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

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Synthesis and Characterization of the Layered Type $(C_nH_{2n+1}NH_3)_2PbCl_4$ System

  • Lee, Su Jong;Kim, Gye Ya;O, Eun Ju;Kim, Gyu Hong;Yeo, Cheol Hyeon
    • Bulletin of the Korean Chemical Society
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    • v.21 no.3
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    • pp.317-320
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    • 2000
  • Layered $K_2NiF_4$type ($C_nH_{2n+1}NH_3)_2PbCl_4$(n=6, 8 and 10) system, or alkylammonium tetrachloroplumbate compound, has been synthesized from $PbCl_2$ and $C_nH_{2n+1}NH_3Cl$ solutions under argon ambient pressure for 12hrs at $90^{\circ}C$. The crystal structure of the compound has been analyzed using X-ray powder diffaction in the range of $5^{\circ}{\leq}2{\theta}{\leq}55^{\circ}$, and all samples assigned to an orthorhombic system. Local distances of the Pb-Cl bond have been determined by Pb $L_{III}$-edge extended X-ray absorption fine structure (EXAFS) spectroscopy. The vibration modes of alkylammonium chains and the absorpton peaks of an excition have been examined by FT-IR and UV-Vis. reflectance spectra, respectively. The phase transition temperatures of the compounds have been studied by using DSC. According to the thermal analysis, two phase transition temperatures have been observed in the compositons of n=8 and 10.

Applications of Ar Gas Cluster Ion Beam Sputtering to Ta2O5 thin films on SiO2/Si (100)

  • Park, Chanae;Chae, HongChol;Kang, Hee Jae
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.119-119
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    • 2015
  • Ion beam sputtering has been widely used in Secondary Ion Mass Spectrometry (SIMS), X-ray Photoelectron Spectroscopy (XPS), and Auger Electron Spectroscopy (AES) for depth profile or surface cleaning. However, mainly due to severe matrix effects such as surface composition change from its original composition and damage of the surface generated by ion beam bombardment, conventional sputtering skills using mono-atomic primary ions with energy ranging from a few hundred to a thousand volts are not sufficient for the practical surface analysis of next-generation organic/inorganic device materials characterization. Therefore, minimization of the surface matrix effects caused by the ion beam sputtering is one of the key factors in surface analysis. In this work, the electronic structure of a $Ta_2O_5$ thin film on $SiO_2/Si$ (100) after Ar Gas Cluster Ion Beam (GCIB) sputtering was investigated using X-ray photoemission spectroscopy and compared with those obtained via mono-atomic Ar ion beam sputtering. The Ar ion sputtering had a great deal of influence on the electronic structure of the oxide thin film. Ar GCIB sputtering without sample rotation also affected the electronic structure of the oxide thin film. However, Ar GCIB sputtering during sample rotation did not exhibit any significant transition of the electronic structure of the $Ta_2O_5$ thin films. Our results showed that Ar GCIB can be useful for potential applications of oxide materials with sample rotation.

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A Study on the S-block Structure in Hexagonal Ferrites (육방정 페라이트의 S-block 구조에 대한 연구)

  • 신형섭;이종협;권순주
    • Journal of the Korean Ceramic Society
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    • v.31 no.1
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    • pp.62-68
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    • 1994
  • It is compared the structures of the S-block in the Ba-Co-Zn Y-type hexagonal ferrites (Ba2Co2-xZnxFe12O22, x=0~2) and the Co-Zn spinel ferrites (Co1-xZnxFe2O4, x=0~1) expressed by a hexagonal axis system (space group R3m). The structures have been refined with a Rietveld analysis of the powder X-ray diffraction pattern with high precision (Rwp<0.13, RI<0.03). The overal dimension of the S-block is slightly different from the 1/3 of a hexagonal spinel unit cell as follow: 1.6~2.0% longer c-axis, 1.3~1.6% shorter a-axis and about 1% smaller volume. Upto Zn:Co=1:1 in the Ba-Co-Zn Y-type hexagonal ferrites, the zinc substitute primarily the tetrahedral sites in the S-block. Beyond that the zinc seems to go into the T-block as well.

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Morphological Analysis of Hydraulically Stimulated Fractures by Deep-Learning Segmentation Method (딥러닝 기반 균열 추출 기법을 통한 수압 파쇄 균열 형상 분석)

  • Park, Jimin;Kim, Kwang Yeom ;Yun, Tae Sup
    • Journal of the Korean Geotechnical Society
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    • v.39 no.8
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    • pp.17-28
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    • 2023
  • Laboratory-scale hydraulic fracturing experiments were conducted on granite specimens at various viscosities and injection rates of the fracturing fluid. A series of cross-sectional computed tomography (CT) images of fractured specimens was obtained via a three-dimensional X-ray CT imaging method. Pixel-level fracture segmentation of the CT images was conducted using a convolutional neural network (CNN)-based Nested U-Net model structure. Compared with traditional image processing methods, the CNN-based model showed a better performance in the extraction of thin and complex fractures. These extracted fractures extracted were reconstructed in three dimensions and morphologically analyzed based on their fracture volume, aperture, tortuosity, and surface roughness. The fracture volume and aperture increased with the increase in viscosity of the fracturing fluid, while the tortuosity and roughness of the fracture surface decreased. The findings also confirmed the anisotropic tortuosity and roughness of the fracture surface. In this study, a CNN-based model was used to perform accurate fracture segmentation, and quantitative analysis of hydraulic stimulated fractures was conducted successfully.

INFLUENCE of SHS-CATALYSTS PHASE STRUCTURE on FORMING PRODUCTS of PARTIAL METHANE OXIDATION

  • Mironenko, A.V.;Rahmetkaliev, K.N.;Mansurov, Z.A.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2000.07a
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    • pp.278-283
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    • 2000
  • The activity of catalysts obtained by self-propagating high temperature synthesis in reaction of partial methane oxidation at atmospheric pressure was investigated. Basing on the compared results of X-ray analysis and gas chromatography analysis of reaction products, the dependence of compounds formation on the phase concentrations in the studied catalyst samples was found.

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Characterization of Nitrogen-Doped $TiO_2$ Thin Films Prepared by Metalorganic Chemical Vapor Deposition (유기금속 화학 기상증착법으로 실리콘 기판위에 증착된 질소치환 $TiO_2$ 박막의 특성분석)

  • 이동헌;조용수;이월인;이전국;정형진
    • Journal of the Korean Ceramic Society
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    • v.31 no.12
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    • pp.1577-1587
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    • 1994
  • TiO2 thin films with the substitution of oxygen with nitrogen were deposited on silicon substrate by metalorganic chemical vapor deposition (MOCVD) using Ti(OCH(CH3)2)4 (titanium tetraisopropoxide, TTIP) and N2O as source materials. X-ray diffraction (XRD) results indicated that the crystal structure of the deposited thin films was anatase TiO2 with only (101) plane observed at the deposition temperatures of 36$0^{\circ}C$ and 38$0^{\circ}C$, and with (101) and (200) plane at above 40$0^{\circ}C$. Raman spectroscopic results indicated that the crystal structure was anatase TiO2 in accordance with the XRD results without any rutile, fcc TiN, or hcp TiN structure. No fundamental difference was observed with temperature increase, but the peak intensity at 194.5 cm-1 increased with strong intensity at 143.0 cm-1 for all samples. The crystalline size of the films varied from 49.2 nm to 63.9 nm with increasing temperature as determined by slow-scan XRD experiments. The refractive index of the films increased from 2.40 to 2.55 as temperature increased. X-ray photoelectron spectroscopy (XPS) study showed only Ti 2s, Ti 2p, C 1s, O 1s and O 2s peaks at the surface of the film. The composition of the surface was estimated to be TiO1.98 from the quatitative analysis. In the bulk of the film Ti 2s, Ti 2p, O 1s, O 2s, N 1s and N 2s were detected, and Ti-N bonding was observed due to the substitution of oxygen with nitrogen. A satellite structure was observed in the Ti 2p due to the Ti-N bonding, and the composition of titanium nitride was determined to be about TiN1.0 from the position of the binding energy of Ti-N 2p3/2 and the quatitative analysis. The spectrum of Ti 2p energy level could be the sum of a 4, 5, or 6 Gaussian curve reconstruction, and the case of the sum of the 6 Gaussian curve reconstruction was physically most meaningful. From the results of Auger electron spectroscopy (AES), it was known that the composition was not varied significantly throughout the whole thickness of the film, and silicon oxide was not observed at the interface between the film and the substrate. The composition of the film was possible (TiO2)1-x.(TiN)x or TiO2-2xNx and in this experimental condition x was found to be about 0.21-0.16.

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A Study on the 3D Imaging of High Temperature Heating Cement Paste and the Analysis of Variation of the Pore Structure (고온 가열 시멘트 페이스트의 3D 영상화 및 세공구조 변화 분석에 관한 연구)

  • Kim, Min-Hyouck;Lee, Gun-Cheol
    • Proceedings of the Korean Institute of Building Construction Conference
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    • 2020.11a
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    • pp.147-148
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    • 2020
  • In case of high temperature damage such as fire, the durability of concrete is reduced due to the collapse of internal pore tissue. Therefore, in this paper, we are going to analyze the pore structure of cement paste hardening agent using MIP analysis and build up 3D data produced using X-ray CT tomography. The test specimen is made of cement paste from W/C 0.4. As the temperature of heating increased, the amount of air gap and the diameter of air gap in cement paste increased. It is judged that the air gap structure inside cement collapsed due to the evaporation of the hydrate, gel count, capillary water, etc. inside the cement due to the high temperature.

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Electronic Structure of Ce-doped ZrO2 Film: Study of DFT Calculation and Photoelectron Spectroscopy

  • Jeong, Kwang Sik;Song, Jinho;Lim, Donghyuck;Kim, Hyungsub;Cho, Mann-Ho
    • Applied Science and Convergence Technology
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    • v.25 no.1
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    • pp.19-24
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    • 2016
  • In this study, we evaluated the change of electronic structure during redox process in cerium-doped $ZrO_2$ grown by sol gel method. By sol-gel method, we could obtain cerium-doped $ZrO_2$ in high oxygen partial pressure and low temperature. After post annealing process in nitrogen ambient, the film is deoxidized. We used spectroscopic and theoretical methods to analysis change of electronic structure. X-ray absorption spectroscopy (XAS) for O K1-edge and Density Functional Theory (DFT) calculation using VASP code were performed to verify the electronic structure of the film. Also, high resolution x-ray photoelectron spectroscopy (HRXPS) for Ce 3d was carried out to confirm chemical bond of cerium doped $ZrO_2$. Through the investigation of the electronic structure, we verified as followings. (1) During reduction process, binding energy of oxygen is increase. Simultaneously, oxidation state of cerium was change to 4+ to 3+. (2) Cerium 4+ and cerium 3+ states were generated at different energy level. (3) Absorption states in O K edge were mainly originated by Ce 4+ $f_0$ and Ce 3+, while occupied states in valance band were mainly originated from Ce 4+ $f_2$.

Ferroelectric Properties of Bi3.25La0.75Ti3O12 Thin Films with Eu Contents for Non-volatile Memory Device Application (비휘발성 메모리 소자응용을 위한 Eu 첨가량에 따른 BET 박막의 강유전 특성)

  • Kim, Kyoung-Tae;Kim, Jong-Gyu;Woo, Jong-Chang;Kim, Gwan-Ha;Kim, Chang-Il
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.20 no.3
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    • pp.223-227
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    • 2007
  • The effect of Eu contents on the ferroelectric properties of $Bi_{4-x}Eu_xTi_3 O_{12}$ (BET) thin films has been investigated. Bismuth Europium titanate thin films with a Eu contents were prepared on the $Pt/Ti/SiO_2/Si$ substrate by metal-organic decomposition technique. The structure and the morphology of the films were analyzed using X-ray diffraction (XRD) and field emission scanning microscopy (FE-SEM), respectively. From the XRD analysis, it was found that BET thin films have polycrystalline structure, and the layered-perovskite phase is obtained when the Eu contents exceeds 0.2 (x > 0.2). Also, the ferroelectric characteristics of the BET thin films were found to be dependent on the Eu content. Particularly, the BET films doped with x = 0.75 show better ferroelectric properties (remanent polarization 2Pr = 60.99 C/$cm^2$ and only a little polarization fatigue up to $3.5{\times}10^9$ bipolar switching cycling) than those doped with other Eu contents.

Influence analysis of heat treatment on crystalline structure of ZrO2-SiO2 glass precursor synthesized by sol-gel method (졸-겔법으로 합성된 ZrO2-SiO2 유리전구체의 결정화구조에 미치는 열처리의 영향분석)

  • Chun, Kyung-Soo
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.3-6
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    • 2012
  • $xZrO_2-(1-x)SiO_2$ glass precursor with relatively high concentration of zirconium propoxide in metal alkoxide solution was obtained by sol-gel method and then heated at various temperature from 500 to $1,100^{\circ}C$ to investigate the effect of the thermal treatment on the crystalline structure of the glass precursor. Based on X-ray diffraction analysis, the crystalline peak was started to develop at temperature higher than $600^{\circ}C$, and the crystalline phase was considerably increased at $850^{\circ}C$ or higher. With increasing the thermal treatment temperature, the characteristic peaks, such as baddelyite, tetragonal-$ZrO_2$ and zircon, was shown at $35^{\circ}$, $50^{\circ}$ and $60^{\circ}$ of $2{\theta}$.