• Title/Summary/Keyword: X-ray structure analysis

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Magnetic Properties of Sn1-xFexO2 Thin Films and Powders Grown by Chemical Solution Method

  • Li, Yong-Hui;Shim, In-Bo;Kim, Chul-Sung
    • Journal of Magnetics
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    • v.14 no.4
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    • pp.161-164
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    • 2009
  • Iron-doped $Sn_{1-x}Fe_xO_2$ (x = 0.0, 0.05, 0.1, 0.2, 0.33) thin films on Si(100) substrates and powders were prepared by a chemical solution process. The x-ray diffraction (XRD) patterns of the $Sn_{1-x}Fe_xO_2$ thin films and powders showed a polycrystalline rutile tetragonal structure. Thermo gravimetric (TG) - differential thermal analysis (DTA) showed the final weight loss above $430{^{\circ}C}$ for all powder samples. According to XRD Rietveld refinement of the powders, the lattice parameters and unit cell volume decreased with increasing Fe content. The magnetic properties were characterized using a vibrating sample magnetometer (VSM) and M$\ddot{o}$ssbauer spectroscopy. The thin film samples with x = 0.1 and 0.2 showed paramagnetic properties but thin films with x = 0.33 exhibited ferromagnetic properties at room temperature. Mossbauer studies revealed the $Fe^{3+}$ valence state in the samples. The ferromagnetism in the samples can be interpreted in terms of the direct ferromagnetic coupling of ferric ions via an electron trapped in a bridging oxygen deficiency, which can be explained using the F-center exchange model.

Synthesis and Characteristics of the Organic Layered Structure Material of $(C_4H_9NH_3)_2Fe_xPb_1-xCl_4$

  • Jeong, Su Jin;In, Ri Ju;O, Eung Ju;Jo, Ung In;Kim, Gyu Hong;Yo, Cheol Hyeon
    • Bulletin of the Korean Chemical Society
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    • v.22 no.7
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    • pp.703-708
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    • 2001
  • K2NiF4-type organic-based perovskites of the (C4H9NH3)2FexPb1-xCl4 (x=0.00, 0.25, 0.50, and 0.75) system have been synthesized using a low-temperatu re solution method under a flowing argon gas. When stoichiometric butylamine, iron chloride, and lead chloride are mixed, a yellow solution are obtained from slow cooling of 90 to -10 $^{\circ}C.$ The final product is a plate-like yellow crystal. The X-ray crystallographic analysis has been carried out using XRD in the range of $5^{\circ}{\leq}$ 2${\theta}$ ${\leq}80^{\circ}.$ The local symmetry around the absorbing Pb atom of the samples has been determined by the EXAFS spectroscopic study. The crystals assign to orthorhombic system by the XRD analysis. The FT-IR spectra are analyzed in the range of 600 to 3300 cm-1 . DSC and TGA are measured to detect thermal stability between 30 and 300 $^{\circ}C.$ Two endothermic peaks are detected in all samples. The electrical conductivity has been measured using the four-probes technique for the (C4H9NH3)2FexPb1-xCl4 system in 300-460 K. Photoluminescence phenomenon was also investigated at room-temperature.

Irradiation enduced In-plane magnetization in Fe/MgO/Fe/Co multilayers

  • Singh, Jitendra Pal;Lim, Weon Cheol;Song, Jonghan;Kim, Jaeyeoul;Asokan, K.;Chae, Keun Hwa
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.188.1-188.1
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    • 2015
  • For present investigation Fe/MgO/Fe/Co multilayer stack is grown on Si substrate using e-beam evaporation in ultrahigh vacuum. This stack is irradiated perpendicularly by 120 MeV $Ag^{8+}$ at different fluences ranging from $1{\times}10^{11}$ to $1{\times}10^{13}ions/cm^2$ in high vacuum using 15UD Pelletron Accelerator at Inter University Accelerator Centre, New Delhi. Magnetic measurements carried out on pre and post irradiated stacks show significant changes in the shape of perpendicular hysteresis which is relevant with previous observation of re-orientation of magnetic moment along the direction of ion trajectory. However increase in plane squareness may be due to the modification of interface structure of stacks. X-ray reflectivity measurements show onset of interface roughness and interface mixing. X-ray diffraction measurements carried out using synchrotron radiation shows amorphous nature of MgO and Co layer in the stack. Peak corresponding body centered Fe [JCPDS-06-0696] is observed in X-ray diffraction pattern of pre and post irradiated stacks. Peak broadening shows granular nature of Fe layer. Estimated crystallite size is $22{\pm}1nm$ for pre-irradiated stack. Crystallite size first increases with irradiation then decreases. Structural quality of these stacks was further studied using transmission electron microscopic measurements. Thickness from these measurements are 54, 36, 23, 58 and 3 nm respectively for MgO, Fe, MgO, Fe+Co and Au layers in the stack. These measurements envisage poor crystallinity of different layers. Interfaces are not clear which indicate mixing at interface. With increase fluence mixing and diffusion was increased in the stack. X-ray absorption spectroscopic measurements carried out on these stacks show changes of Fe valence state after irradiation along with change of O(2p)-metal (3d) hybridized state. Valence state change predicts oxide formation at interface which causes enhanced in-plane magnetization.

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Production Techniques for the Metal Artifacts Excavated in Hasong-ri, Yeongwol and Their Conservation Treatment (영월 하송리 출토 금속유물 보존처리 및 제작기법 연구)

  • Lee, Byeong Hoon;Go, Hyeong Sun;Kim, Soo-Ki
    • Conservation Science in Museum
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    • v.21
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    • pp.53-66
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    • 2019
  • This study describes the processes undertaken for the conservation treatment of metal artifacts excavated in Hasong-ri, Yeongwol, Gangwon-do and the results of the related surface composition analysis. X-ray fluorescence analysis (XRF) was applied to analyze the surface composition of a small gilt-bronze wind chime, two clappers, and a small gourd-shaped bronze bottle. The gourd-shaped bronze bottle was investigated using radiography to examine its internal structure. The wind chime and clappers were excavated from the same location. A gilt layer was identified on the wind chime, but surface corrosion made it difficult to identify any such layers on the clappers. The element analysis revealed that the wind chime was made of bronze in a Cu-Sn-Pb ternary system and was gilt-plated using mercury amalgam. The clappers were made from copper with a small amount of gold detected, but did not show any evidence of mercury. Since a thick corrosion layer was affixed to the surface of each clapper, it was impossible to identify the surface composition and determine if the clappers had been gilded. It is possible that the gold detected from the clappers was a foreign substance or had detached from the giltbronze wind chime buried alongside them. The small gourd-shaped bronze bottle was investigated through surface element analysis and radiography to verify if it was a type of silver bottle used as currency during the Goryeo dynasty. The radiography photography identified that a small hole in the middle of the base had been stopped up. The general surface analysis did not detect silver, which suggests that the bottle was made of bronze instead and was not one of the silver bottles used as a means of currency.

Analysis of Porosity and Distribution of Pores in Rocks by Micro Focus X-Ray CT (미소 초점 X선 CT를 이용한 암석 내 공극의 분포 및 공극률 분석)

  • Jeong, Gyo-Cheol;Takahashi, Manabu
    • The Journal of Engineering Geology
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    • v.20 no.4
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    • pp.461-465
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    • 2010
  • Weathering and permeability in rocks play a very important role in underground disposal of radioactive waste and their long-term management as well as stability security of rock structures. Weathering and permeability of rocks are largely controlled by the characters of inner structures of rocks. In other words, weathering rate can be accelerated depending on the quantity of pore and microcrack in rocks. Quantitative evaluation of inner structures of rocks can serve as a tool that can assess the degree of weathering of rocks. Therefore it can be said that the understanding of three dimensional distribution of the inner structure of rocks is important for long-term management of rock structures. This study was performed to analyze three dimensional distribution of pore in rocks using Micro Focus X-ray CT on fresh granite and weathered granite from Korea. Results of the analysis clearly show distribution of pore and porosity of the inner rock.

Mechanistic investigations on emission characteristics from g-C3N4, gC3N4@Pt and g-C3N4@Ag nanostructures using X-ray absorption spectroscopy

  • Sharma, Aditya;Varshney, Mayora;Chae, Keun Hwa;Won, Sung Ok
    • Current Applied Physics
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    • v.18 no.11
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    • pp.1458-1464
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    • 2018
  • An improved method for the preparation of g-$C_3N_4$ is described. Currently, heating (> $400^{\circ}C$) of urea is the common method used for preparing the g-$C_3N_4$. We have found that sonication of melamine in $HNO_3$ solution, followed by washing with anhydrous ethanol, not only reduce the crystallite size of g-$C_3N_4$ but also facilitate intriguing electronic structure and photoluminescence (PL) properties. Moreover, loading of metal (Pt and Ag) nanoparticles, by applying the borohydride reduction method, has resulted in multicolor-emission from g-$C_3N_4$. With the help of PL spectra and local electronic structure study, at C K-edge, N K-edge, Pt L-edge and Ag K-edge by X-ray absorption spectroscopy (XAS), a precise mechanism of tunable luminescence is established. The PL mechanism ascribes the amendments in the transitions, via defect and/or metal states assimilation, between the ${\pi}^*$ states of tris-triazine ring of g-$C_3N_4$ and lone pair states of nitride. It is evidenced that interaction between the C/N 2p and metal 4d/5d orbitals of Ag/Pt has manifested a net detraction in the ${\delta}^*{\rightarrow}LP$ transitions and enhancement in the ${\pi}^*{\rightarrow}LP$ and ${\pi}^*{\rightarrow}{\pi}$ transitions, leading to broad PL spectra from g-$C_3N_4$ organic semiconductor compound.

Synthesis, Structure and Characterization of Nd2XCd2-3XSiO4 (0.01≤X≤0.21) Solid-Solutions (Nd2XCd2-3XSiO4 (0.01≤X≤0.21) 고용체의 합성과 구조 규명)

  • Ramesh, S.;Das, B.B.
    • Journal of the Korean Chemical Society
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    • v.55 no.3
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    • pp.502-508
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    • 2011
  • Synthesis of $Nd_{2x}Cd_{2-3x}SiO_4$ ($0.01{\leq}x{\leq}0.21$) [S1-S3: x=0.01, 0.11 and 0.21] solid solutions were prepared by solgel method. Powder x-ray diffraction (XRD) results show monoclinic unit cell with space group P21/m. The average crystallite sizes are found to be 20 to 45 nm. The Scanning Electron Microcopy (SEM) images show morphology of the sample is in globular nature. The energy dispersive analysis of x-rays (EDX) and X-ray mapping results confirmed that all the constituent elements of the composites were present and that were distributed in uniformly. The optical absorption band at ~750 nm was due to $^4I_{9/2}{\rightarrow}^4F_{7/2}+^4S_{3/2}$ transition optically active $Nd^{3+}$ ions. Electron Paramagnetic Resonance (EPR) lineshapes of S1-S3 at 10, 40, 77 and 300 K show a broad unresolved isotropic lineshapes were observed due to rapid spin lattice relaxation of $Nd^{3+}$.

Synthesis and structure analysis of the bis(dicyclohexylammonium) chromate dihydrate complex, [(C6H11)2NH2]2[CrO4]·2H2O

  • Kim, Chong-Hyeak;Moon, Hyoung-Sil;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.448-451
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    • 2007
  • A new bis(dicyclohexylammonium) chromate dihydrate complex, $[(C_6H_{11})_2NH_2]_2[CrO_4]{\cdot}2H_2O$, (I), has been synthesized and its structure analyzed by FT-IR, EDS, elemental analysis, ICP-AES, and single crystal X-ray diffraction methods. The Cr(VI) complex (I) is tetragonal system, I${\bar{4}}$2d space group with a = 12.5196(1), b = 12.5196(1), c = $17.3796(3){\AA}$, a = ${\beta}$ = ${\gamma}$ = $90^{\circ}$, V = $2724.09(6){\AA}^3$, Z = 4. The crystal structure of complex (I) consists of tetrahedral chromate $[CrO_4]^{2-}$ anion, two organic dicyclohexylammonium $[(C_6H_{11})_2NH_2]^+$ cations and two lattice water molecules. The chromate anion and protonated dicyclohexylammonium cation is mainly constructed through the ionic bond. The cyclohexylammonium rings of the dicyclohexylammonium cation take the chair form and vertical configuration with each other. The N-H${\cdot}$O and O-H${\cdot}$O hydrogen bond networks between the $N_{dicyclohexylammonium}$, $O_{water}$ and $O_{chromate}$ atom lead to self-assembled molecular conformation and stabilize the crystal structure.

Structural analysis of sialyltransferase PM0188 from Pasteurella multocida complexed with donor analogue and acceptor sugar

  • Kim, Dong-Uk;Yoo, Ji-Ho;Lee, Yong-Joo;Kim, Kwan-Soo;Cho, Hyun-Soo
    • BMB Reports
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    • v.41 no.1
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    • pp.48-54
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    • 2008
  • PM0188 is a newly identified sialyltransferase from P. multocida which transfers sialic acid from cytidine 5'-monophosphonuraminic acid (CMP-NeuAc) to an acceptor sugar. Although sialyltransferases are involved in important biological functions like cell-cell recognition, cell differentiation and receptor-ligand interactions, little is known about their catalytic mechanism. Here, we report the X-ray crystal structures of PM0188 in the presence of an acceptor sugar and a donor sugar analogue, revealing the precise mechanism of sialic acid transfer. Site-directed mutagenesis, kinetic assays, and structural analysis show that Asp141, His311, Glu338, Ser355 and Ser356 are important catalytic residues; Asp141 is especially crucial as it acts as a general base. These complex structures provide insights into the mechanism of sialyltransferases and the structure-based design of specific inhibitors.

A study of physical and chemical properties of internal accumulated material in water mains (상수관로 내부 오염물질의 물리화학적 특성 분석)

  • Bae, Cheol-Ho;Choi, Doo-Yong;Lee, Doo-Jin;Kim, Do-Hwan
    • Journal of Korean Society of Water and Wastewater
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    • v.28 no.5
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    • pp.589-600
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    • 2014
  • Tuberculation and slime accumulated in water mains play an important role in modifying water quality of drinking water. Therefore, in this study, it was investigated that what materials were accumulated, and what components were included in the tuberculation and slime of water mains. The Various tuberculation and slime sample were collected from the 12 water mains to analyze their physical and chemical properties and crystal structure. As a analysis method, VSS(Volatile suspended solid), SEM(scanning electron microscope), EDS(Energy Dispersive X-ray spectroscope), ICP(Inductively Coupled Plasma Mass Spectrometer) and XRD(X-Ray Diffractomete) were used. The results of analysis on the samples, the representative materials were verified such as iron corrosion products, the fine sand particles generated during backwash, fine particles of activated carbon, aluminum used in coagulation process, and manganese included in raw water.