• Transactions of the Korean Society of Mechanical Engineers B
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• v.25 no.10
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• pp.1400-1407
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• 2001

The size distributions of electrospray droplets from the Taylor cone in cone-jet mode are directly measured by using a freezing method and a transmission electron microscope (TEM) image processing technique. These results are compared with the data obtained by an aerodynamic size spectrometer (TSI Aerosizer DSP). The use of glycerol seeded with NaI and a freezing method make it possible to sample droplets with their original sizes preserved. Since pictures of droplets are taken with TEM with very low vapor pressure of the solution, evaporation is suppressed by freezing. For liquid flow rates below 1 nl/sec, the measured droplet diameters by the TEM image processing technique and the aerosizer are in the range of 0.25 to 0.32 m add 0.3B to 0.40m, respectively. Comparing the TEM data with the aerosizer measurements, it has been revealed that the TEM image processing technique can afford more accurate values of droplet size distributions in the submicron range of 0.1 to 0.4m.

• Applied Microscopy
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• v.29 no.3
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• pp.265-274
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• 1999

The microstructure of Cu thin films in various deposition conditions was characterized. Cr films (50 nm thick) and Cu films (500 or 1000 nm thick) were deposited on polyimide films by DC magnetron sputtering. The Ar pressure during Cu deposition was controlled to 5, 50 and 100 mtorr. The microstructure was characterized using conventional and high resolution SEM and TEM. As sputtering pressure increases, open boundaries are observed more frequently. The Cu film deposited at 5 mtorr has a dense and uniform structure, while low-density regions or open boundaries between columns exist in the film deposited at higher pressure. As the film grows thicker, open boundaries are wider and the density of open boundaries are higher. The comparison between SEM and TEM show that the small features shown in high resolution SEM are grains. High resolution SEM is very effective to characterize the microstructure of the thin films. One column in the films deposited at 50 and 100 mtorr consists of several grains, which are smaller than those deposited at 5 mtorr.

• Applied Microscopy
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• v.29 no.3
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• pp.323-329
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• 1999

Synthesis of inorganic nanophase particles was performed to verify and understand the binding of non-ferrous metal ions including Al and $UO_2$ to the apoferritin molecules. Reconstituted inorganic particles of Al or $UO_2$ were identified by TEM as discrete electron dense cores encapsulated within the protein shell. The corresponding EDXA spectra confirm the presence of metal ions in the reconstituted ferritin. The Al cores of ferritin has been studied by TEM for the first time. Bimetallic cores with Al/Fe and $UO_2/Al$ were also produced and examined under TEM. Mixed metal cores encapsulated in the protein shell are well formed and its corresponding EDXA spectra also confirm the presence of metal ions in the mineral cores. Therefore, the present study proves that ferritin can be used to synthesize inorganic nanophase particles of Al and $UO_2$.

• Applied Microscopy
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• v.42 no.1
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• pp.49-52
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• 2012

For TEM study of biological samples or polymers that are contained in organic structure, it is often required that the sample is prepared by using ultramicrotome and stained with proper agents to increase the contrast of organic structure. In this study, we investigated an efficient TEM sample preparation method for ductile heterogeneity material by using ultramicrotomy. Cryo-ultramicrotomy is a suitable method that is capable of rendering sample hardness for various ductile materials. However, it has several factors to consider, such as experimental cost, working time and finding the optimal staining conditions. To satisfy these considerations, we prepared TEM sample by using ultramicrotome without cryofunction, and secured the sample hardness by applying the staining process prior to ultrathin sectioning. The cross-linked polyethylene structure in the sample was stained with the 2% $RuO_4$ solution in a sealed test tube for 24 hours at $4^{\circ}C$. After the sample staining, ultrathin sections of sample were prepared using ultramicrotome. As a result, it was revealed that the difficulties associated with staining of ultrathin sections prepared by low-temperature conditions were improved. In addition, appropriate staining depth of sample could be selected for sectioning process. The quality of TEM sample obtained by using this method was better than that of cryo-ultramicroscopy. Finally, it is expected that our method could be effectively applied in TEM sample preparation for a variety of nano-bio convergence materials.

• Applied Microscopy
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• v.34 no.1
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• pp.23-29
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• 2004

In this study, we introduce the structural analysis of amorphous silica nanoparticles by EF-TEM electron diffraction and in-situ heating experiments. Three diffused rings were observed on the electron diffraction patterns of initial silica nanoparticles, while crystalline spot patterns were gradually appeared during the insitu heating process at $900^{\circ}C$. These patterns indicate the basic unit of $SiO_4$ tetrahedra consisting amorphous silica and gradual crystallization into the ideal layer structure of tridymite by heating. Under high vacuum condition in TEM, SiO nanoparticles were redeposited on the carbon grid after evaporation of SiO gas from $SiO_2$ above $850^{\circ}C$ and the remaining $SiO_2$ were crystallized into orthorhombic tridymite, consistent with ex-situ heating results in furnace at $900^{\circ}C$.

• Applied Microscopy
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• v.39 no.3
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• pp.277-281
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• 2009

Practical difficulties for preparing a good crosssectional specimen of GaN-based materials for transmission electron microscopy have arisen due to large difference of mechanical properties between hard ceramic substrate and soft GaN-layered materials. Uneven polishing, sudden cracking, delamination, and selective sputtering during the conventional wedge polishing technique are often encountered as experimental hindrances. The preparation technique based on Strecker's method can be applied to overcome these difficulties, which eventually leads to mechanically stable TEM samples independent of the mechanical properties of materials. The basic idea is to use hard ceramic dummy filler for embedding the sample of interest into the dummy frame. In this study, we applied this technique into preparing cross-sectional TEM specimen of the GaN-based materials with mechanical instability and demonstrated usefulness of this hard dummy filler method in which the possible modifications of the sample of interest during the preparation must be avoidable. In addition, practical precautions during the preparation were discussed.

• Applied Microscopy
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• v.49
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• pp.3.1-3.7
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• 2019

Graphene, which is one of the most promising materials for its state-of-the-art applications, has received extensive attention because of its superior mechanical properties. However, there is little experimental evidence related to the mechanical properties of graphene at the atomic level because of the challenges associated with transferring atomically-thin two-dimensional (2D) materials onto microelectromechanical systems (MEMS) devices. In this study, we show successful dry transfer with a gel material of a stable, clean, and free-standing exfoliated graphene film onto a push-to-pull (PTP) device, which is a MEMS device used for uniaxial tensile testing in in situ transmission electron microscopy (TEM). Through the results of optical microscopy, Raman spectroscopy, and TEM, we demonstrate high quality exfoliated graphene on the PTP device. Finally, the stress-strain results corresponding to propagating cracks in folded graphene were simultaneously obtained during the tensile tests in TEM. The zigzag and armchair edges of graphene confirmed that the fracture occurred in association with the hexagonal lattice structure of graphene while the tensile testing. In the wake of the results, we envision the dedicated preparation and in situ TEM tensile experiments advance the understanding of the relationship between the mechanical properties and structural characteristics of 2D materials.

• Transactions on Electrical and Electronic Materials
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• v.4 no.3
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• pp.15-18
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• 2003

Aluminum oxide ($Al_2O_3$) materials were coated conformally on ZnO nanorods by atomic layer deposition (ALD). The ZnO nanorods were first synthesized on a Si(100) substrate from ball-milled ZnO powders by a thermal evaporation procedure. $Al_2O_3$ films were then deposited on these ZnO nanorods by ALD at a substrate temperature of $300^{\circ}C$ using trimethylaluminum (TMA) and distilled water ($H_2O$). Transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) images of the deposited ZnO nanorods revealed that amorphous $Al_2O_3$ cylindrical shells surround the ZnO nanorods. These TEM images illustrate that ALD has an excellent capability to coat any shape of nanorods conformally.

• Bulletin of the Korean Chemical Society
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• v.34 no.3
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• pp.773-776
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• 2013

We have prepared 1-D BiSI and 2-D BiOI nanostructures, and characterized them by scanning electron microscopy, transmission electron microscopy (TEM), X-ray diffraction crystallography, thermogravimetric analysis/differential scanning calorimetry, and UV-visible absorption. Here, we first report clear HR-TEM image of BiSI. In addition, we first found that the growth direction of BiSI is [12-1] plane, with the neighboring distance of 0.30 nm. The crystal structures of BiSI and BiOI are found to be orthorhombic (Pnam) and tetragonal (P4/nmm), respectively. The absorption band gaps of BiSI and BiOI are measured to be 1.55 and 1.92 eV, respectively. Our study could further highlight the applications of V-VI-VII compounds.

• Transactions on Electrical and Electronic Materials
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• v.5 no.4
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• pp.143-147
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• 2004

Surface defects and bulk defects on SOI wafers are studied. Two new metrologies have been proposed to characterize surface and bulk defects in epitaxial layer transfer (ELTRAN) wafers. They included the following: i) laser scattering particle counter and coordinated atomic force microscopy (AFM) and Cu-decoration for defect isolation and ii) cross-sectional transmission electron microscope (TEM) foil preparation using focused ion beam (FIB) and TEM investigation for defect morphology observation. The size of defect is 7.29 urn by AFM analysis, the density of defect is 0.36 /cm$^2$ at as-direct surface oxide defect (DSOD), 2.52 /cm$^2$ at ox-DSOD. A hole was formed locally without either the silicon or the buried oxide layer (Square Defect) in surface defect. Most of surface defects in ELTRAN wafers originate from particle on the porous silicon.