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

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Effect of Drying Methods on the Production of Graphenes Oxide Powder Prepared by Chemical Exfoliation (화학적 박리법으로 제조된 산화그래핀 분말의 건조방법에 따른 물성 비교)

  • Rho, Sangkyun;Noh, Kyung-Hun;Eom, Sung-Hun;Hur, Seung Hyun;Lim, Hyung Mi
    • Korean Journal of Materials Research
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    • v.23 no.10
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    • pp.592-598
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    • 2013
  • Graphene oxide powders prepared by two different drying processes, freeze drying and spray drying, were studied to compare the effect of the drying method on the physical properties of graphene oxide powder. The graphene oxide dispersion was prepared from graphite by chemical delamination with the aid of sulfuric acid and permanganic acid, and the dispersion was further washed and re-dispersed in a mixed solvent of water and isopropyl alcohol. A freeze drying method can feasibly minimize damage to the sample, but it requires a long process time. In contrast, spray drying is able to remove a solvent in a relatively short time, though this process requires exposure to a high temperature for a rapid evaporation of the solvent. The powders prepared by freeze drying and spray drying were characterized and compared by Raman spectroscopy, X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, and by an elemental analysis. The graphene oxide powders showed similar chemical compositions; however, the morphologies of the powders differed in that the graphene oxide prepared by spray drying had a winkled morphology and a higher apparent density compared to the powder prepared by freeze drying. The graphene oxide powders were reduced at $900^{\circ}C$ in an atmosphere of $N_2$. The effect of the drying process on the properties of the reduced graphene oxide was examined by SEM, TEM and Raman spectroscopy.

Photocatalysis of TiO2/WO3 Composites Synthesized by Ball Milling (볼밀을 이용한 TiO2/WO3 복합체 제조 및 광촉매 특성)

  • Yu, Su-Yeol;Nam, Chunghee
    • Journal of Powder Materials
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    • v.25 no.4
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    • pp.316-321
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    • 2018
  • Composites of P25 $TiO_2$ and hexagonal $WO_3$ nanorods are synthesized through ball-milling in order to study photocatalytic properties. Various composites of $TiO_2/WO_3$ are prepared by controlling the weight percentages (wt%) of $WO_3$, in the range of 1-30 wt%, and milling time to investigate the effects of the composition ratio on the photocatalytic properties. Scanning electron microscopy, x-ray diffraction, and transmission electron microscopy are performed to characterize the structure, shape and size of the synthesized composites of $TiO_2/WO_3$. Methylene blue is used as a test dye to analyze the photocatalytic properties of the synthesized composite material. The photocatalytic activity shows that the decomposition efficiency of the dye due to the photocatalytic effect is the highest in the $TiO_2/WO_3$ (3 wt%) composite, and the catalytic efficiency decreases sharply when the amount of $WO_3$ is further increased. As the amount of $WO_3$ added increases, dye-removal by adsorption occurs during centrifugation, instead of the decomposition of dyes by photocatalysts. Finally, $TiO_2/WO_3$ (3 wt%) composites are synthesized with various milling times. Experimental results show that the milling time has the best catalytic efficiency at 30 min, after which it gradually decreases. There is no significant change after 1 hour.

NO2 Sensing Properties of β-Bi2O3 Nanowires Sensor Coated with Pd Nanoparticles (Pd 나노입자가 코팅된 β-Bi2O3 나노와이어의 NO2 검출 특성)

  • Park, Sunghoon;Kang, Wooseung
    • Journal of the Korean institute of surface engineering
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    • v.48 no.6
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    • pp.303-308
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    • 2015
  • Pd-functionalized ${\beta}-Bi_2O_3$ nanowires are synthesized by thermal evaporation of Bi powder using VLS mechanism followed by Pd coating and annealing. In this study, sensing properties of Pd-functionalized ${\beta}-Bi_2O_3$ nanowires sensor to selected concentrations of $NO_2$ gas were examined. Scanning electron microscopy showed that the nanowires with diameters in a range of 100 - 200 nm and lengths of up to a few tens of micrometers. Transmission electron microscopy and X-ray diffraction confirmed that the products corresponded to the nanowires of ${\beta}-Bi_2O_3$ crystals and Pd nanoparticles. Pd-functionalized ${\beta}-Bi_2O_3$ nanowires sensor showed an enhanced sensing performance to $NO_2$ gas compared to as-synthesized ${\beta}-Bi_2O_3$ nanowires sensor. As synthesized and Pd-functionalized ${\beta}-Bi_2O_3$ nanowire sensors showed responses of 178% - 338% and 196% - 535% at $300^{\circ}C$, respectively, to 0.05 - 2 ppm $NO_2$. In addition, the underlying mechanism of the enhancement of the sensing properties of ${\beta}-Bi_2O_3$ nanowires by Pd-functionalization is discussed.

Photocatalytic Degradation of Organic Dyes with Nanomaterials (나노소재를 이용한 유기염료 광촉매 분해 반응)

  • Hong, Sung-Kyu;Yu, Gu-Yong;Lim, Chung-Sun;Ko, Weon-Bae
    • Elastomers and Composites
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    • v.45 no.3
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    • pp.206-211
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    • 2010
  • Zinc oxide(ZnO) nanoparticles were synthesized by reacting an aqueous-alcoholic zinc nitrate solution to sodium hydroxide under ultrasonic irradiation at room temperature. The fullerene($C_{60}$) and ZnO nanoparticles were heated individually in an electric furnace for two hours at $700^{\circ}C$. The morphology and optical properties of the $C_{60}$ and ZnO nanoparticles were characterized by X-ray diffraction(XRD), scanning electron microscopy(SEM), transmission electron microscopy(TEM) and ultraviolet/visible (UV-vis) spectroscopy. The photocatalytic activity of the heated and unheated the $C_{60}$ and ZnO nanoparticles for the decomposition of methylene blue(MB), methyl orange(MO) and rhodamine B(RhB) was examined using UV-vis spectroscopy.

Enhanced Si based negative electrodes using RF/DC magnetron sputtering for bulk lithium ion batteries

  • Hwang, Chang-Muk;Park, Jong-Wan
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.277-277
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    • 2010
  • The capacity of the carbonaceous materials reached ca. $350\;mAhg^{-1}$ which is close to theorestical value of the carbon intercalation composition $LiC_6$, resulting in a relatively low volumetric Li capacity. Notwithstanding the capacities of carbon, it will not adjust well to the need so future devices. Silicon shows the highest gravimetric capacities (up to $4000\;mAhg^{-1}$ for $Li_{21}Si_5$). Although Si is the most promising of the next generation anodes, it undergoes a large volume change during lithium insertion and extraction. It results in pulverization of the Si and loss of electrical contact between the Si and the current collector during the lithiation and delithiation. Thus, its capacity fades rapidly during cycling. We focused on electrode materials in the multiphase form which were composed of two metal compounds to reduce the volume change in material design. A combination of electrochemically amorphous active material in an inert matrix (Si-M) has been investigated for use as negative electrode materials in lithium ion batteries. The matrix composited of Si-M alloys system that; active material (Si)-inactive material (M) with Li; M is a transition metal that does not alloy with Li with Li such as Ti, V or Mo. We fabricated and tested a broad range of Si-M compositions. The electrodes were sputter-deposited on rough Cu foil. Electrochemical, structural, and compositional characterization was performed using various techniques. The structure of Si-M alloys was investigated using X-ray Diffractometer (XRD) and transmission electron microscopy (TEM). Surface morphologies of the electrodes are observed using a field emission scanning electron microscopy (FESEM). The electrochemical properties of the electrodes are studied using the cycling test and electrochemical impedance spectroscopy (EIS). It is found that the capacity is strongly dependent on Si content and cycle retention is also changed according to M contents. It may be beneficial to find materials with high capacity, low irreversible capacity and that do not pulverize, and that combine Si-M to improve capacity retention.

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Photocatalytic Properties of the Ag-Doped TiO2 Prepared by Sol-Gel Process/Photodeposition (졸-겔공정/광증착법을 이용한 Ag-Doped TiO2 합성 및 광촉매 특성)

  • Kim, Byeong-Min;Kim, Jung-Sik
    • Korean Journal of Materials Research
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    • v.26 no.2
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    • pp.73-78
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    • 2016
  • $TiO_2$ nanoparticles were synthesized by a sol-gel process using titanium tetra isopropoxide as a precursor at room temperature. Ag-doped $TiO_2$ nanoparticles were prepared by photoreduction of $AgNO_3$ on $TiO_2$ under UV light irradiation and calcinated at $400^{\circ}C$. Ag-doped $TiO_2$ nanoparticles were characterized for their structural and morphological properties by X-ray diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and transmission electron microscopy (TEM). The photocatalytic properties of the $TiO_2$ and Ag-doped $TiO_2$ nanoparticles were evaluated according to the degree of photocatalytic degradation of gaseous benzene under UV and visible light irradiation. To estimate the rate of photolysis under UV (${\lambda}=365nm$) and visible (${\lambda}{\geq}410nm$) light, the residual concentration of benzene was monitored by gas chromatography (GC). Both undoped/doped nanoparticles showed about 80 % of photolysis of benzene under UV light. However, under visible light irradiation Ag-doped $TiO_2$ nanoparticles exhibited a photocatalytic reaction toward the photodegradation of benzene more efficient than that of bare $TiO_2$. The enhanced photocatalytic reaction of Ag-doped $TiO_2$ nanoparticles is attributed to the decrease in the activation energy and to the existence of Ag in the $TiO_2$ host lattice, which increases the absorption capacity in the visible region by acting as an electron trapper and promotes charge separation of the photoinduced electrons ($e^-$) and holes ($h^+$). The use of Ag-doped $TiO_2$ nanoparticles preserved the option of an environmentally benign photocatalytic reaction using visible light; These particles can be applicable to environmental cleaning applications.

Synthesis of CdS with Graphene by CBD(Chemical Bath Deposition) Method and Its Photocatalytic Activity

  • Pawar, R.C.;Lee, Jin-Yong;Kim, Eun-Jeong;Kim, Hyungsub;Lee, Caroline Sunyong
    • Korean Journal of Materials Research
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    • v.22 no.10
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    • pp.504-507
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    • 2012
  • Synthesis of RGO (reduced graphene oxide)-CdS composite material was performed through CBD (chemical bath deposition) method in which graphene oxide served as the support and Cadmium Sulfate Hydrate as the starting material. Graphene-based semiconductor photocatalysts have attracted extensive attention due to their usefulness for environmental and energy applications. The band gap (2.4 eV) of CdS corresponds well with the spectrum of sunlight because the crystalline phase, size, morphology, specic surface area and defects, etc., of CdS can affect its photocatalytic activity. The specific surface structure (morphology) of the photocatalyst can be effective for the suppression of recombination between photogenerated electrons and holes. Graphene (GN) has unique properties such as a high value of Young's modulus, large theoretical specific surface area, excellent thermal conductivity, high mobility of charge carriers, and good optical transmittance. These excellent properties make GN an ideal building block in nanocomposites. It can act as an excellent electron-acceptor/transport material. Therefore, the morphology, structural characterization and crystal structure were observed using various analytical tools, such as X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and Raman spectroscopy. From this analysis, it is shown that CdS particles were well dispersed uniformly in the RGO sheet. Furthermore, the photocatalytic property of the resulting RGO-CdS composite is also discussed in relation to environmental applications such as the photocatalytic degradation of pollutants. It was found that the prepared RGO-CdS nanocomposites exhibited enhanced photocatalytic activity as compared with that of CdS nanoparticles. Therefore, better efficiency of photodegradation was found for water purification applications using RGO-CdS composite.

Variation in optical, dielectric and sintering behavior of nanocrystalline NdBa2NbO6

  • Mathai, Kumpamthanath Chacko;Vidya, Sukumariamma;Solomon, Sam;Thomas, Jijimon Kumpukattu
    • Advances in materials Research
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    • v.2 no.2
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    • pp.77-91
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    • 2013
  • High quality nanoparticles of neodymium barium niobium ($NdBa_2NbO_6$) perovskites have been synthesized using an auto ignition combustion technique for the first time. The nanoparticles thus obtained have been characterized by powder X-ray diffraction, thermo gravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, Raman spectroscopy and transmission electron microscopy. UV-Visible absorption and photoluminescence spectra of the samples are also recorded. The structural analysis shows that the nano powder is phase pure with the average particle size of 35 nm. The band gap determined for $NdBa_2NbO_6$ is 3.9 eV which corresponds to UV-radiation for optical inter band transition with a wavelength of 370nm. The nanopowder could be sintered to 96% of the theoretical density at $1325^{\circ}C$ for 2h. The ultrafine cuboidal nature of nanopowders with fewer degree of agglomeration improved the sinterability for compactness at relatively lower temperature and time. During the sintering process the wide band gap semiconducting behavior diminishes and the material turns to a high permittivity dielectric. The microstructure of the sintered surface was examined using scanning electron microscopy. The striking value of dielectric constant ${\varepsilon}_r=43$, loss factor tan ${\delta}=1.97{\times}10^{-4}$ and the observed band gap value make it suitable for many dielectric devices.

Characterization of Microstructure and Mechanical Properties of Mg-8Li-3Al-1Y Alloy Subjected to Different Rolling Processes

  • Zhou, Xiao;Liu, Qiang;Liu, Ruirui;Zhou, Haitao
    • Metals and materials international
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    • v.24 no.6
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    • pp.1359-1368
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    • 2018
  • The mechanical properties and microstructure evolution of Mg-8Li-3Al-1Y alloy undergoing different rolling processes were systematically investigated. X-ray diffraction, optical microscope, scanning electron microscopy, transmission electron microscopy as well as electron backscattered diffraction were used for tracking the microstructure evolution. Tensile testing was employed to characterize the mechanical properties. After hot rolling, the $MgLi_2Al$ precipitated in ${\beta}-Li$ matrix due to the transformation reaction: ${\beta}-Li{\rightarrow}{\beta}-Li+MgLi_2Al+{\alpha}-Mg$. As for the alloy subjected to annealed hot rolling, ${\beta}-Li$ phase was clearly recrystallized while recrystallization rarely occurred in ${\alpha}-Mg$ phase. With regard to the microstructure undergoing cold rolling, plenty of dislocations and dislocation walls were easily observed. In addition, the microstructure of alloys subjected to annealed cold rolling revealed the formation of new fresh ${\alpha}-Mg$ grains in ${\beta}-Li$ phase due to the precipitation reaction. The mechanical properties and fracture modes of Mg-8Li-3Al-1Y alloys can be effectively tuned by different rolling processes.

Development of Ultra-Thin TiO2 Coated WO3 Inverse Opal Photoelectrode for Dye-Sensitized Solar Cells (염료감응형 태양전지로의 응용을 위한 얇은 TiO2가 코팅 된 WO3 역오팔 광전극의 개발)

  • Arunachalam, Maheswari;Kwag, Seoui;Lee, Inho;Kim, Chung Soo;Lee, Sang-Kwon;Kang, Soon Hyung
    • Korean Journal of Materials Research
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    • v.29 no.8
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    • pp.491-496
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    • 2019
  • In this study, we prepare pure $WO_3$ inverse opal(IO) film with a thickness of approximately $3{\mu}m$ by electrodeposition, and an ultra-thin $TiO_2$ layer having a thickness of 2 nm is deposited on $WO_3$ IO film by atomic layer deposition. Both sets of photoelectrochemical properties are evaluated after developing dye-sensitized solar cells(DSSCs). In addition, morphological, crystalline and optical properties of the developed films are evaluated through field-emission scanning electron microscopy(FE-SEM), High-resolution transmission electron microscopy(HR-TEM), X-ray diffraction(XRD) and UV/visible/infrared spectrophotometry. In particular, pure $WO_3$ IO based DSSCs show low $V_{OC}$, $J_{SC}$ and fill factor of 0.25 V, $0.89mA/cm^2$ and 18.9 %, achieving an efficiency of 0.04 %, whereas the $TiO_2/WO_3$ IO based DSSCs exhibit $V_{OC}$, $J_{SC}$ and fill factor of 0.57 V, $1.18mA/cm^2$ and 50.1 %, revealing an overall conversion efficiency of 0.34 %, probably attributable to the high dye adsorption and suppressed charge recombination reaction.