• 제목/요약/키워드: 분말회절

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Synthesis and characterization of $BaTiO_3$ fine particles by hydrothermal process (수열합성법에 의한 미립의 $BaTiO_3$ 분말합성 및 특성)

  • 배동식;주기태;한경섭;최상흘
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.8 no.4
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    • pp.563-566
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    • 1998
  • $BaTiO_3$ fine particles were prepared by hydrothermal process from titanium tetra-isoproproxide ($Ti(OiPr)_4$) and barium hexa-hydroxide ($Ba(OH)_2{cdot}8H_2O$) as raw materials. The fine particles were obtained at the temperature range of 160 to $185^{\circ}C$. The properties of $BaTiO_3$ particles were studied as a function of various parameters such as reaction temperature, reaction time and Ba/Ti ratio, etc. The average particle size of $BaTiO_3$ increased with increasing reaction temperature and time. After hydrothermal treatment at $170^{\circ}C$ for 8 h, the average particle size of $BaTiO_3$ was about 30 nm and the particle size distribution was narrow.

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Studies on Mineral Composition of Fault Clay in Quaternary Ipsil Fault: High Resolution Powder Diffraction Analysis (제4기 입실 단층 파쇄대에서 나타나는 단층점토의 산출상태에 따른 광물조성 연구: 고해상도분말회절 분석을 중심으로)

  • Park, Sung-Min;Kang, Han;Jang, Yun-Deuk;Im, Chang-Bock;Kim, Jeong-Jin
    • Journal of the Mineralogical Society of Korea
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    • v.20 no.2 s.52
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    • pp.83-89
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    • 2007
  • XRD, HRPD and SEM were used for mineralogical characterization of fault clay in fracture zone from Ipsil. Variations of color in fault clay exhibit significant mineral composition difference. Fault clays from Ipsil are composed mainly of smectite, laumontite, and quartz. Laumontite, a distinct fault clay in Ipsil fault, might be resulted from alteration of bed rock in fracture zone based on the result that no laumontite was found near fault rock. Fault clays from Ipsil are composed mainly of smectite.

Mechanical alloying effect and structural observation of (V, Fe)-N amorphous alloy powders (기계적 합금화에 의한 (V, Fe)-N계 비정질 합금의 제조 및 구조변화)

  • 이충효;전성용;김지순
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.14 no.4
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    • pp.129-134
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    • 2004
  • In this study, we investigated the effect of a nitrogen atom on the amorphization of V-Fe alloy through solid-gas reaction during mechanical alloying (MA). MA by planetary ball mill of $V_{70}Fe_{30}$ elemental powders was carried out under the nitrogen gas atmosphere. Amorphization has been observed after 160 hours of ball milling in this case. The DSC spectrum for the mechanically alloyed ($V_{70}Fe$_{30}$)_{0.89}N_{0.11}$ powders exhibits a sharp exothermic peak due to crystallization at about $600^{\circ}C$. Structural transformation from the bcc crystalline to amorphous states was also observed through X-ray and neutron diffractions. We take a full advantage of a negligibly small scattering length of the V atom in the neutron diffraction measurement. During amorphization process the octahedral unit, which is typical of a polyhedron formed in any crystal structures, was preferentially destroyed and transformed into the tetrahedral unit. Futhermore, neutron diffraction measurements revealed that a nitrogen atom is selectively situated at a center of the polyhedron formed by V atoms.

Determination of mixing ratios in a mixture via non-negative independent component analysis using XRD spectrum (XRD 스펙트럼의 비음독립성분분석을 통한 혼합물 구성비 결정)

  • You, Hanmin;Jun, Chi-Hyuck;Lee, Hyeseon;Hong, Jae-Hwa
    • Analytical Science and Technology
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    • v.20 no.6
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    • pp.502-507
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    • 2007
  • X-ray diffraction method has been widely used for qualitative and quantitative analysis of a mixture of materials since every crystalline material gives a unique X-ray diffraction pattern independently of others, with the intensity of each pattern proportional to that material's concentration in a mixture. For determination of mixing ratios, extracting source spectra correctly is important and crucial. Based on the source spectra extracted, a regression model with non-negativity constraint is applied for determining mixing ratios. In some mixtures, however, X-ray diffraction spectrum has sharp and narrow peaks, which may result in partial negative source spectrum from independent component analysis. We propose several procedures of extracting non-negative source spectra and determining mixing ratios. The proposed method is validated with experimental data on powder mixtures.

On the Growth of GaN Single Crystal from GaOOH Powders (GaOOH 분말로부터 GaN 단결정 성장에 관하여)

  • 이재범;이종원;박인용;김선태
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2003.03a
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    • pp.96-96
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    • 2003
  • 벌크 형태의 CaN 단결정 성장은 매우 곤란한 관계로 아직까지 관련 기술의 개발이 미흡한 실정이다 오랜 기간동안 승화 (sublimation)법으로 대구경 벌크 GaN 단결정을 성장시키고자 하는 노력이 지속되었지만 최근까지도 만족할 만한 결과가 보고되지 않고 있다. 본 논문에서는 종래의 방법과는 달리 출발물질로서 GaOOH 분말을 채택하고, 이를 NH$_3$ 분위기에서 가열 반응시켜 GaN 결정을 성장시켰다. 반응온도와 반응시간 및 NH$_3$ 유량 등의 성장조건에 따른 GaN 결정의 성장거동과 광학적 특성을 조사하였다. 원료인 GaOOH 분말 1g을 석영 용기에 담아 직경이 35mm인 석영 보호관에 위치시키고, 1000~l17$0^{\circ}C$의 온도에서 NH$_3$ 가스를 100~1000 sccm으로 공급하면서 96시간 동안 반응시켰다. 실험이 종료되면 전기로의 온도를 상온까지 냉각시킨 후 석영 보호관 내벽에 성장된 Ga 결정을 채집하였다. 이와 같이 채집된 결정의 형태와 크기를 광학현미경을 사용하여 조사하였고, 결정표면의 상태를 전자현미경을 사용하여 관찰하였다. 시료의 결정성을 알아보기 위하여 X선 회절 분석을 하였고, 저온에서의 광루미네센스 (PL; photoluminescence) 특성을 조사하였다.

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Crystallite Size Measurement of Uranium Oxide Fuel Powders by Neutron Diffraction (중성자 회절에 의한 산화우라늄 핵연료 분말의 결정크기 측정)

  • 류호진;강권호;문제선;송기찬;최용남
    • Journal of Powder Materials
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    • v.10 no.5
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    • pp.318-324
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    • 2003
  • The nano-scale crystallite sizes of uranium oxide powders in simulated spent fuel were measured by the neutron diffraction line broadening method in order to analyze the sintering behavior of the dry process fuel. The mixed $UO_2$ and fission product powders were dry-milled in an attritor for 30, 60, and 120 min. The diffraction patterns of the powders were obtained by using the high resolution powder diffractometer in the HANARO research reactor. Diffraction line broadening due to crystallite size was measured using various techniques such as the Stokes' deconvolution, profile fitting methods using Cauchy function, Gaussian function, and Voigt function, and the Warren-Averbach method. The non-uniform strain, stacking fault and twin probability were measured using the information from the diffraction pattern. The realistic crystallite size could be obtained after separation of the contribution from the non-uniform strain, stacking fault and twin.

Characterization of Hydrolyzed Antheraea yamamai Silk Fibroin Powder (천잠 견단백질 가수분해 분말의 특성 분석)

  • Kweon, Hae-Yong;Lee, Kwang-Gill;Yeo, Joo-Hong;Woo, Soon-Ok;Han, Sang-Mi;Sohn, Bong-Hee;Lee, Heui-Sam;Shin, Bong-Seop
    • Journal of Sericultural and Entomological Science
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    • v.48 no.1
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    • pp.11-15
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    • 2006
  • Antheraea yamamai silk fibroin powder was prepared by treatment with HCl. The prepared A. yamamai fibroin hydrolysate was characterized by gel filtration chromatography, amino acid analysis, X-ray diffractometry, circular dichroism analysis, differential thermal analysis, and thermogravimetry. The average molecular weight of A. yamamai powder was about 430 and the major amino acids composed of the powder were Ala and Ser. According to XRD analysis, A. yamamai silk powder showed sharp diffraction peaks at $2{\theta}=20.34^{\circ}\;and\;31.5^{\circ}$. CD spectrum showed a peak around 220 nm and a should 215 nm, assigned to ${\alpha}-helix\;and\;{\beta}-sheet$ structure, respectively. DSC and TGA showed that the maximum degradation temperature of powder was around $250{\sim}270^{\circ}C$. Moreover, no harmful heavy metal was contained in the A. yamamai silk fibroin hydrolysate.

Growth and Magnetic Properties of $Y_{3-x}La_xFe_5O_{12}(0.0{\le}X{\le}1.0)$ Powders and Thin Films by a Sol-Gel Method (Sol-Gel 법에 의한 $Y_{3-x}La_xFe_5O_{12}(0.0{\le}X{\le}1.0)$ 분말과 박막의 합성 및 자기적 특성에 관한 연구)

  • 엄영랑;김철성;임연수;이재광
    • Journal of the Korean Magnetics Society
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    • v.8 no.6
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    • pp.350-356
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    • 1998
  • $Y_{3-x}La_xFe_5O_{12}$ (x=0.0, 0.25, 0.5, 0.75, 1.0) powders and thin films were fabricated by a sol-gel method and their magnetic properties and crystal structure were investigated by using X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), vibrating sample magnetometer (VSM), and Mossbauer spectroscopy. XRD and Mossbauer spectroscopy measurements show that garnet powders annealed at 900 $^{\circ}C$ for 8 hours were single-phased and that thin films fired at 800 $^{\circ}C$ for 2 hours were crystallized without any preferred direction. X-ray diffraction patterns of $Y_{3-x}La_xFe_5O_{12}$ powders annealed at 1000 $^{\circ}C$ had only peaks of the garnet structure in case of x$\leq$0.75 but those of $Y_2LaFe_5O_{12}$ powders consisted of peaks from garnets and $LaFeO_3$. Mossbauer sepectra of garnet powders grown by the sol-gel method had a similar shape of those of powders grown by a conventional ceramic method. Grain sizes of garnet powders were 200~300 nm and the averaged surface roughness was 3.17 nm. Results of VSM measurements show the powders and thin films had soft magnetic properties and that the garnet powders had the largest saturation magnetization, 30 emu/g, and the lowest coercivity, 52 Oe.

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In-situ Phase Transition Study of Minerals using Micro-focusing Rotating-anode X-ray and 2-Dimensional Area Detector (집속 회전형 X-선원과 이차원 검출기를 이용한 광물의 실시간 상전이 연구)

  • Seoung, Dong-Hoon;Lee, Yong-Moon;Lee, Yong-Jae
    • Economic and Environmental Geology
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    • v.45 no.2
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    • pp.79-88
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    • 2012
  • The increased brightness and focused X-ray beams now available from laboratory X-ray sources facilitates a variety of powder diffraction experiments not practical using conventional in-house sources. Furthermore, the increased availability of 2-dimensional area detectors, along with implementation of improved software and customized sample environmental cells, makes possible new classes of in-situ and time-resolved diffraction experiments. These include phase transitions under variable pressure- and temperature conditions and ion-exchange reactions. Examples of in-situ and time-resolved studies which are presented here include: (1) time-resolved data to evaluate the kinetics and mechanism of ion exchange in mineral natrolite; (2) in-situ dehydration and thermal expansion behaviors of ion-exchanged natrolite; and (3) observations of the phases forming under controlled hydrostatic pressure conditions in ion-exchanged natrolite. Both the quantity and quality of the in-situ diffraction data are such to allow evaluation of the reaction pathway and Rietveld analysis on selected dataset. These laboratory-based in-situ studies will increase the predictability of the follow-up experiments at more specialized beamlines at the synchrotron.