• Title/Summary/Keyword: raman microscopy

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Evaluation of Structural Changes and Dispersibility of Boron Nitride Nanotubes under Different Ultrasonication Conditions (초음파 처리 조건에 따른 질화붕소나노튜브 구조 변화 및 분산성 평가)

  • Da Bin Cheon;Won Jung Choi;Seung Hwa Yoo
    • Composites Research
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    • v.37 no.4
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    • pp.350-355
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    • 2024
  • Boron nitride nanotubes (BNNT) are materials of significant interest in next-generation technological fields due to their outstanding physicochemical properties, including excellent chemical and thermal stability. However, for effective utilization, dispersion of BNNT is essential. Unfortunately, BNNT exhibit hydrophobic surfaces and strong van der Waals forces, making their dispersion challenging. Current dispersion methods include the addition of surfactants and surface functionalization, but these chemical treatments often damage BNNT and involve cumbersome processes. In this study, we dispersed BNNT in water under various tip ultrasonication conditions and identified conditions that do not affect BNNT using FT-IR spectroscopy, Raman spectroscopy, and X-ray diffraction analysis. Subsequently, enhanced dispersibility was confirmed through turbidity measurements, and the solubility range in 15 different solvents was evaluated using the Hansen solubility parameter.

Characterization of SiC nanowire Synthesized by Thermal CVD (열 화학기상증착법을 이용한 탄화규소 나노선의 합성 및 특성연구)

  • Jung, M.W.;Kim, M.K.;Song, W.;Jung, D.S.;Choi, W.C.;Park, C.J.
    • Journal of the Korean Vacuum Society
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    • v.19 no.4
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    • pp.307-313
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    • 2010
  • One-dimensional cubic phase silicon carbide nanowires (${\beta}$-SiC NWs) were efficiently synthesized by thermal chemical vapor deposition (TCVD) with mixtures containing Si powders and nickel chloride hexahydrate $(NiCl_2{\cdot}6H_2O)$ in an alumina boat with a carbon source of methane $(CH_4)$ gas. SEM images are shown that the growth temperature (T) of $1,300^{\circ}C$ is not enough to synthesize the SiC NWs owing to insufficient thermal energy for melting down a Si powder and decomposing the methane gas. However, the SiC NWs could be synthesized at T>$1,300^{\circ}C$ and the most efficient temperature for growth of SiC NWs is T=$1,400^{\circ}C$. The synthesized SiC NWs have the diameter with an average range between 50~150 nm. Raman spectra clearly revealed that the synthesized SiC NWs are forming of a cubic phase (${\beta}$-SiC). Two distinct peaks at 795 and $970 cm^{-1}$ in Raman spectra of the synthesized SiC NWs at T=$1,400^{\circ}C$ represent the TO and LO mode of the bulk ${\beta}$-SiC, respectively. XRD spectra are also supported to the Raman spectra resulting in the strongest (111) peaks at $2{\Theta}=35.7^{\circ}$, which is the (111) plane peak position of 3C-SiC. Moreover, the gas flow rate of 300 sccm for methane is the optimal condition for synthesis of a large amount of ${\beta}$-SiC NW without producing the amorphous carbon structure shown at a high methane flow rate of 800 sccm. TEM images are shown two kinds of the synthesized ${\beta}$-SiC NWs structures. One is shown the defect-free ${\beta}$-SiC NWs with a (111) interplane distance of 0.25 nm, and the other is the stacking-faulted ${\beta}$-SiC NWs. Also, TEM images exhibited that two distinct SiC NWs are uniformly covered with $SiO_2$ layer with a thickness of less 2 nm.

Reliable and High Spatial Resolution Method to Identify the Number of MoS2 Layers Using a Scanning Electron Microscopy

  • Sharbidre, Rakesh Sadanand;Park, Se Min;Lee, Chang Jun;Park, Byong Chon;Hong, Seong-Gu;Bramhe, Sachin;Yun, Gyeong Yeol;Ryu, Jae-Kyung;Kim, Taik Nam
    • Korean Journal of Materials Research
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    • v.27 no.12
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    • pp.705-709
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    • 2017
  • The electronic and optical characteristics of molybdenum disulphide ($MoS_2$) film significantly vary with its thickness, and thus a rapid and accurate estimation of the number of $MoS_2$ layers is critical in practical applications as well as in basic researches. Various existing methods are currently available for the thickness measurement, but each has drawbacks. Transmission electron microscopy allows actual counting of the $MoS_2$ layers, but is very complicated and requires destructive processing of the sample to the point where it will no longer be useable after characterization. Atomic force microscopy, particularly when operated in the tapping mode, is likewise time-consuming and suffers from certain anomalies caused by an improperly chosen set point, that is, free amplitude in air for the cantilever. Raman spectroscopy is a quick characterization method for identifying one to a few layers, but the laser irradiation causes structural degradation of the $MoS_2$. Optical microscopy works only when $MoS_2$ is on a silicon substrate covered with $SiO_2$ of 100~300 nm thickness. The last two optical methods are commonly limited in resolution to the micrometer range due to the diffraction limits of light. We report here a method of measuring the distribution of the number of $MoS_2$ layers using a low voltage field emission electron microscope with acceleration voltages no greater than 1 kV. We found a linear relationship between the FESEM contrast and the number of $MoS_2$ layers. This method can be used to characterize $MoS_2$ samples at nanometer-level spatial resolution, which is below the limits of other methods.

A Study on the Annealing Effect of SnO Nanostructures with High Surface Area (높은 표면적을 갖는 SnO 나노구조물의 열처리 효과에 관한 연구)

  • Kim, Jong-Il;Kim, Ki-Chul
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.19 no.9
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    • pp.536-542
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    • 2018
  • Tin dioxide, $SnO_2$, is a well-known n-type semiconductor that shows change in resistance in the presence of gas molecules, such as $H_2$, CO, and $CO_2$. Considerable research has been done on $SnO_2$ semiconductors for gas sensor applications due to their noble property. The nanomaterials exhibit a high surface to volume ratio, which means it has an advantage in the sensing of gas molecules. In this study, SnO nanoplatelets were grown densely on Si substrates using a thermal CVD process. The SnO nanostructures grown by the vapor transport method were post annealed to a $SnO_2$ phase by thermal CVD in an oxygen atmosphere at $830^{\circ}C$ and $1030^{\circ}C$. The pressure of the furnace chamber was maintained at 4.2 Torr. The crystallographic properties of the post-annealed SnO nanostructures were investigated by Raman spectroscopy and XRD. The change in morphology was confirmed by scanning electron microscopy. As a result, the SnO nanostructures were transformed to a $SnO_2$ phase by a post-annealing process.

Role of Aluminum Top-layer on Synthesis of Carbon Nanotubes using Laminated Catalyst(Al/Fe/Al) layer (적층구조 촉매층(Al/Fe/Al)을 이용한 탄소나노튜브의 합성에서 최상층 알루미늄 층의 역할)

  • Song, W.;Choi, W.C.;Jeon, C.;Ryu, D.H.;Lee, S.Y.;Shin, Y.S.;Park, C.Y.
    • Journal of the Korean Vacuum Society
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    • v.16 no.5
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    • pp.377-382
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    • 2007
  • In this study, we report the synthesis of the single-walled carbon nanotubes(SWCNTs) using laminated catalyst(Al/Fe/Al) layer deposited by sputter on Si(001). SWCNTs are grown by thermal chemical vapor deposition (TCVD) method. As the results of scanning electron microscopy(SEM), high resolution transmission electron microscopy(HR-TEM) and Raman spectroscopy, we confirmed the SWCNTs bundles with narrow diameter distribution of $1.14{\sim}1.32\;nm$ and average G&D ratio of 22.76. Compare to the sample having Fe/Al catalyst layer, it can be proposed that the top-aluminum incorporated with iron catalyst plays an important role in growing process of CNTs as a agglomeration barrier of the Fe catalyst. Thus, we suggest that a proper quantity of aluminium metal incorporated in Fe catalyst induce small and uniform iron catalysts causing SWCNTs with narrow diameter distribution.

Effect of Temperature on Growth of Tin Oxide Nanostructures (산화주석 나노구조물의 성장에서 기판 온도의 효과)

  • Kim, Mee-Ree;Kim, Ki-Chul
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.4
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    • pp.497-502
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    • 2019
  • Metal oxide nanostructures are promising materials for advanced applications, such as high sensitive gas sensors, and high capacitance lithium-ion batteries. In this study, tin oxide (SnO) nanostructures were grown on a Si wafer substrate using a two-zone horizontal furnace system for a various substrate temperatures. The raw material of tin dioxide ($SnO_2$) powder was vaporized at $1070^{\circ}C$ in an alumina crucible. High purity Ar gas, as a carrier gas, was flown with a flow rate of 1000 standard cubic centimeters per minute. The SnO nanostructures were grown on a Si substrate at $350{\sim}450^{\circ}C$ under 545 Pa for 30 minutes. The surface morphology of the as-grown SnO nanostructures on Si substrate was characterized by field-emission scanning electron microscopy (FE-SEM) and atomic force microscopy (AFM). Raman spectroscopy was used to confirm the phase of the as-grown SnO nanostructures. As the results, the as-grown tin oxide nanostructures exhibited a pure tin monoxide phase. As the substrate temperature was increased from $350^{\circ}C$ to $424^{\circ}C$, the thickness and grain size of the SnO nanostructures were increased. The SnO nanostructures grown at $450^{\circ}C$ exhibited complex polycrystalline structures, whereas the SnO nanostructures grown at $350^{\circ}C$ to $424^{\circ}C$ exhibited simple grain structures parallel to the substrate.

The Formation of ConTiOn+2 Compounds in CoOx/TiO2 Catalysts and Their Activity for Low-Temperature CO Oxidation (CoOx/TiO2 촉매상에 ConTiOn+2 화합물의 생성과 저온 CO 산화반응에 대한 촉매활성)

  • Kim, Moon-Hyeon;Ham, Sung-Won
    • Journal of Environmental Science International
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    • v.17 no.8
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    • pp.933-941
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    • 2008
  • The formation of $Co_nTiO_{n+2}$ compounds, i.e., $CoTiO_3$ and $CO_2TiO_4$, in a 5wt% $CoO_x/TiO_2$ catalyst after calcination at different temperatures has been characterized via scanning electron microscopy (SEM), Raman and X-ray photoelectron spectroscopy (XPS) measurements to verify our earlier model associated with $CO_3O_4$ nanoparticles present in the catalyst, and laboratory-synthesized $Co_nTiO_{n+2}$ chemicals have been employed to directly measure their activity profiles for CO oxidation at $100^{\circ}C$. SEM measurements with the synthetic $CoTiO_3$ and $CO_2TiO_4$ gave the respective tetragonal and rhombohedral morphology structures, in good agreement with the earlier XRD results. Weak Raman peaks at 239, 267 and 336 $cm^{-1}$ appeared on 5wt% $CoO_x/TiO_2$ after calcination at $570^{\circ}C$ but not on the catalyst calcined at $450^{\circ}C$, and these peaks were observed for the $Co_nTiO_{n+2}$ compounds, particularly $CoTiO_3$. All samples of the two cobalt titanate possessed O ls XPS spectra comprised of strong peaks at $530.0{\pm}0.1$ eV with a shoulder at a 532.2-eV binding energy. The O ls structure at binding energies near 530.0 eV was shown for a sample of 5 wt% $CoO_x/TiO_2$, irrespective to calcination temperature. The noticeable difference between the catalyst calcined at 450 and $570^{\circ}C$ is the 532.2 eV shoulder which was indicative of the formation of the $Co_nTiO_{n+2}$ compounds in the catalyst. No long-life activity maintenance of the synthetic $Co_nTiO_{n+2}$ compounds for CO oxidation at $100^{\circ}C$ was a good vehicle to strongly sup port the reason why the supported $CoO_x$ catalyst after calcination at $570^{\circ}C$ had been practically inactive for the oxidation reaction in our previous study; consequently, the earlier proposed model for the $CO_3O_4$ nanoparticles existing with the catalyst following calcination at different temperatures is very consistent with the characterization results and activity measurements with the cobalt titanates.

Electrochemical properties of heat-treated multi-walled carbon nanotubes (열처리된 탄소나노튜브 상대전극의 전기화학적 특성 연구)

  • Lee, S.K.;Moon, J.H.;Hwang, S.H.;Kim, G.C.;Lee, D.Y.;Kim, D.H.;Jeon, M.H.
    • Journal of the Korean Vacuum Society
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    • v.17 no.1
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    • pp.67-72
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    • 2008
  • We have studied the effect of heat treatment of multi-walled carbon nanotubes (MWNTs) as a counter electrode on the electro-chemical properties of dye-snsitized solar cells. MWNTs on the p-type Si substrate were synthesized by thermal chemical vapor deposition (CVD) using Fe catalysts. We prepared the two types of MWNTs samples with the different diameters. The rapid thermal annealing (RTA) treatment for the MWNTs was carried out at the growth temperature ($900^{\circ}C$) for 1 minute with $N_2$ gas atmosphere. The structural, electrical and electrochemical properties of MWNTs were investigated by field-emission scanning electron microscopy (FE-SEM), Raman spectroscopy, 2-point probe station and electrochemical impedance spectroscopy (EIS). The I(D)/I(G) ratio of heat-treated MWNTs in Raman spectra was considerably decreased. It was also found that the heat-treated MWNTs showed better redox reaction of iodide at the interface between MWNTs surface and electrolyte than that of as-grown MWNTs. The redox resistance value of heat-treated electrodes was measured to be much lower than that of as-grown electrode at the interface. As a result, the counter electrode using the heat-treated MWNTs showed better electrochemical properties.

A Study on Morphology and Mechanical Properties of Biodegradable Polymer Nanocomposites (생분해성 고분자 나노복합체의 형태학 및 기계적 특성 연구)

  • Jang, Sang Hee
    • Clean Technology
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    • v.19 no.4
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    • pp.401-409
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    • 2013
  • BBiodegradable polymers have attracted great attention because of the increased environmental pollution by waste plastics. In this study, PLA (polylactic acid)/Clay-20 (Cloisite 20) and PLA (polylactic acid)/PBS (poly(butylene succinate)/Clay-20 (Cloisite 20) nanocomposites were manufactured in a twin-screw extruder. Specimens for mechanical properties of PLA/Clay-20 and PLA/PBS (90/10)/Clay-20 nanocomposites were prepared by injection molding. Thermal, mechanical, morphological and raman spectral properties of two nanocomposites were investigated by differential scanning calorimetry (DSC), tensile tester, scanning electron microscopy (SEM) and raman-microscope spectrophotometer, respectively. In addition, hydrolytic degradation properties of two nanocomposites were investigated by hydrolytic degradation test. It was confirmed that the crystallinity of PLA/Clay-20 and PLA/PBS/Clay-20 nanocomposite was increased with increasing Clay-20 content and the Clay-20 is miscible with PLA and PLA/PBS resin from DSC and SEM results. Tensile strength of two nanocomposites was decreased, but thier elongation, impact strength, tensile modulus and flexural modulus were increased with an increase of Clay-20 content. The impact strength of PLA/Clay-20 and PLA/PBS/Clay-20 nanocomposites with 5 wt% of Clay-20 content was increased above twice than that of pure PLA and PLA/PBS (90/10). The hydrolytic degradation rate of PLA/Clay-20 nanocomposite with 3 wt% of Clay-20 content was accelerated about twice than that of pure PLA. The reason is that degradation may occur in the PLA and Clay-20 interface easily because of hydrophilic property of organic Clay-20. It was confirmed that a proper amount of Clay-20 can improve the mechanical properties of PLA and can control biodegradable property of PLA.

A Study on the Changing Properties of Iron Oxides in Black Glazes using Raman Microscope -Focused on Black Glazes Excavated in Shinan Shipwreck- (라만분광현미경을 이용한 흑유자 유약 내 철산화물의 변화 양상 연구 -신안선 출수 흑유자를 중심으로-)

  • Park, Jin Ho;Yu, Heisun;Chung, Yong Jae
    • Journal of Conservation Science
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    • v.35 no.2
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    • pp.117-129
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    • 2019
  • In this study, black-glazed porcelain excavated from the Shinan shipwreck is analyzed to distinguish its characteristics. Glazes of Hong-Tang kiln are thin and exhibit little vitrification, whereas the Ci-Zhou-type and Cha-Yang kilns are similar in terms of their cross section. However, Raman mapping images reveal difference in the distribution area of magnetite. In this study, firing experiments are conducted to determine how iron oxides change properties in black glazes. The results show that when hematite is fired to a temperature greater than $1250^{\circ}C$, it becomes magnetite. Therefore, it is estimated that a firing temperature of approximately $1200^{\circ}C$ is suitable for the Hong-Tang kiln. In addition, glazes of the Ci-Zhou-type and Cha-Yang kilns are fired at approximately $1300^{\circ}C$. However, when the characteristics of firing in ancient kilns are considered, porcelain can be fired for a sufficiently long period to extend to glaze surfaces.