• Title/Summary/Keyword: X-ray회절법

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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, $LiND_{3.05}H_{0.95}SO_4$.

The X-Ray Study on Macrostress and Microstress for Two-Phase Stainless Steel (二相스테인리스鋼의 X線에 의한 巨視的.微視的 應力에 關한 硏究)

  • ;;廣賴幸雄
    • Journal of Welding and Joining
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    • v.12 no.4
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    • pp.141-150
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    • 1994
  • The residual stress is inevitably introduced into composites because of the mismatch of the coefficient of thermal expansion, and it is different in each phase. The X-ray technique can detect separately the stress in each phase, so will wield useful information for analyzing the toughening mechanisms of composites. In order to apply the law of mixture to alloy steels with composite microstructures, two phase stainless steel, consisted of ferrite (.alpha.-Fe) and austenite (.gamma.-Fe) structures, was selected. The tensile elastic deformation was loaded, and then the X-ray diffraction technique was used to measure the X-ray elastic constants, the X-ray stress constants and the phase stresses. The law of mixture was investigated and the separation of macrostress and microstress was carried out. The phase stresses (the residual stresses of phase) in each phase, which were measured by X-ray technique, was directly proportional to the applied stress. The macrostress calculated from the phase stresses by using the law of mixture was nearly equal to the applied stress.

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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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Correction Method of the Hydrogen Bond-Distance from X-ray Diffraction: Use of Neutron Data and Bond Valence Method (X-선 회절로 얻은 수소결합의 결합거리 보정 방법: 중성자 회절결과와 결합원자가 방법 이용)

    • Journal of the Mineralogical Society of Korea
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    • v.16 no.1
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    • pp.65-73
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    • 2003
  • In this study we have derived the two correction methods of hydrogen bonding distance. In case of the intermediate or long hydrogen bond(>2.5 $\AA$), hydrogen bonding distances can be corrected by using the function d(O-H)=exp((2.173-d(O…O))/0.138)+0.958 obtained by least- squares fit to the data from the neutron diffraction at low temperatures. The valence-least-squares method is effective for the distance correction of very short hydrogen bond(<2.5 $\AA$). The distance correction is necessary for the long intermolecular hydrogen bond obtained from X-ray diffraction analysis.

Microscopic analysis of gas hydrates using X-ray diffraction method (X-ray diffraction을 이용한 가스 하이드레이트 미세구조 분석)

  • Lee, Jong-Won;Seol, Ji-Woong;Koh, Dong-Yeun;Lee, Huen
    • 한국신재생에너지학회:학술대회논문집
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    • 2008.10a
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    • pp.178-181
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    • 2008
  • 다양한 조성을 갖는 $CH_4+CO_2$ 혼합 기체 하이드레이트 샘플의 미세 구조 분석을 위하여 X-ray 회절 방법을 이용하였다. X-ray 회절 분석을 이용할 경우, 하이드레이트로의 전환율과 같은 정성적인 분석뿐 아니라 각 객체별 cage occupancy와 같은 정량적인 분석까지도 가능한 것으로 나타났다. 또한 이렇게 얻어진 X-ray 회절 분석 결과 및 refinement 결과를 $^{13}C$ 고체 NMR 방법과 교차 비교함으로써 측정 결과의 신뢰도를 높이려 하였다. 얻어진 분석 결과는 이후 가스 하이드레이트를 이용한 다양한 연구 분야에서 저장용량 평가 및 객체 점유율과 같은 미세 구조 정보를 얻는 데에 유용하게 사용될 것으로 전망된다.

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Elastic Moduli Determination of MgO Using Ultrasonic Interferometry (초음파 간섭법을 이용한 MgO 단결정의 체적탄성률 측정)

  • Kim, Young-Ho
    • Journal of the Mineralogical Society of Korea
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    • v.13 no.3
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    • pp.138-146
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    • 2000
  • Using the ultrasonic interferometry on the single crystal MgO-periclase, adiabatic bulk moduli were determined to be 163.2 GPa and 162.6 GPa from (100) and (110) lattice plane measurements, respectively. Density was measured on polycrystalline MgO by the X-ray diffraction technique. Results from this study were compared with the previously reported values. Further, the present results were converted to the isothermal bulk moduli and, then compared with the published data available including the energy dispersive X-ray diffraction result which was performed on the same single crystal MgO. The principle and techniques ultrasonic interferometry were introduced too.

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X-선 Lang 토포그래피를 이용한 사파이어 단결정 웨이퍼 결함 분석

  • Jeon, Hyeon-Gu;Bin, Seok-Min;Lee, Yu-Min;O, Byeong-Seong;Kim, Chang-Su
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.371-371
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    • 2013
  • 사파이어 단결정 웨이퍼는 제조과정에서 결정 성장 조건 및 기계적 연마에 의하여 내부적인 결함이 발생할 수 있다. 사파이어 단결정은 일반적으로 LED용 기판 재료로 사용되며, 내부결함이 발생 시 기판 위의 GaN 등 layer의 결함도 함께 증가하므로 기판의 결함을 줄이는 과정이 중요한 이슈이다. 이 과정에 X-선 토포그래피는 단결정의 내부 결함을 모니터링 하는데 있어서 매우 유용한 방법이다. 이에 본 연구에서는 사파이어 단결정 웨이퍼에 내재하는 결함 형태를 X-선 Lang 토포그래피 방법(X-ray Lang Topography)으로 이미징하여 관찰, 분석하였다. Lang 토포그래피 방법은 X-선 투과법으로 넓은 부분을 우수한 강도와 분해능으로 내부 결함을 관찰할 수 있는 장점을 지니고 있다. X-선 source는 Mo $k{\alpha}$ 1을 사용하였으며, 시료는 c-plane 사파이어 웨이퍼를 사용하였다. 사파이어 웨이퍼의 (110), (102) 회절면의 X-선 토포그래피 이미지를 통해 전위 결함의 유형에 따른 이미지 패턴의 형성 메커니즘에 대해 연구하였고, 측정 회절면과 두께, 표면 데미지에 따른 전위 결함 이미지의 변화를 확인하였다. X-선 토포그래피 이미지를 통해 단결정 c-plane 사파이어 웨이퍼의 전위 결함의 형성 메카니즘 연구와 유형별 이미지와 회절면, 두께, 표면 데미지에 따른 이미지 변화 등을 확인하였다.

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Phase Analysis of Mechanically Alloyed $\sigma$-VFe Alloy Powders by Neutron and X-ray Diffraction (기계적 합금화한 $\sigma$-VFe합금의 중성자 및 X선 회절에 의한 상분석)

  • 이충효;조재문;이상진;심해섭;이창희
    • Korean Journal of Materials Research
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    • v.11 no.8
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    • pp.664-664
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    • 2001
  • The mechanical alloying (MA) effect in $\sigma$-VFe intermetallic compound was studied by neutron and X-ray diffraction. The structure of MA $\sigma$-VFe powders were characterized by the X- ray diffraction with Cu- $K\alpha$ radiation and neutron diffraction with monochromatic neutrons of $1.835\AA$ using a high resolution powder diffractometer (HRPD). Mechanical alloying of $\sigma$-VFe compound gives rise to a dramatic structural change. After 60 hours of MA, the Fe-Fe distribution of the $\sigma$- phase VFe tetragonal structure with 30 atoms in a unit cell is found to change into that of the $\sigma$-(V,Fe) solid solution with bcc structure, which is a stable phase at elevated temperature above $1200^{\circ}C$. A comparison of X-ray diffraction data for the $\alpha$-phase has been also made with the corresponding neutron diffraction data. The (101) and (111) diffraction peaks of the $\sigma$-phase was clearly observed only in neutron diffraction pattern, which is believed to be a characteristic feature due to the chemical atomic ordering of $\sigma$- VFe phase.

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.

Possibility about Application and Interpretation of Surface Nondestructive X-ray Diffraction Method for Cultural Heritage Samples by Material (유형별 문화재 시료의 비파괴 표면 X-선 회절분석법 적용과 해석 가능성)

  • Moon, Dong Hyeok;Lee, Myeong Seong
    • Journal of the Mineralogical Society of Korea
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    • v.32 no.4
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    • pp.287-301
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    • 2019
  • Preservation of the original form is the principle for conservation, management and utilization of cultural heritages. Thus, non-destructive analysis of these samples are important field of the conservation science. In this study, examined the applicability of nondestructive surface X-ray diffraction analysis (ND-XRD) for cultural heritage by materials (rock specimen, jade stone, pigment painted specimen, earthen artifact, metal artifact). In result, all type of sample is recorded suitable X-ray diffraction patterns for identifying mineral composition in case of surface condition with adequate particle size and arrangement. And diffraction pattern is reflected surface information than matrix. Therefore, ND-XRD is thought to be applicable not only mineral identification but also interpretation of manufacturing technique and alteration trend about layered sample (in horizontally or vertically). Whereas some exceptional diffraction patterns were recorded due to overlapping information on specific crystal planes. It caused by skip the sample treatment (powdering and randomly orientation). It could be advantageously used for mineral identification, such as preferred orientation of clay minerals. In contrast, irregular diffraction pattern caused by single crystalline effect is required careful evaluation.