• 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.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.

• 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.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 $900^{\circ}C$.

• Journal of Korea Foundry Society
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• v.15 no.3
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• pp.252-261
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• 1995

The purposes of this study were to investigate the microstructural changes in alloy ribbons of Al-Fe-Mo-Si quarternary system at $450{\sim}500^{\circ}C$, and to study the coarsening mechanism of fine precipitates. Using the hot stage in TEM, in situ microstructural changes in Al-4Fe-0.5Mo-1.5Si alloy ribbon and Al-8Fe-2Mo-1.5Si alloy ribbon have been examined successively up to 60 hours at $450^{\circ}C$ and $500^{\circ}C$. Cell structure in zone B of Al-4Fe-0.5Mo-1.5Si alloy ribbon was observed to collapse even in 10 minutes by in-situ heating at $450^{\circ}C$ and the size of precipitates in zone B increased twice in 60 hours. The precipitates in zone A of Al-4Fe-0.5Mo-1.5Si alloy ribbon showed slower coarsening rate than those in zone B by in-situ heating at $450^{\circ}C$. The precipitates in zone A of Al-8Fe-2Mo-1.5Si alloy ribbon increased 50% by in-situ heating at $500^{\circ}C$ in 50 hours compared to the initial precipitates while any microstructual change in zone B was not observed by in-situ heating at $500^{\circ}C$ up to 50 hours. Only the precipitates in zone A of Al-4Fe-0.5Mo-1.5Si alloy ribbon satisfied $r^3{\propto}t$ relationship of coarsening mechanism.

• Applied Microscopy
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• v.36 no.spc1
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• pp.19-24
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• 2006

The alumina-aluminum solid-liquid interfaces were directly observed at atomic scale by heating the alumina single crystal in high-voltage electron microscope (HVEM) owing to the electron beam damage processes, Atomic ordering in the first several layers of the liquid was clearly resolved adjacent to the alumina surface and its relevance to the single crystal growth was examined with the real-time observations.

• Applied Microscopy
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• v.48 no.4
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• pp.128-129
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• 2018

Soft ferromagnetic materials are utilized for various electromagnetic devices such as magnetic recording heads and magnetic shielding. In situ observation of magnetic microstructures and domain wall motions are prerequisite for understanding and improving their magnetic properties. In this work, by the Fresnel (out-of-focus) method of Lorentz microscopy, we observe the domain wall motions of polycrystalline Ni/Ti thin film layers triggered by single-shot laser pulse. Random motions of domain walls were visualized at every single pulse.

• Applied Microscopy
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• v.33 no.1
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• pp.49-58
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• 2003

The ${\alpha}-{\beta}$ phase transition of titanium was investigated through in-situ EF-TEM heating experiments. Three different areas of a titanium foil were observed to minimize statistical errors. Systematic recording of diffraction patterns and images was carried out from $RT{\rightarrow}600^{\circ}C{\rightarrow}900^{\circ}C{\rightarrow}RT$ on each area. The following results were obtained: (1) Transition of titanium takes place very rapidly at $900^{\circ}C$. Two phases of titanium, ${\alpha}\;and\;{\beta}$, coexist at this temperature. (2) The transited ${\beta}$-phase appears in the form of twinned plates which are arranged in rotation relationship one another. (3) Analyses of electron diffraction patterns and EDS data indicate that the thermal oxidation layer is gradually formed on the surface of titanium above $900^{\circ}C$, which hinders the reversible ${\beta}{\rightarrow}{\alpha}$ phase transition upon cooling.

• Applied Microscopy
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• v.36 no.spc1
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• pp.35-40
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• 2006

Self-assembled InAs/GaAs quantum dots (QDs) were grown by the atomic layer epitaxy (ALE) and molecular beam epitaxy (MBE) techniques, The structure and the thermal stability of QDs have been studied by high resolution electron microscopy with in-situ heating experiment capability, The ALE and MBE QDs were found to form a hemispherical structure with side facets in the early stage of growth, Upon capping by GaAs layer, however, the apex of QDs changed to a flat one. The ALE QDs have larger size and more regular shape than those of MBE QDs. The QDs collapse due to elevated temperature was observed directly in atomic scale, In situ heating experiment within TEM revealed that the uncapped QDs remained stable up to $580^{\circ}C$, However, at temperature above $600^{\circ}C$, the QDs collapsed due to the diffusion and evaporation of In and As from the QDs, The density of the QDs decreased abruptly by this collapse and most of them disappeared at above $600^{\circ}C$.

• 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.