• Title/Summary/Keyword: powder X-ray diffraction

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An Study on the Structure of Maghemite(${\gamma}$-Fe$_2$O$_3$) I -Rietveld Analysis of Powder XRD Patterns- (마게마이트(${\gamma}$-Fe$_2$O$_3$)대한 연구 I -분말 X-선 회절무늬의 Rietveld 분석-)

  • 신형섭
    • Journal of the Korean Ceramic Society
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    • v.35 no.10
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    • pp.1113-1119
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    • 1998
  • Crystal structure of needle-shaped maghemite(${\gamma}$-{{{{ { {Fe }_{2 }O }_{3 } }}) has been studied by the Rieveld analysis of powder X-ray diffraction patterns. The tetragonal space group P41,.3212 and cubic space group P41,.32 have been have been used for the refinement of X-ray diffraction patterns. The crystal system of maghemite is closed to tetragonal more than cubic. The tetragonal lattice parameters are a=8.3460$\AA$ and c=25.034$\AA$ The standard X-ray diffraction pattern of the tetragonal maghemite analyzed with space group P41,.3212 is proposed.

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X-Ray Diffraction Patterns and Acid Consuming Capacity of Aluminum Hydroxide Gel. (수산화알루미늄.겔의 X선회절상과 제산도)

  • 조문혜
    • YAKHAK HOEJI
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    • v.8 no.2
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    • pp.37-44
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    • 1964
  • The relationships involving acid-consuming capacity and X-ray powder diffraction patterns of aluminum hydroxide gel were studied. The aging of antacid efficacy of aluminum hydroxide gel has also been characterized by using X-ray powder diffraction. The acid-consuming capacity decreased with progress of crystallization from amorphous alumino gel, and it was found that aged product at 80.deg. C had crystal structure of bohmite (.alpha.-Al.sub 2/O$_{2}$(OH)$_{2}$). It was also noted that the rate of aging decreased with decreasing pH of aluminum hydroxide gel.

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X-Ray Diffraction Analysis of Various Calcium Silicate-Based Materials

  • An, So-Youn;Lee, Myung-Jin;Shim, Youn-Soo
    • Journal of dental hygiene science
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    • v.22 no.3
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    • pp.191-198
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    • 2022
  • Background: The purpose of this study was to evaluate the composition of the crystal phases of various calcium silicate-based materials (CSMs): ProRoot white MTA (mineral trioxide aggregate) (WMTA), Ortho MTA (OM), Endocem MTA (EM), Retro MTA (RM), Endocem Zr (EN-Z), BiodentineTM (BD), EZ-sealTM (EZ), and OrthoMTA III (OM3). Methods: In a sample holder, 5 g of the powder sample was placed and the top surface of the material was packed flat using a sterilized glass slide. The prepared slides were mounted on an X-ray diffraction (XRD) instrument (D8 Advance; Bruker AXS GmbH, Germany). The X-ray beam 2θ angle range was set at 10~90° and scanned at 1.2° per minute. The Cu X-ray source set to operate at 40 kV and 40 mA in the continuous mode. The peaks in the diffraction pattern of each sample were analyzed using the software Diffrac (version 2.1). Then, the peaks were compared and matched with those of standard materials in the corresponding Powder Diffraction File (PDF-2, JCPDS International Center for Diffraction Data). A powder samples of the materials were analyzed using XRD and the peaks in diffraction pattern were compared to the Powder Diffraction File data. Results: Eight CSMs showed a similar diffraction pattern because their main component was calcium silicate. Eight CSMs showed similar diffraction peaks because calcium silicate was their main component. Two components were observed to have been added as radiopacifiers: bismuth oxide was detected in WMTA, OM, and EM while zirconium oxide was detected in RM, EN-Z, BD, EZ, and OM3. Unusual patterns were detected for the new material, OM3, which had strong peaks at low angles. Conclusion: It was caused by the presence of Brushite, which is believed to have resulted in crystal growth in a particular direction for a specific purpose.

Synchrotron X-ray Powder Diffraction Study of CFC-13 Loaded Zeolite LSX (제올라이트 LSX에서의 CFC-13 분자체 흡착에 관한 결정학적 연구)

  • Lee, Yong-Jae;Lee, Jong-Won;Yoon, Ji-Ho
    • Journal of the Mineralogical Society of Korea
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    • v.21 no.3
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    • pp.307-312
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    • 2008
  • Rietveld analysis using synchrotron X-ray powder diffraction data collected at 15 K reveals that CFC-13 ($CF_{3}Cl;$ chlorotrifluoromethane) sorbed on Na,K-LSX binds through fluorine to sodium ions around the single 6-ring aperture in the supcrgage.

The Structure Determination of La2/3-xLi3x1/3-2xTiO3 by the Powder Neutron and X-ray Diffraction

  • Kang, Eun-Tae;Kwon, Young-Jean
    • Journal of the Korean Ceramic Society
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    • v.40 no.6
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    • pp.513-518
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    • 2003
  • La/sub 2/3-x/Li/sub 3x/□/sub 1/3-2x/TiO₃ compounds with x=0.13 and 0.12 were prepared by slow cooling (x=0.13) and rapid quenching (x=0.12) into the liquid nitrogen after sintering at 1350℃ for 6 h. Their crystal structure has been determined by Rietveld refinement of both the powder neutron and X-ray diffraction data. From neutron diffraction data, we found that the main phase was not tetragonal (P4/mmm), but trigonal (R3cH). The refinement of neutron diffraction for the slow cooled samples were in a good agreement with a new model; a mixture of trigonal (R3cH, 45.7 wt%), tetragonal (p4/mmm, 37.0 wt%), and Li/sub 0.57/Ti/sub 0.86/O₂(pbnm, 17.2 wt%), but the quenched sample was found not to contain tetragonal (p4/mmm). X-ray diffraction data couldn't be well fitted because of the Poor scattering factor of lithium ions and the similar reflection patterns among trigonal (R3cH), tetragonal (p4/mmm), and cubic (Pm3m). We also knew that one transport bottlenecks is destroyed by one La vacancy in the case of trigonal (R3cH).

High Pressure X-Ray Diffraction Study on a Goethite using Synchrotron Radiation (방사광을 이용한 괴타이트에 대한 고압 X-선 회절연구)

  • 김영호;이지은
    • Journal of the Mineralogical Society of Korea
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    • v.10 no.2
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    • pp.75-81
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    • 1997
  • High pressure X-ray diffraction study was carried out on a natural FeO(OH)-goethite to investigate its compressibility at room temperature. Energy dispersive X-ray diffraction method was employed using Mao-Bell type diamond anvil cell with Synchrotron Radiation. MgO powder was compressed together with goethite for the high pressure determinations. Bulk modullus was determined to be 147.9 GPa by the Birch-Murnaghan equation of state under assumption of K0' of 4. This value was subjected to compare with its structural analogs and related materials.

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A Study of Mineral Quantification on Clay-Rich Rocks (점토질 암석의 광물정량 분석법 연구)

  • Byeong-Kook, Son;Gi-O, An
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.4
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    • pp.431-445
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    • 2022
  • A quantitative phase analysis method of X-ray powder diffraction was studied to determine the mineral content of clay-rich rocks practically as well as effectively. For quantitative X-ray powder diffraction analysis of the clay-rich rocks, it is necessary to prepare whole-rock powder samples with a random orientation by side mounting method. In addition, for the identification of the clay minerals in the rock, it is required to prepare an oriented mount specimen with a clay particle size of 2 ㎛ or less, ethylene glycol treatment, and heat treatment. RIR (reference intensity ratio) and Rietveld method were used for the quantitative analysis of the clay-rich rocks. It was possible to obtain the total clay and the non-clay minerals contents from the whole-rock X-ray diffraction profiles using the RIR values. In addition, it was possible to calculate the relative content of each clay mineral from the oriented X-ray diffraction profiles of the clay particle size and assign it to the total clay. In the Rietveld method of whole-rock X-ray diffraction, effective quantitative values were obtained from the Rietveld diffraction patterns excluded the region of less than 10 degrees (2θ). Similar quantitative values were shown in not only the RIR but the Rietveld methods. Therefore, the analysis results indicate a possibility of a routine quantitative analysis of clay-rich rocks in the laboratory. However, quantitative analysis of clay minerals is still a challenge because there are numerous varieties of clay minerals with different chemical and structural characteristics.

Synthesis, Structures and Properties of Two Metal-organic Frameworks Derived from 3-Nitro-1,2-benzenedicarboxylic Acid

  • Xu, Wen-Jia;Zhang, Ling-Yu;Tang, Jin-Niu;Wang, Dai-Yin;Pan, Gang-Hong;Feng, Yu
    • Bulletin of the Korean Chemical Society
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    • v.34 no.8
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    • pp.2375-2380
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    • 2013
  • Two metal-organic frameworks based on the connectivity co-effect between rigid benzenedicarboxylic acid and bridging ligand have been synthesized $[Zn_2(3-NO_2-bdc)_2(4,4'-bpy)_2H_2O]_n$ (1), $[Co(3-NO_2-bdc)(4,4'-bpy)H_2O]_n$ (2) (where $3-NO_2-bdcH_2$ = 3-nitro-1,2-benzenedicarboxylic acid, 4,4'-bpy = 4,4'-bipyridine). The two novel complexes were characterized by IR spectrum, elemental analysis, fluorescent properties, thermogravimetric analysis, single-crystal X-ray diffraction and powder X-ray diffraction (PXRD). X-ray structure analysis reveals that 1 and 2 are two-dimensional (2D) network structures. Complex 1 and complex 2 belong to triclinic crystal with P-1 space group. The luminescence measurements reveal that two complexes exhibit good fluorescent emissions in the solid state at room temperature. Also, thermal decomposition process and powder X-ray diffraction of complexes were investigated.

A Study of Practical and Optimized Mineral Quantification (실용적이고 최적화된 광물정량분석법 연구)

  • Son, Byeong-Kook;An, Gi-O
    • Korean Journal of Mineralogy and Petrology
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    • v.34 no.4
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    • pp.227-239
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    • 2021
  • A practical and effective method of X-ray powder diffraction analysis was investigated for quantitative analysis of the mineral content of natural samples. Sample mounting experiments were conducted to select the best randomly oriented powder sample mount. A comparative experiment was also made between a reference intensity ratio (RIR) method, which compares a single peak intensity with standard material, and the Rietveld method, which calculates a full X-ray diffraction pattern, to search for the effective method of mineral quantification. In addition, samples containing amorphous minerals were quantitatively analyzed by the Rietveld method and the efficiency was reviewed. As a result of the study, the optimal random orientation could be reached by the side mounting method. The Rietveld method using the full pattern of X-ray diffraction was more suitable for mineral quantitative analysis, rather than the RIR method using a specific peak. However, either method could depend on the analyst's experience in addition to analytical technique. Moreover, amorphous minerals can be quantitatively analyzed by the Rietveld method, and the analysis results make the geological analysis possible.

The Synthesis of Maghemite and Hematite Nanospheres

  • Dar, Mushtaq Ahmad;Ansari, Shafeeque G.;Wahab, Rizwan;Kim, Young-Soon;Shin, Hyung-Shik
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 2006.09a
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    • pp.472-473
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    • 2006
  • Maghemite and hematite nanospheres were synthesized by using the Sol-gel technique. The structural properties of these nanosphere powders were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), and pore size distribution. Hematite phase shows crystalline structures. The mean particle size that resulted from BET and XRD analyses were 4.9 nm and 2 nm. It can be seen from transmission electron microscopy that the size of the particles are very small which is in good agreement with the FESEM and the X-ray diffraction. The BET and pore size method were employed for specific surface area determination.

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