• 제목/요약/키워드: X-ray Diffraction Method

검색결과 2,317건 처리시간 0.031초

Physicochemical Characterization and Dissolution Properties of CS-891 with Different Crystallinity

  • Lee, Woo-Young;Park, Byoung-Woo;Park, Yong-Sun
    • Journal of Pharmaceutical Investigation
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    • 제35권4호
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    • pp.279-285
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    • 2005
  • Ground CS-891 (N-[1-(4-methoxyphenyl)-1-methylethyl]-3-oxo-4-aza-5a-androst-1-ene-$17{\beta}$-carboxamide) of poorly water soluble drug was obtained using a Heiko Seisakusho model TI-100 vibration mill, and samples with different crystallinity were prepared at mixture ratios of 10:0, 7:3, 5:5, 3:7 and 0:10 (intact;ground CS-891). Physicochemical characterizations were obtained using qualitative and quantitative X-ray diffractometry, different scanning calorimetry (DSC), scanning electron microscopy (SEM), Quantasorb surface area analyzer, and controlled atmosphere microbalance. With increase of amorphous CS-891 in mixture ratios, the intensities of X-ray diffraction peaks of crystalline CS-891 were decreased, whereas surface area, water absorption, and exothermic peaks in DSC were increased. The apparent solubility of ground CS-891 was $4.4\;{\mu}g/ml$ and the solubility of intact CS-891 was $3.1\;{\mu}g/ml$ at $37{\pm}1^{\circ}C$. The apparent precipitation rates of CS-891 in a supersaturated solution during the solubility test were increased with an increase of amorphous CS-891, and a crystalline form of CS-891 transformed from amorphous CS-891 after the solubility test was found by X-ray diffraction analysis, DSC and SEM. The dissolution profiles of CS-891 with different crystallinity at $37{\pm}1^{\circ}C$ by the USP paddle method were investigated, and the apparent dissolution rate constant of ground CS-891 was about 5.9-fold higher than that of intact CS-891. A linear relationships between the crystallinity of CS-891 and the apparent dissolution rate constant (r>0.96) were obtained.

순차 스퍼터법으로 제작한 BiSrCaCuO 박막의 부착 특성 (Sticking Characteristics in BiSrCaCuO Thin Film Fabricated by Layer-by-Layer Sputtering Method)

  • 천민우;박용필;김정호
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2003년도 제5회 학술대회 논문집 일렉트렛트 및 응용기술연구회
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    • pp.45-48
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    • 2003
  • BiSrCaCuO thin films were fabricated by atomic layer-by-layer deposition using an ion beam sputtering method. 10 wt% and 90 wt% ozone mixed with oxygen were used with ultraviolet light irradiation to assist oxidation. At early stages of the atomic layer by layer deposition, two dimensional epitaxial growth which covers the substrate surface would be suppressed by the stress and strain caused by the lattice misfit, then three dimensional growth takes place. Since Cu element is the most difficult to oxidize, only Sr and Bi react with each other predominantly, and forms a buffer layer on the substrate in an amorphous-like structure, which is changed to $SrBi_2O_4$ by in-situ anneal.

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HWE 방법에 의한 $AgGaS_2$단결정 박막성장과 특성에 관한 연구 (A study on the growth and characteristics of $AgGaS_2$ single crystal thin film by hot wall epitaxy)

  • 홍광준;정준우
    • 한국결정성장학회지
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    • 제8권2호
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    • pp.211-220
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    • 1998
  • 수평 전기로에서 $AgGaS_2$ 다결정을 합성하여 HWE 방법으로 $AgGaS_2$ 단결정 박막을 성장하였다. $AgGaS_2$ 단결정 박막을 성잘할 때 증발원과 기판의 온도를 각각 $590^{\circ}C$, $440^{\circ}C$로 성장하였을 때 이중결정 X-선 요동곡선(double crystal X-ray diffraction rocking curve, DCRC)의 반폭치(FWHM)값이 124 arcsec로 가장 작아 최적 성장조건이었다. 상온에서 $AgGaS_2$ 단결정 박막의 광흡수 특성으로부터 에너지 띠간격이 2.61cV였다. Band edge에 해당하는 광전도도 peak의 온도 의존성은 Varshni 관계식으로 설명되었으며, Vaeshni 관계식의 상수값은 Eg(0) = 2.7284eV, $\alpha$= 8.695$\times$10-4 eV/K, $\beta$= 332K 로 주어졌다. 광발광 봉우리는 20K에서 414.3nm(2.9926eV)와 414.1nm(2.7249eV)는 free exciton(Ex)의 upper polariton과 lower polariton인 {{{{{E}`_{x} ^{u} }}}}와 {{{{{E}`_{x} ^{L} }}}}, 423.6nm(2.9269eV)는 bound exciton emission에 의한 I로 관측되었다. 또한 455nm(2.7249eV)의 peak는 donor-acceptor pair(DAP)에 기인하는 광발광 봉우리로 관측되었다.

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Reinvestigation of Dion-Jacobson Phases CsCa2Nb2MO9 (M = Fe and Al)

  • Hong, Young-Sik
    • Bulletin of the Korean Chemical Society
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    • 제27권6호
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    • pp.853-856
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    • 2006
  • Dion-Jacobson phases $CsCa_2Nb_2FeO_9$ and $CsCa_2Nb_2AlO_9$ were reinvestigated by the Rietveld analysis of powder X-ray diffraction (XRD) method, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). These nominal compounds, previously known as the oxygen-deficient layered perovskites with the sequences of $NbO_6-MO_4-NbO_6$ in tripled slab, in fact, were mixed phases of n = 3 Dion-Jacobson phases and impurities such as $Ca_2NbFeO_6$ and $Ca_3Al_2O_6$. The difference of morphology and chemical in-homogeneity between Dion-Jacobson phases and impurities could be clearly identified by scanning electron microscopy with energy-dispersive X-ray spectroscopy. The chemical composition of $CsCa_2Nb_2FeO_9$ was calculated into $Cs_{0.59}Ca_{2.64}Nb_{2.92}Fe_{0.81}$ in small agglomerate crystals and $Cs_{0.95}Ca_{1.97}Nb_{3.08}Fe_{0.15}$ in long plate-like crystals.

Surface Analysis of Copper-Tin Thin Films Synthesized by rf Magnetron Co-sputtering

  • 강유진;박주연;강용철
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2016년도 제50회 동계 정기학술대회 초록집
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    • pp.272.2-272.2
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    • 2016
  • Copper-Tin (CuSn) thin films were synthsized by rf magnetron co-sputtering method with pure Cu and Sn metal targets with various rf powers and sputtering times. The obtained CuSn thin films were characterized by a surface profiler (alpha step), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), X-ray induced Auger electron spectroscopy (XAES), and contact angle measurement. The deposition rates were calculated by the thickness of CuSn thin films and sputtering times. We observed hexagonal Cu20Sn6 and cubic Cu39Sn11 phases from the films by XRD measurement. From the survey XPS spectra, the Cu and Sn main peaks were observed. Therefore, we could conclude CuSn thin films were successfully fabricated on the substrate in this study. The changes of oxidation states and chemical environment of the films were investigated with high resolution XPS spectra in the regions of Cu 2p, Cu LMM, and Sn 3d. Surface free energy (SFE) and wettability of the CuSn thin films were studied with distilled water (DW) and ethylene glycol (EG) using the contact angle measurement. The total SFE of CuSn thin films decreased as rf power on Cu target increased. The contribution to the total SFE of dispersive SFE was relatively superior to polar SFE.

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Crystallization and Preliminary X-Ray Crystallographic Analysis of PAS Factor from Vibrio vulnificus

  • Lee, Jun Hyuck;Kim, Soo Young;Rho, Seong-Hwan;Im, Young Jun;Kim, Young Ran;Kim, Mun-Kyoung;Kang, Gil Bu;Rhee, Joon Haeng;Eom, Soo Hyun
    • Molecules and Cells
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    • 제20권3호
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    • pp.361-363
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    • 2005
  • Plasmid Achromobacter secretion (PAS) factor is a putative secretion factor that induces the secretion of periplasmic proteins. PAS factor from Vibrio vulnificus was crystallized at 294 K by the hanging drop vapor-diffusion method. It was isolated as a monomer during the purification procedures. The native crystal belongs to the F222 space group with unit cell parameters a = 56.1, b = 74.4, $c=80.0{\AA}$, ${\alpha}={\beta}={\gamma}=90^{\circ}$. The crystal was soaked in cryoprotectant containing 1 M NaBr for 1 h for MAD phasing. The diffraction limit of the Br-MAD data set was $1.9{\AA}$ using synchrotron X-ray irradiation at beam line BL-18B at the Photon Factory, Japan.

Synthesis of Silver Nanocrystallites by a New Thermal Decomposition Method and Their Characterization

  • Lee, Don-Keun;Kang, Young-Soo
    • ETRI Journal
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    • 제26권3호
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    • pp.252-256
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    • 2004
  • We formed silver nanocrystallites by the thermal decomposition of a $Ag^{+1}$-oleate complex, which was prepared by a reaction with $AgNO_{3}$ and sodium oleate in a water solution. The resulting monodispersed silver nanocrystallites were produced by controlling the temperature (290$^{\circ}$C). Transmission electron microscopic (TEM) images of the particles showed a 2-dimensional assembly of the particles with a diameter of $9.5{\pm}0.7nm$, demonstrating the uniformity of these nanocrystallites. An energy-dispersive X-ray (EDX) spectrum and X-ray diffraction (XRD) peaks of the nanocrystallites showed the highly crystalline nature of the silver structure. We analyzed the decomposition of the $Ag^{+1}$-oleate complex using a Thermo Gravimetric Analyzer (TGA) and observed the crystallization process using XRD.

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The molecular structure of (+) -6-methoxy-.alpha. 1-2-naphtha-leneacetic acid determined by X-Ray method

  • Kim, Yang-Bae;Song, Hyun-June
    • Archives of Pharmacal Research
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    • 제7권2호
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    • pp.137-139
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    • 1984
  • The molecular structure of (+)-6-Me hoxy-.alpha.-methyl-2-naphthaleneacetic acid (Naproxen), $C_{14}H_{14}O_{ 3}$, was determined by X-Ray diffraction technique. Naproxen crystallized in $P2_1$ with two molecules on the unit cell of dimensions a = 7.855, b = 5.783, c = 13.347$\AA$ and $\beta$ = $93.9^{\circ}$

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Quantitative Photocatalytic Activity under Visible Light with Mn-ACF/TiO2

  • Ye, Shu;Kim, Hyun-il;Oh, Won-Chun
    • 한국세라믹학회지
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    • 제53권3호
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    • pp.343-348
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    • 2016
  • Manganese and $TiO_2$ grown on Activated Carbon Fiber (ACF) was synthesized by hydrothermal method. The prepared composites were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) with energy dispersive X-ray (EDX). The catalytic behavior was investigated through the decomposition of methylene blue (MB) and methyl orange (MO) as standard dyes under visible light. The degradation performance of the degraded standard dye solutions was determined by UV-Vis spectrophotometry. This enhanced photocatalytic activity arises from the positive synergetic effect among the Mn, $TiO_2$ and ACF in this heterogeneous photocatalyst. The process contributes to the release of abundant photocatalytic sites of Mn and $TiO_2$ and improves the photocatalytic efficiency. The excellent adsorption and photocatalytic effect with the explanation of the synergetic mechanism are very useful not only for fundamental research but also for potential practical applications.

Synthesis of CdSe-TiO2 Photocatalyst and Their Enhanced Photocatalytic Activities under UV and Visible Light

  • Lim, Chang-Sung;Chen, Ming-Liang;Oh, Won-Chun
    • Bulletin of the Korean Chemical Society
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    • 제32권5호
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    • pp.1657-1661
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    • 2011
  • In this study, CdSe-$TiO_2$ photocatalyst were synthesized by a facile solvothermal method and characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis and UV-vis diffuse reflectance spectrophotometer. The photocatalytic activity was investigated by degrading methylene blue (MB) in aqueous solution under irradiation of UV light as well as visible light. The absorbance of degraded MB solution was determined by UV-vis spectrophotometer. The results revealed that the CdSe-$TiO_2$ photocatalyst exhibited much higher photocatalytic activity than $TiO_2$ both under irradiation of UV light as well as visible light.