• Title, Summary, Keyword: XRD

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Relationship between Expandability, MacEwan Crystallite Thickness, and Fundamental Particle Thickness in Illite-Smectite Mixed Layers (일라이트-스멕타이트 혼합층광물의 팽창성과 MacEwan 결정자 및 기본입자두께에 관한 연구)

  • 강일모;문희수;김재곤;송윤구
    • Journal of the Mineralogical Society of Korea
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    • v.15 no.2
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    • pp.95-103
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    • 2002
  • The object of this study was to interpret the ralationship between expandability (% $S_{XRD}$), MacEwan crystallite thickness ( $N_{CSD}$), and mean fundamental particle thickness ( $N_{F}$ ) in illite-semctite mixed layer (I-S), quantitatively. This interpretation was extracted from comparison of two structural models (MacEwan crystallite model and fundamental particle model) of I-S mixed layers. In I-S structure, % $S_{XRD}$, $N_{CSD}$, and $N_{F}$ are not independent parameters but are related to each others by particular geometric relations. % $S_{XRD}$ is dependent on $N_{CSD}$ by short-stack effect, whereas, % $S_{XRD}$ and $N_{F}$ have relation to smectite interlayer number (Ns)=( $N_{F-}$1)/(100%/% $S_{XRD-}$ $N_{F}$ . Therefore, % $S_{XRD}$ and $N_{F}$ should satisfy a specific physical condition, 1< $N_{F}$ <100%/% $S_{XRD}$, because $N_{s}$ is positive. Based on this condition, this study suggested % $S_{XRD}$ vs $N_{F}$ diagram which can be used to interpret % $S_{XRD}$, $N_{F}$ , $N_{S}$ , and ordering, quantitatively. The diagram was examined by XRD data for I-S samples from Ceumseongsan volcanic complex, Korea. I-S samples showed that $N_{F}$ departs from the physical upper-limit ( $N_{F}$ =100%/% $S_{XRD}$) with decrease in % $S_{XRD}$. This phenomenon may happen due to decrease of stacking-capability of fundamental particles with their thickening.g.s with their thickening.g.

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

  • 강일모;문희수
    • Proceedings of the Mineralogical Society of Korea Conference
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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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Estimation of Phase Ratio for TiO2 Powders by XRD and XAS (XRD와 XAS에 의한 TiO2 분말의 상분율 결정)

  • Rha, Sa-Kyun;Lee, Youn Seoung
    • Journal of the Korean Ceramic Society
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    • v.49 no.5
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    • pp.469-474
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    • 2012
  • The crystallinity and phase ratio of anatase to rutile in $TiO_2$ were estimated by x-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS). Traditionally, the structural characterization of $TiO_2$ powders has been carried out by XRD techniques, which are comparatively easy in use and analysis. However, materials with amorphous phase, nano-sized or nano-structured crystallinities cannot be fully characterized by XRD because XRD analysis has a limit for abnormal contributions of the nano-crystal such as the surface contribution. From the comparison with the experimental and calculated Ti K-edge XAS spectra, we found the possibility of efficient estimation in the crystalinites and the phase ratio of anatase to rutile for nano-sized $TiO_2$ mixture.

XRD Analysis of Portland Limestone Cement Paste (포틀랜드 석회석 시멘트에 관한 XRD 분석)

  • Bang, Mi-Jin;Shin, Ki-Su;Park, Ki-Bong
    • Proceedings of the Korean Institute of Building Construction Conference
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    • pp.189-190
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    • 2018
  • This study produced Portland limestone cement at the rate of limestone substitution by grinding limestone and clinker together, and it conducted an XRD analysis to determine the sign language response structure as a basic study on Portland Limestone Cement. As a result of the XRD analysis, the higher the substitution rate of limestone, the more likely it is that the detection rate of ettringite is decreased. Additionally, we could see that the production volume of Mono-carbonate was increasing.

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Structural Study of the Oxidized High Modulus Carbon Fiber using Laser Raman Spectroscopy

  • Roh, Jae-Seung;Kim, Suk-Hwan
    • Carbon letters
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    • v.10 no.1
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    • pp.38-42
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    • 2009
  • This study aims to find a correlation between XRD and Raman result of the oxidized high modulus carbon fibers as a function of its oxidation degrees, and compare with the isotropic carbon fiber reported early. La of the high modulus carbon fiber prepared by oxidation in carbon dioxide gas have been observed using laser Raman spectroscopy. The basic structural parameters of the fibers were evaluated by XRD as well. The La of the original high modulus carbon fibers were measured to be 144 ${\AA}$ from Raman analysis and 135 ${\AA}$ from XRD analysis. La of the 92% oxidized fiber were 168 ${\AA}$ by using Raman and 182 ${\AA}$ by using XRD. There was some correlation between the La value obtained from Raman and XRD. However the La value changes of the high modulus carbon fiber through whole oxidation process showed opposite tendency compare with the isotropic carbon fiber because of the fiber structure basically.

Structural Changes during Oxidation Process of Anisotopic Mesophase Carbon fibers(I) - TEM and XRD Study (산화반응에 의한 이방성 메조페이스 탄소섬유의 구조 변화(I) - TEM 및 XRD를 이용한 분석)

  • Roh, J.S.
    • Korean Journal of Materials Research
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    • v.13 no.12
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    • pp.825-830
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    • 2003
  • Structural changes during oxidation of anisotopic mesophase carbon fiber(AMCFs) have been observed with TEM and XRD. It was shown that the AMCFs are three dimensionally stacked structure of turbostratic layers, and are non-homogeneous structure which consist of the highly ordered areas and the random areas. The $d_{ 002}$, Lc, and La of AMCFs which were measured by XRD were 3.44, 146, and $135\AA$, respectively. It was observed that the oxidation initiated at the random areas, because the $d_{002}$ / decreased to the value of 3.41 $\AA$ during initial oxidation stage. It was also observed that the La of the oxidized AMCFs increased up to 182 $\AA$ during the whole oxidation process, and the $d_{002}$ of that increases up to 9.44 $\AA$ when the burn-off is over the degree of 20%. Therefore, it was suggested that the micro-crystalline grew up by heat treatment effects during the fibers were oxidized, In addition, it was shown that there was difference in the measured value of La by XRD and TEM, in case of 39% oxidized fibers for example, the measured La was $ 165\AA$ by XRD and in the range of 180∼220 $\AA$ by TEM.

About Short-stacking Effect of Illite-smectite Mixed Layers (일라이트-스멕타이트 혼합층광물의 단범위적층효과에 대한 고찰)

  • Kang, Il-Mo
    • Economic and Environmental Geology
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    • v.45 no.2
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    • pp.71-78
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    • 2012
  • Illite-smectite mixed layers (I-S) occurring authigenically in diagenetic and hydrothermal environments reacts toward more illite-rich phases as temperature and potassium ion concentration increase. For that reason, I-S is often used as geothermometry and/or geochronometry at the field of hydrocarbons or ore minerals exploration. Generally, I-S shows X-ray powder diffraction (XRD) patterns of ultra-thin lamellar structures, which consist of restricted numbers of sillicate layers (normally, 5 ~ 15 layers) stacked in parallel to a-b planes. This ultra-thinness is known to decrease I-S expandability (%S) rather than theoretically expected one (short-stacking effect). We attempt here to quantify the short stacking effect of I-S using the difference of two types of expandability: one type is a maximum expandability ($%S_{Max}$) of infinite stacks of fundamental particles (physically inseparable smallest units), and the other type is an expandability of finite particle stacks normally measured using X-ray powder diffraction (XRD) ($%S_{XRD}$). Eleven I-S samples from the Geumseongsan volcanic complex, Uiseong, Gyeongbuk, have been analyzed for measuring $%S_{XRD}$ and average coherent scattering thickness (CST) after size separation under 1 ${\mu}m$. Average fundamental particle thickness ($N_f$) and $%S_{Max}$ have been determined from $%S_{XRD}$ and CST using inter-parameter relationships of I-S layer structures. The discrepancy between $%S_{Max}$ and $%S_{XRD}$ (${\Delta}%S$) suggests that the maximum short-stacking effect happens approximately at 20 $%S_{XRD}$, of which point represents I-S layer structures consisting of ca. average 3-layered fundamental particles ($N_f{\approx}3$). As a result of inferring the $%S_{XRD}$ range of each Reichweite using the $%S_{XRD}$ vs. $N_f$ diagram of Kang et al. (2002), we can confirms that the fundamental particle thickness is a determinant factor for I-S Reichweite, and also that the short-stacking effect shifts the $%S_{XRD}$ range of each Reichweite toward smaller $%S_{XRD}$ values than those that can be theoretically prospected using junction probability.

Comparison of Analytical Methods for α-Quartz by FTIR and XRD (FTIR과 XRD를 이용한 α-Quartz 분석법 비교)

  • Kim, Boo-Wook;Lee, Jong-Seong;Choi, Byung-Soon
    • Journal of Environmental Health Sciences
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    • v.35 no.2
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    • pp.130-142
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    • 2009
  • This study compared FTIR with XRD method for the analysis of quartz by % recovery, coefficient of variation (CV) and influence of the interference. the results were as the following. 1. In FTIR method, the coefficient of determination ($r^2$) was 0.9998 in a calibration curve of $695\;cm^{-1}$, and the limit of detection was $4.9{\mu}g/sample$. 2. The highest recovery was $799\;cm^{-1}$ (98.2%). 3. The CVpooled of the FTIR method was approximately 10% in three wave numbers. 4. The analysis of qualitative and quantitative for quartz is difficult with mixed cristobalite and iron oxide. 5. In XRD method with rotating sample holder and LynxEye detector, the coefficient of determination was 0.9996 in a calibration curve, and the limit of detection was $5.9{\mu}g/sample$. 6. The recovery and CV pooled were 104.3%, and 11 %, respectively. 7. In muffle furnace ashing, the quartz weight decreased to 34% when the maximum weight of the iron oxide was more than eight times. In conclusion, the accuracy (% recovery) and precision (CV) of FTIR and XRD method for analyzing $\alpha$-quartz were similar. FTIR method was a disadvantage for sample matrix because it indicates possibility of interference. However, XRD method distinguished specific crystalline forms of silica, and the majority of silicate minerals. In addition, XRD method recommend filter dissolution to pretreatment method.

Effect of substrate temperature and hydrogen dilution on solid-phase crystallization of plasma-enhanced chemical vapor deposited amorphous silicon films (PECVD로 증착된 a-Si박막의 고상결정화에 있어서 기판 온도 및 수소희석의 효과)

  • 이정근
    • Journal of the Korean Vacuum Society
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    • v.7 no.1
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    • pp.29-34
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    • 1998
  • The solid-phase crystallization (SPC) of plasma-enhanced chemical vapor depsoited (PECVD) amorphous silicon (a-Si) films ha s been investigated by x-ray diffraction (XRD). The a-Si films were prepared on Si (100) wafers using $SiH_4$ gas and without $H_2$ dilution at the substrate temperatures between $120^{\circ}C$ and $380^{\circ}C$, and than annealed at $600^{\circ}C$ for crystallization. The annealed samples exhibited (111), (220), and (311) XRD peaks with preferential orientation of (111). The XRD peak intensities increased as the substrate temperature decreased, and the $H_2$dilution suppressed the solid-phase crystallization. The average grain size estimated by XRD analysis for the (111) texture has increased from about 10 nm to about 30 nm, as the substrate temperature decreased. The deposition rate also increased with the decreasing substrate temperature and the grain size was closely dependent on the deposition rate of the films. The grain size enhancement was attributed to an increase of the structural disorder of the Si network.

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Microstructural Evaluation of $CO_2$ Activation Process of Isotopic Carbon Fibers by XRD Analysis (XRD를 이용한 등방성 탄소섬유의 이산화탄소 활성화 과정 중 발생하는 구조변화 해석)

  • 노재승
    • Proceedings of the Materials Research Society of Korea Conference
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    • pp.227-227
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    • 2003
  • 흑연(graphite), 석탄(coal), 숯(char), soot(검댕이) 등의 탄소로 이루어진 재료들은 비정질부터 완전한 흑연결정까지 다양한 구조를 나타낸다. 이러한 탄소재료의 구조의 출발물질 뿐 아니라 열처리에 따라 강한 영향을 받는다 이러한 구조는 여러 구조인자에 의해 특성화되는데, 구조인자로는 층간거리 d, 결정립 크기 Lc 그리고 결정립 직경 La이다. 이런 구조 인자의 지식은 흑연화, 탄소화, 가스화 등과 같은 다양한 공정을 이해하는데 매우 중요하다. 많은 연구자들은 XRD, Raman 분광, 고분해능 TEM 등과 같은 여러 기술을 통하여 이러한 구조인자에 대한 해석을 시도하였다. 그 중 XRD는 정량적 분석에 있어서 가장 많이 이용되는 기술이다. XRD 회절피크의 위치로부터 층간거리 d를 구할 수 있으며, 결정립 크기 Lc 및 결정립 직경 La는 피크의 line 퍼짐(반가폭)으로 직접 구할 수 있다. 한편 섬유상 흡착제로 이용되는 등방성 탄소섬유는 이산화탄소 또는 수증기에 의해 쉽게 활성화되어 최고 약 2,500 $m^2$/g의 고 비 표면적을 얻을 수 있다. 이렇게 활성화 후 고 비표면적을 나타내는 이유는 좁은 분포를 나타내는 미세기공의 기공구조 때문에 발생하는 것으로 알려져 있다.

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