• Title/Summary/Keyword: In situ transmission electron microscopy

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In-situ rf treatment of multiwall carbon nanotube with various post techniques for enhanced field emission

  • Ahn, Kyoung-Soo;Kim, Jun-Sik;Kim, Ji-Hoon;Kim, Chae-Ok;Hong, Jin-Pyo
    • 한국정보디스플레이학회:학술대회논문집
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    • 2003.07a
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    • pp.859-862
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    • 2003
  • Well-aligned multiwall carbon nanotubes (MWCNTs) were prepared at low temperature of 400 $^{\circ}C$ by utilizing a radio frequency plasma-enhanced chemical vapor deposition (rf-PECVD) system. The MWCNTs were treated by an external rf plasma source and an ultra-violet laser in order to modify structural defect of carbon nanotube and to ablate possible contamination on carbon nanotube surface. Structural properties of carbon nanotubes were investigated by using a scanning electron microscopy (SEM), Raman spectroscopy, Fourier transformer Infrared spectroscopy (FTIR) and transmission electron microscope (TEM). In addition, the emission properties of the MWNTs were measured for the application of field emission display (FED) in near future. Various post treatments were found to improve the field emission property of carbon nanotubes.

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Electrical Conductivity, Dielectric Behavior and EMI Shielding Effectiveness of Polyaniline-Yttrium Oxide Composites

  • Faisal, Muhammad;Khasim, Syed
    • Bulletin of the Korean Chemical Society
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    • v.34 no.1
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    • pp.99-106
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    • 2013
  • Polyaniline-yttrium trioxide (PAni-$Y_2O_3$) composites were synthesized by the in-situ polymerization of aniline in the presence of $Y_2O_3$ The composite formation and structural changes in these composites were investigated by X-ray diffraction (XRD), Fourier transform infra red spectroscopy (FTIR), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM). The direct current (DC) electrical conductivity of the order of $0.51{\times}10^{-2}\;S\;cm^{-1}-0.283\;S\;cm^{-1}$ in the temperature range 300 K-473 K indicates semiconducting behavior of the composites. Room temperature AC conductivity and dielectric response of the composites were studied in the frequency range of 10 Hz to 1 MHz. The variation of AC conductivity with frequency obeyed the power law, which decreased with increasing weight percentage (wt %) of $Y_2O_3$. Studies on dielectric properties shows the relaxation contribution coupled by electrode polarization effect. The dielectric constant and dielectric loss in these composites depend on the content of $Y_2O_3$ with a percolation threshold at 20 wt % of $Y_2O_3$ in PAni. Electromagnetic interference shielding effectiveness (EMI SE) of the composites in the frequency range 100 Hz to 2 GHz was in the practically useful range of -12.2 dB to -17.2 dB. The observed electrical and shielding properties were attributed to the interaction of $Y_2O_3$ particles with the PAni molecular chains.

Epitaxial Growth and Characterization of Zinc-blende CrAs/GaAs/MnAs/GaAs Multilayers

  • Wang W.H.;Manago T.;Akinaga H.
    • Journal of Magnetics
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    • v.11 no.1
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    • pp.1-4
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    • 2006
  • We report on the growth, structural and transport properties of zinc-blende CrAs/GaAs/MnAs/GaAs multilayers on GaAs(001) substrates. Structural analyses using in-situ reflection high-energy electron diffraction and exsitu cross-sectional transmission electron microscopy confirmed the realization of a zinc-blende crystal structure. Room temperature Hall measurements reveal that the as-grown multilayer exhibits p-type conductivity with a very low resistivity of $0.052\;\omega{cm}$, a high carrier concentration of $6.2X10^{19}\;cm^{-3}$ and a Hall mobility of $1.8\;cm^2/Vs$. We also observed a clear decrease of the resistivity in samples after low temperature annealing.

Electrochemical and surface investigations of copper corrosion in dilute oxychloride solution

  • Gha-Young Kim ;Junhyuk Jang;Jeong-Hyun Woo;Seok Yoon;Jin-Seop Kim
    • Nuclear Engineering and Technology
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    • v.55 no.8
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    • pp.2742-2746
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    • 2023
  • The corrosion behavior of copper immersed in dilute oxychloride solution (100 mM) was studied through surface investigation and in-situ monitoring of open-circuit potential. The copper corrosion was initiated with copper dissolution into a form of CuCl-2, resulting in mass decrease within the first 40 h of immersion. This was followed by a hydrolysis reaction initiated by the CuCl-2 at the copper surface, after which oxide products were formed and deposited on the surface, resulting in a mass increase. The formation of nucleation sites for copper oxide and its lateral extension during the corrosion process were examined using focused ion beam (FIB)-scanning electron microscopy (SEM). The presence of metastable compounds such as atacamite (CuCl2·3Cu(OH)2) on the corroded copper surface was revealed by X-ray photoelectron spectra (XPS) and transmission electron microscopy (TEM)-energy dispersive spectrometry (EDS) analysis.

One Pot Synthesis and Characterization of Alginate Stabilized Semiconductor Nanoparticles

  • Sundarrajan, Parani;Eswaran, Prabakaran;Marimuthu, Alexander;Subhadra, Lakshmi Baddireddi;Kannaiyan, Pandian
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3218-3224
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    • 2012
  • Uniform and well dispersed metal sulfide semiconductor nanoparticles incorporated into matrices of alginate biopolymer are prepared by using a facile in situ method. The reaction was accomplished by impregnation of alginate with divalent metal ions followed by reaction with thioacetamide. XRD analysis showed that the nanoparticles incorporated in the polymer matrix were of cubic structure with the average particle diameter of 1.8 to 4.8 nm. Field emission scanning electron microscopy and high resolution transmission electron microscopy images indicated that the particles were well dispersed and distributed uniformly in the matrices of alginate polymer. FT-IR spectra confirmed the presence of alginate in the nanocomposite. The crystalline nature and thermal stability of the alginate polymer was found to be influenced by the nature of the divalent metal ions used for the synthesis. The proposed method is considered to be a simple and greener approach for large scale synthesis of uniform sized nanoparticles.

In-situ electron beam growth of $YBa_2Cu_3O_{7-x}$ coated conductors on metal substrates

  • Jo, W.;Ohnishi, T.;Huh, J.;Hammond, R.H.;Beasley, M.R.
    • Progress in Superconductivity
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    • v.8 no.2
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    • pp.175-180
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    • 2007
  • High temperature superconductor $YBa_2Cu_3O_{7-x}$ (YBCO) films have been grown by in-situ electron beam evaporation on artificial metal tapes such as ion-beam assisted deposition (IBAD) and rolling assisted biaxially textured substrates (RABiTS). Deposition rate of the YBCO films is $10{\sim}100{\AA}/sec$. X-ray diffraction shows that the films are grown epitaxially but have inter-diffusion phases, like as $BaZrO_3\;or\;BaCeO_3$, at their interfaces between YBCO and yttrium-stabilized zirconia (YSZ) or $CeO_2$, respectively. Secondary ion mass spectroscopy depth profile of the films confirms diffused region between YBCO and the buffer layers, indicating that the growth temperature ($850{\sim}900^{\circ}C$) is high enough to cause diffusion of Zr and Ba. The films on both the substrates show four-fold symmetry of in-plane alignment but their width in the -scan is around $12{\sim}15^{\circ}$. Transmission electron microscopy shows an interesting interface layer of epitaxial CuO between YBCO and YSZ, of which growth origin may be related to liquid flukes of Ba-Cu-O. Resistivity vs temperature curves of the films on both substrates were measured. Resistivity at room temperature is between 300 and 500 cm, the extrapolated value of resistivity at 0 K is nearly zero, and superconducting transition temperature is $85{\sim}90K$. However, critical current density of the films is very low, ${\sim}10^3A/cm^2$. Cracking of the grains and high-growth-temperature induced reaction between YBCO and buffer layers are possible reasons for this low critical current density.

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High-temperature oxidation behaviors of ZrSi2 and its coating on the surface of Zircaloy-4 tube by laser 3D printing

  • Kim, Jae Joon;Kim, Hyun Gil;Ryu, Ho Jin
    • Nuclear Engineering and Technology
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    • v.52 no.9
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    • pp.2054-2063
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    • 2020
  • The high-temperature oxidation behavior of ZrSi2 used as a coating material for nuclear fuel cladding was investigated for developing accident-tolerant fuel cladding of light water reactors. Bulk ZrSi2 samples were prepared by spark plasma sintering. In situ X-ray diffraction was conducted in air at 900, 1000, and 1100 ℃ for 20 h. The microstructures of the samples before and after oxidation were examined by scanning electron microscopy and transmission electron microscopy. The results showed that the oxide layer of zirconium silicide exhibited a layer-by-layer structure of crystalline ZrO2 and amorphous SiO2, and the high-temperature oxidation resistance was superior to that of Zircaloy-4 owing to the SiO2 layer formed. ZrSi2 was coated on the Zircaloy-4 tube surface using laser 3D printing, and the coated tube was oxidized for 2000 s at 1200 ℃ under a vapor/argon mixture atmosphere. The outer surface of the coated tube was hardly oxidized (10-30 ㎛), while the inner surface of the uncoated tube was significantly oxidized to approximately 300 ㎛.

The Characterization of ZnO Hybrid Structure Grown by Metal-organic Chemical Vapor Deposition

  • Kim, A-Yeong;Jang, Sam-Seok;Lee, Do-Han;Im, So-Yeong;Byeon, Dong-Jin
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.10a
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    • pp.37.2-37.2
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    • 2011
  • The growth of three-dimensional ZnO hybrid structures by metal-organic chemical vapor deposition was controlled through their growth pressure. Vertically aligned ZnO nanorods were grown on c-plane sapphire substrate at $600^{\circ}C$ and 400 Torr. ZnO film was then formed in-situ on the ZnO nanorods at $600^{\circ}C$ and 10 Torr. High-resolution X-ray diffraction and transmission electron microscopy measurements showed that the ZnO film on the nanorods/sapphire grew epitaxially, and that the ZnO film/nanorods hybrid structures had well-ordered wurtzite structures. The hybrid ZnO structure was shown to be about 5 ${\mu}m$ by field-emission scanning electron microscopy. The hybrid structure showed better crystalline quality than mono-layer film on sapphire substrate. Consequently, purpose of this work is developing high quality hybrid epi-growth technology using nano structure. These structures have potential applicability as nanobuilding blocks in nanodevices.

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Templated Formation of Silver Nanoparticles Using Amphiphilic Poly(epichlorohydrine-g-styrene) Film

  • Park, Jung-Tae;Koh, Joo-Hwan;Seo, Jin-Ah;Roh, Dong-Kyu;Kim, Jong-Hak
    • Macromolecular Research
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    • v.17 no.5
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    • pp.301-306
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    • 2009
  • This work has demonstrated that a novel amphiphilic poly(epichlorohydrine)-graft-polystyrene (PECH-g-PS) copolymer at 34:66 wt% was synthesized via atom transfer radical polymerization (ATRP) of styrene using PECH as a macroinitiator. The structure of the graft copolymer was characterized by nuclear magnetic resonance ($^1H$ NMR) and FTIR spectroscopy, demonstrating that the "grafting from" method using ATRP was successful. The self-assembled graft copolymer was used as a template film for the in-situ growth of silver nanoparticles from $AgCF_3SO_3$ precursor under UV irradiation. The in situ formation of silver nanoparticles with 6-8 nm in average size in the solid state template film was confirmed by transmission electron microscopy (TEM), UV-visible spectroscopy and wide angle X-ray scattering (WAXS). Differential scanning calorimetry (DSC) also displayed the selective incorporation and the in situ formation of silver nanoparticles within the hydrophilic PECH domains, probably due to stronger interaction of the silvers with the ether oxygens of PECH backbone than that with hydrophobic PS side chains.

PBMS의 교정 및 이를 이용한 진공 내 나노입자의 실시간 분석 연구

  • Kim, Dong-Bin;Mun, Ji-Hun;Kim, Hyeong-U;Kim, Deuk-Hyeon;Lee, Jun-Hui;Gang, Sang-U;Kim, Tae-Seong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.91-91
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    • 2015
  • 반도체 공정의 발전에 의해 최근 생산되는 메모리 등은 십 수 나노미터까지 좁아진 선 폭을 갖게 되었다. 이러한 이유로, 기존에는 큰 문제를 발생시키지 않던 나노미터 영역의 입자들이 박막 증착 공정과 같은 반도체 제조공정 수율을 저감시키게 되었다. 따라서 오염입자의 유입을 막거나 제어하기 위해 transmission electron microscopy (TEM)나 scanning electron microscopy (SEM)과 같은 전자현미경을 활용한 비 실시간 입자 측정 방법 및 광원을 이용하는 in-situ particle monitor (ISPM) 및 전기적 이동도를 이용한 scanning mobility particle sizer (SMPS) 등 다양한 원리를 이용한 실시간 입자 측정방법이 현재 사용중에 있다. 이 중 진공 내 입자의 수농도를 측정하기 위해 개발된 particle beam mass spectrometer (PBMS) 기술은 박막 증착 공정 등 chemical vapor deposition (CVD) 방법을 이용하는 진공공정에서 활용 가능하여 개발이 진행되어 왔다. 본 연구에서는 PBMS의 한계점인 입자 밀도, 형상 등의 특성분석이 용이하도록 PBMS와 scanning electron microscopy (SEM), 그리고 energy dispersive spectroscopy (EDS) 기술을 결합하여 입자의 직경별 개수농도, 각 입자의 형상 및 성분을 함께 측정 가능하도록 하였다. 협소한 반도체 제조공정 내부 공간에 적용 가능하도록 기존 PBMS 대비 크기 또한 소형화 하였다. 각 구성요소인 공기역학 집속렌즈, electron gun, 편향판, 그리고 패러데이 컵의 설치 및 물리적인 교정을 진행한 후 입자발생장치를 통해 발생시킨 sodium chloride 입자를 상압 입자 측정 및 분류장치인 SMPS 장치를 이용하여 크기별로 분류시켜 압력차를 통해 PBMS로 유입시켜 측정을 진행하였다. 나노입자의 입경분포, 형상 및 성분을 측정결과를 토대로 장치의 측정정확도를 교정하였다. 교정된 장치를 이용하여 실제 박막 증착공정 챔버의 배기라인에서 발생하는 입자의 수농도, 형상 및 성분의 복합특성 측정이 가능하였으며, 최종적으로 실제 공정에 적용가능하도록 장치 교정을 완료하였다.

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