법을 이용한 BaTiO3 합성 및 특성 평가)

  • Kim, Yong Jin;Choi, Moon Hee;Shin, Hyo Soon;Ju, Byeong-Kwon;Chun, Myoung Pyo
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.33 no.6
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    • pp.483-489
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    • 2020
  • BaTiO3 powder was synthesized by a solid-state reaction using BaCO3 and TiO2. Different calcination temperatures (800℃, 850℃, 900℃, and 950℃) were set to investigate their effects on the properties of BaTiO3 powder. The synthesized BaTiO3 phase was confirmed to be a single phase by XRD, and the tetragonality (c/a) and crystallite size were calculated. Thereafter, each calcinated BaTiO3 was sintered at five different sintering temperatures (1,100℃, 1,150℃, 1,200℃, 1,250℃, and 1,300℃), and the tetragonality, density, porosity, dielectric constant, and grain size were measured. As the calcination temperature increased, the tetragonality and crystallite size also increased, to 1.008 and 66 nm, respectively, at 950℃. Moreover, most pellets showed increased density, dielectric constant, and tetragonality as the sintering temperature increased up to 1,250℃; the same parameters slightly decreased at 1,300℃. It is noteworthy that the tetragonality of BaTiO3 at 1,250℃ exhibits a very high c/a value of 1.0084. In addition, the grain size and dielectric constant measured near the Curie temperature increased as the sintering temperature increased.

Peeling Behavior of Backsheet according to Surface Temperature of Photovoltaic Module (태양광 모듈 표면 온도 제어에 따른 백시트 박리 거동)

  • Kim, Jeong-Hun;Lee, Jun-Kyu;Ahn, Young-Soo;Yeo, Jeong-Gu;Lee, Jin-Seok;Kang, Gi-Hwan;Cho, Churl-Hee
    • Korean Journal of Materials Research
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    • v.29 no.11
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    • pp.703-708
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    • 2019
  • In this study, we investigate the relationship between the peeling behavior of the backsheet of a photovoltaic(PV) module and its surface temperature in order facilitate removal of the backsheet from the PV module. At low temperatures, the backsheet does not peel off whereas, at high temperatures, part of the backsheet remains on the surface of the PV module after the peeling process. The backsheet material remaining on the surface of the PV module is confirmed by X-ray diffraction(XRD) analysis to be poly-ethylene(PE). Differential scanning calorimetry(DSC) is also performed to investigate the interfacial characteristics of the layers of the PV module. In particular, DSC provides the melting temperature($T_m$) of laminated ethylene vinyl acetate(EVA) and of the backsheet on the PV module. It is found that the backsheet does not peel off below the $T_m$ of ethylene of EVA, while the PE layer of the backsheet remains on the surface of the PV module above the $T_m$ of the PE. Thus, the backsheet is best removed at a temperature between the $T_m$ of ethylene and that of PE layer.

High-temperature Thermal Decomposition of Cs-adsorbed CHA-Cs and CHA-PCFC-Cs Zeolite System, and Sr-adsorbed 4A-Sr and BaA-Sr Zeolite System (Cs-흡착 CHA-Cs 및 CHA-PCFC-Cs 제올라이트계와 Sr-흡착 4A-Sr 및 BaA-Sr 제올라이트계의 고온 열분해)

  • Lee, Eil-Hee;Kim, Ji-Min;Kim, Hyung-Ju;Kim, Ik-Soo;Chung, Dong-Yong;Kim, Kwang-Wook;Lee, Keun-Young;Seo, Bum-Kyoung
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.16 no.1
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    • pp.49-58
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    • 2018
  • For the immobilization of high-radioactive nuclides such as Cs and Sr by high-temperature thermal decomposition, this study was carried out to investigate the phase transformation with calcined temperature by using TGA (thermogravimetric analysis) and XRD (X-ray diffraction) in the Cs-adsorbed CHA (chabazite zeolite of K type)-Cs and CHA-PCFC (potassium cobalt ferrocyanide)-Cs zeolite system, and Sr-adsorbed 4A-Sr and BaA-Sr zeolite system, respectively. In the case of CHA-Cs zeolite system, the structure of CHA-Cs remained at up to $900^{\circ}C$ and recrystallized to pollucite ($CsAlSi_2O_6$) at $1,100^{\circ}C$ after undergoing amorphous phase at $1,000^{\circ}C$. However, the CHA-CFC-Cs zeolite system retained the CHA-PCFC-Cs structure up to $700^{\circ}C$, but its structure collapsed in $900{\sim}1,000^{\circ}C$, and then transformed to amorphous phase, and recrystallized to pollucite at $1,100^{\circ}C$. In the case of 4A-Sr zeolite system, on the other hand, the structure of 4A-Sr maintained up to $700^{\circ}C$ and its phase transformed to amorphous at $800^{\circ}C$, and recrystallized to Sr-feldspar ($SrAl_2Si_2O_8$, hexagonal) at $900^{\circ}C$ and to $SrAl_2Si_2O_8$ (triclinic) at $1,100^{\circ}C$. However, the BaA-Sr zeolite system structure began to break down at below $500^{\circ}C$, and then transformed to amorphous phase in $500{\sim}900^{\circ}C$ and recrystallized to Ba/Sr-feldspar (coexistence of $Ba_{0.9}Sr_{0.1}Al_2Si_2O_8$ and $Ba_{0.5}Sr_{0.5}Al_2Si_2O_8$) at $1,100^{\circ}C$. All of the above zeolite systems recrystallized to mineral phase through the dehydration/(decomposition) ${\rightarrow}$ amorphous ${\rightarrow}$ recrystallization with increasing temperature. Although further study of the volatility and leachability of Cs and Sr in the high-temperature thermal decomposition process is required, Cs and Sr adsorbed in each zeolite system are mineralized as pollucite, Sr-feldspar and Ba/Sr-feldspar. Therefore, Cs and Sr seen to be able to completely immobilize in the calcining wasteform/(solidified wasteform).