• Title/Summary/Keyword: TEM Journal

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Fabrication and Characterization of Titanate Nanotube Supported ZSM-5 Zeolite Composite Catalyst for Ethanol Dehydration to Ethylene

  • Wu, Liangpeng;Li, Xinjun;Yuan, Zhenhong;Chen, Yong
    • Bulletin of the Korean Chemical Society
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    • v.35 no.2
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    • pp.525-530
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    • 2014
  • Titanium dioxide nanotube supported ZSM-5 zeolite composite catalyst was fabricated by decorating ZSM-5 zeolite on the hydrothermally synthesized titanium dioxide via hydrothermal process and subsequent annealing. The catalyst was characterized by X-ray powder diffraction (XRD), Transmission electron microscopy (TEM) and Nitrogen adsorption-desorption (BET). The surface acidity of the catalyst was measured by means of Fourier transform infrared (FT-IR) spectrum of pyridine adsorption. And the catalytic activity for ethanol dehydration to ethylene was evaluated in a continuous flow fixed-bed reactor. Attributed to the increase of the effective surface acid sites caused by titanium dioxide nanotube as electron acceptor, titanium dioxide nanotube supported ZSM-5 zeolite composite catalyst exhibits strongly enhanced activity for ethanol dehydration to ethylene.

Photoluminescence Imaging of SiO2@ Y2O3:Eu(III) and SiO2@ Y2O3:Tb(III) Core-Shell Nanostructures

  • Cho, Insu;Kang, Jun-Gill;Sohn, Youngku
    • Bulletin of the Korean Chemical Society
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    • v.35 no.2
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    • pp.575-580
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    • 2014
  • We uniformly coated Eu(III)- and Tb(III)-doped yttrium oxide onto the surface of $SiO_2$ spheres and then characterized them by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction crystallography and UV-Visible absorption. 2D and 3D photoluminescence image map profiles were reported for the core-shell type structure. Red emission peaks of Eu(III) were observed between 580 to 730 nm and assigned to $^5D_0{\rightarrow}^7F_J$ (J = 0 - 4) transitions. The green emission peaks of Tb(III) between 450 and 650 nm were attributed to the $^5D_4{\rightarrow}^7F_J$ (J = 6, 5, 4, 3) transitions. For annealed samples, Eu(III) ions were embedded at a $C_2$ symmetry site in $Y_2O_3$, which was accompanied by an increase in luminescence intensity and redness, while Tb(III) was changed to Tb(IV), which resulted in no green emission.

Preparation of Micro-/Macroporous Carbons and Their Gas Sorption Properties

  • Hwang, Yong-Kyung;Shin, Hye-Seon;Hong, Jin-Yeon;Huh, Seong
    • Bulletin of the Korean Chemical Society
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    • v.35 no.2
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    • pp.377-382
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    • 2014
  • Micro-/macroporous carbons (MMCs) were prepared using a hollow mesoporous silica capsule (HMSC) as a sacrificial hard template. The carbonization process after the infiltration of furfuryl alcohol into the template-free HMSC material afforded MMC materials in high yield. The hard template HMSC could be removed by HF etching without deteriorating the structure of MMC. The MMC materials were fully characterized by SEM, TEM, PXRD, XPS, and Raman spectroscopy. The replication processes were so successful that MMCs exhibited a hollow capsular structure with multimodal microporosity. Detailed textural properties of MMC materials were investigated by volumetric $N_2$ adsorption-desorption analysis at 77 K. To explore the gas sorption abilities of MMCs for other gases, $H_2$ and $CO_2$ sorption analyses were also performed at various temperatures. The multimodal MMC materials were found to be good sorbents for both $H_2$ and $CO_2$ at low pressure.

Synthesis of CdS Nanocrystals with Different Shapes via a Colloidal Method

  • Bai, Jie;Liu, Changsong;Niu, Jinzhong;Wang, Hongzhe;Xu, Shasha;Shen, Huaibin;Li, Lin Song
    • Bulletin of the Korean Chemical Society
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    • v.35 no.2
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    • pp.397-400
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    • 2014
  • Size- and shape-controlled monodisperse wurtzite structured CdS nanorods have been successfully synthesized using a facile solution-based colloidal method. Depending on the control of injection/growth temperatures and the variation of Cd-to-S molar ratios, the morphology of the CdS nanocrystals (NCs) can be adjusted into bullet-like, rod-like, and dot-like shapes. X-ray diffraction (XRD), transition electron microscopy (TEM), and absorption spectroscopy were used to characterize the structure, morphology, and optical properties of as-synthesized CdS NCs. It was found that uniform CdS nanorods could be successfully synthesized when the injection and growth temperatures were very high (> $360^{\circ}C$). The aspect ratios of different shaped (bullet-like or rod-like) CdS NCs could be controlled by simply adjusting the molar ratios between Cd and S.

Heteroepitaxial Growth of Single 3C-SiC Thin Films on Si (100) Substrates Using a Single-Source Precursor of Hexamethyldisilane by APCVD

  • Chung, Gwiy-Sang;Kim, Kang-San
    • Bulletin of the Korean Chemical Society
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    • v.28 no.4
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    • pp.533-537
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    • 2007
  • This paper describes the heteroepitaxial growth of single-crystalline 3C-SiC (cubic silicon carbide) thin films on Si (100) wafers by atmospheric pressure chemical vapor deposition (APCVD) at 1350 oC for micro/nanoelectromechanical system (M/NEMS) applications, in which hexamethyldisilane (HMDS, Si2(CH3)6) was used as a safe organosilane single-source precursor. The HMDS flow rate was 0.5 sccm and the H2 carrier gas flow rate was 2.5 slm. The HMDS flow rate was important in obtaing a mirror-like crystalline surface. The growth rate of the 3C-SiC film in this work was 4.3 μm/h. A 3C-SiC epitaxial film grown on the Si (100) substrate was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), reflection high energy electron diffraction (RHEED), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and Raman scattering, respectively. These results show that the main chemical components of the grown film were single-crystalline 3C-SiC layers. The 3C-SiC film had a very good crystal quality without twins, defects or dislocations, and a very low residual stress.

Novel Method for the Preparation of Mesoporous BaSO4 Material with Thermal Stability by Spray Pyrolysis

  • Nagaraja, Bhari Mallanna;Abimanyu, Haznan;Jung, Kwang-Deog;Yoo, Kye-Sang
    • Bulletin of the Korean Chemical Society
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    • v.29 no.5
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    • pp.1007-1012
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    • 2008
  • Spray pyrolysis has been found as an excellent method for the preparation of mesoporous barium sulfate at higher temperature. Ethylene glycol, a reducing agent, and solvents had good inhibition effect for the preparation of $BaSO_4$ nano particles. The $BaSO_4$ solution was sprayed at 500 & 800 ${^{\circ}C}$ using different solvents such as methanol, ethanol, propanol and n-butyl alcohol. $N_2$ adsorption-desorption isotherm revealed that $BaSO_4$ is micropore free, possessing narrow mesopores size distribution and high BET surface areas of 72.52 $m^2\;g^{-1}$ at 800 ${^{\circ}C}$ using propanol as an additive. Scanning electron microscopy (SEM) indicates that the morphology of $BaSO_4$ nano material shows uniform shell like particles. Transmission electron microscopy (TEM) proved that the resulting BaSO4 nano particles were uniform in size and the average particle size was 4-8 nm. The surface functionality and ethylene glycol peaks were assessed by Fourier transform infrared resonance (FTIR) spectroscopy. Low intensity ethylene glycol specific absorption peak was observed in propanol which proved that propanol had good inhibition effect on the structural morphology of nano particles.

Submicrospheres as Both a Template and the Catalyst Source. Silica Submicro-reactor Dotted with Palladium Nanoparticles as Catalysts

  • Kim, Sung Min;Noh, Tae Hwan;Jung, Ok-Sang
    • Bulletin of the Korean Chemical Society
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    • v.34 no.4
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    • pp.1127-1130
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    • 2013
  • Formation of the monodisperse submicrospheres consisting of ionic palladium(II) complexes, $[(Me_4en)Pd(L)]_2(X)_4$($Me_4en$ = N,N,N',N'-tetramethylethylenediamine; L = bis(4-(4-pyridylcarboxyl)phenyl)methane; $X^-=BF_4{^-}$ and $ClO_4{^-}$), has been carried out without any templates or additives. The submicrospheres were coated with silicates, and then calcined in air at $550^{\circ}C$ for 1 h, to efficiently form hollow-spherical $SiO_2$ submicro-reactors dotted with palladium(0) nanoparticles (PdNPs). That is, the submicrospheres act as both a template and a source of the palladium metal nanoparticles. The submicro-reactors containing nano-catalysts have been characterized by means of SEM, TEM, and XPS. Notably, the reactors were proved to be very effective for Suzuki-Miyaura cross-coupling and hydrogenation reactions.

Synthesis of Ni-Ag Core-shell Nanoparticles by Polyol process and Microemulsion Process

  • Nguyen, Ngoc Anh Thu;Park, Joseph G.;Kim, Sang-Hern
    • Bulletin of the Korean Chemical Society
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    • v.34 no.10
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    • pp.2865-2870
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    • 2013
  • Ni-Ag core-shell nanoparticles were synthesized by polyol process and microemulsion technique successfully. In the polyol process, a chemical reduction method for preparing highly dispersed pure nickel and Ag shell formation have been reported. The approach involved the control of reaction temperature and reaction time in presence of organic solvent (ethylene glycol) as a reducing agent for Ag cation with poly(vinyl-pyrrolidone) (PVP. Mw = 40000) as a capping agent. In microemulsion method, the emulsion was prepared by water/cetyltrimetylammonium bromide (CTAB)/cyclohexane. The size of microemulsion droplet was determined by the molar ratio of water to surfactant (${\omega}_o$). The core-shell formation along with the change in structural phase and stability against oxidation at high temperature heat treatments of nanoparticles were investigated by X-ray diffraction and TEM analysis. Under optimum conditions the polyol process gives the Ni-Ag core-shell structures with 13 nm Ni core covered with 3 nm Ag shell, while the microemulsion method gives Ni core diameter of 8 nm with Ag shell of thickness 6 nm. The synthesized Ni-Ag core-shell nanoparticles were stable against oxidation up to $300^{\circ}C$.

Outer Diameter Stress Corrosion Cracking Susceptibility of Steam Generator Tubing Materials (증기발생기 전열관 재료의 2차측 응력부식균열 민감성)

  • Kim, Dong-Jin;Kim, Hyun Wook;Kim, Hong Pyo
    • Corrosion Science and Technology
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    • v.10 no.4
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    • pp.118-124
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    • 2011
  • Alloy 600 (Ni 75 wt%, Cr 15 wt%, Fe 10 wt%) as a heat exchanger tube of the steam generator (SG) in nuclear power plants (NPP) has been degraded by various corrosion mechanism during the long-term operation. Especially lead (Pb) is known to be one of the most deleterious species in the secondary system causing outer diameter stress corrosion cracking (ODSCC). Oxide formation and breakdown is requisite for SCC initiation and propagation. Therefore it is expected that a property change of the oxide formed on SG tubing materials by lead addition into a solution is closely related to PbSCC. In the present work, the SCC susceptibility was assessed by using a slow strain rate test (SSRT) in caustic solutions with and without lead for Alloy 600 and Alloy 690 (Ni 60 wt%, Cr 30 wt%, Fe 10 wt%) used as an alternative of Alloy 600 because of outstanding superiority to SCC. The results were discussed in view of the oxide property formed on Alloy 600 and Alloy 690. The oxides formed on Alloy 600 and Alloy 690 in aqueous solutions with and without lead were examined by using a transmission electron microscopy (TEM), equipped with an energy dispersive x-ray spectroscopy (EDXS).

Development of Poly(methyl methacrylate)-Clay Nanocomposites by Using Power Ultrasonic Wave

  • Ryu, Joung Gul;Lee, Jae Wook;Kim, Hyungsu
    • Macromolecular Research
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    • v.10 no.4
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    • pp.187-193
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    • 2002
  • Several methods have been used to synthesize polymer-clay nanocomposites. In-situ polymerization with clay belongs to a classical way to develop nano-structured materials, while melt intercalation is being recognized as another useful approach due to its versatility and environmentally benign character. In this research, we prepared polymer-clay nanocomposites based on the poly (methyl methacrylate) and organically modified montmorillonite via two-stage sonication process. According to the unique mode of power ultrasonic wave, the sonication during processing led to enhanced breakup of the clay agglomerates and reduction in size of the dispersed phase. Optimum conditions to form stable exfoliated nanocomposites were studied for various compositions and conditions. It was found that a novel attempt carried out in this study yielded further improvement in the mechanical performance of the nanocomposites compared to those produced by the conventional melt mixing process, as revealed by DMA, XRD and TEM. And rheological properties of nanocomposites were measured by ARES. As a result, sonicated PMMA-clay nanocomposites exhibits enhanced properties such as storage modulus and thermal stability than that of neat PMMA.