• Title/Summary/Keyword: In situ TEM

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Measuring the Tensile Properties of the Nanostructure Using a Force Sensor (힘센서를 이용한 나노구조체의 인장물성 측정)

  • Jeon, Sang-Gu;Jang, Hoon-Sik;Kwon, Oh-Heon;Nahm, Seung-Hoon
    • Transactions of the Korean Society of Mechanical Engineers A
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    • v.34 no.2
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    • pp.211-217
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    • 2010
  • It is important to measure the mechanical properties of nanostructures because they are required to determine the lifetime and reliability of nanodevices developed for various fields. In this study, tensile tests for a multi-walled carbon nanotube (MWCNT) and a ZnO nanorod were performed in a scanning electron microscope (SEM). The force sensor was a cantilever type and was mounted in front of a nanomanipulator placed in the chamber. The nanomanipulator was controlled using a joystick and personal computer. The nanostructures dispersed on the cut area of a transmission electron microscope (TEM) grid were gripped with the force sensor by exposing an electron beam in the SEM; the tensile tests were the performed. The in situ tensile loads of the nanostructure were obtained. After the tensile test, the cross-sectional areas of the nanostructures were observed by TEM and SEM. Based on the TEM and SEM results, the elastic modulus of the MWCNT and ZnO nanorod were calculated to be 0.98 TPa and 55.85 GPa, respectively.

In-situ Particle Characterization of Cu Nanopowder using Scanning Mobility Particle Sizer in Pulsed Wire Evaporation Method (전기폭발법에서 SMPS를 이용한 Cu 나노분말의 실시간 입자특성평가)

  • 이창우;맹덕영;박중학;유지훈;이재훈;이창규;김흥회
    • Journal of Powder Materials
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    • v.10 no.4
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    • pp.275-280
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    • 2003
  • Synthesis and characteristics of Cu nanopowder were considered by in-situ characterization method using SMPS in pulsed wire evaporation process. With increasing pressure in chamber, particle size and degree of agglomeration increased by increase of collision frequency. Also, it was found from the XRD analyses and BET measurements that crystallite size and particle size decreased with elevating applied voltage. However, SMPS measurements and TEM observation revealed the increase of particle size and degree of agglomeration with increase of applied voltage. These results suggested that particle growth and agglomeration depend on overheating factor in chamber at the early stage and thermal coagulation in filtering system during powder formation until collection.

A New Trend of In-situ Electron Microscopy with Ion and Electron Beam Nano-Fabrication

  • Furuya, Kazuo;Tanaka, Miyoko
    • Applied Microscopy
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    • v.36 no.spc1
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    • pp.25-33
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    • 2006
  • Nanofabrication with finely focused ion and electron beams is reviewed, and position and size controlled fabrication of nano-metals and -semiconductors is demonstrated. A focused ion beam (FIB) interface attached to a column of 200keV transmission electron microscope (TEM) was developed. Parallel lines and dots arrays were patterned on GaAs, Si and $SiO_2$ substrates with a 25keV $Ga^+-FIB$ of 200nm beam diameter at room temperature. FIB nanofabrication to semiconductor specimens caused amorphization and Ga injection. For the electron beam induced chemical vapor deposition (EBI-CVD), we have discovered that nano-metal dots are formed depending upon the beam diameter and the exposure time when decomposable gases such as $W(CO)_6$ were introduced at the beam irradiated areas. The diameter of the dots was reduced to less than 2.0nm with the UHV-FE-TEM, while those were limited to about 15nm in diameter with the FE-SEM. Self-standing 3D nanostructures were also successfully fabricated.

Surface Migration in Al and Cu Films (알루미늄 및 구리 박막에서의 표면전자이주)

  • 박종원;김윤태;이진호
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 1994.11a
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    • pp.106-108
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    • 1994
  • Electromigration(EM) tests were carried out on Al and Cu films in HV systems to study surface migration. The Al films were made on oxidized silicon wafers by thermal evaporation, in-situ annealed at 300$^{\circ}C$, patterned, and EM tested at 260$^{\circ}C$ and 4.5MA/$\textrm{cm}^2$. SEM observation with back scattered electron mode on the EM tested Al films disclosed that thinning took place under the native Al oxide. In the case of Cu films, tested using in-situ TEM, thinning was also observed at the early stage of void formation even though the thinned areas were much less than those of the Al films.

Methods to evaluate the twin formation energy: comparative studies of the atomic simulations and in-situ TEM tensile tests

  • Hong-Kyu Kim;Sung-Hoon Kim;Jae-Pyoung Ahn
    • Applied Microscopy
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    • v.50
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    • pp.19.1-19.9
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    • 2020
  • Deformation twinning, one of the major deformation modes in a crystalline material, has typically been analyzed using generalized planar fault energy (GPFE) curves. Despite the significance of these curves in understanding the twin nucleation and its effect on the mechanical properties of crystals, their experimental validity is lacking. In this comparative study based on the first-principles calculation, molecular dynamics simulation, and quantitative in-situ tensile testing of Al nanowires inside a transmission electron microscopy system, we present both a theoretical and an experimental approach that enable the measurement of a part of the twin formation energy of the perfect Al crystal. The proposed experimental method is also regarded as an indirect but quantitative means for validating the GPFE theory.

Effects of Hydrogen on the PWSCC Initiation Behaviours of Alloy 182 Weld in PWR Environments

  • Kim, H.-S.;Hong, J.-D.;Lee, J.;Gokul, O.S.;Jang, C.
    • Corrosion Science and Technology
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    • v.14 no.3
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    • pp.113-119
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    • 2015
  • Alloy 82/182 weld metals had been extensively used in joining the components of the PWR primary system. Unfortunately, there have been a number of incidents of cracking caused by PWSCC in Alloy 82/182 welds during the operation of PWR worldwide. To mitigate PWSCC, optimization of water-chemistry conditions, especially dissolved hydrogen (DH) and Zn contents, is considered as the most promising and effective remedial method. In this study, the PWSCC behaviours of Alloy 182 weld were investigated in simulated PWR environments with various DH content. Both in-situ and ex-situ oxide characterizations as well as PWSCC initiation tests were performed. The results showed that PWSCC crack initiation time was shortest in PWR water (DH: 30cc/kg). Also, high stress reduced crack initiation time. Oxide layer showed multi-layered structures consisted of the outer needle-like Ni-rich oxide layer, Fe-rich crystalline oxide, and inner Cr-rich inner oxide layers, which was not altered by the level of applied stress. To analyse the multi-layer structure of oxides, EIS measurement were fitted into an equivalent circuit model. Further analyses including TEM and EDS are underway to verify appropriateness of the equivalent circuit model.

Growth Characteristics of Silica Particles Using In situ Sampling from $H_2/O_2TEOS$ Diffusion Flame (수소/산소/TEOS 확산화염 중 직접포집을 이용한 실리카 입자의 성장특성에 관한 연구)

  • Jung, Chang-Hoon;Ahn, Kang-Ho;Choi, Man-Soo;Lee, Joon-Sik
    • Proceedings of the KSME Conference
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    • 2000.04b
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    • pp.404-409
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    • 2000
  • Growth characteristics of silica particles have been studied experimentally using in situ sampling technique from $H_2/O_2TEOS$ diffusion flame with carefully devised sampling probe. Verification of sampling result was done through new method and effects of flame condition and TEOS flow rate on growth characteristics of silica particles were investigated. By comparing particles sampled by thermophoretic sampling in flame with those by collector sampling after probe, particles do not change before and after probe sampling, which was clearly proved from the fact that the result of TEM image analysis makes good agreement with that of SMPS measurement. As flame temperature increases, the effect of coalescence or sintering becomes important mechanism during growth of silica particles, resulting in canceling the effect of coagulation, which makes mean diameter of silica particles increase slowly. With increase in TEOS flow rate, the number concentration of generated silica particle increases but residence time of particles in flame decreases. As a result, there exists upper limit to which the diameter of silica particle increases under same flame condition.

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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.

Transmission Electron Microscopy Characterization of Early Pre-Transition Oxides Formed on ZIRLOTM

  • Bae, Hoyeon;Kim, Taeho;Kim, Ji Hyun;Bahn, Chi Bum
    • Corrosion Science and Technology
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    • v.14 no.6
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    • pp.301-312
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    • 2015
  • Corrosion of zirconium fuel cladding is known to limit the lifetime and reloading cycles of fuel in nuclear reactors. Oxide layers formed on ZIRLO4^{TM}$ cladding samples, after immersion for 300-hour and 50-day in a simulated primary water chemistry condition ($360^{\circ}C$ and 20 MPa), were analyzed by using the scanning transmission electron microscopy (STEM), in-situ transmission electron microscopy (in-situ TEM) with the focused ion beam (FIB) technique, and X-ray diffraction (XRD). Both samples (immersion for 300 hours and 50 days) revealed the presence of the ZrO sub-oxide phase at the metal/oxide interface and columnar grains developed perpendicularly to the metal/oxide interface. Voids and micro-cracks were also detected near the water/oxide interface, while relatively large lateral cracks were found just above the less advanced metal/oxide interface. Equiaxed grains were mainly observed near the water/oxide interface.

Electrochemical Performance of Activated Carbons/Mn3O4-Carbon Blacks for Supercapacitor Electrodes

  • Kim, Ki-Seok;Park, Soo-Jin
    • Bulletin of the Korean Chemical Society
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    • v.34 no.8
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    • pp.2343-2347
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    • 2013
  • In this work, manganese dioxide ($Mn_3O_4$)/carbon black (CB) composites (Mn-CBs) were prepared by an in situ coating method as electrical fillers and the effect of the Mn-CBs on the electrical performance of activated carbon (AC)-based electrodes was investigated. Structural features of Mn-CBs produced via in situ coating using a $KMnO_4$ solution were confirmed by XRD and TEM images. The electrical performances, including cv curves, charge-discharge behaviors, and specific capacitance of the ACs/Mn-CBs, were determined by cyclic voltammograms. It was found that the composites of $Mn_3O_4$ and CBs were successfully formed by in situ coating method. ACs/Mn-CBs showed higher electrical performance than that of AC electrodes fabricated with conventional CBs due to the pesudocapacitance reaction of manganese oxides in the aqueous electrolyte. Consequently, it is anticipated that the incorporation of $Mn_3O_4$ into CBs could facilitate the utilization of CBs as electrical filler, leading to enhanced electrochemical performance of AC electrodes for supercapacitors.