• Title/Summary/Keyword: X-ray microscopy

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Physicochemical and Electrochemical Characteristics of Carbon Nanomaterials and Carbon Nanomaterial-Silicon Composites

  • Kim, Soo-Jin;Hyun, Yura;Lee, Chang-Seop
    • Journal of the Korean Chemical Society
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    • v.60 no.5
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    • pp.299-309
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    • 2016
  • In this study, the physicochemical and electrochemical properties of carbon nanomaterials and synthesized nano-carbon/Si composites were studied. The nano-carbon/Si composites were ball-milled to a nano size and coated with pyrolytic carbon using Chemical Vapor Deposition (CVD). They were then finely mixed with respective nano-carbon materials. The physicochemical properties of samples were analyzed using Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), Raman spectroscopy, X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), and surface area analyzer. The electrochemical characteristics were investigated using the galvanostatic charge-discharge and cyclic voltammetry (CV) measurements. Three-electrode cells were fabricated using the carbon nanomaterials and nano-carbon/Si composites as anode materials and LiPF6 and LiClO4 as electrolytes of Li secondary batteries. Reversibility using LiClO4 as an electrolyte was superior to that of LiPF6 as the electrolyte. The initial discharge capacities of nano-carbon/Si composites were increased compared to the initial discharge capacities of nano-carbon materials.

X-ray Diffraction Studies of Poly(aryl ether ether ketone) Fibers with Different Degrees of Crystallinity and Orientation

  • Karacan Ismail
    • Fibers and Polymers
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    • v.6 no.3
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    • pp.206-218
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    • 2005
  • Structural studies of series of 'as spun' and drawn PEEK fibers have been carried out using X-ray diffraction and optical microscopy techniques. The analysis of results suggest that fibers produced at a constant draw ratio with increasing draw temperatures show enhanced orientation and crystalline behaviour. The resolved equatorial and meridional traces provide additional structural parameters in terms of crystallinity, crystallite size, and crystallite thickness. It is concluded that drawing at a temperature below $T_g(i.e.,\;144^{\circ}C)$ results in poorly oriented non-crystalline materials, whereas drawing above $T_g$ results in highly oriented semi crystalline materials. Additional drawing proved to increase the overall orientation with slight improvements in lateral order of the chain molecules. Quantitative analysis revealed that the crystallite size increases with increasing drawing temperature. The results also revealed the increased crystallite size upon additional drawing. Crystalline orientation parameter, $_c$, suggests almost perfect orientation. In all cases, the amorphous orientation is found to be lower than the overall orientation parameter obtained from the optical birefringence. As a result of additional drawing, crystalline orientation was found to increase slightly but the increase in the orientation of non-crystalline material was found to be substantial. An average crystalline density was determined from the orthorhombic unit cell dimensions. It was found to vary as a result of processing conditions. It was also found that the value of the maximum birefringence shows heavy dependence on the chain conformation.

Metal-insulator Transition in $(Sr_{0.75},\;La_{0.25})TiO_3$ Ultra-thin Films

  • Choi, Jae-Du;Choi, Eui-Young;Lee, Yun-Sang;Lee, Jai-Chan
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.10a
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    • pp.19.2-19.2
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    • 2011
  • The $(Sr_{0.75},\;La_{0.25})TiO_3$ (SLTO) ultra-thin films with various thicknesses have been grown on Ti-O terminated $SrTiO_3$(100) substrate using Laser-Molecular Beam Epitaxy (Laser MBE). By monitoring the in-situ specular spot intensity oscillation of reflection high energy electron diffraction (RHEED), we controlled the layer-by-layer film growth. The film structure and topography were verified by atomic force microscopy (AFM) and high resolution thin film x-ray diffraction by the synchrotron x-ray radiation. We have also investigated the electronic band structure using x-ray absorption spectroscopy (XAS). The ultra thin SLTO film exhibits thickness driven metal-insulator transition around 8 unit cell thickness when the film thickness progressively reduced to 2 unit cell. The SLTO thin films with an insulating character showed band splitting in Ti $L_3-L_2$ edge XAS spectrum which is attributed to Ti 3d band splitting. This narrow d band splitting could drive the metal-insulator transition along with Anderson Localization. In optical conductivity, we have found the spectral weight transfer from coherent part to incoherent part when the film thickness was reduced. This result indicates the possibility of enhanced electron correlation in ultra thin films.

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Wood Identification of Historical Architecture in Korea by Synchrotron X-ray Microtomography-Based Three-Dimensional Microstructural Imaging

  • HWANG, Sung-Wook;TAZURU, Suyako;SUGIYAMA, Junji
    • Journal of the Korean Wood Science and Technology
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    • v.48 no.3
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    • pp.283-290
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    • 2020
  • For visual inspection-based wood identification, optical microscopy techniques typically require a relatively large sample size, and a scanning electron microscope requires a clean surface. These novel techniques experience limitations for objects with highly limited sampling capabilities such as important and registered wooden cultural properties. Synchrotron X-ray microtomography (SR-µCT) has been suggested as an effective alternative to avoid such limitations and various other imaging issues. In this study, four pieces of wood fragments from wooden members used in the Manseru pavilion of Bongjeongsa temple in Andong, Korea, wereused for identification. Three-dimensional microstructural images were reconstructed from these small wood samples using SR-µCT at SPring-8. From the analysis of the reconstructed images, the samples were identified as Zelkova serrata, Quercus sect. Cerris, and Pinus koraiensis. The images displayed sufficient spatial resolution to clearly observe the anatomical features of each species. In addition, the three-dimensional imaging allowed unlimited image processing.

Synchrotron X-ray Reflectivity Studies on Nanoporous Low Dielectric Constant Organosilicate Thin Films

  • Oh, Weon-Tae;Park, Yeong-Do;Hwang, Yong-Taek;Ree, Moon-Hor
    • Bulletin of the Korean Chemical Society
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    • v.28 no.12
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    • pp.2481-2485
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    • 2007
  • Spatially resolved, quantitative, non-destructive analysis using synchrotron x-ray reflectivity (XR) with subnano-scale resolution was successfully performed on the nanoporous organosilicate thin films for low dielectric applications. The structural information of porous thin films, which were prepared with polymethylsilsesquioxane and thermally labile 4-armed, star-shaped poly(ε-caprolactone) (PCL) composites, were characterized in terms of the laterally averaged electron density profile along with a film thickness as well as a total thickness. The thermal process used in this work caused to efficiently undergo sacrificial thermal degradation, generating closed nanopores in the film. The resultant nanoporous films became homogeneous, well-defined structure with a thin skin layer and low surface roughness. The average electron density of the calcined film reduced with increase of the initial porogen loading, and finally leaded to corresponding porosity ranged from 0 to 22.8% over the porogen loading range of 0-30 wt%. In addition to XR analysis, the surface and the inner structures of films are investigated and discussed with atomic force and scanning electron microscopy images.

Electron Crystallography of CaMoO4 Using High Voltage Electron Microscopy

  • Kim, Jin-Gyu;Choi, Joo-Hyoung;Jeong, Jong-Man;Kim, Young-Min;Suh, Il-Hwan;Kim, Jong-Pil;Kim, Youn-Joong
    • Bulletin of the Korean Chemical Society
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    • v.28 no.3
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    • pp.391-396
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    • 2007
  • The three-dimensional structure of an inorganic crystal, CaMoO4 (space group I 41/a, a = 5.198(69) A and c = 11.458(41) A), was determined by electron crystallography utilizing a high voltage electron microscope. An initial structure of CaMoO4 was determined with 3-D electron diffraction patterns. This structure was refined by crystallographic image processing of high resolution TEM images. X-ray crystallography of the same material was performed to evaluate the accuracy of the TEM structure determination. The cell parameters of CaMoO4 determined by electron crystallography coincide with the X-ray crystallography result to within 0.033-0.040 A, while the atomic coordinates were determined to within 0.072 A.

Soft X-ray Nano-spectroscopy for Electronic Structures of Transition Metal Oxide Nano-structures

  • Oshima, Masaharu
    • Applied Science and Convergence Technology
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    • v.23 no.6
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    • pp.317-327
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    • 2014
  • In order to develop nano-devices with much lower power consumption for beyond-CMOS applications, the fundamental understanding and precise control of the electronic properties of ultrathin transition metal oxide (TMO) films are strongly required. The metal-insulator transition (MIT) is not only an important issue in solid state physics, but also a useful phenomenon for device applications like switching or memory devices. For potential use in such application, the electronic structures of MIT, observed for TMO nano-structures, have been investigated using a synchrotron radiation angle-resolved photoelectron spectroscopy system combined with a laser molecular beam epitaxy chamber and a scanning photoelectron microscopy system with 70 nm spatial resolution. In this review article, electronic structures revealed by soft X-ray nano-spectroscopy are presented for i) polarity-dependent MIT and thickness-dependent MIT of TMO ultrathin films of $LaAlO_3/SrTiO_3$ and $SrVO_3/SrTiO_3$, respectively, and ii) electric field-induced MIT of TMO nano-structures showing resistance switching behaviors due to interfacial redox reactions and/or filamentary path formation. These electronic structures have been successfully correlated with the electrical properties of nano-structured films and nano-devices.

Enhanced Optical Properties of Au Nanoparticles/ZnO Nanowires Fabiracted by X-ray Induced Wet Process

  • Lee, Mu-Seong;Gang, Hyeon-Cheol
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.318.1-318.1
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    • 2014
  • Metal nano-crystals have been received much attentions owing to their excellent catalytic property and surface plasmon effect. In the last decade, many studies on synthesizing well-dispersive nanoparticles and on understanding their distinct physical properties have been performed. There were tremendous reports revealing the electrochemical activities and enhancement of surface plasmonic effect were dependent mainly on the size, shape, and composition. So far, most fabrication methods have been based on vacuum based deposition techniques, such as chemical vapor deposition and electron-beam evaporation, and then annealed them to transform into the nanoparticles. Recently, there were several reports regarding to the photoinduced nano-crystal synthesis as an effective way to produce the metal nanoparticles. In this study, we report synchrotron x-ray mediated synthesis of Au nanoparticles on ZnO nanowires. ZnO nanowires were fabricated by hydrothermal method, and then they were dip into a solution having Au clusters. Detailed structural evolution of Au nanoparticles was investigated using scanning electron microscopy and photoluminescence measurements. The results on formation of well-dispersive Au nanoparticles on ZnO nanowires will be presented.

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Characterizations of Thermal Compound Using CuO Particles Grown by Wet Oxidation Method (습식 산화법으로 성장된 산화구리입자를 이용한 방열 컴파운드 제조 및 특성 연구)

  • Lee, Dong Woo;Um, Chang Hyun;Chu, Jae Uk
    • Korean Journal of Materials Research
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    • v.27 no.4
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    • pp.221-228
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    • 2017
  • Various morphologies of copper oxide (CuO) have been considered to be of both fundamental and practical importance in the field of electronic materials. In this study, using Cu ($0.1{\mu}m$ and $7{\mu}m$) particles, flake-type CuO particles were grown via a wet oxidation method for 5min and 60min at $75^{\circ}C$. Using the prepared CuO, AlN, and silicone base as reagents, thermal interface material (TIM) compounds were synthesized using a high speed paste mixer. The properties of the thermal compounds prepared using the CuO particles were observed by thermal conductivity and breakdown voltage measurement. Most importantly, the volume of thermal compounds created using CuO particles grown from $0.1{\mu}m$ Cu particles increased by 192.5 % and 125 % depending on the growth time. The composition of CuO was confirmed by X-ray diffraction (XRD) analysis; cross sections of the grown CuO particles were observed using focused ion beam (FIB), field emission scanning electron microscopy (FE-SEM), and energy dispersive analysis by X-ray (EDAX). In addition, the thermal compound dispersion of the Cu and Al elements were observed by X-ray elemental mapping.

Spectral Analysis of $CO_2$ Corrosion Product Scales on 13Cr Tubing Steel

  • Lin, Guan-fa;Xu, Xun-yuan;Bai, Zhen-quan;Feng, Yao-rong
    • Corrosion Science and Technology
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    • v.7 no.4
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    • pp.201-207
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    • 2008
  • $CO_2$ corrosion product scales formed on 13 Cr tubing steel in autoclave and in the simulated corrosion environment of oil field are investigated in the paper. The surface and cross-section profiles of the scales were observed by scanning electron microscopy (SEM), the chemical compositions of the scales were analyzed using energy dispersion analyzer of X-ray (EDAX), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) to confirm the corrosion mechanism of the 13 Cr steel in the simulated $CO_2$ corrosion environment. The results show that the corrosion scales are formed by the way of fashion corrosion, consist mainly of four elements, i.e. Fe, Cr, C and O, and with a double-layer structure, in which the surface layer is constituted of bulky and incompact crystals of $FeCO_3$, and the inner layer is composed of compact fine $FeCO_3$ crystals and amorphous $Cr(OH)_3$. Because of the characteristics of compactness and ionic permeating selectivity of the inner layer of the corrosion product scales, 13 Cr steel is more resistant in $CO_2$ corrosion environment.