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

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Effect of Steady-State Oxidation on Tensile Failure of Zircaloy Cladding

  • Kim, Taeho;Choi, Kyoung Joon;Yoo, Seung Chang;Lee, Yunju;Kim, Ji Hyun
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.20 no.2
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    • pp.161-170
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    • 2022
  • The effect of oxidation time on the characteristics and mechanical properties of spent nuclear fuel cladding was investigated using Raman spectroscopy, tube rupture test, and tensile test. As oxidation time increased, the Raman peak associated with the tetragonal zirconium oxide phase diminished and merged with the Raman peak associated with the monoclinic zirconium oxide phase near 333 cm-1. Additionally, the other tetragonal zirconium oxide phase peak at 380 cm-1 decreased after 100 d of oxidation, whereas the zirconium monoclinic oxide peak became the dominant peak. The oxidation time had no effect on the tube rupture pressure of the oxidized zirconium alloy tube. However, the yield and tensile stresses of the oxidized nuclear fuel cladding tube decreased after 100 d of oxidation. The results of the scanning electron microscopy and transmission electron microscopy were represented with the in-situ Raman analysis result for the oxide characteristics generated on the cladding of spent nuclear fuel.

Dual Responsive Pectin Hydrogels and Their Silver Nanocomposites: Swelling Studies, Controlled Drug Delivery and Antimicrobial Applications

  • Reddy, P. Rama Subba;Eswaramma, S.;Krishna Rao, K.S.V.;Lee, Yong Ill
    • Bulletin of the Korean Chemical Society
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    • v.35 no.8
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    • pp.2391-2399
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    • 2014
  • Novel dual responsive pectin hydrogels composed from poly(acrylamidoglycolic acid-co-vinylcaprolactam)/Pectin (PAV-PC) and also PAV-PC hydrogels are used as templates for the production of silver nanoparticles. 5-Fluorouracil is an anticancer drug and has been loaded in situ into PAV-PC hydrogels. Structure and morphology characterization of PAV-PC hydrogels were investigated by fourier transform infrared spectroscopy, differential scanning calorimetry, thermo gravimetric analysis, X-ray diffraction studies, scanning electron microscopy and transmission electron microscopy. The results revealed a molecular level dispersion of the drug in PAV-PC hydrogels. In vitro release of 5-fluorouracil from the PAV-PC hydrogels has been carried out in GIT fluids as well as in various temperatures. 5-Fluorouracil released from PAV-PC hydrogels was 50% at pH 1.2, and 85% at pH 7.4 within 24 h. The release profile was characterized with PAV-PC hydrogels and initial burst effect was significantly reduced in two buffer media (1.2 and 7.4), followed by a continuous and controlled release phase, the drug release mechanism from polymer was due to Fickian diffusion. In situ fabrication of silver nanoparticles inside the hydrogel network via the reduction of sodium borohydrate by PAV-PC chains led to hydrogel nanocomposites. The diameter of the nanocomposites was about 50-100 nm, suitable for uptake within the gastrointestinal tract due to their nanosize range and mucoadhesive properties. These nanocomposite PAV-PC hydrogels showed strong antimicrobial activity towards Bacillus subtilis (G+ve) and Escherichia coli (G-ve).

In-Situ Electrical Resistance and Microstructure for Ultra-Thin Metal Film Coated by Magnetron Sputtering (마그네트론 스파터시 금속 극박막의 실시간 전기저항과 미세구조 변화)

  • Kwon, Na-Hyun;Kim, Hoi-Bong;Hwang, Bin;Bae, Dong-Su;Cho, Young-Rae
    • Korean Journal of Materials Research
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    • v.21 no.3
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    • pp.174-179
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    • 2011
  • Ultra-thin aluminum (Al) and tin (Sn) films were grown by dc magnetron sputtering on a glass substrate. The electrical resistance R of films was measured in-situ method during the film growth. Also transmission electron microscopy (TEM) study was carried out to observe the microstructure of the films. In the ultra-thin film study, an exact determination of a coalescence thickness and a continuous film thickness is very important. Therefore, we tried to measure the minimum thickness for continuous film (dmin) by means of a graphical method using a number of different y-values as a function of film thickness. The raw date obtained in this study provides a graph of in-situ resistance of metal film as a function of film thickness. For the Al film, there occurs a maximum value in a graph of in-situ electrical resistance versus film thickness. Using the results in this study, we could define clearly the minimum thickness for continuous film where the position of minimum values in the graph when we put the value of Rd3 to y-axis and the film thickness to x-axis. The measured values for the minimum thickness for continuous film are 21 nm and 16 nm for sputtered Al and Sn films, respectively. The new method for defining the minimum thickness for continuous film in this study can be utilized in a basic data when we design an ultra-thin film for the metallization application in nano-scale devices.

In situ reduction of gold nanoparticles in PDMS matrices and applications for large strain sensing

  • Ryu, Donghyeon;Loh, Kenneth J.;Ireland, Robert;Karimzada, Mohammad;Yaghmaie, Frank;Gusman, Andrea M.
    • Smart Structures and Systems
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    • v.8 no.5
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    • pp.471-486
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    • 2011
  • Various types of strain sensors have been developed and widely used in the field for monitoring the mechanical deformation of structures. However, conventional strain sensors are not suited for measuring large strains associated with impact damage and local crack propagation. In addition, strain sensors are resistive-type transducers, which mean that the sensors require an external electrical or power source. In this study, a gold nanoparticle (GNP)-based polymer composite is proposed for large strain sensing. Fabrication of the composites relies on a novel and simple in situ GNP reduction technique that is performed directly within the elastomeric poly(dimethyl siloxane) (PDMS) matrix. First, the reducing and stabilizing capacities of PDMS constituents and mixtures are evaluated via visual observation, ultraviolet-visible (UV-Vis) spectroscopy, and transmission electron microscopy. The large strain sensing capacity of the GNP-PDMS thin film is then validated by correlating changes in thin film optical properties (e.g., maximum UV-Vis light absorption) with applied tensile strains. Also, the composite's strain sensing performance (e.g., sensitivity and sensing range) is also characterized with respect to gold chloride concentrations within the PDMS mixture.

Low-Temperature Si and SiGe Epitaxial Growth by Ultrahigh Vacuum Electron Cyclotron Resonance Chemical Vapor Deposition (UHV-ECRCVD)

  • Hwang, Ki-Hyun;Joo, Sung-Jae;Park, Jin-Won;Euijoon Yoon;Hwang, Seok-Hee;Whang, Ki-Woong;Park, Young-June
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1996.06a
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    • pp.422-448
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    • 1996
  • Low-temperature epitaxial growth of Si and SiGe layers of Si is one of the important processes for the fabrication of the high-speed Si-based heterostructure devices such as heterojunction bipolar transistors. Low-temperature growth ensures the abrupt compositional and doping concentration profiles for future novel devices. Especially in SiGe epitaxy, low-temperature growth is a prerequisite for two-dimensional growth mode for the growth of thin, uniform layers. UHV-ECRCVD is a new growth technique for Si and SiGe epilayers and it is possible to grow epilayers at even lower temperatures than conventional CVD's. SiH and GeH and dopant gases are dissociated by an ECR plasma in an ultrahigh vacuum growth chamber. In situ hydrogen plasma cleaning of the Si native oxide before the epitaxial growth is successfully developed in UHV-ECRCVD. Structural quality of the epilayers are examined by reflection high energy electron diffraction, transmission electron microscopy, Nomarski microscope and atomic force microscope. Device-quality Si and SiGe epilayers are successfully grown at temperatures lower than 600℃ after proper optimization of process parameters such as temperature, total pressure, partial pressures of input gases, plasma power, and substrate dc bias. Dopant incorporation and activation for B in Si and SiGe are studied by secondary ion mass spectrometry and spreading resistance profilometry. Silicon p-n homojunction diodes are fabricated from in situ doped Si layers. I-V characteristics of the diodes shows that the ideality factor is 1.2, implying that the low-temperature silicon epilayers grown by UHV-ECRCVD is truly of device-quality.

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Studies on Properties of Polyaniline-Dodecylbenzene Sulfonic Acid Composite Films Synthesized Using Different Oxidants

  • Basavaraja, C.;Pierson, R.;Huh, Do-Sung;Venkataraman, A.;Basavaraja, S.
    • Macromolecular Research
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    • v.17 no.8
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    • pp.609-615
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    • 2009
  • Two types of nano composite were obtained by in situ chemical method in polyaniline (PANI)/dodecyl-benzenesulfonic acid (DBSA) system depending on the use of either ammonium persulfate (APS) or ferric chloride ($FeCl_3$) as the oxidant. In order to study the difference of the two composites in the surface characteristics, thermal stability, and electric properties, the composite films were studied by transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and temperature dependent DC electrical conductivity. The results revealed a large difference in the surface morphology, thermal stability, and the microstructure properties between the two composites, and these differences were considered responsible for the molecular order and conductivity.

MWCNT/Fibrin Bionanocomposites by in situ Enzymatic Polymerization

  • Kim, Mi-Jin;Jang, Jun-Ho;Han, Jung-Hun;Lee, Yong-Won;Cho, Sang-Min;Son, Sung-Yong;Hulme, John;Choi, In-Sung S.;Paik, Hyun-Jong;An, Seong-Soo A.
    • Bulletin of the Korean Chemical Society
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    • v.30 no.2
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    • pp.405-408
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    • 2009
  • In this work multiwalled carbon nanotube (MWCNT)/fibrin hybrid structures were synthesized via the transglutaminase- catalyzed polymerization of fibrinogen (FBG). Specifically, FBG was tethered onto oxidized MWCNTs by amide coupling, and the in situ polymerization of FBG to fibrin was performed by plasma transglutaminase (Factor XIIIa) in the presence of thrombin. The attached FBG was found to be biologically active and was polymerized to fibrin by thrombin and Factor XIIIa. MWCNT-FBG and MWCNT-Fibrin structures were characterized by FT-IR spectroscopy, transmission electron microscopy, and energy-dispersive X-ray (EDX) spectroscopy.

Electromagnetic Interference Reflectivity of Nanostructured Manganese Ferrite Reinforced Polypyrrole Composites

  • Chakraborty, Himel;Chabri, Sumit;Bhowmik, Nandagopal
    • Transactions on Electrical and Electronic Materials
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    • v.14 no.6
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    • pp.295-298
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    • 2013
  • Nano-size manganese ferrite reinforced conductive polypyrrole composites reveal a core-shell structure by in situ polymerization, in the presence of dodecyl benzene sulfonic acid as the surfactant and dopant, and iron chloride as the oxidant. The structure and magnetic properties of manganese ferrite nano-fillers were measured, by using X-ray diffraction and vibrating sample magnetometer. The morphology, microstructure, and conductivity of the composite were characterized by transmission electron microscopy, Fourier transform infrared spectroscopy, and four-wire technique. The microwave-absorbing properties of composites reinforcement dispersed in resin coating with the coating thickness of 1.2 nm were investigated, by using vector network analyzers, in the frequency range of 8~12 GHz. A reflection loss of -8 dB was observed at 10.5 GHz.

Order-to-disorder Behavior of Block Copolymer Films

  • Ryu, Du-Yeol;Kim, Eun-Hye;Choe, Seung-Hun
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.05a
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    • pp.6.2-6.2
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    • 2011
  • Block copolymer (BCP) self-assembly in a film geometry has recently been the focus of increased research interest due to their potential use as templates and scaffolds for the fabrication of nanostructured materials. The phase behavior in a thin film geometry that confines polymer chains to the interfaces will be influenced by the interfacial interactions at substrate/polymer and polymer/air and the commensurability between the equilibrium period (L0) of the BCP and the total film thickness. We investigated the phase transitions for the films of block copolymers (BCPs) on the modified surface, like the order-to-disorder transition (ODT) by in-situ grazing incidence small angle x-ray scattering (GISAXS) and transmission electron microscopy (TEM). The selective interactions on the surface by a PS-grafted substrate provide the preferential interactions with the PS component of the block, while a random copolymer (PS-r-PMMA) grafted substrate do the balanced interfacial interactions on the surface. The thickness dependence of order-to-disorder behavior for BCP films will be discussed in terms of the surface interactions.

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Preparation of Poly(methyl methacrylate)/Na-MMT Nanocomposites via in-Situ Polymerization with Macroazoinitiator

  • Jeong Han Mo;Ahn Young Tae
    • Macromolecular Research
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    • v.13 no.2
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    • pp.102-106
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    • 2005
  • Poly(methyl methacrylate) (PMMA)/sodium montmorillonite (Na-MMT) nanocomposites were prepared with a novel method utilizing a macroazoinitiator (MAI). To induce the intergallery polymerization of methyl methacrylate (MMA), the MAI containing a po1y(ethylene glycol) (PEG) segment was intercalated between the lamellae of Na-MMT and swelled with water to enhance the diffusion of MMA into the gallery. The structure of the nanocomposite was examined using X-ray diffraction and transmission electron microscopy, and the thermal properties were examined using differential scanning calorimetry and thermogravimetry. The PMMA/Na-MMT nanocomposite prepared by intergallery polymerization showed a distinct enhancement of its thermal properties; an approximately $30^{\circ}C$ increase in its glass transition temperature and an $80\sim100^{\circ}C$ increase in its thermal decomposition temperature for a $10\%$ weight loss.