• 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.43 no.2
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• pp.88-97
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• 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
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• v.33 no.2
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• pp.118-122
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• 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.

• 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.

• Transactions of Materials Processing
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• v.16 no.3 s.93
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• pp.210-214
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• 2007

Manufacturing bulk nanostructured materials with least grain growth from initial powders is challenging because of the bottle neck of bottom-up methods using the conventional powder metallurgy via compaction and sintering. In the study, densification behavior of nano Cu powders during pressureless sintering was investigated using an in-situ optical dilatometer technique. The initial heating and steady temperature stages during the sintering of nano Cu powder compacts were observed. At the initial heating stage, the powder compact has many porosities and full densification needs high temperature and/or high pressure sintering. In the experimental analysis, changes in geometry and density were measured and discussed for optimal consolidation and densification by the in-situ optical dilatometer.

• Transactions on Electrical and Electronic Materials
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• v.6 no.3
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• pp.106-109
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• 2005

We have investigated the generation of pretilt angle for a nematic liquid crystal (NLC) alignment with in-situ photoalignment method on polyimide (PI) surfaces using polymer films. Especially, we studied in-situ photoalignment changing heating temperature from $50^{\circ}C\;to\;120^{\circ}C$ on the polymer film. The LC aligning capabilities and pretilt angle on the polymer substrates were better than those on the glass substrate using in-situ photoalignment method. It is considered that this increase in pretilt angle may be attributed to the roughness of the micro-groove substrate induced by the in-situ photoalignment. As temperature of heated subtrate and UV exposure time increase, pretilt angle of the cell used polymer film increased. It is considered that the heating temperature of substrate is attributed to generate pretilt angle. Also, electro-optical performances of the in-situ photoaligned TN cell using the polymer substrate are almost the same as that of the TN cell using the glass substrate.

• 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.

• Applied Microscopy
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• v.45 no.2
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• pp.95-100
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• 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
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• v.47 no.3
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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.

• Transactions on Electrical and Electronic Materials
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• v.7 no.3
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• pp.145-148
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• 2006

In this study, the response surface modeling of the pretilt angle control using in-situ photoalignment method with oblique UV exposure .on plastic substrate is investigated. The pretilt angle is the main factor to determine the alignment of the liquid crystal display. The response surface model is used to analyze the variation of the pretilt angle on the various process conditions. Heating temperature and UV exposure time are considered as input factors. The liquid crystal (LC) pretilt angle increased with increasing heating temperature and UV exposure time. The analysis of variance is used to analyze the statistical significance and the effect plots are also investigated to examine the relationship between the process parameters and the response.