• Title/Summary/Keyword: Electron diffraction data

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Self-Assembled ZnO Hexagonal Nano-Disks Grown by RF Sputtering

  • Jeong, Eun-Ji;Kim, Ji-Hyeon;Kim, Su-Jin;Gang, Hyeon-Cheol
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.461-461
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    • 2013
  • Over the last decade, zinc oxide (ZnO) thin films have attracted considerable attention owing to large band gap of 3.37 eV and large exciton binding energy of 60 meV at room temperature [1-3]. Recent interest in ZnO related researches has been switched into the fabrication and characterization of low-dimensional nanostructures, such as nano-wires and nano-dots that can be applicable to manufacture the optoelectronic devices such as ultraviolet lasers, light-emitting-diodes and detectors. Since the optical properties of ZnO nano-structures might be distinct from those of bulk materials or thin films, the low-dimensional phenomena should be examined further. In order to utilize such advanced optoelectronic devices, one of the challenges is how to control the surface state related emissions that are drastically increased with increasing the density of the nano-structures and the surface-to-volume ratio. This paper reports the synthesis and characterization of self-assembled ZnO hexagonal nano-disks grown by radio-frequency magnetron sputtering. X-ray diffraction data and scanning electron microscopy data showed that ZnO hexagonal nano-disks were nucleated on top of the flat surfaces as the film thickness reached to 1.56 ${\mu}m$ and then the number of nano-disks increased with increasing the film thickness. The lateral size of hexagonal nano-disks was ~720 nm and height was ~74 nm. The strong photo luminescence spectra obtained at 10 K was also observed, which was assigned to a surface exciton emission at 3.3628 eV arising from the surface sites of hexagonal nano-disks.

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Arsenic Contamination of Groundwater a Grave Concern: Novel Clay-based Materials for Decontamination of Arsenic (V)

  • Amrita Dwivedi;Diwakar Tiwari;Seung Mok Lee
    • Applied Chemistry for Engineering
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    • v.34 no.2
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    • pp.199-205
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    • 2023
  • Arsenic is a highly toxic element, and its contamination is widespread around the world. The natural materials with high selectivity and efficiency toward pollutants are important in wastewater treatment technology. In this study, the mesoporous synthetic hectorite was synthesized by facile hydrothermal crystallization of gels comprising silica, magnesium hydroxide, and lithium fluoride. Additionally, the naturally available clay was modified using zirconium at room temperature. Both synthetic and modified natural clays were employed in the removal of arsenate from aquatic environments. The materials were fully characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), and Fourier transform-infrared (FT-IR) analyses. The synthesized materials were used to remove arsenic (V) under varied physicochemical conditions. Both materials, i.e., Zr-bentonite and Zr-hectorite, showed high percentage removal of arsenic (V) at lower pH, and the efficiency decreased in an alkaline medium. The equilibrium-state sorption data agrees well with the Langmuir and Freundlich adsorption isotherms, and the maximum sorption capacity is found to be 4.608 and 2.207 mg/g for Zr-bentonite and Zr-hectorite, respectively. The kinetic data fits well with the pseudo-second order kinetic model. Furthermore, the effect of the background electrolytes study indicated that arsenic (V) is specifically sorbed at the surface of these two nanocomposites. This study demonstrated that zirconium intercalated synthetic hectorite as well as zirconium modified natural clays are effective and efficient materials for the selective removal of arsenic (V) from aqueous medium.

A Transmission Electron Microscopy Study on the Crystallization Behavior of In-Sb-Te Thin Films (In-Sb-Te 박막의 결정화 거동에 관한 투과전자현미경 연구)

  • Kim, Chung-Soo;Kim, Eun-Tae;Lee, Jeong-Yong;Kim, Yong-Tae
    • Applied Microscopy
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    • v.38 no.4
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    • pp.279-284
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    • 2008
  • The phase change materials have been extensively used as an optical rewritable data storage media utilizing their phase change properties. Recently, the phase change materials have been spotlighted for the application of non-volatile memory device, such as the phase change random access memory. In this work, we have investigated the crystallization behavior and microstructure analysis of In-Sb-Te (IST) thin films deposited by RF magnetron sputtering. Transmission electron microscopy measurement was carried out after the annealing at $300^{\circ}C$, $350^{\circ}C$, $400^{\circ}C$ and $450^{\circ}C$ for 5 min. It was observed that InSb phases change into $In_3SbTe_2$ phases and InTe phases as the temperature increases. It was found that the thickness of thin films was decreased and the grain size was increased by the bright field transmission electron microscopy (BF TEM) images and the selected area electron diffraction (SAED) patterns. In a high resolution transmission electron microscopy (HRTEM) study, it shows that $350^{\circ}C$-annealed InSb phases have {111} facet because the surface energy of a {111} close-packed plane is the lowest in FCC crystals. When the film was heated up to $400^{\circ}C$, $In_3SbTe_2$ grains have coherent micro-twins with {111} mirror plane, and they are healed annealing at $450^{\circ}C$. From the HRTEM, InTe phase separation was occurred in this stage. It can be found that $In_3SbTe_2$ forms in the crystallization process as composition of the film near stoichiometric composition, while InTe phase separation may take place as the composition deviates from $In_3SbTe_2$.

The effect of low temperature aging on the mechanical property & phase stability of Y-TZP ceramics

  • Kim, Hyung-Tae;Han, Jung-Suk;Yang, Jae-Ho;Lee, Jai-Bong;Kim, Sung-Hun
    • The Journal of Advanced Prosthodontics
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    • v.1 no.3
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    • pp.113-117
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    • 2009
  • STATEMENT OF PROBLEM. Recently Yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) has been introduced due to superior flexural strength and fracture toughness compared to other dental ceramic systems. Although zirconia has outstanding mechanical properties, the phenomenon of decrease in the life-time of zirconia resulted from degradation in flexural strength after low temperature aging has been reported. PURPOSE. The objective of this study was to investigate degradation of flexural strength of Y-TZP ceramics after various low temperature aging treatments and to evaluate the phase stability and micro-structural change after aging by using X-ray diffraction analysis and a scanning electron microscope (SEM). MATERIAL AND METHODS. Y-TZP blocks of Vita In-Ceram YZ (Vita Zahnfabrik, Bad $S\ddot{a}ckingen$, Germany) were prepared in 40 mm (length) $\times$ 4 mm (width) $\times$ 3 mm (height) samples. Specimens were artificially aged in distilled water by heat-treatment at a temperature of 75, 100, 125, 150, 175, 200, and $225^{\circ}C$ for 10 hours, in order to induce the phase transformation at the surface. To measure the mechanical property, the specimens were subjected to a four-point bending test using a universal testing machine (Instron model 3365; Instron, Canton, Mass, USA). In addition, X-ray diffraction analysis (DMAX 2500; Rigaku, Tokyo, Japan) and SEM (Hitachi s4700; Jeol Ltd, Tokyo, Japan) were performed to estimate the phase transformation. The statistical analysis was done using SAS 9.1.3 (SAS institute, USA). The flexural strength data of the experimental groups were analyzed by one-way analysis of variance and to detect statistically significant differences ($\alpha$= .05). RESULTS. The mean flexural strength of sintered Vita In-Ceram YZ without autoclaving was 798 MPa. When applied aging temperature at below $125^{\circ}C$ for 10 hours, the flexural strength of Vita In-Ceram YZ increased up to 1,161 MPa. However, at above $150^{\circ}C$, the flexural strength started to decrease. Although low temperature aging caused the tetragonal-to-monoclinic phase transformation related to temperature, the minimum flexural strength was above 700 MPa. CONCLUSION. The monoclinic phase started to appear after aging treatment above $100^{\circ}C$. With the higher aging temperature, the fraction of monoclinic phase increased. The ratio of monoclinic/tetragonal + monoclinic phase reached a plateau value, circa 75% above $175^{\circ}C$. The point of monoclinic concentration at which the flexural strength begins to decrease was between 12% and 54%.

Talc Mineralization in the Middle Ogcheon Metamorphic Belt (II) : Poongjeon Talc Deposit (중부옥천변성대의 활석광화작용에 관한 연구 (II) : 풍전활석광상을 중심으로)

  • Park, Hee-In;Lee, In Sung;Hur, Soon Do;Shin, Dong Bok
    • Economic and Environmental Geology
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    • v.30 no.6
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    • pp.543-551
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    • 1997
  • Poongjeon talc deposits is emplaced in dolomite and dolomitic limestone of the Cambro-Ordovician Samtaesan Formation. Ore in Poongjeon is low grade talc and the deposit has been known as the contact metasomatic or hydrothermal replacement type related to the intrusion of late Cretaceous granite in this area. X-ray diffraction, electron microprobe analysis, fluid inclusion and stable isotope analysis were utilized to examine the mineralogy of the ore and the origin of the ore fluid. The ore from Poongjeon mine mainly consists of talc and tremolite with minor amount of illite, vermiculite, smectite, and chlorite-vermiculite mixed layer. Occurrence of ore body indicates that the talc-tremolite ore was formed through the replacement by the $SiO_2$-rich hydrothermal fluid along the bedding and dike boundaries, or contact of amphibolite and basic dike with carbonate rocks. The temperature and pressure of the ore forming fluids at the time of the talc mineralization were estimated as $350^{\circ}C$ and 400 bar, respectively, based on the heating and freezing data of the fluid inclusions in quartz from talc-tremolite veins. During the talc-tremolite formation, fluids were divided into $CO_2$-enriched fluid and $CO_2$-poor fluid from $CO_2$ immiscibility (or effervescence). Oxygen isotope values (${\delta}^{18}O$) of the talc-tremolite fall within a range between 12.2 and 12.9‰. Hydrogen isotope values(${\delta}D$) of the ore range from -60 to -85‰ and $H_2O$ contents range from 2.0 to 3.4 wt.%. ${\delta}^{18}O$ and ${\delta}D$ values of talc ore indicate that the hydrothermal fluid involved in talc-tremolite formation was of igneous origin. Oxygen and hydrogen isotopic exchange between talc ore and the surface water was negligible after talc-tremolite ore formation.

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Synthesis and characterization of carbon doped TiO2 photocatalysts supported on stainless steel mesh by sol-gel method

  • Tijani, JO.;Fatoba, OO.;Totito, TC.;Roos, WD.;Petrik, LF.
    • Carbon letters
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    • v.22
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    • pp.48-59
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    • 2017
  • This study synthesized pure anatase carbon doped $TiO_2$ photocatalysts supported on a stainless steel mesh using a sol-gel solution of 8% polyacrylonitrile (PAN)/dimethylformamide (DMF)/$TiCl_4$. The influence of the pyrolysis temperature and holding time on the morphological characteristics, particle sizes and surface area of the prepared catalyst was investigated. The prepared catalysts were characterized by several analytical methods: high resolution scanning electron microscopy (HRSEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), and X-ray photoelectron spectroscopy (XPS). The XRD patterns showed that the supported $TiO_2$ nanocrystals are typically anatase, polycrystalline and body-centered tetragonal in structure. The EDS and XPS results complemented one another and confirmed the presence of carbon species in or on the $TiO_2$ layer, and the XPS data suggested the substitution of titanium in $TiO_2$ by carbon. Instead of using calcination, PAN pyrolysis was used to control the carbon content, and the mesoporosity was tailored by the applied temperature. The supported $TiO_2$ nanocrystals prepared by pyrolysis at 300, 350, and $400^{\circ}C$ for 3 h on a stainless steel mesh were actual supported carbon doped $TiO_2$ nanocrystals. Thus, $PAN/DMF/TiCl_4$ offers a facile, robust sol-gel related route for preparing supported carbon doped $TiO_2$ nanocomposites.

Graphitization of PAN-based carbon fibers by CO2 laser irradiation

  • Yao, Liangbo;Yang, Weimin;Li, Sanyang;Sha, Yang;Tan, Jing;An, Ying;Li, Haoyi
    • Carbon letters
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    • v.24
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    • pp.97-102
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    • 2017
  • Graphite fibers are materials with a high specific modulus that have attracted much interest in the aerospace industry, but their high manufacturing cost and low yield are still problems that prevent their wide applications in practice. This paper presents a laser-based process for graphitization of carbon fiber (CF) and explores the effect of laser radiation on the microstructure of CF. The obtained Raman spectra indicate that the outer surface of CF evolves from turbostratic structures into a three-dimensional ordered state after being irradiated by a laser. The X-ray diffraction data revealed that the growth of crystallite was parallel to the fiber axis, and the interlayer spacing $d_{002}$ decreased from 0.353 to 0.345 nm. The results of scanning electron microscopy revealed that the surface of irradiated CFs was rougher than that of the unirradiated ones and there were scale-like small fragments that had peeled off from the fibers. The tensile modulus increased by 17.51% and the Weibull average tensile strength decreased by 30.53% after being irradiated by a laser. These results demonstrate that the laser irradiation was able to increase the graphitization degree of the CFs, which showed some properties comparable to graphite fibers.

Preparation and Characterization of Simvastatin Solid Dispersion using Aqueous Solvent

  • Kim, Kwang-Hyeon;Park, Jun-Bom;Choi, Won-Jae;Lee, Han-Seung;Kang, Chin-Yang
    • Journal of Pharmaceutical Investigation
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    • v.41 no.4
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    • pp.239-247
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    • 2011
  • Simvastatin is an inhibitor of 3-hydroxy-3-methylglutaryl-coenzyme A (HMG-CoA) reductase, which catalyzes the conversion of HMG-CoA to mevalonate, an early and rate-limiting step in the biosynthesis of cholesterol. Simvastatin has good permeability, but it also has low solubility (BCS class II), which reduces its bioavailability. To overcome this problem, a solid dispersion is formed using a spray-dryer with polymeric material carrier to potentially enhance the dissolution rate and extend drug absorption. As carriers for solid dispersion, Gelucire$^{(R)}$44/14 and Gelucire$^{(R)}$ 50/13 are semisolid excipients that greatly improve the bioavailability of poorly-soluble drugs. To avoid any toxic effects of an organic solvent, we used aqueous medium to melt Tween$^{(R)}$ 80 and distilled water. The structural behaviors of the raw materials and the solid dispersion were analyzed by differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD) and scanning electron microscopy (SEM). The DSC and PXRD data indicated that the crystalline structure of simvastatin was transformed to an amorphous structure through solid dispersion. Then, solid dispersion-based tablets containing 20 mg simvastatin were prepared with excipients. Dissolution tests were performed in distilled water and artificial intestinal fluid using the USP paddle II method. Compared with that of the commercial tablet (Zocor$^{(R)}$ 20 mg), the release of simvastatin from solid dispersion based-tablet was more efficient. Although the stability study is not complete, this solid dispersion system is expected to deliver poorly water-soluble drugs with enhanced bioavailability and less toxicity.

Phases and phase Equilibria of the Pt-Sb System (백금-안티모니 계의 식평구 및 화합흉에 대한 연구)

  • 김원사
    • Korean Journal of Crystallography
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    • v.4 no.1
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    • pp.18-24
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    • 1993
  • The phase diagram of the Pt-Sb system was reinvestigated, using the conventional sealedcapsule technique. The identification of phases present in the reaction products was made by reflected light microscopy, X-ray diffraction and electron microprobe analysis. The existence of compounds, Pt5Sb, Pt3Sb, Pt3Sb2, PtSb and PtSb5 was confirmed. A new phase, Pt5Sb with a composition of 83at% Pt and tetragonal structure of the lattice parameters a=3.948(3), c=16.85(1)A, was found. The X-ray powder data of Ptsb may be indexable on a tetragonal cell with a=3.9455(7), c=16.959(5)A. PtSb is stoichiometric up to 800t and becomes Pt-deficient as much as lat% at 1000t. Solid solubility limits of Sb in Pt were determined to be 7.5,10.0 and 6.1at% at 1000˚,800˚ and 600˚ , respectively. The earlier reported Pts Sbf was not found in this study. The liquidus curve between the Ptsb2 and Sb phases was revised.

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Effects of B Doping on Structural, Optical, and Electrical Properties of ZnO Nanorods Grown by Hydrothermal Method

  • Kim, Soaram;Nam, Giwoong;Park, Hyunggil;Yoon, Hyunsik;Kim, Byunggu;Kim, Jin Soo;Kim, Jong Su;Leem, Jae-Young
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.337-337
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    • 2013
  • ZnO seed layers were deposited on a quartz substrate using the sol-gel method, and B-doped ZnO (BZO) nanorods with different B concentrations ranging from 0 to 2.5 at.% were grown on the ZnO seed layers by the hydrothermal method. The structural, optical, electrical propertiesof the ZnO and BZO nanorods were investigated using field-emission scanning electron microscopy, X-ray diffraction (XRD), photoluminescence (PL), ultraviolet-visible spectroscopy, and hall effect. The ZnO and BZO nanorods grew well aligned on the surface of the quartz substrates. From the XRD data, it can be seen that the B doping is responsible for the distortion of the ZnO lattice. The PL spectra show near-band-edge emission and deep-level emission, and they also show that B doping significantly affects the PL properties of ZnO nanorods. The optical band gaps are changed by B doping, and thus the Urbach energy value changed with the optical band gap of the ZnO nanorods. From the hall measurements, it can be observed that the values of electrical resistivity, carrier concentration, and mobility are changed by B doping.

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