• Title/Summary/Keyword: X-ray Diffractometer

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Modification of conventional X-ray diffractometer for the measurement of phase distribution in a narrow region

  • Park, Yang-Soon;Han, Sun-Ho;Kim, Jong-Goo;Jee, Kwang-Yong;Kim, Won-Ho
    • Analytical Science and Technology
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    • v.19 no.5
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    • pp.407-414
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    • 2006
  • An X-ray diffractometer for spatially resolved X-ray diffraction measurements was developed to identify phase in the narrow (micron-scaled) region of high burn-up fuels and some nuclear materials. The micro-XRD was composed of an X-ray microbeam alignment system and a sample micro translation system instead of a normal slit and a fixed sample stage in a commercial XRD. The X-ray microbeam alignment system was fabricated with a microbeam concentrator having two Ni deposited mirrors, a vertical positioner, and a tilt table for the generation of a concentrated microbeam. The sample micro translation system was made with a sample holder and a horizontal translator, allowing movement of a specimen at $5{\mu}m$ steps. The angular intensity profile of the microbeam generated through a concentrator was symmetric and not distorted. The size of the microbeam was $4,000{\times}20{\mu}m$ and the spatial resolution of the beam was $47{\mu}m$ at the sample position. When the diffraction peaks were measured for a $UO_2$ pellet specimen by this system, the reproducibility ($2{\Theta}={\pm}0.01^{\circ}$) of the peaks was as good as a conventional X-ray diffractometer. For the cross section of oxidized titanium metal, not only $TiO_2$ in an outer layer but also TiO near an oxide-metal interface was observed.

Phase identification and degree of orientation measurements far fine-grained rock forming minerals using micro-area X-ray diffractometer -$Al_{2}SiO_{5}$ Polymorphs- (미소부 X-선 회절분석기를 이용한 미립조암광물의 상동정 및 배향도 측정 -$Al_{2}SiO_{5}$ 3상다형-)

  • 박찬수;김형식
    • The Journal of the Petrological Society of Korea
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    • v.9 no.4
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    • pp.205-210
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    • 2000
  • Measurements of phase identification and degree of orientation for fine-grained (about 0.3 mm in diameter) minerals in rock samples performed by micro-area X-ray diffractometer.$Al_{2}SiO_{5}$ polymorphs (andalusite, kyanite and sillimanite) were chosen for the measurements and target minerals were existed on thin sections. Micro-area X-ray diffractometer is composed of 3(${\omega}\;{\chi}\;{\phi}$)-circle oscillating goniometer and position sensitive proportional counter (PSPC). $CuK_{\alpha}$ radiation was used as X-ray source and a pin hole ($50\;\mu\textrm{m}$$ in diameter) collimator was selected to focus radiation X-ray onto the target minerals. Phase identification and diffracted X-ray peak indexing were carried out by 3(${\omega}\;{\chi}\;{\phi}$)-circle oscillation measurement. Then, 2(${\omega}\;{\phi}$)-circle oscillation measurement was made for the purpose of searching the prevailing lattice plane of the minerals on thin section surface. Finally, for a selected peak by 2-circle oscillation measurement, X-ray pole figure measurement was executed for the purpose of check the degree of orientation of the single lattice direction and examine its pole distribution. As a result of 3-circle oscillation measurement, it was possible that phase identification among $Al_{2}SiO_{5}$ polymorphs. And from the results of 2-circle oscillation measurement and X-ray pole figure measurement, we recognized that poles of andalusite (122), kyanite (200) and sillimanite (310) lattice plances were well developed with direction normal to each mineral surface plane respectively. Therfore, the measurements used with micro-area X-ray diffractometer in this study will be a useful tool of phase identification and degree of orientation measurement for fine-grained rock forming minerals.

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Development and Evaluation of Parallel Beam Optic for X-ray (엑스선용 평행빔 광학소자 개발 및 평가)

  • Park, Byunghun;Cho, Hyungwook;Chon, Kwonsu
    • Journal of the Korean Society of Radiology
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    • v.6 no.6
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    • pp.477-481
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    • 2012
  • An X-ray diffractometer which has various X-ray optics can give qualitative and quantitative information for a sample using a nondestructive analysis method. A parallel beam optic passes the parallel beam and removes divergent beam generated from an X-ray tube. The parallel beam optic used in the X-ray diffractometer was fabricated by wire cut and grading of stainless steel plates and was evaluated its performance using an X-ray imaging system. The measured parallelization of 6.6 mrad for the fabricated the parallel beam optic was a very close to the expected value of 6 mrad. An X-ray imaging technique for evaluating the parallel beam optics can estimate parallelization for each plate and can be used to other X-ray optics.

Improvement of Measurement Accuracy by Correcting Systematic Error Associated with the X-ray Diffractometer (X-선 회절 장비의 기계적 오차 수정을 통한 분석 정확도 향상)

  • Choi, Dooho
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.18 no.10
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    • pp.97-101
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    • 2017
  • X-ray diffractometers are used to characterize material properties, such as the phase, texture, lattice constant and residual stress, based on the diffracted beams obtained from specimens. Quantitative analyses using X-rays are typically conducted by measuring the peak positions of the diffracted beams. However, the long-term use of the diffractomer, like any other machine, results in errors associated with the mechanical parts, which can deteriorate the accuracy of the quantitative analyses. In this study, the process of correcting systematic errors in the $2{\theta}$ range of $30{\sim}90^{\circ}$ is discussed, for which strain-free Si powders from NIST were used as the standard specimens. For the evaluation of the impact of such error correction, we conducted a quantitative analysis of the true lattice constant for tungsten thin films.

Crystal Structure of $KD_2PO_4$: Neutron and X-ray Diffraction Studies ($KD_2PO_4$의 결정구조: 중성자와 X-선 회절에 의한 연구)

  • 김신애;심해섭;이창희
    • Korean Journal of Crystallography
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    • v.11 no.3
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    • pp.162-166
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    • 2000
  • KD₂PO₄ single crystals were grown from D₂O with reagent KH₂PO₄ and the crystal structure was determined by X-ray and neutron diffraction methods. The crystals are tetragonal at room temperature, I42d, with lattice parameters of a=7.4633(7), c=6.9785(5) Å and Z=4. Intensity data were collected on an Enraf-nonius CAD4 diffractometer with a graphite monochromated MoK/sub α/ radiation (λ=0.7107Å) and on the neutron four circle single crystal diffractometer with Ge(331) monochromated neutron beam (λ=0.997Å). The structure was refined by full-matrix least-square to final R and wR values of 0.030 and 0.072, respectively, for 204 observed reflections with I>2σ(I) by X-ray diffraction and to final R=0.041 and wR=0.096 for 144 observed relfecdtions by neutron diffraction. The O…O distance of 2.516(4)Å obtained by X-ray diffraction is the same as that of 2.515(4)Å by neutron diffraction. On the other hand, the O-D/H distance of 0.84(4)Å by X-ray diffraction is considerably shorter than 1.029(7) Åby neutron diffraction. Hydrogen and deuterium can be readily distinguished by neutrons. In this crystal 66% of H-positions were substituted by D and the rest 34% occupied by H. The phase transition temperature of DKDP obtained with deuteration levels is f193K. This value agrees fairly well with the result of DSC measurement. The nuclear density distribution by neutron diffraction provides an observation of the disordered state of D/H in KD₂PO₄ at room temperature.

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Synthesis of Ultrathin Polymer Films by Self Assembly (자기 집합에 의한 고분자 초박막의 합성)

  • Shin, Jae Sup
    • Applied Chemistry for Engineering
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    • v.7 no.6
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    • pp.1142-1146
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    • 1996
  • Cholesterol-containing surfactant was synthesized, and it was sonicated with monomer in water to form a vesicle solution. This vesicle solution was dried to construct a membrane which had a molecular multilayer structure. Using UV irradiation the monomer in this membrane were polymerized, and then surfactant was extracted by organic solvent. Using a X-ray diffractometer, the thickness of one layer and the regularity of the multilayer were measured. And scanning electron microscopy was conducted for fractured polymer film.

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A Study on Material Properties and Fabrication of ITO Thin Films by Unbalanced-Magnet Structure in Magnetron Sputtering (DC 마그네트론 스파터링의 비대칭 자석강조에 의한 ITO 박막 제조 및 물성에 관한 연구)

  • 신성호;김현후;박광자
    • Electrical & Electronic Materials
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    • v.10 no.7
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    • pp.700-705
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    • 1997
  • Transparent conducting indium tin oxide (TC-ITO) thin films are deposited on soda lime glass by a dc magnetron sputtering technique having the unbalanced-magnet structure in order to improve the electrical/material characteristics and to avoid the surface damages. The material properties are measured by the x-ray diffractometer (XRD) and atomic force microscope (AFM). The (400) peak as the preferred orientation of <100> direction for ITO thin films is stabilized with the increase of substrate temperature. The surface roughness estimated by AFM 3D image at the substrate temperature of 40$0^{\circ}C$ is extremely uniform. The best resistivity of ITO films (5500 $\AA$ thick) at 40$0^{\circ}C$ is about 1.3$\times$10$^{-4}$ $\Omega$cm on the position of 4 cm from substrate center.

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The Result of the Pigment Analysis of the Mural in Ssangyeongchong (Tomb of Two Pillars) from Goguryeo (고구려(高句麗) 쌍영총(雙楹塚) 벽화(壁畫)의 안료분석(顔料分析))

  • Yu, Heisun
    • Conservation Science in Museum
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    • v.6
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    • pp.47-54
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    • 2005
  • The elements of the pigments used on the wall painting in Ssangyeongchong (Tomb of Two Pillars) from Goguryeo in the Nampo area of Pyeongyang were analyzed to confirm their mineral compositions and features of the painting. Specifically, the non-destructive X-ray fluorescence spectrometer (XRF) was used. On the other hand, the mineral composition of the background and pigment layers were analyzed using an X-ray diffractometer (XRD). The results of these analyses suggested that the lips of the characters in the painting were painted with HgS, and their faces, painted with HgS(Cinnabar/ vermilion) mixed with CaCO3. Note that lead white pigment [2PbCO3·Pb(OH)2] was found only on the bottom layer of the painting, indicating that the wall painting was likely to have been created using the Secco method.

Formation and Characterization of Silicon Carbide Whiskers by Acheson Method (에치슨법에 의한 탄화규소 휘스카의 성장과 특성분석)

  • 주한용;김형준
    • Journal of the Korean Ceramic Society
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    • v.27 no.1
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    • pp.136-146
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    • 1990
  • Whiskers of SiC were grown from the mixture of silica and graphite powders by Acheson method(direct heating method). The structrua, morphological and chemical characterizations have been performed by X-ray diffractometer(XRD), transmission electron microscopy(TEM), optical microscopy(OM), scanning electron microscopy(SEM), X-ray photoelectron spectroscopy(XPS) and energy dispersive spectrometer(EDS). The growth mechanism of SiC whiskers is also discussed.

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Crystal Structure Analysis of $LiN(D_xH_{1-x}){_4}SO_4$ by X-ray and Neutron Diffraction (X-선과 중성자 회절을 이용한 강유전체 단결정 $LiN(D_xH_{1-x}){_4}SO_4$의 결정구조 연구)

  • Kim, Shin-Ae;Kim, Seong-Hoon;So, Ji-Yong;Lee, Jeong-Soo;Lee, Chana-Hee
    • Journal of the Mineralogical Society of Korea
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    • v.20 no.4
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    • pp.351-356
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    • 2007
  • The crystal structure of $Li(ND_4)SO_4$ was analyzed by X-ray and neutron diffraction methods. The crystal is a deuterated $Li(NH_4)SO_4$ and one of the ferroelectric materials with hydrogen atoms. The crystal is orthorhombic at room temperature, $P2_1nb$, with lattice parameters of $a=5.2773(5)\;{\AA},\;b=9.1244(23)\;{\AA},\;c=8.7719(11)\;{\AA}$ and Z=4. Neutron intensity data were collected on the Four-Circle diffractometer (FCD) at HANARO in Korea Atomic Energy Research Institute and X-ray date were given by Prof. Y. Noda of Tohoku University Japan. The structure was refined by full-matrix least-square to final R value of 0.070 for 1450 observed reflections by X-ray diffraction and to final R=0.049 for 745 observed reflections by neutron diffraction. With X-ray data we obtained only one hydrogen atomic position. However, not only all atomic positions of four hydrogen atoms at $NH_4$ but also the occupation factors of D and H were refined with neutron data. From this results we obtained the average chemical structure of this sample, $LiND_{3.05}H_{0.95}SO_4$.