• Applied Microscopy
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• v.47 no.2
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• pp.77-83
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• 2017

Drastic development of ubiquitous devices requires more advanced batteries with high specific capacitance and high rate capability. Large-area microstructure characterization across the stacks of cathode, electrolyte and anode might reveal the origin of the instability or degradation of batteries upon cycling charge. In this study, sample preparation methods to observe the cross-section view of the electrodes for battery in SEM and several imaging tips are reviewed. For an accurate evaluation of the microstructure, ion milling which flats the surface uniformly is recommended. Pros and cons of cross-section polishing (CP) with Ar ion and focused ion beam (FIB) with Ga ion were compared. Additionally, a modified but new cross-section milling technique utilizing precision ion polishing system (PIPS) which can be an alternative method of CP is developed. This simple approach will make the researchers have more chances to prepare decent large-area cross-section electrode for batteries.

• Corrosion Science and Technology
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• v.14 no.6
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• pp.301-312
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• 2015

Corrosion of zirconium fuel cladding is known to limit the lifetime and reloading cycles of fuel in nuclear reactors. Oxide layers formed on ZIRLO4^{TM}$ cladding samples, after immersion for 300-hour and 50-day in a simulated primary water chemistry condition ($360^{\circ}C$ and 20 MPa), were analyzed by using the scanning transmission electron microscopy (STEM), in-situ transmission electron microscopy (in-situ TEM) with the focused ion beam (FIB) technique, and X-ray diffraction (XRD). Both samples (immersion for 300 hours and 50 days) revealed the presence of the ZrO sub-oxide phase at the metal/oxide interface and columnar grains developed perpendicularly to the metal/oxide interface. Voids and micro-cracks were also detected near the water/oxide interface, while relatively large lateral cracks were found just above the less advanced metal/oxide interface. Equiaxed grains were mainly observed near the water/oxide interface.

• Applied Microscopy
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• v.40 no.4
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• pp.177-183
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• 2010

A focused ion beam (FIB) system produces a beam of positive ions (usually gallium) which are heavier than electrons and can be focused by electrostatic lenses into a spot on the specimen. With its ability milling of the specimen material by 10 to 100 nm with each pass of the beam, FIB is widely adopted in materials science, semiconductor industry, and ceramics research. Recently, FIB has been increasingly employed in the field of biomedical sciences. Here we provide a brief introduction to FIB and its applications for a wide variety of biomedical research. The surface of specimen can be in situ processed and quasi-real time visualized by two beam combination of FIB and field emission scanning electron microscope (FESEM). Due to its milling process, internal structures can be exposed and analyzed: yeast cells, fungus-inoculated wheat leaf, mannitol particles in inhalation aerosols, and oyster shell. Serial blockface tomography with the system kindles 3-dimensional reconstruction researches in the realm of nervous system and life sciences. Two-beam system of FIB/FESEM is a versatile tool to be utilized in the biomedical sciences, especially in 3-dimensional reconstruction studies.

• Korean Journal of Materials Research
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• v.20 no.12
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• pp.645-648
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• 2010

The structure and morphology of epitaxial layer defects in epitaxial Si wafers produced by the Czochralski method were studied using focused ion beam (FIB) milling, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Epitaxial growth was carried out in a horizontal reactor at atmospheric pressure. The p-type Si wafers were loaded into the reactor at about $800^{\circ}C$ and heated to about $1150^{\circ}C$ in $H_2$. An epitaxial layer with a thickness of $4{\mu}m$ was grown at a temperature of 1080-$1100^{\circ}C$. Octahedral void defects, the inner walls of which were covered with a 2-4 nm-thick oxide, were surrounded mainly by $\{111\}$ planes. The formation of octahedral void defects was closely related to the agglomeration of vacancies during the growth process. Cross-sectional TEM observation suggests that the carbon impurities might possibly be related to the formation of oxide defects, considering that some kinds of carbon impurities remain on the Si surface during oxidation. In addition, carbon and oxygen impurities might play a crucial role in the formation of void defects during growth of the epitaxial layer.

• Nuclear Engineering and Technology
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• v.46 no.2
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• pp.147-158
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• 2014

In order to investigate how the microstructure of fuel/matrix-interaction (FMI) layers change during irradiation, different U-7Mo dispersion fuel plates have been irradiated to high fission density and then characterized using scanning electron microscopy (SEM). Specifially, samples from irradiated U-7Mo dispersion fuel elements with pure Al, Al-2Si and AA4043 (~4.5 wt.%Si) matrices were SEM characterized using polished samples and samples that were prepared with a focused ion beam (FIB). Features not observable for the polished samples could be captured in SEM images taken of the FIB samples. For the Al matrix sample, a relatively large FMI layer develops, with enrichment of Xe at the FMI layer/Al matrix interface and evidence of debonding. Overall, a significant penetration of Si from the FMI layer into the U-7Mo fuel was observed for samples with Si in the Al matrix, which resulted in a change of the size (larger) and shape (round) of the fission gas bubbles. Additionally, solid fission product phases were observed to nucleate and grow within these bubbles. These changes in the localized regions of the microstructure of the U-7Mo may contribute to changes observed in the macroscopic swelling of fuel plates with Al-Si matrices.

• Transactions of the Korean Society of Pressure Vessels and Piping
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• v.17 no.2
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• pp.109-118
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• 2021

In the periodic surveillance material test for the spacer component of fuel channel assembly in CANDU, a microstructural characterization analysis is required in addition to the mechanical property evaluation test. In this study, detailed microstructure analysis and simple mechanical property evaluation of archive spacer parts were conducted to indirectly support the surveillance test and assist in the study of spacer material degradation. We investigated the microstructural characteristics of the spacer garter spring coil through comparative analysis with the plate material. The main microstructure characteristics of the garter spring coil X-750 are represented by the fine grain size distribution, the ordering phase distribution developed inside the matrix, the high dislocation density inside the grains, and the arrangement of coarse carbides. In addition, the yield strength of the garter spring coil X-750 was indirectly evaluated to be approximately 1 GPa. We also established an analytical method to elucidate the microstructural evolution of the radioactive spacer garter spring coil X-750 based on Canadian research experiences. Finally, we confirmed the measurement technique for helium bubble formation through TEM examination on the helium implanted X-750 material.

• Nuclear Engineering and Technology
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• v.55 no.8
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• pp.2742-2746
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• 2023

The corrosion behavior of copper immersed in dilute oxychloride solution (100 mM) was studied through surface investigation and in-situ monitoring of open-circuit potential. The copper corrosion was initiated with copper dissolution into a form of CuCl^-₂, resulting in mass decrease within the first 40 h of immersion. This was followed by a hydrolysis reaction initiated by the CuCl^-₂ at the copper surface, after which oxide products were formed and deposited on the surface, resulting in a mass increase. The formation of nucleation sites for copper oxide and its lateral extension during the corrosion process were examined using focused ion beam (FIB)-scanning electron microscopy (SEM). The presence of metastable compounds such as atacamite (CuCl₂·3Cu(OH)₂) on the corroded copper surface was revealed by X-ray photoelectron spectra (XPS) and transmission electron microscopy (TEM)-energy dispersive spectrometry (EDS) analysis.

• Journal of Sensor Science and Technology
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• v.30 no.5
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• pp.273-278
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• 2021

Here, we studied the change in the mechanical stiffness of a diaphragm according to the corrugation pattern. The diaphragm consists of a silicon oxide and nitride double layer; a corrugation pattern was formed by dry etching, and the diaphragm was released by wet etching. The fabrication of the thin film was verified using focused ion beam and scanning electron microscopy images. The mechanical stiffness of the diaphragm was obtained by measuring the surface vibration using a laser Doppler vibrometer while applying external sound pressure. Flat squares, diaphragms with square corrugations, and circular corrugation patterns were measured and compared. The stiffness of the diaphragm with a corrugation structure was found to be smaller than that without a corrugation structure; in particular, circular corrugation showed a better effect because of the high symmetry. Furthermore, the effect of corrugation was theoretically predicted. The proposed corrugated diaphragm showed comparable flexibility with the state-of-the-art MEMS microphone diaphragm.

• Nuclear Engineering and Technology
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• v.53 no.8
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• pp.2629-2639
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• 2021

Within the frame of the EMPIrE test, four monolithic mini-plates were irradiated in the ATR reactor. In two of them, the monolithic U(Mo) foil had been PVD-coated with Zr before the plate manufacturing. Extensive microstructural characterizations were performed on a fresh archive mini-plate, using Optical Microscopy (OM), Scanning Electron Microscopy (SEM) combined with Energy Dispersive Spectroscopy (EDS), Electron Backscattered Diffraction (EBSD) and Focused Ion Beam (FIB)/Transmission Electron Microscopy (TEM) with nano EDS. A particular attention was paid to the examination of the U(Mo) foil, the PVD coating, the cladding/Zr and Zr/U(Mo) interfaces. The Zr coating has a thickness around 15 ㎛. It has a columnar microstructure and appears dense. The cohesion of the cladding/Zr and Zr/U(Mo) interfaces seems to be satisfactory. An almost continuous layer with a thickness of the order of 100-300 nm is present at the cladding/Zr interface and corresponds to an oxidized part of the Zr coating. At the Zr/U(Mo) interface, a thin discontinuous layer is observed. It could correspond to locally oxidized U(Mo). This work provides a basis for interpreting the results of characterizations on EMPIrE irradiated plates.

• Journal of Welding and Joining
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• v.32 no.3
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• pp.60-67
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• 2014

The ability of electronic packages and assemblies to resist solder joint failure is becoming a growing concern. This paper reports on a study of high speed shear energy of Sn-4.0wt%Ag-0.5wt%Cu (SAC405) solder with different electroless Ni-P thickness, with $HNO_3$ vapor's status, and with various pre-conditions. A high speed shear testing of solder joints was conducted to find a relationship between the thickness of Ni-P deposit and the brittle fracture in electroless Ni-P deposit/SAC405 solder interconnection. A focused ion beam (FIB) was used to polish the cross sections to reveal details of the microstructure of the fractured pad surface with and without $HNO_3$ vapor treatment. A scanning electron microscopy (SEM) and an energy dispersive x-ray analysis (EDS) confirmed that there were three intermetallic compound (IMC) layers at the SAC405 solder joint interface: $(Ni,Cu)_3Sn_4$ layer, $(Ni,Cu)_2SnP$ layer, and $(Ni,Sn)_3P$ layer. The high speed shear energy of SAC405 solder joint with $3{\mu}m$ Ni-P deposit was found to be lower in pre-condition level#2, compared to that of $6{\mu}m$ Ni-P deposit. Results of focused ion beam and energy dispersive x-ray analysis of the fractured pad surfaces support the suggestion that the brittle fracture of $3{\mu}m$ Ni-P deposit is the result of Ni corrosion in the pre-condition level#2 and the $HNO_3$ vapor treatment.