• Title/Summary/Keyword: Scanning transmission X-ray microscopy

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Preparation of Al@Fe2O3 Core-Shell Composites Using Amphiphilic Graft Copolymer Template

  • Patel, Rajkumar;Kim, Sang Jin;Kim, Jin Kyu;Park, Jung Su;Kim, Jong Hak
    • Korean Chemical Engineering Research
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    • v.52 no.2
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    • pp.209-213
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    • 2014
  • A graft copolymer of poly(vinyl chloride)-g-poly(oxyethylene methacrylate) (PVC-g-POEM) was synthesized via atom transfer radical polymerization (ATRP) and used as a structure-directing agent to prepare $Al@Fe_2O_3$ core-shell nanocomposites through a sol-gel process. The amphiphilic property of PVC-g-POEM allows for good dispersion of Al particles and leads to specific interaction with iron ethoxide, a precursor of $Fe_2O_3$. Secondary bonding interaction in the sol-gel composites was characterized by Fourier transform-infrared (FT-IR) spectroscopy. The well-organized morphology of $Al@Fe_2O_3$ core-shell nanocomposites was observed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Energy dispersive X-ray (EDX) and X-ray diffraction (XRD) were used to analyze the elemental composition and crystallization structure of the composites.

Synthesis of Praseodymium-Doped TiO2 Nanocatalysts by Sol-Microwave and Their Photocatalytic Activity Study

  • Huang, Fengping;Wang, Shuai;Zhang, Shuang;Fan, Yingge;Li, Chunxue;Wang, Chuang;Liu, Chun
    • Bulletin of the Korean Chemical Society
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    • v.35 no.8
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    • pp.2512-2518
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    • 2014
  • The praseodymium-doped $TiO_2$ photocatalyst samples, which could degrade methyl orange under UV irradiation, were prepared by sol-microwave method for improving the photocatalytic activity of $TiO_2$. The resulting materials were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), Transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Raman spectra, Fourier transform infrared spectra (FTIR) and Ultraviolet-visible diffuse reflectance spectra (UV-vis DRS). It was found Pr doping retarded the growth of crystalline size and the phase transformation from anatase to rutile, and narrowed the band gap energy. Praseodymium doping brought about remarkable improvement in the photoactivity. The optimal dopant amount of Pr was 2% by molar of cement and the calcination temperature was $500^{\circ}C$ for the best photocatalytic activity. The improvement of photocatalytic activity was ascribed to the occurrence of lattice distortion and the effective containment of the recombination of the electron-hole by $Pr^{3+}$.

Pt Electrocatalysts Composited on Electro-Spun Pt Nanowires for Direct Methanol Fuel Cells

  • An, Geon-Hyoung;Ahn, Hyo-Jin
    • Korean Journal of Materials Research
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    • v.22 no.8
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    • pp.421-425
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    • 2012
  • Two types of Pt nanoparticle electrocatalysts were composited on Pt nanowires by a combination of an electrospinning method and an impregnation method with NaBH4 as a reducing agent. The structural properties and electrocatalytic activities for methanol electro-oxidation in direct methanol fuel cells were investigated by means of scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry. In particular, SEM, HRTEM, XRD, and XPS results indicate that the metallic Pt nanoparticles with polycrystalline property are uniformly decorated on the electro-spun Pt nanowires. In order to investigate the catalytic activity of the Pt nanoparticles decorated on the electro-spun Pt nanowires, two types of 20 wt% Pt nanoparticles and 40 wt% Pt nanoparticles decorated on the electro-spun Pt nanowires were fabricated. In addition, for comparison, single Pt nanowires were fabricated via an electrospinning method without an impregnation method. As a result, the cyclic voltammetry and chronoamperometry results demonstrate that the electrode containing 40 wt% Pt nanoparticles exhibits the best catalytic activity for methanol electro-oxidation and the highest electrochemical stability among the single Pt nanowires, the 20 wt% Pt nanoparticles decorated with Pt nanowires, and the 40 wt% Pt nanoparticles decorated with Pt nanowires studied for use in direct methanol fuel cells.

The Effect of $Y_2O_3$ Addition on the Mechanical Alloying of $Ni_3$Al ($Ni_3$Al의 기계적합금화에 미치는 $Y_2O_3$ 첨가의 영향)

  • 이상태
    • Journal of Powder Materials
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    • v.4 no.3
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    • pp.205-213
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    • 1997
  • Mechanical alloying of $Ni_3Al$ and $Y_2O_3$ added ODS $Ni_3Al$ from elemental powders was investigated by the X-ray diffraction, differential scanning calorimeter, transmission electron microscopy and optical microscopy. The steady states of $Ni_3Al$ and ODS $Ni_3Al$ powders were reached after mechanical alloying with the condition of the ball-to-powder input ratio of 20:1 for 20 hours and 10 hours, respectively. The addition of nano-sized $Y_2O_3$ particles enhanced cold working and fracture, and subsequently accelerated MA of $Ni_3Al$ powders. DSC results of MAed $Ni_3Al$ powders showed four exothermic peaks at 14$0^{\circ}C$, 234$^{\circ}C$, 337$^{\circ}C$ and 385$^{\circ}C$. From the high temperature X-ray diffraction analysis, it was concluded that the peaks were resulted from the recovery solution of unalloyed Al in Ni, the formation of intermediate phase NiAl, and $LI_2$ ordering of MAed $Ni_3Al$ powders.

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Synthesis and Characterization of ZnS and ZnS/TiO2 Nanocomposites and Their Enhanced Photo-decolorization of MB and 1,5-Diphenyl Carbazide

  • Meng, Ze-Da;Ullah, Kefayat;Zhu, Lei;Ye, Shu;Oh, Won-Chun
    • Journal of the Korean Ceramic Society
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    • v.51 no.4
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    • pp.307-311
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    • 2014
  • ZnS and $ZnS/TiO_2$ were prepared by chemical deposition. The prepared photocatalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), and transmission electron microscopy (TEM). The generation of reactive oxygen species was detected by monitoring the oxidation reaction from 1,5-diphenyl carbazide (DPCI) to 1,5-diphenyl carbazone (DPCO). Excellent catalytic degradation of methylene blue (MB) solution was observed using the $ZnS/TiO_2$ composites during irradiation with visible light. The results show that the photocatalytic performance of $TiO_2$ nanoparticles is improved by loading with ZnS.

Effect of Al Precursor Type on Mesoporous Alumina Particles Prepared by Spray Pyrolysis (분무열분해공정에 의한 메조기공 알루미나 제조에 있어 Al 전구체 영향)

  • Kim, Joo-Hyun;Jung, Kyeong-Youl;Park, Kyun-Young
    • Journal of Powder Materials
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    • v.17 no.3
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    • pp.209-215
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    • 2010
  • Mesoporous alumina particles were prepared by spray pyrolysis using cetyltrimethyl-ammonium bromide (CTAB) as a structure directing agent and the effect of Al precursor types on the texture properties was studied using $N_2$ adsorption isotherms, small-angle X-ray scattering (SAXS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The surface area and the microstructure of alumina particles were significantly influenced by the Al precursor type. The largest BET surface area was obtained when Al chloride was used, whereas alumina particles prepared from Al acetate had the largest pore volume. According to small-angle X-ray scattering (SAXS) analysis, the alumina powders prepared using nitrate and acetate precursors had a clear single SAXS peak around $2{\theta}=1.0{\sim}1.5^{\circ}$, indicating that regular mesopores with sponge-like structure were produced. On the basis of TEM, SAXS, and $N_2$ isotherm results, the chloride precursor was most profitable to obtain the largest surface area ($265\;m^2/g$), whereas, the nitrate precursor is useful for the preparation of non-hollow mesoporous alumina with regular pore size, maintaining high surface area (${\sim}233\;m^2/g$).

The Photodegradation Effect of Organic Dye for Metal Oxide (Cr2O3, MgO and V2O3) Treated CNT/TiO2 Composites

  • Chen, Ming-Liang;Bae, Jang-Soon;Yoon, Hee-Seung;Lim, Chang-Sung;Oh, Won-Chun
    • Bulletin of the Korean Chemical Society
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    • v.32 no.3
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    • pp.815-820
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    • 2011
  • Three kinds of organometallic compounds (chromium acetylacetonate, magnesium acetate and vanadyl acetylacetonate) were used as transition metal precursor, titanium n-butoxide and multi-walled carbon nanotube as titanium and carbon precursor to prepare metal oxide-CNT/$TiO^2$ composites. The surface properties and morphology of metal oxide-CNT/$TiO^2$ composites were by Brauer-Emett-Teller (BET) surface area measurement, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and energy dispersive X-ray (EDX) analysis. The photocatalytic activity of prepared metal oxide-CNT/$TiO^2$ composites was determined by the degradation effect of methylene blue in an aqueous solution under irradiation of visible light.

Improved Tri-iodide Reduction Reaction of Co-TMPP/C as a Non-Pt Counter Electrode in Dye-Sensitized Solar Cells

  • Kim, Jy-Yeon;Lee, Jin-Kyu;Han, Sang-Beom;Lee, Young-Woo;Park, Kyung-Won
    • Journal of Electrochemical Science and Technology
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    • v.1 no.2
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    • pp.75-80
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    • 2010
  • We report Co-tetramethoxyphenylporphyrin on carbon particles (Co-TMPP/C) as a non-Pt catalyst for tri-iodide reduction in dye-sensitized solar cells (DSSCs). The presence of well-dispersed carbon and cobalt source in the catalyst surface is confirmed by transmission electron microscopy, scanning electron microscopy, and energy dispersive X-ray analysis. In the C 1s, Co 2p, and N 1s peaks measured by X-ray photoelectron spectroscopy, the C-N, Co-$N_4$, and N-C are assigned to the component at 285.7, 781.8, and 401 eV, respectively. Especially, the Co-TMPP/C shows improved current density, diffusion coefficient, and charge-transfer resistance in the ${I_3}^-/I^-$ redox reaction compared to conventional catalysts. Furthermore, in the DSSCs performance, the Co-TMPP/C shows increased short circuit current density, higher open circuit voltage, and improved cell efficieny in comparison with Pt/C.

Hydrothermal Synthesis, Characterization and Improved Activity of a Visible-Light-Driven ZnSe-Sensitized TiO2 Composite Photocatalyst

  • Zhu, Lei;Peng, Mei-Mei;Cho, Kwang Youn;Ye, Shu;Sarkar, Sourav;Ullah, Kefayat;Meng, Ze-Da;Oh, Won-Chun
    • Journal of the Korean Ceramic Society
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    • v.50 no.6
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    • pp.504-509
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    • 2013
  • In this study, ZnSe-$TiO_2$ composites were synthesized by a facile hydrothermal-assisted sol-gel process and characterized by nitrogen adsorption isotherms (77 K), X-ray diffraction (XRD), scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM) and UV-vis diffuse reflectance spectrophotometry. The photocatalytic activity was investigated by decoloration methylene blue (MB), methyl orange (MO), and rhodamine B (Rh.B) in an aqueous solution under visible light irradiation. The results revealed that the photocatalytic activity of the ZnSe-$TiO_2$ photocatalyst was much higher than that of pure$TiO_2$. The ZnSe nanoparticles, which act as a photosensitizer, not only extend the spectral response of $TiO_2$ to the visible region but also reduce charge recombinations.

Preparation of MWCNT/TiO2 Composites by Using MWCNTs and Titanium(IV) Alkoxide Precursors in Benzene and their Photocatalytic Effect and Bactericidal Activity

  • Oh, Won-Chun;Zhang, Feng-Jun;Chen, Ming-Liang
    • Bulletin of the Korean Chemical Society
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    • v.30 no.11
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    • pp.2637-2642
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    • 2009
  • In this present paper, we prepared $MWCNT/TiO_2$ composites by using pre-oxidized multi-walled carbon nanotubes (MWCNTs) with different titanium alkoxide precursors in benzene solvent. The composites were comprehensively characterized by BET surface area, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX) and UV-Vis absorption spectroscopy. The photoactivity of the prepared materials, under UV irradiation, was tested using methylene blue (MB) in aqueous solution. Finally, according to the results of MB removal experiment, it can be considered that the MB degradation infect mainly caused by photocatalytic effect of $TiO_2$. Furthermore, the bactericidal test of the composites was also determined. It was indicated that $MWCNT/TiO_2$ composites with sunlight had greater effectiveness for B. cereus, S. aureus and E. coli than any other experimental conditions.