• Korean Journal of Metals and Materials
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• v.46 no.2
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• pp.58-64
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• 2008

Surface-void defects observed on the galvannealed(GA) steel sheets in Interstitial-free high-strengthened steels containing Si and Mn have been investigated using the combination of the FIB(Focused Ion Beam) and FE-TEM(Field Emission-Transmission Electron Microscope) techniques. The scanning ion micrographs of cross-section microstructure of defects showed that these defects were identified as craters which were formed on the projecting part of the substrate surface. Also, those craters were formed on the Si or Mn-Si oxides film through the whole interface between galvannealed coating and steel substrate. Interface enrichments and oxidations of the active alloying elements such as Si and Mn during reduction annealing process for galvanizing were found to interrupt Zn and Fe interdiffusion during galvannealing process. During galvannealing, Zn and Fe interdiffusion is preferentially started on the clean substrate surface which have no oxide layer on. And then, during galvannealing, crater is developed with consumption of molten zinc on the oxide layer.

• 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.

• 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.

• Corrosion Science and Technology
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• v.14 no.2
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• pp.64-75
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• 2015

Single $TiO_2$ coating prepared by sol-gel process usually experiences cracks in coating layer. In order to prevent cracks, an inorganic-organic hybrid $TiO_2-SiO_2$ coating was synthesized by combining precursors with an organic functional group. Five different coatings with various ratios of (1:8, 1:4, 1:1, 1:0.25 and 1:0.125) titanium alkoxide (TBOT, Tetrabutylorthotitanate) to organo-alkoxysilane (MAPTS, ${\gamma}$-Methacryloxy propyltrimethoxysilane) on carbon steel substrate were made by sol-gel dip coating. The prepared coatings were analyzed to study the coating properties (surface crack, thickness, composition) by scanning electron microscope (SEM), focused ion beam (FIB), and Fourier transform infrared spectroscopy (FT-IR). Potentiodynamic polarization tests and electrochemical impedance spectroscopy (EIS) were also performed to evaluate the corrosion characteristics of the coatings. Crack free $TiO_2-SiO_2$ hybrid coatings were prepared with the optimization of the ratio of TBOT to MAPTS. The corrosion rates were significantly decreased in the coatings for the optimized precursor ratio without cracks.

• Journal of the Microelectronics and Packaging Society
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• v.21 no.4
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• pp.63-68
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• 2014

For a nanoscale Cu/low-k wafer, inter-layer dielectric (ILD) and metal layers peelings, cracks, chipping, and delamination are the most common dicing defects by traditional diamond blade saw process. Sidewall void in sawing street is one of the key factors to bring about cracks and chipping. The aim of this research is to evaluate laser grooving & mechanical sawing parameters to eliminate sidewall void and avoid top-side chipping as well as peeling. An ultra-fast pico-second (ps) laser is applied to groove/singulate the 28-nanometer node wafer with Cu/low-k dielectric. A series of comprehensive parametric study on the recipes of input laser power, repetition rate, grooving speed, defocus amount and street index has been conducted to improve the quality of dicing process. The effects of the laser kerf geometry, grooving edge quality and defects are evaluated by using scanning electron microscopy (SEM) and focused ion beam (FIB). Experimental results have shown that the laser grooving technique is capable to improve the quality and yield issues on Cu/low-k wafer dicing process.

• Proceedings of the KSME Conference
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• 2003.04a
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• pp.438-444
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• 2003

A new method to measure residual stress in micron and nano scale films is described. In the theory it is based on Linear Elastic Fracture Mechanics. And in the techniques it depends on the combined capability of the focused ion beam (FIB) imaging system and of high-resolution digital image correlation (DIC) software. The method can be used for any film material (whether amorphous or crystalline) without thinning the substrate. In the method, a region of the film surface is highlighted and scanning electron images of that region taken before and after a long slot, depth a, is introduced using the FIB. The DIC software evaluates the displacement of the surface normal to the slot due to the stress relaxation by using features on the film surface. To minimize the influence of signal noise and rigid body movement, not a few, but all of the measure displacements are used for determining the real residual stress. The accuracy of the method has been assessed by performing measurements on a nano film of diamond like carbon (DLC) on glass substrate and on micro film of aluminum oxide thermally grown on Fecrally substrate. It is shown that the new method determines the residual stress ${\sigma}_R=-1.73$ GPa for DLC and ${\sigma}_R=-5.45$ GPa for the aluminum oxide, which agree quite well with ones measured independently.

• Korean Journal of Materials Research
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• v.27 no.4
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• pp.221-228
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• 2017

Various morphologies of copper oxide (CuO) have been considered to be of both fundamental and practical importance in the field of electronic materials. In this study, using Cu ($0.1{\mu}m$ and $7{\mu}m$) particles, flake-type CuO particles were grown via a wet oxidation method for 5min and 60min at $75^{\circ}C$. Using the prepared CuO, AlN, and silicone base as reagents, thermal interface material (TIM) compounds were synthesized using a high speed paste mixer. The properties of the thermal compounds prepared using the CuO particles were observed by thermal conductivity and breakdown voltage measurement. Most importantly, the volume of thermal compounds created using CuO particles grown from $0.1{\mu}m$ Cu particles increased by 192.5 % and 125 % depending on the growth time. The composition of CuO was confirmed by X-ray diffraction (XRD) analysis; cross sections of the grown CuO particles were observed using focused ion beam (FIB), field emission scanning electron microscopy (FE-SEM), and energy dispersive analysis by X-ray (EDAX). In addition, the thermal compound dispersion of the Cu and Al elements were observed by X-ray elemental mapping.

• Korean Journal of Materials Research
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• v.30 no.11
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• pp.589-594
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• 2020

Many electronic applications require magnetic materials with high permeability and frequency properties. We improve the magnetic permeability of soft magnetic powder by controlling the shape magnetic anisotropy of the powders and through the preparation of amorphous nanoparticles. For this purpose, the effect of the shape magnetic anisotropy of amorphous Fe-B-P nanoparticles is observed through a magnetic field and the frequency characteristics and permeability of these amorphous nanoparticles are observed. These characteristics are investigated by analyzing the composition of particles, crystal structure, microstructure, magnetic properties, and permeability of particles. The composition, crystal structure, and microstructure of the particles are analyzed using inductively coupled plasma optical emission spectrometry-, X-ray diffraction, scanning electron microscopy and focused ion beam analysis. The saturation magnetization and permeability are measured using a vibrating sample magnetometer and an LCR meter, respectively. It is confirmed that the shape magnetic anisotropy of the particles influences the permeability. Finally, the permeability and frequency characteristics of the amorphous Fe-B-P nanoparticles are improved.

• 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.