• Applied Microscopy
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• 제38권4호
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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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• 제47권3호
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• pp.208-213
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• 2017

The microstructural changes in Co nanoparticles and an Au-10at.%Pd thin film have been investigated using an in situ heating holder with a micro-electro-mechanical system (MEMS). In Co nanoparticles, two phases (face-centered cubic and hexagonal close-packed crystal structures) were found to coexist at room temperature and microstructures at temperatures, higher than $1,000^{\circ}C$, were observed with a quick response time and significant stability. The actual temperature of each specimen was directly estimated from the changes in the lattice spacing (Bragg-peak separation). For the Au-10at.%Pd thin film, at a set temperature of $680^{\circ}C$, the actual temperature of the sample was estimated to be $1,020^{\circ}C{\pm}123^{\circ}C$. Note that the specimen temperature should be carefully evaluated because of the undesired effects, i.e., the temperature non-uniformity due to the sample design of the MEMS chip, and distortion due to thermal expansion.

• Carbon letters
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• 제14권4호
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• pp.228-233
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• 2013

In this work, we report in-situ observations of changes in catalyst morphology, and of growth termination of individual carbon nanotubes (CNTs), by complete loss of the catalyst particle attached to it. The observations strongly support the growth-termination mechanism of CNT forests or carpets by dynamic morphological evolution of catalyst particles induced by Ostwald ripening, and sub-surface diffusion. We show that in the tip-growth mode, as well as in the base-growth mode, the growth termination of CNT by dissolution of catalyst particles is plausible. This may allow the growth termination mechanism by evolution of catalyst morphology to be applicable to not only CNT forest growth, but also to other growth methods (for example, floating-catalyst chemical vapor deposition), which do not use any supporting layer or substrate beneath a catalyst layer.

• Applied Microscopy
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• 제45권3호
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• pp.107-114
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• 2015

Two-dimensional (2D) materials containing hole defects are a promising substitute for conventional nanopore membranes like silicon nitride. Hole defects on 2D materials, as atomically thin nanopores, have been used in nanopore devices, such as DNA sensor, gas sensor and purifier at lab-scale. For practical applications of 2D materials to nanopore devices, researches on characteristics of hole defects on graphene, hexagonal boron nitride and molybdenum disulfide have been conducted precisely using transmission electron microscope. Here, we summarized formation, features, structural preference and stability of hole defects on 2D materials with atomic-resolution transmission electron microscope images and theoretical calculations, emphasizing the future challenges in controlling the edge structures and stabilization of hole defects. Exploring the properties at the local structure of hole defects through in situ experiments is also the important issue for the fabrication of realistic 2D nanopore devices.

• Applied Microscopy
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• 제45권1호
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• pp.16-22
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• 2015

The reaction kinetics of the growth of Ni germanide in the Ni/Zr-interlayer/Ge system was investigated using isothermal in situ annealing at three different temperatures in a transmission electron microscope. The growth rate of Ni germanide in the Ni/Zr-interlayer/Ge system was determined to be diffusion controlled and depended on the square root of the time, with the activation energy of $1.04P{\pm}0.04eV$. For the Ni/Zr-interlayer/Ge system, no intermediate or intermixing layer between the Zr-interlayer and Ge substrate was formed, and thus the Ni germanide was formed and grew uniformly due to Ni diffusion through the diffusion path created in the amorphous Zr-interlayer during the annealing process in the absence of any intermetallic compounds. The reaction kinetics in the Ni/Zr-interlayer/Ge system was affected only by the Zr-interlayer.

• Applied Microscopy
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• 제36권spc1호
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• pp.63-69
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• 2006

By utilizing a field emission gun and a biprism installed on a transmission electron microscope (TEM), electron holography is extensively carried out to visualize the electric and magnetic fields of nanomaterials. In the electric field analysis, the distribution of electric potential in a sharp tip made of W coated with $ZrO_2$ is visualized by applying the voltage to the tip. Denser contour lines due to the electric potential are observed with an increase in the bias voltage. In the magnetic field analysis by producing the strong magnetic field with a sharp magnetic needle made of a permanent magnet, the in situ experiment is carried out to investigate the magnetization of hard magnetic materials. The results of these experiments clearly demonstrate that electron holography is a promising advanced transmission electron microscopy technique to characterize the electric and magnetic properties of nanomaterials.

• Bulletin of the Korean Chemical Society
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• 제33권8호
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• pp.2535-2538
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• 2012

$SnO_2@carbon$ tube-core nanowire was synthesized via a facile self-organized method, which was in situ by one step via Chemical Vapor Deposition. The resulting composite was characterized by scanning electron microscopy, X-ray diffraction and transmission electron microscope. The diameter of the single nanowire is between 5 nm and 60 nm, while the length would be several tens to hundreds of micrometers. Then X-ray diffraction pattern shows that the composition is amorphous carbon and tin dioxide. Transmission electron microscope images indicate that the nanowire consists of two parts, the outer carbon tube and the inner tin dioxide core. Meanwhile, the possible growth mechanism of $SnO_2@carbon$ tube-core nanowire is also discussed.

• 대한수의학회지
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• 제36권4호
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• pp.845-858
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• 1996

The purpose of this study was to establish early diagnostic methods for the detection of Aujeszky's disease viral antigens and nucleic acid in nasal cells, and buffy coats from experimentally infected living pigs by a combination of immunocytochemistry, in situ hybridization with digoxigenin(DIG)-labled probe and electron microscopy. Forty days old piglets were inoculated intranasally with $10^{7.0}TCID_{50}$ of Aujeszky's disease virus (ADV, NYJ-1-87 strain). The viral antigens and nucleic acid of ADV were detected in nasal cells, and buffy coat for 20 days after inoculation by immunocytochemistry, in situ hybridization with DIG-labeled probe and electron microscopical method. The results were compared with conventional methods such as a porcine Aujeszky's disease serodiagnostic(PAD) kit, neutralization test(NT) and virus isolation. 1. The viral antigens, nucleic acids and capsids of ADV were detected in nasal cells, buffy coats from 3 days to 20 days after inoculation by immunocytochemistry, in situ hybridization with DIG-labeled probe and electron microscopy, respectively. 2. When viral antigens were detected by the immunocytochemical technique, a diffuse brown deposit was observed in the nucleus and cytoplasm of nasal cells, buffy coats and PK-15 cells under a microscope. 3. DIG-labeled DNA probe was prepared by amplification of conserved sequence of recombinant ADV-gp50 clone with polymerase chain reacction. When ADV-DNA was detected by ISH with DIG-labeled probe, purplish blue pigmentation were observed in the nuclei and cytoplasms of ADV-infected cells under a microscope. Positive signals were observed in nasal cells and in the buffy coat and PK-15 cells at the first day after inoculation. 4. Where ADV-capsids were detected by transmission electron microscopical method, aggregation of capsids was observed in the nuclei and cytoplasms of nasal cells, buffy coats and PK-15 cells. The results suggested that these methods were considered as the highly sensitive and reliable tools for rapid and confirmative diagnosis of Aujeszky's disease in living pigs.

• Applied Microscopy
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• 제36권spc1호
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• pp.25-33
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• 2006

Nanofabrication with finely focused ion and electron beams is reviewed, and position and size controlled fabrication of nano-metals and -semiconductors is demonstrated. A focused ion beam (FIB) interface attached to a column of 200keV transmission electron microscope (TEM) was developed. Parallel lines and dots arrays were patterned on GaAs, Si and $SiO_2$ substrates with a 25keV $Ga^+-FIB$ of 200nm beam diameter at room temperature. FIB nanofabrication to semiconductor specimens caused amorphization and Ga injection. For the electron beam induced chemical vapor deposition (EBI-CVD), we have discovered that nano-metal dots are formed depending upon the beam diameter and the exposure time when decomposable gases such as $W(CO)_6$ were introduced at the beam irradiated areas. The diameter of the dots was reduced to less than 2.0nm with the UHV-FE-TEM, while those were limited to about 15nm in diameter with the FE-SEM. Self-standing 3D nanostructures were also successfully fabricated.

• Applied Microscopy
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• 제52권
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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.