• Title/Summary/Keyword: In situ TEM

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Caffeine as a source for nitrogen doped graphene, and its functionalization with silver nanowires in-situ

  • Ramirez-Gonzalez, Daniel;Cruz-Rivera, Jose de J.;Tiznado, Hugo;Rodriguez, Angel G.;Guillen-Escamilla, Ivan;Zamudio-Ojeda, Adalberto
    • Advances in nano research
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    • v.9 no.1
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    • pp.25-32
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    • 2020
  • In this work, we report the use of caffeine as an alternative source of nitrogen to successfully dope graphene (quaternary 400.6 eV and pyridinic at 398 eV according XPS), as well as the growth of silver nanowires (in-situ) in the surface of nitrogen doped graphene (NG) sheets. We used the improved graphene oxide method (IGO), chemical reduction of graphene oxide (GOx), and impregnation with caffeine as source of nitrogen for doping and subsequently, silver nanowires (NW) grow in the surface by the reduction of silver salts in the presence of NG, achieving a numerous of growth of NW in the graphene sheets. As supporting experimental evidence, the samples were analyzed using conventional characterization techniques: SEM-EDX, XRD, FT-IR, micro RAMAN, TEM, and XPS.

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.

Fabrication of Au Nanoparticle for Au-conjugate Immuno Chemistry Probe (Au-conjugate 면역화학 진단용 금 나노입자 제조)

  • Park, Sung-Tae;Lee, Kwang-Min
    • Korean Journal of Materials Research
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    • v.13 no.8
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    • pp.550-554
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    • 2003
  • Current nanogold cluster synthesized by chemical routine with 11 or 55 atoms of gold has been widely used for immuno chemistry probe as a form of nanocluster conjugated with biomolecules. It would be an undeveloped region that the 1 nm size of nanogold could be made by materials engineering processing. Therefore, objective of this study is to minimize the size of gold nanocluster as a function of operating temperature and chamber pressure in inert gas condensation (IGC) processing. Evaporation temperature was controlled by input current from 50 A to 65 A. Chamber pressure was controlled by argon gas with a range of 0.05 to 2 torr. The gold nanocluster by IGC was evaluated by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The gold nanocluster for TEM analysis was directly sampled with special in-situ method during the processing. Atomic force microscopy (AFM) was used to observe 3-D nanogold layer surfaces on a slide glass for the following biomolecule conjugation step. The size of gold nanoclusters had a close relationship with the processing condition such as evaporation temperature and chamber pressure. The approximately 1 nm size of nanogold was obtained at the processing condition for 1 torr at $1124 ^{\circ}C$.

In-Situ Synthesis of $\textrm{Si}_{3}\textrm{N}_{4}$-AIN Ceramic Composites ($\textrm{Si}_{3}\textrm{N}_{4}$-AIN 복합세라믹스의 In-Situ합성)

  • Lee, Byeong-Taek;Kim, Hae-Du;Heo, Seok-Hwan;Lee, Chan-Gyu
    • Korean Journal of Materials Research
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    • v.8 no.1
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    • pp.27-32
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    • 1998
  • In-Sit반응소결에의해 Si과 AI금속분말을 이용하여 Si$_{3}$N$_{4}$-AIN 복합세라믹스를 합성하였다. 합성된 Si$_{3}$N$_{4}$-AIN복합세라믹스의 미세조직과 결정구조를 해석하기 위해, OM, TEM, XRD및 EDX를 이용하였으며, Si$_{3}$N$_{4}$-AIN -20wt.%AIN복합세라믹스에서 Si의 질화율은 97%로 가장 높았다. Si$_{3}$N$_{4}$-AIN 복합세라믹스에서 Si의 질화율은 AI첨가량 증가에 따라 감소하였다. 대부분의 AI입자들은 다결정 AI입자들은 다결정 AIN(4-H구조)로 완전질화되었으며, 따라서 잔류 AI상은 반응소결체내에서 관찰되지 않았다. Si$_{3}$N$_{4}$의 결정구조는 $\alpha$$\beta$구조가 혼재된 상태이며, 잔류 Si입자내에서는 미소균열 및 전위가 관찰되었다. AI/Si$_{3}$N$_{4}$와 Si$_{3}$N$_{4}$ 두계면에서 이들은 거친 형상을 보이지만, 계면반응상은 관찰되지 않았다.

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Preparation of poly(methyl methacrylate)/clay nanocomposites by microwaveassisted in-situ radical polymerization

  • Jeong, Ji-Won;Kim, Dong-Hyun;Jang, Jae-Ho;Lee, Jung-Taek;Yoo, Kyung-Hyeon;Yoon, Seog-Young
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.29 no.1
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    • pp.19-23
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    • 2019
  • The PMMA (polymethyl methacrylate)/clay nanocomposites were synthesized by in situ radical polymerizations with different clay contents (3 and 7 wt%) using microwave heating. The nanostructure, optical, and thermal properties of the synthesized PMMA/clay nanocomposites were measured by XRD, TEM, AFM, UV-vis, and TGA. It was found that the intercalated- or exfoliated structure of PMMA/clay nanocomposites was strongly dependent on the content of clay. Thus, the imposition of microwave-assisted polymerization facilitated a delamination process of layered silicates to achieve exfoliation state of interlayer distance. The PMMA/3 wt% C10A nanocomposite with well-dispersed and exfoliated clay nano-layers showed the good optical transparency similar to pure PMMA in this study. The thermal decomposition rates of the PMMA/clay nanocomposites become to be lower compared to that of the pure PMMA, indicating the intercalated- or exfoliated inorganic silicate has high thermal stability. A possible reason is that the thermally segmental motion of PMMA polymer into inorganic silicate interlayer spacing has increased the thermal stability of the PMMA/clay nanocomposites.

Poly(ethylene terephthalate) Nanocomposite Fibers with Thermally Stable Organoclays (내열성 유기화 점토를 이용한 폴리(에틸렌 테레프탈레이트) 나노복합체 섬유)

  • Jung, Min-Hye;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.31 no.6
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    • pp.518-525
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    • 2007
  • The thermomechanical properties and morphologies of nanocomposite fibers of poly(ethylene terephthalate)(PET) incorporating thermally stable organoclays are compared. Dodecyltriphenyl-phosphonium-mica($C_{12}PPh-Mica$) and 1-hexadecane benzimidazole-mica ($C_{16}BIMD-Mica$) were used as reinforcing fillers in the fabrication of PET hybrid fibers. Dispersions of organoclays with PET were studied by using the in-situ polymerization method at various organoclay contents to produce nano-scale composites. The thermo-mechanical properties and morphologies of the PET hybrid fibers were determined using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), wide angle X-ray diffraction (XRD), electron microscopy (SEM and TEM), and a universal tensile machine (UTM). Transmission electron microscopy (TEM) micrographs show that some of the clay layers are dispersed homogeneously within the polymer matrix on the nano-scale, although some clay particles are agglomerated. We also found that the addition of only a small amount of organoclay is enough to improve the thermal stabilities and mechanical properties of the PET nanocomposite fibers. Even polymers with low organoclay content (<5 wt%) were found to exhibit much higher thermo-mechanical values than pure PET fibers.

Improved Electrical Properties by In Situ Nitrogen Incorporation during Atomic Layer Deposition of HfO2 on Ge Substrate (Ge 기판 위에 HfO2 게이트 산화물의 원자층 증착 중 In Situ 질소 혼입에 의한 전기적 특성 변화)

  • Kim, Woo-Hee;Kim, Bum-Soo;Kim, Hyung-Jun
    • Journal of the Korean Vacuum Society
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    • v.19 no.1
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    • pp.14-21
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    • 2010
  • Ge is one of the attractive channel materials for the next generation high speed metal oxide semiconductor field effect transistors (MOSFETs) due to its higher carrier mobility than Si. But the absence of a chemically stable thermal oxide has been the main obstacle hindering the use of Ge channels in MOS devices. Especially, the fabrication of gate oxide on Ge with high quality interface is essential requirement. In this study, $HfO_xN_y$ thin films were prepared by plasma-enhanced atomic layer deposition on Ge substrate. The nitrogen was incorporated in situ during PE-ALD by using the mixture of nitrogen and oxygen plasma as a reactant. The effects of nitrogen to oxygen gas ratio were studied focusing on the improvements on the electrical and interface properties. When the nitrogen to oxygen gas flow ratio was 1, we obtained good quality with 10% EOT reduction. Additional analysis techniques including X-ray photoemission spectroscopy and high resolution transmission electron microscopy were used for chemical and microstructural analysis.

Use of Modern Non­destructive Techniques in High Temperature Degradation of Material and Coatings

  • Lee, C.K.;Sohn, Y.H.
    • International Journal of Korean Welding Society
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    • v.3 no.2
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    • pp.29-39
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    • 2003
  • The durability and reliability of thermal barrier coatings (TBCs) play an important role in the service reliability, availability and maintainability (RAM) of hot­section components in advanced turbine engines for aero and utility applications. Photostimulated luminescence spectroscopy (PSLS) and electrochemical impedance spectroscopy (EIS) are being concurrently developed as complimentary non­destructive evaluation (NDE) techniques for quality control and life­remain assessment of TBCs. This paper overviews the governing principles and applications of the luminescence and the impedance examined in the light of residual stress, phase constituents and resistance (or capacitance) in TBC constituents including the thermally grown oxide (TGO) scale. Results from NDE by PSLS and EIS are discussed and related to the microstructural development during high temperature thermal cycling, examined by using a variety of microscopic techniques including focused ion beam (FIB) in­situ lift­out (INLO), transmission and scanning transmission electron microscopy (TEM and STEM).

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Synthesis and Thermo-mechanical Property of Multi-walled Carbon Nanotubes/Poly(methyl methacrylate-co-butyl acrylate) Nanocomposites Prepared Using Emulsion Polymerizations in the Presence of Amphiphilic Random Terpolymer

  • Chang, Woo-Hyuck;Ki, Ho-Seong;Cheong, In-Woo
    • Proceedings of the Polymer Society of Korea Conference
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    • 2006.10a
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    • pp.289-289
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    • 2006
  • The carboxylated MWNTs were successfully prepared by conventional acid treatment, and their structures were confirmed by FT-IR, Raman and TEM analysis. The water-dispersibility of the surface modified WNTs were good. The COOH-MWNT will show better stability during the emulsion polymerization as compared with Pristine MWNT. In-situ emulsion polymerizations of methyl methacrylate N(MMA) and n-butyl acrylate (BA) were carried out. Aggregate size and dispersion stability of the CNTs in water phase were measured using dynamic light scattering, turbidity, UV-visible spectrophotometer, and electron microscope. In addition, thermo-mechanical properties of MWNT/polymer nanocomposites were investigated.

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A Study of Production, Hot Consolidation, Secondary Recrystallization and Mechnical Property Assesment of Mechanically Alloyed $NiAl-Fe-AiN-Al_2O_3$ (기계적 합금화에 의한 $NiAl-Fe-AIN-Al_2O_3$ 합금분말의 제조, 열간 성형, 이차재결정화 및 기계적 성질 평가에 관한 연구)

  • 이순철
    • Journal of Powder Materials
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    • v.6 no.1
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    • pp.111-118
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    • 1999
  • Ni(Fe)Al powders containing a homogeneous distribution of the in-situ formed AIN and $Al_2O_3$ dispersoids have been produced by mechanical alloying process in a controlled atmosphere using high energy attrition mill. The powders have been successfully consolidated by hot extrusion process. The phase information investigated by TEM and XRD analysis reveals that Fe can be soluble up to 20% to the NiAl phase ($\beta$) at room temperature after MA process. Subsequent thermomechanical treatment under specific condition has been tried to induce secondary recrystallization (SRx) to improve high temperature properties, however, the clear evidence of SRx was not obtained in this material. Mechanical properties in term of strength at room temperature as well as at high temperatures have been improved by the addition pf AIN, and the room temperature ductility has been shown to be improved after heat treatment, presumably due to the precipitation of second phase of $\alpha$ in this material.

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