• Applied Microscopy
• /
• v.36 no.spc1
• /
• pp.9-17
• /
• 2006

An interface and a grain boundary in the solid state can be quite unstable and vibrate violently under special circumstances. Two examples of such a vibration, as observed by in-situ transmission electron microscopy, were presented.

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

• Applied Microscopy
• /
• v.38 no.4
• /
• pp.383-386
• /
• 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
• /
• v.43 no.2
• /
• pp.88-97
• /
• 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.

• Transactions of Materials Processing
• /
• v.33 no.2
• /
• pp.118-122
• /
• 2024

Micro-electromechanical systems (MEMS) based in-situ heating holders have been developed to enable high resolution imaging of heat treatment analysis. However, unlike the standard 3 mm metal disk specimens used in the furnace-based heating holder and general transmission electron microscopy holder, the MEMS-based in-situ heating holder requires thin specimens that can be penetrated by electrons to be transferred onto the MEMS chip. Previously, focused ion beam milling was used to transfer metal specimens, but it has the disadvantage of being expensive and the risk of specimen damage due to gallium ions. Therefore, in this study, we devised a method of transferring metallic materials by ultrasonic treatment using a transmission electron microscopy specimen made by electro jet polishing. A 3mm electropolished metal disk was placed in an appropriate solution, ultrasonicated, and then drop casted. The transfer of the specimen was successful, but it was confirmed that dislocations were formed inside the specimen due to ultrasonic treatment. This study provides a novel method for transferring metallic materials onto MEMS chips, which is cost-effective and less gallium ion damaging to the specimen. The results of this study can be used to improve the efficiency of heat treatment analysis using MEMS-based in-situ heating holders.

• Applied Microscopy
• /
• v.50
• /
• pp.22.1-22.6
• /
• 2020

In-situ transmission electron microscopy (TEM) holders that employ a chip-type specimen stage have been widely utilized in recent years. The specimen on the microelectromechanical system (MEMS)-based chip is commonly prepared by focused ion beam (FIB) milling and ex-situ lift-out (EXLO). However, the FIB-milled thin-foil specimens are inevitably contaminated with Ga⁺ ions. When these specimens are heated for real time observation, the Ga⁺ ions influence the reaction or aggregate in the protection layer. An effective method of removing the Ga residue by Ar⁺ ion milling within FIB system was explored in this study. However, the Ga residue remained in the thin-foil specimen that was extracted by EXLO from the trench after the conduct of Ar⁺ ion milling. To address this drawback, the thin-foil specimen was attached to an FIB lift-out grid, subjected to Ar⁺ ion milling, and subsequently transferred to an MEMS-based chip by EXLO. The removal of the Ga residue was confirmed by energy dispersive spectroscopy.

• Applied Microscopy
• /
• v.45 no.2
• /
• pp.95-100
• /
• 2015

The in-situ heating transmission electron microscopy experiment allows us to observe the time- and temperature-dependent dynamic processes in nanoscale materials by examining the same specimen. The temperature, which is a major experimental parameter, must be measured accurately during in-situ heating experiments. Therefore, calibrating the thermocouple readout of the heating holder prior to the experiment is essential. The calibration can be performed using reference materials whose phase-transformation (melting, oxidation, reduction, etc.) temperatures are well-established. In this study, the calibration experiment was performed with four reference materials, i.e., pure Sn, Al-95 wt%Zn eutectic alloy, NiO/carbon nanotube composite, and pure Al, and the calibration curve and formula were obtained. The thermocouple readout of the holder used in this study provided a reliable temperature value with a relative error of <4%.

• Applied Microscopy
• /
• v.45 no.4
• /
• pp.208-213
• /
• 2015

Nanomanipulators installed in focused ion beam (FIB), which is used in the lift-out of lamella when preparing transmission electron microscopy specimens, have recently been employed for electrical resistance measurements, tensile and compression tests, and in situ reactions. During the pick-up process of a single nanowire (NW), there are crucial problems such as Pt, C and Ga contaminations, damage by ion beam, and adhesion force by electrostatic attraction and residual solvent. On the other hand, many empirical techniques should be considered for successful pick-up process, because NWs have the diverse size, shape, and angle on the growth substrate. The most important one in the in-situ precedence, therefore, is to select the optimum pick-up process of a single NW. Here we provide the advanced methodologies when manipulating NWs for in-situ mechanical and electrical measurements in FIB.

• 한국전자현미경학회:학술대회논문집
• /
• 1998.05a
• /
• pp.15-15
• /
• 1998

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
• /
• v.13 no.2
• /
• pp.125-130
• /
• 2000

Two step growth of reduced pressure chemical vapor eposition has been successfully developed to achieve in-situ phosphorus-doped silicon epilayers, and the characteristic evolution on their microstructures has been investigated using scanning electron microscopy, transmission electron microscopy, and secondary ion mass spectroscopy. The two step growth, which employs heavily in-situ P doped silicon buffer layer grown at low temperature, proposes crucial advantages in manipulating crystal structures of in-situ phosphorus doped silicon. In particular, our experimental results showed that with annealing of the heavily P doped silicon buffer layers, high-quality epitaxial silicon layers grew on it. the heavily doped phosphorus in buffer layers introduces into native oxide and plays an important role in promoting the dispersion of native oxides. Furthermore, the phosphorus doping concentration remains uniform depth distribution in high quality single crystalline Si films obtained by the two step growth.