• Title/Summary/Keyword: XRD 분석

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X-선 회절분석을 이용한 일라이트-스멕타이트 기본입자의 적층성에 관한 연구

  • 강일모;문희수
    • Proceedings of the Mineralogical Society of Korea Conference
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    • 2003.05a
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    • pp.10-10
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    • 2003
  • 일라이트-스멕타이트 혼합층광물(I-S)은 열역학적으로 상호 대립적인 두 가지 모델로 이해되고 있다. 첫째, MacEwan 결정자 모델은 I-S를 5-20개의 스멕타이트와 일라이트 층으로 구성된 결정자로 해석한다. 이러한 모델은 분산과 재응집 과정을 기초로 하는 X-선 회절분석(XRD)에서 기인한 것으로 Reynolds의 XRD 모델과 동일하다. 둘째, 기본입자 모델은 I-S를 물리적으로 분리될 수 있는 최소 입자인 기본입자가 $c^{*-}$축 방향으로 응집된 응집체로 해석한다. 이러한 모델은 분산 과정을 기초로 하는 주사전자현미경(TEM) 관찰에서 기인한 모델이다. 강일모 등(2002)은 이 두 가지 모델을 비교함으로써 1< $N_{F}$<100/% $S_{XRD}$ ( $N_{F}$=평균 기본입자 층개수, %$S_{XRD}$=XRD 분석을 통하여 측정된 팽창성)을 도출하였다. 이 식은 기본입자모델과 Eberl & Srodon(1988)이 제시한 최대 팽창성(%$S_{MAX}$)을 동시에 해석할 수 있게 해준다. %$S_{MAX}$는 XRD 모델에서는 고려하지 않는 I-S 결정자 상$\cdot$하부에 존재하는 두 개의 0.5nm 규산염층을 하나의 스멕타이트 층으로 간주하여 얻어진 팽창성이다. Srodon et al.(1992)은 %$S_{MAX}$=100/ $N_{F}$을 제시하였으며, 강일모 등(2002)은 %$S_{MAX}$는 기하학적으로 기본입자가 무한적층을 하였을 때 관찰되는 %$S_{XRD}$와 동일함을 밝힌 바 있다. 만약, XRD 분석을 위한 시료 준비과정에서 I-S 결정자가 분산되었다가 재응집을 한다면, XRD에서 관찰되는 결과는 일차적으로 기본입자의 적층성에 영향을 받게 된다. 따라서, 기본 입자의 적층성은 XRD 분석을 이용하여 I-S 구조를 해석하는데 매우 중요한 요인이다. 본 연구는 기본입자의 적층성을 정량화하기 위해 %$S_{XRD}$=A/ $N_{F}$ (0$S_{MAX}$=100/ $N_{F}$로부터 얼마나 벗어나 있는가는 지시해 준다 금성산화산암복합체에서 산출되는 11개 I-S 시료와 14개의 Drits et al.(1998) 자료로부터 1nA=-0.14 $N_{F}$+4.7의 실험식을 도출할 수 있었으며, 기본입자의 적층성은 일차적으로 기본입자의 두께에 의해 영향을 받는 것으로 관찰되었다. Nadeau(1985)는 기본입자두께분포로부터 I-S 결정자의 팽창성을 측정하기 위하여 Ps=$\Sigma$p(N)/N을 제시하였다(Ps=스멕타이트 층 비율, N=기본 입자 층개수, p(N)=N의 확율). 그러나 위식은 실질적으로 %$S_{MAX}$를 제공해주기 때문에 %$S_{XRD}$를 유추하는데는 부적합하다. 본 연구는 이를 변형하여 Ps=$\Sigma$p(N)A(N)/N을 제시하였다(A(N)=N에 대한 A값). 위의 실험식을 사용하여 헝가리산 Zempleni 시료(15%$S_{XRD}$)의 기본입자분포로부터 %$S_{XRD}$를 계산한 결과, 16%$S_{XRD}$의 결과값을 얻을 수 있었다. 따라서, 본 연구에서 도출한 관계식들이 유효함을 확인할 수 있었다.계식들이 유효함을 확인할 수 있었다.

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Quntitative Analysis of Calcium Carbonate Polymorphs by Peak Area of XRD (XRD 피크 면적을 이용한 탄산칼슘 결정 형태의 정량분석)

  • Bak, Young-Cheol
    • Korean Chemical Engineering Research
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    • v.60 no.4
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    • pp.564-573
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    • 2022
  • Calcium carbonate (CaCO3) exhibits three polymorphs: calcite with arhombohedral, vaterite with a spherical, and aragonite with a needle-like structure. Qualitative and quantitative analyses of the morphology of CaCO3 are very important to investigate the synthesis of single-crystal vaterite and aragonite. In this work, the polymorphs of calcium carbonate were quantitatively analyzed using XRD. Pure vaterite and pure aragonite were synthesized and the peak distribution of a single phase was analyzed. The vaterite fraction of a mixture of calcite and vaterite was calculated based on the intensity of a specific diffraction peak, and compared to the results based on the peak area. The mean value of fsV (the correction factor for the peak area of vaterite) was 0.654. The phase analysis of calcite-aragonite mixtures was performed, and the mean value of fsA (the correction factor for the peak area of aragonite) was obtained as 0.6713. Using these factors, Eq. (24)~Eq. (32) for the quantitative analysis based on the total peak area of XRD were derived to calculate the phase contents of ternary phase CaCO3. And three-component XRD section was defined considering overlapping sections.

A study on the nature of needle-like inclusions in corundum crystals (커런덤의 침상내포물 본질에 관한 연구)

  • 배상덕;김상기;최종건;김판채
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.14 no.3
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    • pp.101-104
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    • 2004
  • It was realized that MC-XRD is useful for phase analyzing of inclusions in crystals because it can focus the X-Ray beam to the small particles sized dozens of $\mu\textrm{m}$ with high S/N ratio. By using this MC-XRD, needle-like inclusions which are seen generally in corundum crystals known as rutile was found to be the iron titanium oxide and iron oxide which has the chemical composition of $Fe_2TiO_4,\; Fe_2TiO_5,\; Fe_2O_3$respectively

A study of semi-quantification of the Friedel's salt using the X-ray diffraction method in concrete (콘크리트 내 Friedel염의 XRD를 이용한 반정량적 측정기법에 관한 연구)

  • Lee, Ho-Jae;Lee, Jang-Hwa;Kim, Do-Gyeum
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.33-38
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    • 2012
  • Despite the importance of chloride binding, it is very difficult to measure the binding capacity, in particular, for the concrete body in an existing structure: in fact, the measurement procedure for chloride binding is much influenced by the environmental condition such as temperature, fineness of sample and pore water extraction techniques. The present study concerns the quantification of the binding capacity of chloride ions in concrete using the X-ray diffraction (XRD) technique. Once the binding isotherm of chlorides was determined by the Langmuir isotherm, as a function of the W/C, curing age and binder type, the generation of bound chlorides (i.e. Friedel's salt) was simultaneously ensured by the XRD technique. The amount of bound chloride was then determined by analyzing the peak intensity for the bound chlorides in the XRD curve. It was found that an increase in the curing age and a decrease in the W/C resulted in an increase in the binding capacity.

In situ Electric-Field-Dependent X-Ray Diffraction Experiments for Ferroelectric Ceramics (강유전 세라믹의 전기장 인가에 따른 in situ X-선 회절 실험)

  • Choi, Jin San;Kim, Tae Heon;Ahn, Chang Won
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.35 no.5
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    • pp.431-438
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    • 2022
  • In functional materials, in situ experimental techniques as a function of external stimulus (e.g., electric field, magnetic field, light, etc.) or changes in ambient environments (e.g., temperature, humidity, pressure, etc.) are highly essential for analyzing how the physical properties of target materials are activated/evolved by the given stimulation. In particular, in situ electric-field-dependent X-ray diffraction (XRD) measurements have been extensively utilized for understanding the underlying mechanisms of the emerging electromechanical responses to external electric field in various ferroelectric, piezoelectric, and electrostrictive materials. This tutorial article briefly introduces basic principles/key concepts of in situ electric-field-dependent XRD analysis using a lab-scale XRD machine. We anticipate that the in situ XRD method provides a practical tool to systematically identify/monitor a structural modification of various electromechanical materials driven by applying an external electric field.

Mineralogical Properties of Asian Dust in April 6 and 15, 2018, Korea (2018년 4월 6일과 15일 황사의 광물학적 특성)

  • Jeong, Gi Young
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.2
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    • pp.103-111
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    • 2018
  • Mineralogical properties of two Asian dust (Hwangsa) samples collected during dust events in April 6 and 15, 2018 were examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD analyses showed that Asian dusts were dominated by phyllosilicates (62 wt%) comprising illite-smectite series clay minerals (ISCMs) (55%), chlorite (3%) and kaolinite (4%). Nonphyllosilicate minerals were quartz (18%), plagioclase (9%), K-feldspar (3%), calcite (3%), and gypsum (2-4%). Mineral compositions determined by SEM chemical analyses were consistent with XRD data. ISCMs occur as submicron grains forming aggregate particles or coating coarse mineral grains such as quartz, plagioclase, K-feldspar, chlorite, and calcite. The ISCMs are often associated with calcite nanofibers and gypsum blades. Mineralogical properties of 2018 dusts were similar to those of previous dusts although clay contents were higher than that of coarse 2012 dust.

Estimation Study of Firing Temperature for Fired Clay Brick Relics Excavated from Buddhist Temple in Karatepa Using Analytical Method of High Temperature X-ray Diffraction (고온 XRD 분석법을 이용한 카라테파 불교사원 출토 점토벽돌의 소성온도 추정연구)

  • Han, Min Su;Lee, Jang Jon;Kim, Jae Hwan
    • Journal of Conservation Science
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    • v.32 no.4
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    • pp.511-520
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    • 2016
  • The purpose of this study was to estimate the firing temperature of fired clay brick by applying high temperature X-ray diffraction(XRD) analysis. The clay bricks, which were excavated from a Buddhist temple in Karatepa, Uzbekistan were composed of quartz, plagioclase, alkali feldspar, mica, chlorite, limestone, hornblende, etc. Some clay bricks contained gypsum, which was presumed to have been used to improve the adhesive strength of the brick. Estimating the firing temperature using a geologic thermometer, the UZ-1 sample was identified as being in the quartz, plagioclase, pyroxene series, and the firing temperature was estimated to be $900-1200^{\circ}C$. On the other hand, applying the high temperature XRD method to the UZ-5 sample, it was found that the limestone was destroyed at $1000^{\circ}C$ and the diffraction peak of chlorite was weakened at $1050^{\circ}C$. Moreover, pyroxene series minerals developed at $1050^{\circ}C$ in the reproduction experiment. These results indicate that the clay bricks used in the temple were produced in a kiln that reached a temperature of more than $1000^{\circ}C$. Thus, high temperature XRD analysis can more accurately estimate firing temperatures as compared to the firing temperature mineral identification method and it can be used to determine the creation and extinction temperature range of minerals.

Characterization of relationship between particle size and powder properties for $BaTiO_3$ ($BaTiO_3$의 입도와 분체특성과의 상관 관계 연구)

  • Chun, M.P.;Cho, J.H.;Kim, B.I.
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.15 no.6
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    • pp.244-251
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    • 2005
  • The relationship between particle size of hydro-thermally synthesized barium titanate powders (BT01, BT02, BT03, BT04, BT05) and the powder properties was investigated by means of particle size, specific surface area, zeta potential, XPS, XRD and SEM. Particle size determined by laser light scattering is closely related with specific surface area and the tetragonality (c/a) obtained from XRD. The specific surface area of the samples inversely decreased with increasing particle size except BT03 powder. BT03 sample showed higher surface area than BT04 sample of equivalent particle size, which was attributed mostly to the agglomeration of particles in terms of SEM image and XRD analysis. Zeta potential increased with increasing particle size with the exception of BT02 and BT03 which showed larger minus value of zeta potential in comparison with other BT powders. Beta potential results of BT02 and BT03 are considered to be related with the dissolution of $Ba^{2+}$ ion in these powers which was examined by XPS.

Synthesis of Nickel Oxide (NiO) nanoparticles using nickel(II) nitrate hexahydrate as a precursor (Nickel(II) nitrate hexahydrate를 전구체로 사용한 산화니켈(NiO) 나노입자의 합성)

  • Soo-Jong Kim
    • The Journal of the Convergence on Culture Technology
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    • v.9 no.3
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    • pp.593-599
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    • 2023
  • Nickel oxide (NiO) nanoparticles were successfully synthesized by a simple liquid phase process for producing ceramics powder using a precursor impregnated with a nickel(II) nitrate hexahydrate aqueous solution in an industrial pulp. The microfibrile structure of the precursor impregnated with nickel nitrate hexahydrate aqueous solution was confirmed by scanning electron microscope (SEM), and the crystal structure and particle size of nickel oxide (NiO) particles produced as the heat treatment temperature of the precursor were analyzed by X-ray diffraction (XRD) and SEM. As a result, it was confirmed through XRD and SEM analysis that the temperature at which the organic material of the precursor is completely thermally decomposed was 495-500℃, and the size and crystallinity of the nickel oxide particles produced increased as the heat treatment temperature increased. The size of the nickel oxide particles obtained by heat treatment at 500-800℃ for 1 hour was 50-200 nm. It was confirmed by XRD and SEM analysis that a NiO crystal phase was formed at a heat treatment temperature of 380℃, only a single NiO phase existed until 800℃.