• Title/Summary/Keyword: X-ray crystal diffraction

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A Study on the Luminescence Properties of LiGd9(SiO4)6O2:Ce3+ (LiGd9(SiO4)6O2:Ce3+ 형광 특성 연구)

  • Jin, Seongjin
    • Journal of the Korean Society of Radiology
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    • v.9 no.3
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    • pp.169-174
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    • 2015
  • $LiGd_9(SiO_4)_6O_2:Ce^{3+}$ phosphors were synthesized by solid-state reaction method. The structural characteristic was investigated by X-ray powder diffraction analysis. The emission and excitation spectra of the $Ce^{3+}$ ions doped $LiGd_9(SiO_4)_6O_2$ phosphors were obtained under the UV excitation. The emission spectra of $LiGd_9(SiO_4)_6O_2:Ce^{3+}$ shows the band at 410 nm corresponding to the $^2F_{5/2}$ and $^2F_{7/2}$ states of $Ce^{3+}$. The red shift of $Ce^{3+}$ emission is found as the $Ce^{3+}$ concentration increases, which could be explained by the change in crystal-field symmetry and strength with increasing $Ce^{3+}$ concentration. Fluorescence decay time of $Ce^{3+}$ was about 20 ns. When the concentration of $Ce^{3+}$ increases life time was slightly reduced.

A Study on the Preparation of Aluina & Titania Sols for Coatings (코팅용 알루미타, 티타니아솔 제조에 관한 연구)

  • Kim, Chu-Hui;Choe, Hyeong-Su;Jo, Yeong-Sang;Im, Jong-Ju
    • Korean Journal of Materials Research
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    • v.4 no.3
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    • pp.319-328
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    • 1994
  • Aluminium and titanium precursors containing $\beta$-diketonate ligands were used for the synthesis of polymeric sols of alumina and titania by sol-gel methods. To prepare polymeric sols by solgel processing, we synthesized modified precursors having chelating organic ligands. With these precursors it was found to be possible to control both hydrolysis and polycondensation reaction rates which resulted in ultrafine particles few nms of average size. The optimum molar ratio of acid to alkoxide for alumina sol was 0.3-0.4 and that of water to alkoxide &as 1. On the other hand, the corresponding ratios for titania sol were found be 0.25-0.20 and 1 respectively. Dynamic light scattering measurements indicated that the average particle size in both sols was in the order of few nms. SEM photographs were taken to observe crack-free and smooth surfaces of coated membranes after sintering at $450^{\circ}C$. Alumina coated membrane on a slide glass had about 4-4.5$\mu \textrm{m}$, thickness and titania coated one had 2-2.5$\mu \textrm{m}$, thickness. And according to TEM photographs, the grain size of titania was smaller than 30nm and that of alumina was in the range of few $\AA$s to 2nms. An X-ray diffraction study revealed that alumina was $\gamma$ phase and titania was anatase crystal.

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A Study of the Photoluminescence of ZnO Thin Films Deposited by Radical Beam Assisted Molecular Beam Epitaxy (라디칼 빔 보조 분자선 증착법 (Radical Beam Assisted Molecular Beam Epitaxy) 법에 의해 성장된 ZnO 박막의 발광 특성에 관한 연구)

  • Suh, Hyo-Won;Byun, Dong-jin;Choi, Won-Kook
    • Korean Journal of Materials Research
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    • v.13 no.6
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    • pp.347-351
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    • 2003
  • II-Ⅵ ZnO compound semiconductor thin films were grown on $\alpha$-Al$_2$O$_3$(0001) single crystal substrate by radical beam assisted molecular beam epitaxy and the optical properties were investigated. Zn(6N) was evaporated using Knudsen cell and O radical was assisted at the partial pressure of 1$\times$10$^{4}$ Torr and radical beam source of 250-450 W RF power. In $\theta$-2$\theta$ x-ray diffraction analysis, ZnO thin film with 500 nm thickness showed only ZnO(0002)and ZnO(0004) peaks is believed to be well grown along c-axis orientation. Photoluminescence (PL) measurement using He-Cd ($\lambda$=325 nm) laser is obtained in the temperature range of 9 K-300 K. At 9 K and 300 K, only near band edge (NBE) is observed and the FWHM's of PL peak of the ZnO deposited at 450 RF power are 45 meV and 145 meV respectively. From no observation of any weak deep level peak even at room temperature PL, the ZnO grains are regarded to contain very low defect density and impurity to cause the deep-level defects. The peak position of free exciton showed slightly red-shift as temperature was increased, and from this result the binding energy of free exciton can be experimentally determined as much as $58\pm$0.5 meV, which is very closed to that of ZnO bulk. By van der Pauw 4-point probe measurement, the grown ZnO is proved to be n-type with the electron concentration($n_{e}$ ) $1.69$\times$10^{18}$$cm^3$, mobility($\mu$) $-12.3\textrm{cm}^2$/Vㆍs, and resistivity($\rho$) 0.30 $\Omega$$\cdot$cm.

Effect of Metal Interlayers on Nanocrystalline Diamond Coating over WC-Co Substrate (초경합금에 나노결정질 다이아몬드 코팅 시 금속 중간층의 효과)

  • Na, Bong-Kwon;Kang, Chan Hyoung
    • Journal of the Korean institute of surface engineering
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    • v.46 no.2
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    • pp.68-74
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    • 2013
  • For the coating of diamond films on WC-Co tools, a buffer interlayer is needed because Co catalyzes diamond into graphite. W and Ti were chosen as candidate interlayer materials to prevent the diffusion of Co during diamond deposition. W or Ti interlayer of $1{\mu}m$ thickness was deposited on WC-Co substrate under Ar in a DC magnetron sputter. After seeding treatment of the interlayer-deposited specimens in an ultrasonic bath containing nanometer diamond powders, $2{\mu}m$ thick nanocrystalline diamond (NCD) films were deposited at $600^{\circ}C$ over the metal layers in a 2.45 GHz microwave plasma CVD system. The cross-sectional morphology of films was observed by FESEM. X-ray diffraction and visual Raman spectroscopy were used to confirm the NCD crystal structure. Micro hardness was measured by nano-indenter. The coefficient of friction (COF) was measured by tribology test using ball on disk method. After tribology test, wear tracks were examined by optical microscope and alpha step profiler. Rockwell C indentation test was performed to characterize the adhesion between films and substrate. Ti and W were found good interlayer materials to act as Co diffusion barriers and diamond nucleation layers. The COFs on NCD films with W or Ti interlayer were measured as less than 0.1 whereas that on bare WC-Co was 0.6~1.0. However, W interlayer exhibited better results than Ti in terms of the adhesion to WC-Co substrate and to NCD film. This result is believed to be due to smaller difference in the coefficients of thermal expansion of the related films in the case of W interlayer than Ti one. By varying the thickness of W interlayer as 1, 2, and $4{\mu}m$ with a fixed $2{\mu}m$ thick NCD film, no difference in COF and wear behavior but a significant change in adhesion was observed. It was shown that the thicker the interlayer, the stronger the adhesion. It is suggested that thicker W interlayer is more effective in relieving the residual stress of NCD film during cooling after deposition and results in stronger adhesion.

Structure and Properties of Syndiotactic Polystyrene Fibers Prepared in High-speed Melt Spinning Process

  • Hada Yoshiaki;Shikuma Haruo;Ito Hiroshi;Kikutani Takeshi
    • Fibers and Polymers
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    • v.6 no.1
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    • pp.19-27
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    • 2005
  • High-speed melt spinning of syndiotactic polystyrene was carried out using high and low molecular weight poly­mers, HM s-PS and LM s-PS, at the throughput rates of 3 and 6 g/min. The effect of take-up velocity on the structure and properties of as-spun fibers was investigated. Wide angle X-ray diffraction (WAXD) patterns of the as-spun fibers revealed that the orientation-induced crystallization started to occur at the take-up velocities of 2-3 km/min. The crystal modification was a-form. Birefringence of as-spun fibers showed negative value, and the absolute value of birefringence increased with an increase in the take-up velocity. The cold crystallization temperature analyzed through the differential scanning calorimetry (OSC) decreased with an increase in the take-up velocity in the low speed region, whereas as the melting temperature increased after the on-set of orientation-induced crystallization. It was found that the fiber structure development proceeded from lower take-up velocities when the spinning conditions of higher molecular weight and lower throughput rate were adopted. The highest tensile modulus of 6.5 GPa was obtained for the fibers prepared at the spinning conditions of LM s-PS, 6 g/min and 5 km/min, whereas the highest tensile strength of 160 MPa was obtained for the HM s-PS fibers at the take-up velocity of 2 km/min. Elongation at break of as-spun fibers showed an abrupt increase, which was regarded as the brittle-duc­tile transition, in the low speed region, and subsequently decreased with an increase in the take-up velocity. There was a uni­versal relation between the thermal and mechanical properties of as-spun fibers and the birefringence of as-spun fibers when the fibers were still amorphous. The orientation-induced crystallization was found to start when the birefringence reached -0.02. After the starting of the orientation-induced crystallization, thermal and mechanical properties of as-spun fibers with similar level of birefringence varied significantly depending on the processing conditions.

Effect of Solubilizing and Microemulsifying Excipients in Polyethylene Glycol 6000 Solid Dispersion on Enhanced Dissolution and Bioavailability of Ketoconazole

  • Heo, Min-Young;Piao, Zong-Zhu;Kim, Tae-Wan;Cao, Qing-Ri;Kim, Ae-Ra;Lee, Beom-Jin
    • Archives of Pharmacal Research
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    • v.28 no.5
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    • pp.604-611
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    • 2005
  • Polyethylene glycol (PEG) 6000-based solid dispersions (SDs), by incorporating various pharmaceutical excipients or microemulsion systems, were prepared using a fusion method, t o compare the dissolution rates and bioavailabilities in rats. The amorphous structure of the drug in SDs was also characterized by powder X-ray diffractometry (XRD) and differential scanning calorimetry (DSC). The ketoconazole (KT), as an antifungal agent, was selected as a model drug. The dissolution rate of KT increased when solubilizing excipients were incorporated into the PEG-based SDs. When hydrophilic and lipophilic excipients were combined and incorporated into PEG-based SDs, a remarkable enhancement of the dissolution rate was observed. The PEG-based SDs, incorporating a self microemulsifying drug delivery system (SMEDDS) or microemulsion (ME), were also useful at improving the dissolution rate by forming a microemulsion or dispersible particles within the aqueous medium. However, due to the limited solubilization capacity, these PEG-based SDs showed dissolution rates, below 50% in this study, under sink conditions. The PEG-based SD, with no pharmaceutical excipients incorporated, increased the maximum plasma concentration (C$_{max}$) and area under the plasma concentration curve (AUC$_{0-6h}$) two-fold compared to the drug only. The bioavailability was more pronounced in the cases of solubilizing and microemulsifying PEG-based SDs. The thermograms of the PEG-based SDs showed the characteristic peak of the carrier matrix around 60$^{\circ}C$, without a drug peak, indicating that the drug had changed into an amorphous structure. The diffraction pattern of the pure drug showed the drug to be highly crystalline in nature, as indicated by numerous distinctive peaks. The lack of the numerous distinctive peaks of the drug in the PEG-based SDs demonstrated that a high concentration of the drug molecules was dissolved in the solid-state carrier matrix of the amorphous structure. The utilization of oils, fatty acid and surfactant, or their mixtures, in PEG-based SD could be a useful tool to enhance the dissolution and bioavailability of poorly water-soluble drugs by forming solubilizing and microemulsifying systems when exposed to gastrointestinal fluid.

Formation of Magnesium Films on Galvanized Steel Substrates by PVD Method at Nitrogen Gas Pressures and Their Corrosion Resistances (질소가스 중 PVD법에 의해 용융아연도금 강판 상에 형성한 마그네슘 막의 내식특성)

  • Eom, Jin-Hwan;Park, Jae-Hyeok;Hwang, Seong-Hwa;Park, Jun-Mu;Yun, Yong-Seop;Lee, Myeong-Hun
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2016.11a
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    • pp.182-182
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    • 2016
  • 철강은 기본적으로 강도가 우수하고 그 매장량이 풍부할 뿐만 아니라 대량생산이 가능하다 또한 다른 금속과 합금을 구성하여 또 다른 특성을 부여할 수 있기 때문에 현재 전 세계 금속 생산량의 95%를 차지할 정도로 많이 사용되며, 각종 산업과 기술이 발달함에 따라 그 중요도는 점점 더 커져가고 있다. 하지만 철강은 사용 환경 중 부식에 의해 그 수명과 성능이 급격히 저하되기 때문에 내식성을 향상시키기 위하여 도장이나 도금 등의 표면처리를 포함한 다양한 방법이 적용되고 있다. 그 중 철강재의 도금 표면처리방법은 주로 아연을 이용한 용융도금이나 전기도금 등과 같은 습식 프로세스가 널리 사용되고 있다. 여기서 아연은 철보다 이온화 경향은 크나 대기 환경 중 산소와 물과 반응하여 Zn(OH)2와 같은 화합물을 형성함으로써 철강재 표면상 부식인자를 차단(Barrier)함은 물론 사용 중 철 모재가 노출되는 결함이 발생하는 경우에는 철을 대신하여 희생양극(Sacrificial Anode) 역할을 하기 때문에 철의 부식방식용 금속으로 가장 많이 사용되고 있다. 한편 최근에는 철강의 사용 환경이 다양해짐은 물론 가혹해지고 있어서 이에 따른 내식성 향상이 계속해서 요구되고 있는 추세이다. 따라서 본 연구에서는 철강재의 내식성을 향상시키기 위한 일환으로 현재 많이 사용되고 있는 용융아연도금 강판 상에 아연보다 활성이 높은 마그네슘(Mg)을 건식 프로세스 방법 중에 하나인 PVD(Physical Vapour Deposition)법에 의해 코팅하는 것을 시도하였다. 일반적으로 PVD법에 의해 진공증착하는 경우에는 그 도입가스로써 불활성가스인 아르곤(Ar)을 사용하는 경우가 대부분이나 여기서는 상대적으로 비활성이면서 그 크기가 작은 질소(N2)가스를 도입하여 그 증착 막의 몰포로지는 물론 결정구조도 제어하여 그 내식특성을 향상시키고자 하였다. 본 연구에서는 철강재의 내식성을 향상시키기 위한 방법으로 마그네슘(Mg)를 PVD(Physical Vapor Deposition)법 중 진공증착법(Vacuum Deposition)을 사용하여 용융아연도금 강판 상에 마그네슘 증착 막을 형성하였다. 즉, 여기서는 진공증착 중 질소(Nitrogen, N2)가스를 도입하여 진공챔버(Vacuum Chamber)내의 진공도를 $1{\times}10^{-1}$, $1{\times}10^{-2}$, $1{\times}10^{-3}$, $1{\times}10^{-4}$로 조절하며 제작하였다. 또한 제작된 시편에 대해서는 SEM(Scanning Electron Microscope) 및 XRD(X-Ray Diffraction)을 사용하여 형성된 아연도금상 마그네슘 막의 표면 몰포로지 및 결정구조의 변화를 분석함은 물론 침지시험, 염수분무시험, 분극시험을 통해 이 막들에 대한 내식특성을 분석 평가하였다. 상기 실험결과에 의하면, 진공 가스압이 증가됨에 따라 마그네슘 막의 두께는 감소하였으며, 그 몰포로지의 단면은 주상정(Columnar)에서 입상정(Granular) 구조로 변화하며 표면의 결정립은 점점 미세화 되는 경향을 나타냈다. 이때의 표면의 결정배향성(Crystal orientation)은 표면에너지가 상대적으로 큰 면이 우세하게 나타나는 경향이 있었다. 또한 본 실험에서 형성한 진공증착 막은 비교재인 용융아연도금강판보다 우수한 내식성을 나타냈고, 본 형성 막 중에는 마그네슘 막 두께가 작음에도 불구하고 질소 가스압이 가장 큰 조건일수록 내식성이 우수한 경향을 나타냈다. 이상의 결과는 철강재의 내식성 향상을 위한 응용표면처리설계에 기초적인 지침을 제공할 수 있을 것으로 기대된다.

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Optical properties of $Ag_2CdSnSe_4$ and $Ag_2CdSnSe_4:CO^{2+}$ single crystals ($Ag_2CdSnSe_4$$Ag_2CdSnSe_4:Co^{+2}$단결정의 광학적 특성)

  • 이충일
    • Journal of the Korean Vacuum Society
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    • v.10 no.1
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    • pp.16-21
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    • 2001
  • Optical properties of $Ag_2CdSnSe_4$ and $Ag_2CdSnSe_4:Co^{+2}$ quaternary semiconductor single crystals grown by the chemical transport reaction method were investigated. The analysis of the X - ray powder diffraction measurements showed that these crystals have a wurtzite structure with lattice constants a = 4.357 $\AA$, c = 7.380 $\AA$, for $Ag_2CdSnSe_4$ and a = 4.885 $\AA$, c = 7.374 $\AA$, for $Ag_2CdSnSe_4:CO^{2+}$. The direct band gap at 298K, obtained from the optical absorption measurement, is found to be 1.21 eV for $Ag_2CdSnSe_4$ and 1.02 eV for $Ag_2CdSnSe_4:CO^{2+}$. The shrinkage of the band gap due to Co-doping is observed and is about 190 meV, We observed four absorption bands of $Co^{2+}$ ions in two near infrared regions of optical absorption spectra of $Ag_2CdSnSe_4$:$Co^{+2}$. These absorption bands were assigned as due to electronic transitions between the split energy levels of $Co^{2+}$ ions in $T_d$ crystal field under spin-orbit interactions.

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A Study on the Characterization of Anthracite Fly Ash for the Fabrication of Calcinated Brick (소성블릭 제조를 위한 무연탄 석탄회의 특성 연구)

  • Yu Yeon-Tae;Kim Byoung-Gyu;Choi Young-Yoon;Nam Chul-Woo;Lee Yeng-Seok;Kim Cheon-Sun
    • Resources Recycling
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    • v.13 no.2
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    • pp.16-23
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    • 2004
  • To increase the recycling rate of anthracite fly ash, the properties of anthracite fly ash were compared to that of bituminous fly ash. Especially, the high temperature properties of the fly ash are investigated by using thermal analysis, high temperature microscope and X-ray diffraction analysis for utilizing anthracite fly ash to prepare the calcinated bricks. The average ratio of $A1_2$$O_3$/$SiO_2$ for anthracite is 0.62 and the ratio for bituminous is 0.34. The content of $SiO_2$ in anthracite fly ash was higher than that of bituminous fly ash. The $A1_2$$O_3$ of anthracite fly ash reacted with the $A1_2$$O_3$ in the fly ash and formed new mullite crystal at over $1000^{\circ}C$, so anthracite fly ash showed high fire resistance. And, the fly ash mixtures having kaolin were prepared, and then extruded in vacuum to evaluate the extruding property of anthracite fly ash mixture. The extruding velocity was decrease with increasing the addition amount of fly ash in the mixture, and the maximum addition amount of fly ash that could be extruded was 60 wt%.

Effect of Mesoporous TiO2 in Facilitated Olefin Transport Membranes Containing Ag Nanoparticles (나노입자가 포함된 촉진수송 분리막에서의 메조기공 티타늄산화물의 영향)

  • Kim, Sang Jin;Jung, Jung Pyu;Kim, Dong Jun;Kim, Jong Hak
    • Membrane Journal
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    • v.25 no.5
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    • pp.398-405
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    • 2015
  • Facilitated transport is considered to be a possible solution to simultaneously improve permeability and selectivity, which is challenging in normal polymeric membranes based on solution-diffusion transport only. We investigated the effect of adding mesoporous $TiO_2$ ($m-TiO_2$) upon the separation performance of facilitated olefin transport membranes comprising poly(vinyl pyrrolidone), Ag nanoparticles, and 7,7,8,8-tetracyanoquinodimethane as the polymer matrix, olefin carrier, and electron acceptor, respectively. In particular, $m-TiO_2$ was prepared by means of a facile, mass-producible method using poly(vinyl chloride)-g-poly(oxyethylene methacrylate) graft copolymer as the template. The crystal phase of $m-TiO_2$ consisted of an anatase/rutile mixture, of crystallite size approximately 16 nm as determined by X-ray diffraction. The introduction of $m-TiO_2$ increased the membrane diffusivity, thereby increasing the mixed-gas permeance from 1.6 to 16.0 GPU ($1GPU=10^{-6}cm^3$(STP)/($s{\times}cm^2{\times}cmHg$), and slightly decreased the propylene/propane selectivity from 45 to 37. However, both the mixed-gas permeance and selectivity of the membrane containing $m-TiO_2$ rapidly decreased over time, whereas the membrane without $m-TiO_2$ had more stable long-term performance. This difference might be attributed to specific chemical interactions between $TiO_2$ and Ag nanoparticles, causing Ag to lose activity as an olefin carrier.