• Carbon letters
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• v.27
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• pp.42-49
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• 2018

A citric acid functionalized graphene oxide nanocomposite was successfully synthesized and the structure and morphology of the nanocatalyst were comprehensively characterized by Fourier transform infrared spectroscopy, energy-dispersive X-ray analysis, X-ray diffraction patterns, atomic force microscopy images, scanning electron microscopy images, transmission electron microscopy images, and thermogravimetric analysis. The application of this nanocatalyst was exemplified in an important condensation reaction to give imidazole derivatives in high yields and short reaction times at room temperature. The catalyst shows high catalytic activity and could be reused after simple work up and easy purification for at least six cycles without significant loss of activity, which indicates efficient immobilizing of citrate groups on the surface of graphene oxide sheets.

• Applied Microscopy
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• v.51
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• pp.19.1-19.7
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• 2021

The main purpose of this paper is the preparation of transmission electron microscopy (TEM) samples from the microsized powders of lithium-ion secondary batteries. To avoid artefacts during TEM sample preparation, the use of ion slicer milling for thinning and maintaining the intrinsic structure is described. Argon-ion milling techniques have been widely examined to make optimal specimens, thereby making TEM analysis more reliable. In the past few years, the correction of spherical aberration (Cs) in scanning transmission electron microscopy (STEM) has been developing rapidly, which results in direct observation at an atomic level resolution not only at a high acceleration voltage but also at a deaccelerated voltage. In particular, low-kV application has markedly increased, which requires a sufficiently transparent specimen without structural distortion during the sample preparation process. In this study, sample preparation for high-resolution STEM observation is accomplished, and investigations on the crystal integrity are carried out by Cs-corrected STEM.

• The Journal of Advanced Prosthodontics
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• v.16 no.1
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• pp.25-37
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• 2024

PURPOSE. To investigate the effect of sintering programs and surface treatments on surface properties, phase transformation and flexural strength of monolithic zirconia. MATERIALS AND METHODS. Zirconia specimens were sintered using three distinct sintering programs [classic (C), speed (S), and superspeed (SS)] (n = 56, each). One sample from each group underwent scanning electron microscopy (SEM) and grain size analysis following sintering. Remaining samples were divided into five subgroups (n = 11) based on the surface treatments: control (CL), polish (P), glaze (G), grind + polish (GP), and grind + glaze (GG). One sample from each subgroup underwent SEM analysis. Remaining samples were thermally aged. Monoclinic phase volume, surface roughness, and three-point flexural strength were measured. Monoclinic phase volume and surface roughness were analyzed by Kruskal-Wallis and Dunn tests. Flexural strength was analyzed by two-way ANOVA and Weibull analysis. The relationships among the groups were analyzed using Spearman's correlation analysis. RESULTS. Sintering program, surface treatment, and sintering × surface treatment (P ≤ .010) affected the monoclinic phase volume, whereas the type of surface treatment and sintering × surface treatment affected the surface roughness (P < .001). Type of sintering program or surface treatment did not affect the flexural strength. Weibull analysis revealed no significant differences between the m and σ_o values. Monoclinic phase volume was positively correlated with surface roughness in the SGG and SSP groups. CONCLUSION. After sintering monolithic zirconia in each of the three sintering programs, each of the surface treatments can be used. However, for surface quality and aging resistance, G or GG can be recommended as a surface finishing method.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.23 no.5
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• pp.235-240
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• 2013

Pure-carbon materials such as graphite, graphene, carbon nanotubes, and diamond have very high thermal conductivities. The reported thermal conductivity of graphene is in the range 3000~5000W/m-K at room temperature. Here, we developed graphene/cu foam hybrid type heat spreader to obtain higher thermal conductivity than Cu foam. Hybrid materials were characterized using optical microscopy (OM), scanning electron microscopy (SEM) and thermal conductivity measurement system; LFA (Laser Flash Analysis @ LFA 447, NETZSCH). We suggest that excellent thermal properties of graphene/cu foam hybrid structures are beneficial for all proposed electrical applications and can lead to a thermal management application.

• Applied Microscopy
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• v.43 no.2
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• pp.88-97
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• 2013

Technical investigation to figure out the problems arising during in-situ heating electron backscatter diffraction (EBSD) analysis inside scanning electron microscopy (SEM) was carried out. EBSD patterns were successfully acquired up to $830^{\circ}C$ without degradation of EBSD pattern quality in steels. Several technical problems such as image drift and surface microstructure pinning were taking place during in-situ experiments. Image drift problem was successfully prevented in constant current supplying mode. It was revealed that the surface pinning problem was resulted from the $TiO_2$ oxide particle formation during heating inside SEM chamber. Surface pinning phenomenon was fairly reduced by additional platinum and carbon multi-layer coating before in-situ heating experiment, furthermore was perfectly prevented by improvement of vacuum level of SEM chamber via leakage control. Plane view in-situ observation provides better understanding on the overall feature of recrystallization phenomena and cross sectional in-situ observation provides clearer understanding on the recrystallization mechanism.

• Polymer(Korea)
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• v.26 no.4
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• pp.535-542
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• 2002

We have prepared the surfactant-free nanoparticles of poly(DL-lactide-co-glycolide) (PLGA) by dialysis method and their physicochemical properties such as particle size and drug contents were investigated against various solvent. The size of PLGA nanoparticles prepared by using dimethylacetamide (DMAc), dimethylformamide (DMF), and dimethylsulfoxide (DMSO) was smaller than that from acetone. Also, the order of drug contents was DMAc>DMF>DMSO=acetone. These phenomena could be expected from the fact that solvent affects the size of nanoparticles and drug contents. The PLGA nanoparticles have a good spherical shapes as observed from scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Also, surfactant-free nanoparticles entrapping norfloxacin (NFx) have a good drug loading capacity without free-drug on the surface of nanoparticles confirmed by the analysis of X-ray powder diffraction. Release kinetics of NFx used as a model drug was governed not only by drug contents but also by particle size. Also, the biodegradation rate of PLGA nanoparticles prepared from DMF was faster than that prepared from acetone, indicating that the biodegradation of PLGA nanoparticles is size-dependent.

• Bulletin of the Korean Chemical Society
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• v.33 no.6
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• pp.1949-1954
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• 2012

We have developed a novel and eco-friendly synthetic route for the preparation of a two-dimensional layered zinc hydroxide with intercalated nitrate anions. The layered zinc hydroxide nitrate, called 'zinc basic salt', was, in general, successfully synthesized, using an electron beam irradiation technique. The 2-propanol solutions containing hydrated zinc nitrate were directly irradiated with an electron-beam at room temperature, under atmospheric conditions, without stabilizers or base molecules. Under electron beam irradiation, the reactive OH radicals were generated by radiolysis of water molecules in precursor metal salts. After further radiolytic processes, the hydroxyl anions might be formed by the reaction of solvated electrons and the OH radical. Finally, the $Zn_5(OH)_8(NO_3)_2{\cdot}2H_2O$ was precipitated by the reaction of zinc cation and hydroxyl anions. Structure and morphology of obtained compounds were characterized by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and high resolution transmission electron microscopy (HR-TEM). The chemical components of the products were determined by Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA). The thermal behavior of products was studied by thermogravimetric (TG) and differential thermal analysis (DTA).

• 한국전자현미경학회:학술대회논문집
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• 2001.11a
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• pp.18-22
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• 2001

A technique to characterize specific site of materials using a combination of a dedicated focused ion beam system(FIB), and Intermediate-voltage scanning transmission electron microscope(STEM) or transmission electron microscope(TEM) equipped with a scanning electron microscope(SEM) unit has been developed. The FIB system is used for preparation of electron transparent thin samples, while STEM or TEM is used for localization of a specific site to be milled in the FIB system. An FIB-STEM(TEM) compatible sample holder has been developed to facilitate thin sample preparation with high positional accuracy Positional accuracy of $0.1{\mu}m$ or better can be achieved by the technique. In addition, an FIB micro-sampling technique has been developed to extract a small sample directly from a bulk sample in a FIB system These newly developed techniques were applied for the analysis of specific failure in Si devices and also for characterization of a specific precipitate In a metal sample.

• Applied Microscopy
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• v.24 no.3
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• pp.87-93
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• 1994

In order to elucidate the machinability of lead brass, orthogonal machining experiment was conducted in SEM(Scanning Electron Microscope) equipped with a micro-machining device at a cutting speed of $7{\mu}m/s$ for brass containing 0.2 to 3wt% Pb. The microfactors (i.e., shear angle, contact length between chip and tool) were determined by in-situ observations. Machinability of brass containing lead is discussed in terms of the microfactors and the cutting resistant force tested by lathe cutting. The dynamic behavior of the chip formation of lead brass during the machining process was examined: The chips of lead brass form as a shear angle type. The shear angle increases with the content of lead in (6:4) brass. The pronounced effect of lead on the contact length between chip and tool was observed above 1% Pb. The cutting resistant force tested by lathe decreases remarkably with the lead content in brass. The observed microfactors are in close relation to the tested resistant force in macromachining.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.08a
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• pp.187-187
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• 2012

In this report, the plasmonic nanopores of less than 5 nm diameter were fabricated on the apex of the pyramidal cavity array. The metallic pyramidal pit cavity can also utilized as the plasmonic bioreactor, and the fabricated Au or Al metallic nanopore can provide the controllable translocation speed down using the plasmonic optical force. Initially, the SiO2 nanopore on the pyramidal pit cavity were fabricated using conventional microfabrication techniques. Then, the metallic thin film was sputter-deposited, followed by surface modification of the nanometer thick membrane using FESEM, TEM and EPMA. The huge electron intensity of FESEM with ~microsecond scan speed can provide the rapid solid phase surface transformation. However, the moderate electron beam intensity from the normal TEM without high speed scanning can only provide the liquid phase surface modification. After metal deposition, the 100 nm diameter aperture using FIB beam drilling was obtained in order to obtain the uniform nano-aperture. Then, the nanometer size aperture was reduced down to ~50 nm using electron beam surface modification using high speed scanning FESEM. The followed EPMA electron beam exposure without high speed scanning presents the reduction of the nanosize aperture down to 10 nm. During these processes, the widening or the shrinking of the nanometer pore was observed depending upon the electron beam intensity. Finally, using 200 keV TEM, the diameter of the nanopore was successively down from 10 nm down to 1.5 nm.