• Applied Microscopy
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• v.38 no.4
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• pp.383-386
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• 2008

In performing in situ heating transmission electron microscopy (TEM) for materials characterizations, arising concerns such as specimen drifts and unintentional Cu contamination are discussed. In particular, we analysed the thermal and mechanical characteristics of in situ heating holders to estimate thermal drift phenomena. From the experimental results, we suggest an empirical model to describe the thermal drift behavior so that we can design an effective plan for in situ heating experiment. Practical approaches to minimize several hindrances arisen from the experiment are proposed. We believe that our experimental recommendations will be useful for a microscopist fascinated with the powerful potential of in situ heating TEM.

• Applied Microscopy
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• v.51
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• pp.8.1-8.7
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• 2021

Growing demands for comprehending complicated nano-scale phenomena in atomic resolution has attracted in-situ transmission electron microscopy (TEM) techniques for understanding their dynamics. However, simple to safe TEM sample preparation for in-situ observation has been limited. Here, we suggested the optical microscopy based micro-manipulating system for transferring TEM samples. By adopting our manipulator system, several types of samples from nano-wires to plate-like thin samples were transferred on micro-electro mechanical systems (MEMS) chip in a single step. Furthermore, the control of electrostatic force between the sample and the probe tip is found to be a key role in transferring process.

• 한국정보디스플레이학회:학술대회논문집
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• 2005.07b
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• pp.1081-1086
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• 2005

Dynamic behavior of carbon nanotubes (CNTs) in an electric field is directly observed by in-situ transmission electron microscopy (TEM). The CNT field emitters examined by in-situ TEM are multiwalled, double-walled and single walled CNTs. Threshold fields for electron emission and sustainable emission currents depending on the structure of CNTs are presented, and degradation mechanism of the CNT field emitters is discussed. In addition to the microscopy studies on individual CNTs, our recent development in surface treatment of CNT layers grown by chemical vapor deposition, which brings about high density of emission current and high uniformity, is also presented.

• 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.

• Journal of the Mineralogical Society of Korea
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• v.18 no.4 s.46
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• pp.289-299
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• 2005

Annealing experiments on albite powders, thin sections, and TEM specimens have been performed utilizing an optical microscope heating stage. Sample orientations were determined by optical microscope and XRD, and then confirmed by TEM diffraction patterns. Partial melting of samples occurred at $1030^{\circ}C$-l2 hr for powder, but at $1060^{\circ}C$-12 hr for TEM specimen. It is difficult to get TEM images of albite microstructures above this temperature due to thickening and the amorphous phase of the melted part. Correlative studies between optical microscopy and TEM indicated that the $1050^{\circ}C$-12 hr annealing in ambient condition was most adequate to observe tweed microstructures in albite through TEM. In situ TEM heating experiments for direct observation of tweed microstructures in albite may require annealing at slightly higher temperatures than $1050^{\circ}C$ considering the high vacuum condition inside TEM.

• Applied Microscopy
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• v.31 no.4
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• pp.315-323
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• 2001

In situ TEM heating experiments utilizing kaolinite powder samples result in the following facts. (1) The water recirculation system adopted in the Gatan's heating holder is required to prevent specimen drift above $500^{\circ}C$. (2) Since the degree of phase changes depends on the thickness of powders below $600^{\circ}C$, examinations of both thin and thick specimens are required. (3) Sample preparation using Mo-grids is required for TEM heating experiments above $900^{\circ}C$. At these temperature ranges the effect of heating rate and holding time on the phase transition process increases drastically, so that a programmed temperature control is required. (4) TEM heating experiments of the embedded powders by epoxy for the cross-sectional view was limited due to the severe epoxy movement during heating above $300^{\circ}C$. Better methods of sample preparation are required to overcome this problem.

• Proceedings of the Materials Research Society of Korea Conference
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• 2007.05a
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• pp.14.1-14.1
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• 2007

• Elastomers and Composites
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• v.44 no.1
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• pp.34-40
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• 2009

New coupling agent or surface modified agent (9-decenoic acid) was used to enhance the compatibility between silica and polystyrene in silica/polystyrene hybrid nanocomposite, synthesized by in situ miniemulsion polymerization. Composites contain well dispersed nanosize silica particles. Related tests and analyses confirmed the success of synthesis. Functionalization of silica by 9-decenoic acid and silica on the polystyrene was confirmed by FTIR. TGA showed presence and amount of silica in final latex. The glass transition temperature of the hybrid nanocomposite was increased with the silica amount. SEM and TEM analysis showed the spherical morphology of PS and composite with an average diameter of 55 nm. The presence of silica within composite was confirmed by EDS attached to the existing TEM.

• 한국신재생에너지학회:학술대회논문집
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• 2010.11a
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• pp.38.1-38.1
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• 2010

The trend to thinner crystalline silicon solar wafers in production of solar cells investigates re-evolution of back surface field (BSF) formation. We have studied mechanisms of back contact formation in Al evaporation and screen printed Al paste for Si solar cells by TEM analysis. We observed that Si diffuse into Al during heat up. The Si diffusion process made vacancies in Si wafer. The Al began to seep into the Si wafer (Al spike). During heat down, the Al spike were shrink which causes the doped region (BSF).

• 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 $900^{\circ}C$.