• Title/Summary/Keyword: scanning/transmission electron microscopy (STEM)

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In-situ formation of co particles encapsulated by graphene layers

  • Minjeong Lee;Gyutae Kim;Gyu Hyun Jeong;Aram Yoon;Zonghoon Lee;Gyeong Hee Ryu
    • Applied Microscopy
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    • v.52
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    • pp.7.1-7.6
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    • 2022
  • The process of encapsulating cobalt nanoparticles using a graphene layer is mainly direct pyrolysis. The encapsulation structure of hybrids prepared in this way improves the catalyst stability, which greatly reduces the leaching of non-metals and prevents metal nanoparticles from growing beyond a certain size. In this study, cobalt particles surrounded by graphene layers were formed by increasing the temperature in a transmission electron microscope, and they were analyzed using scanning transmission electron microscopy (STEM). Synthesized cobalt hydroxide nanosheets were used to obtain cobalt particles using an in-situ heating holder inside a TEM column. The cobalt nanoparticles are surrounded by layers of graphene, and the number of layers increases as the temperature increases. The interlayer spacing of the graphene layers was also investigated using atomic imaging. The success achieved in the encapsulation of metallic nanoparticles in graphene layers paves the way for the design of highly active and reusable heterogeneous catalysts for more challenging molecules.

Comparative study on the specimen thickness measurement using EELS and CBED methods

  • Yoon-Uk Heo
    • Applied Microscopy
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    • v.50
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    • pp.8.1-8.7
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    • 2020
  • Two thickness measurement methods using an electron energy loss spectroscopy (EELS) and 10a convergent beam electron diffraction (CBED) were compared in an Fe-18Mn-0.7C alloy. The thin foil specimen was firstly tilted to satisfy 10a two-beam condition. Low loss spectra of EELS and CBED patterns were acquired in scanning transmission electron microscopy (STEM) and TEM-CBED modes under the two-beam condition. The log-ratio method was used for measuring the thin foil thickness. Kossel-Möllenstedt (K-M) fringe of the $13{\ba{1}}$ diffracted disk of austenite was analyzed to evaluate the thickness. The results prove the good coherency between both methods in the thickness range of 72 ~ 113 nm with a difference of less than 5%.

Structural Characteristics on InAs Quantum Dots multi-stacked on GaAs(100) Substrates

  • Roh, Cheong-Hyun;Park, Young-Ju;Kim, Eun-Kyu;Shim, Kwang-Bo
    • Journal of the Microelectronics and Packaging Society
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    • v.7 no.1
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    • pp.25-28
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    • 2000
  • The InAs self-assembled quantun dots (SAQDS) were grown on a GaAs(100) substrate using a molecular beam epitaxy (MBE) technique. The InAs QDs were multi-stacked to have various layer structures of 1, 3, 6, 10, 15 and 20 layers, where the thickness of the GaAs spacer and InAs QD layer were 20 monolayers (MLs) and 2 MLs, respectively. The nanostructured feature was characterized by photoluminescence (PL) and scanning transmission electron microscopy (STEM). It was found that the highest PL intensity was obtained from the specimen with 6 stacking layers and the energy of the PL peak was split with increasing the number of stacking layers. The STEM investigation exhibited that the quantum dots in the 6 stacking layer structure were well aligned in vertical columns without any deflect generation, whereas the volcano-like deflects were formed vertically along the growth direction over 10 periods of InAs stacking layers.

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Comprehensive Structural Characterization of Commercial Blue Light Emitting Diode by Using High-Angle Annular Dark Filed Scanning Transmission Electron Microscopy and Transmission Electron Microscopy (고각 환형 암시야 주사투과전자현미경기법과 투과전자현미경기법을 이용한 상용 청색 발광다이오드의 종합적인 구조분석)

  • Kim, Dong-Yeob;Hong, Soon-Ku;Chung, Tae-Hoon;Lee, Sang Hern;Baek, Jong Hyeob
    • Korean Journal of Materials Research
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    • v.25 no.1
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    • pp.1-8
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    • 2015
  • This study suggested comprehensive structural characterization methods for the commercial blue light emitting diodes(LEDs). By using the Z-contrast intensity profile of Cs-corrected high-angle annular dark field scanning transmission electron microscope(HAADF-STEM) images from a commercial lateral GaN-based blue light emitting diode, we obtained important structural information on the epilayer structure of the LED, which would have been difficult to obtain by conventional analysis. This method was simple but very powerful to obtain structural and chemical information on epi-structures in a nanometer-scale resolution. One of the examples was that we could determine whether the barrier in the multi-quantum well(MQW) was GaN or InGaN. Plan-view TEM observations were performed from the commercial blue LED to characterize the threading dislocations(TDs) and the related V-pit defects. Each TD observed in the region with the total LED epilayer structure including the MQW showed V-pit defects for almost of TDs independent of the TD types: edge-, screw-, mixed TDs. The total TD density from the region with the total LED epilayer structure including the MQW was about $3.6{\times}10^8cm^{-2}$ with a relative ratio of Edge- : Screw- :Mixed-TD portion as 80%: 7%: 13%. However, in the mesa-etched region without the MQW total TD density was about $2.5{\times}10^8cm^{-2}$ with a relative ratio of Edge- : Screw- :Mixed-TD portion of 86%: 5%: 9 %. The higher TD density in the total LED epilayer structure implied new generation of TDs mostly from the MQW region.

Structural Characterization of CoCrFeMnNi High Entropy Alloy Oxynitride Thin Film Grown by Sputtering (스퍼터링 방법으로 성장한 코발트크롬철망간니켈 고엔트로피 질산화물 박막의 구조특성)

  • Lee, Jeongkuk;Hong, Soon-Ku
    • Korean Journal of Materials Research
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    • v.28 no.10
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    • pp.595-600
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    • 2018
  • This study investigates the microstructural properties of CoCrFeMnNi high entropy alloy (HEA) oxynitride thin film. The HEA oxynitride thin film is grown by the magnetron sputtering method using nitrogen and oxygen gases. The grown CoCrFeMnNi HEA film shows a microstructure with nanocrystalline regions of 5~20 nm in the amorphous region, which is confirmed by high-resolution transmission electron microscopy (HR-TEM). From the TEM electron diffraction pattern analysis crystal structure is determined to be a face centered cubic (FCC) structure with a lattice constant of 0.491 nm, which is larger than that of CoCrFeMnNi HEA. The HEA oxynitride film shows a single phase in which constituting elements are distributed homogeneously as confirmed by element mapping using a Cs-corrected scanning TEM (STEM). Mechanical properties of the CoCrFeMnNi HEA oxynitride thin film are addressed by a nano indentation method, and a hardness of 8.13 GPa and a Young's modulus of 157.3 GPa are obtained. The observed high hardness value is thought to be the result of hardening due to the nanocrystalline microstructure.

Preparation of Gold-Peptide Hybrid Nanoparticles and Its Applications in Catalytic Reduction of Methylene Blue (금-펩타이드 하이브리드 나노입자의 제조와 메틸렌 블루의 촉매 환원 응용)

  • Hur, Yun-Mi;Min, Kyoung-Ik
    • Applied Chemistry for Engineering
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    • v.32 no.2
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    • pp.163-167
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    • 2021
  • In the present work, we studied a method for the synthesis of uniform gold-peptide hierarchical superstructures using tyrosine rich peptide, Tyr-Tyr-Leu-Tyr-Tyr (YYLYY). Peptide nanoparticles self-assembled by dityrosine bonds were synthesized through the photo-crosslinking reaction of the peptide, and gold-peptide hybrid nanoparticles were synthesized using biomineralization properties of tyrosine in a green synthetic manner. The synthesized gold-peptide hybrid nanoparticles were then characterized by transmission electron microscopy, scanning electron microscopy, dynamic light scattering, UV-vis spectroscopy, scanning transmission electron microscopy-energy dispersive X-ray spectroscopy, and X-ray diffraction. Furthermore, the catalytic activity of gold-peptide hybrid nanoparticles was confirmed by the reduction reaction of methylene blue where the catalytic reaction rate constant was 13.4 × 10-3 s-1.

Microstructure and Mechanical Properties of ODS Ferrite Produced by Reactive Milling for the MSR Suppression (MSR (Mechanically induced Self-sustaining Reaction)이 억제된 반응성 밀링에 의해 제조된 분산강화 페라이트의 미세조직과 기계적 특성)

  • Hwang, Seung J.
    • Journal of the Korean Society for Heat Treatment
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    • v.26 no.6
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    • pp.279-287
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    • 2013
  • Oxide Dispersion Strengthened (ODS) Fe with $Al_2O_3$ dispersoid was successfully produced by reactive milling with a mixture of Fe, $Fe_3O_4$ (Magnetite), $Fe_2O_3$ (Hematite) and Al reactants at cryogenic temperature. The milled powders were consolidated by Vacuum Hot Press (HP) at 1323 K, and the consolidated materials were characterized by Transmission Electron Microscopy (TEM), Scanning Transmission Electron Microscopy (STEM), and Energy Dispersive Spectroscopy (EDS); the yield strength and the hardness of the consolidated materials were determined by compressive test and Vickers hardness test at room temperature. The grain size of the materials was estimated by X-ray Diffraction technique using the scherrer's formula. The TEM observations showed that the microstructure was comprised with a mixture of nanocrystalline Fe matrix and $Al_2O_3$ nano-dispersoids with a bimodal size distribution; the 0.2% off-set yield strength of the materials was as high as $758{\pm}29$ MPa and the Vickers hardness was $358{\pm}2$. The effect of the cryogenic milling and addition of extra Fe powder was discussed on the suppression of MSR (Mechanically induced Self-sustaining Reaction) for the desired microstructural evolution of ODS alloys.

High Speed and Sensitive X-ray Analysis System with Automated Aberration Correction Scanning Transmission Electron Microscope

  • Inada, Hiromi;Hirayama, Yoichi;Tamura, Keiji;Terauchi, Daisuke;Namekawa, Ryoji;Shichiji, Takeharu;Sato, Takahiro;Suzuki, Yuya;Ohtsu, Yoshihiro;Watanabe, Keitaro;Konno, Mitsuru;Tanaka, Hiroyuki;Saito, Koichiro;Shimoyama, Wataru;Nakamura, Kuniyasu;Kaji, Kazutoshi;Hashimoto, Takahito
    • Applied Microscopy
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    • v.45 no.1
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    • pp.1-8
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    • 2015
  • We have developed a new HD-2700 (Hitachi High-Technologies Corp., Japan) scanning transmission electron microscope (STEM) that includes an automatic aberration correction function, and a large-solid-angle energy-dispersive X-ray spectroscopy detector that enables high-resolution and sensitive analysis. For observation with atomic resolution, using spherical-aberration-corrected STEM, in order that satisfactory performance of the device can be achieved readily, and within a short time, irrespective of the operator's skill level, a spherical-aberration-correction device with an automatic aberration-correction function was developed. This automatic aberration-correction function carries out the entire correction-related process (aberration measurement, selection and correction) automatically, with automatic selection of the aberrations that require correction, and automatic measurement of the appropriate corrections.

Facile Synthesis of Gold Nanoparticles Using Tyrosine-Rich Peptide and Its Applications to Catalytic Reduction of 4-Nitrophenol (타이로신이 풍부한 펩타이드를 사용한 금 나노입자의 손쉬운 합성과 4-니트로페놀의 촉매 환원 응용)

  • Hur, Yun-Mi;Min, Kyoung-Ik
    • Applied Chemistry for Engineering
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    • v.32 no.1
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    • pp.15-19
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    • 2021
  • In this study, we studied a facile method for the synthesis of stable and nearly spherical gold nanoparticles using a tyrosine-rich peptide, Tyr-Tyr-Gly-Tyr-Tyr (YYGYY), as both the reducing and capping agent. The peptide coated spherical and polycrystalline gold nanoparticles with diameters from 3 to 15 nm were successfully synthesized by varying the concentration of the peptide and metal precursor under UV irradiation. The nanoparticles were then characterized by transmission electron microscopy (TEM), UV-Vis spectroscopy, scanning transmission electron microscopy-energy dispersive X-ray spectroscopy (STEM-EDS), Fourier transform infrared spectroscopy (FT-IR), and X-ray diffraction (XRD). Furthermore, the catalytic activity of gold nanoparticles was confirmed by the reduction of 4-nitrophenol to 4-aminophenol, in which the catalytic reaction rate constant was 7.3 × 10-3 s-1.

Reset-first Resistance Switching Mechanism of HfO2 Films Based on Redox Reaction with Oxygen Drift-Diffusion

  • Kim, Jong-Gi;Lee, Sung-Hoon;Lee, Kyu-Min;Na, Hee-Do;Kim, Young-Jae;Ko, Dae-Hong;Sohn, Hyun-Chul
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.286-287
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    • 2012
  • Reset-first resistive switching mechanism based on reduction reaction in HfO2-x with oxygen drift-diffusion was studied. we first report that the indirect evidence of local filamentary conductive path formation in bulk HfO2 film with local TiOx region at Ti top electrode formed during forming process and presence of anion-migration at interface between electrode and HfO2 during resistive switching through high resolution transmission electron microscopy (HRTEM), electron disperse x-ray (EDX), and electron energy loss spectroscopy (EELS) mapping. Based on forming process mechanism, we expected that redox reaction from Ti/HfO2 to TiOx/HfO2-x was responsible for an increase of initial current with increasing the post-annealing process. First-reset resistive switching in above $350^{\circ}C$ annealed Ti/HfO2 film was exhibited and the redox phenomenon from Ti/HfO2 to TiOx/HfO2-x was observed with high angle annular dark field (HAADF) - scanning transmission electron microscopy (STEM), EDX and x-ray photoelectron spectroscopy. Therefore, we demonstrated that the migration of oxygen ions at interface region under external electrical bias contributed to bipolar resistive switching behavior.

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