• 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.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.08a
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• pp.222-222
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• 2012

Metal oxide gas sensors based on semiconductor type have attracted a great deal of attention due to their low cost, flexible production and simple usability. However, most works have been focused on n-type oxides, while the characteristics of p-type oxide gas sensors have been barely studied. An investigation on p-type oxides is very important in that the use of them makes possible the novel sensors such as p-n diode and tandem devices. Monoclinic cupric oxide (CuO) is p-type semiconductor with narrow band gap (~1.2 eV). This is composed of abundant, nontoxic elements on earth, and thus low-cost, environment-friendly devices can be realized. However, gas sensing properties of neat CuO were rarely explored and the mechanism still remains unclear. In this work, the neat CuO layers with highly ordered mesoporous structures were prepared by a template-free, one-pot solution-based method using novel ink solutions, formulated with copper formate tetrahydrate, hexylamine and ethyl cellulose. The shear viscosity of the formulated solutions was 5.79 Pa s at a shear rate of 1 s-1. The solutions were coated on SiO2/Si substrates by spin-coating (ink) and calcined for 1 h at the temperature of $200{\sim}600^{\circ}C$ in air. The surface and cross-sectional morphologies of the formed CuO layers were observed by a focused ion beam scanning electron microscopy (FIB-SEM) and porosity was determined by image analysis using simple computer-programming. XRD analysis showed phase evolutions of the layers, depending on the calcination temperature, and thermal decompositions of the neat precursor and the formulated ink were investigated by TGA and DSC. As a result, the formation of the porous structures was attributed to the vaporization of ethyl cellulose contained in the solutions. Mesoporous CuO, formed with the ink solution, consisted of grains and pores with nano-meter size. All of them were strongly dependent on calcination temperature. Sensing properties toward H2 and C2H5OH gases were examined as a function of operating temperature. High and fast responses toward H2 and C2H5OH gases were discussed in terms of crystallinity, nonstoichiometry and morphological factors such as porosity, grain size and surface-to-volume ratio. To our knowledge, the responses toward H2 and C2H5OH gases of these CuO gas sensors are comparable to previously reported values.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2017.05a
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• pp.77-77
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• 2017

Titanium and its alloys offer attractive properties in a variety of applications. These are widely used for the field of biomedical implants because of its good biocompatibility and high corrosion resistance. Titanium anodizing is often used in the metal finishing of products, especially those can be used in the medical devices with dense oxide surface. Based on SAE/AMS (Society of Automotive Engineers/Aerospace Material Specification) 2488D, it has the specification for industrial titanium anodizing that have three different types of titanium anodization as following: Type I is used as a coating for elevated temperature forming; Type II is used as an anti-galling coating without additional lubrication or as a pre-treatment for improving adherence of film lubricants; Type III is used as a treatment to produce a spectrum of surface colours on titanium. In this study, we have focused on Type II anodization for the medical (dental and orthopedic) application, the anodized surface was modified with gray color under alkaline electrolyte. The surface characteristics were analyzed with Focused Ion Beam (FIB), Scanning Electron Microscopy (SEM), surface roughness, Vickers hardness, three point bending test, biocompatibility, and corrosion (potentiodynamic) test. The Ti-6Al-4V alloy was used for specimen, the anodizing procedure was conducted in alkaline solution (NaOH based, pH>13). Applied voltage was range between 20 V to 40 V until the ampere to be zero. As results, the surface characteristics of anodic oxide layer were analyzed with SEM, the dissecting layer was fabricated with FIB method prior to analyze surface. The surface roughness was measured by arithmetic mean deviation of the roughness profile (Ra). The Vickers hardness was obtained with Vickers hardness tester, indentation was repeated for 5 times on each sample, and the three point bending property was verified by yield load values. In order to determine the corrosion resistance for the corrosion rate, the potentiodynamic test was performed for each specimen. The biological safety assessment was analyzed by cytotoxic and pyrogen test. Through FIB feature of anodic surfaces, the thickness of oxide layer was 1.1 um. The surface roughness, Vickers hardness, bending yield, and corrosion resistance of the anodized specimen were shown higher value than those of non-treated specimen. Also we could verify that there was no significant issues from cytotoxicity and pyrogen test.

• Journal of Powder Materials
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• v.16 no.2
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• pp.138-145
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• 2009

The combination of focused ion beam (FIB) and 4 point probe nanomanipulator could make various nano manufacturing and electrical measurements possible. In this study, we manufactured individual ZnO nanowire devices and measured those electrical properties. In addition, tensile experiments of metallic Au and Pd nanowires was performed by the same directional alignment of two nanomanipulators and a nanowire. It was confirmed from I-V curves that Ohmic contact is formed between electrodes and nanomanipulators, which is able to directly measure the electrical properties of a nanowire itself. In the mechanical tensile test, Au and Pd nanowires showed a totally different fracture behavior except the realignment from <110> to <002>. The deformation until the fracture was governed by twin for Au and by slip for Pd nanowires, respectively. The crystallographic relationship and fracture mechanism was discussed by TEM observations.

• Journal of the Microelectronics and Packaging Society
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• v.21 no.3
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• pp.43-50
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• 2014

By the trends of electronic package to be smaller, thinner and more integrative, the reliability of interconnection between Si chip and printed circuit board is required. This paper reports on a study of high speed shear energy of Sn-4.0wt%Ag-0.5wt%Cu (SAC405) solder joints with different the thicknesses of electroless Ni-P deposit. 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. 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. The high speed shear energy of SAC405 solder joint with $1{\mu}m$ Ni-P deposit was found to be lower without $HNO_3$ vapor, compared to those of over $3{\mu}m$ Ni-P deposit. This could be due to the edge of solder resist in $1{\mu}m$ Ni-P deposit, which provides a fracture location for the weakened shear energy of solder joints and brittle fracture in high speed shear test. With $HNO_3$ vapor, the brittle fracture mode in high speed shear test decreased with increasing the thickness of Ni-P deposit. Then the roughness (Ra) of Ni-P deposits decreased with increasing its thickness. Thus, this gives the evidence that the decrease in roughness of Ni-P deposit for Eelectroless Ni/ Electroless Pd/ Immersion Au (ENEPIG) surface play a critical role for improving the robustness of SAC405 solder joint.

• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.413-413
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• 2014

In this paper, we present a fabrication method of functionalized gold nanostructures on flexible substrate that can be implemented for plasmonic sensing application. For biomolecular sensing, many researchers exploit unconventional lithography method like nanoimprint lithography (NIP), contact transfer lithography, soft lithography, colloidal transfer printing due to its usability and easy to functionalization. In particular, nanoimprint and contact transfer lithography need to have anti-adhesion layer for distinctive metallic properties on the flexible substrates. However, when metallic thin film was deposited on the anti-adhesion layer coated substrates, we discover much aggravation of the mold by repetitive use. Thus it would be impossible to get a high quality of metal nanostructure on the transferred substrate for developing flexible electronics based transfer printing. Here we demonstrate a method for nano-pillar mold and transfer the controllable nanoparticle array on the flexible substrates without an anti-adhesion layer. Also functionalization of gold was investigated by the different length of thiol applied for effectively localized surface plasmonic resonance sensing. First, a focused ion beam (FIB) and ICP-RIE are used to fabricate the nanoscale pillar array. Then gold metal layer is deposited onto the patterned nanostructure. The metallic 130 nm and 250 nm nanodisk pattern are transferred onto flexible polymer substrate by bi-layer functionalized contact imprinting which can be tunable surface energy interfaces. Different thiol reagents such as Thioglycolic acid (98%), 3-Mercaptopropionic acid (99%), 11-Mercaptoundecanoic acid (95%) and 16-Mercaptohexadecanoic acid (90%) are used. Overcoming the repeatedly usage of the anti-adhesion layer mold which has less uniformity and not washable interface, contact printing method using bi-layer gold array are not only expedient access to fabrication but also have distinctive properties including anti-adhesion layer free, functionalized bottom of the gold nano disk, repeatedly replicate the pattern on the flexible substrate. As a result we demonstrate the feasibility of flexible plasmonic sensing interface and anticipate that the method can be extended to variable application including the portable bio sensor via mass production of stable nanostructure array and other nanophotonic application.

• Journal of the Korean Vacuum Society
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• v.17 no.5
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• pp.408-418
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• 2008

The rectangular resonant cavity was designed and characterized as a microwave plasma source for focused ion beam. The optimum cavity was calculated analytically and analyzed in detail by using HFSS(High Frequency Structure Simulator). Since the resonant cavity can be affected by the permittivity of quartz chamber and plasma, the cavity is designed to be changeable in one direction. By observing the microwave input power at which the breakdown begins, the optimum cavity length for breakdown is measured and compared with the calculated one, showing in good agreement with the optimum length reduced by 10cm according to the permittivity change in the presence of quartz chamber. The shape of breakdown power curve as a function of pressure appears to be similar to Paschen-curve. After breakdown, plasma densities increase with microwave power and the reduced effective permittivity in the cavity with plasma results in larger optimum length. However, it is not possible to optimize the cavity condition for high density plasmas with increased input power, because too high input power causes expansion of density cutoff region where microwave cannot penetrate. For more accurate microwave cavity design to generate high density plasma, plasma column inside and outside the density cutoff region needs to be treated as a conductor or dielectric.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.18 no.4
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• pp.1-7
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• 2017

Cobalt silicide was used as a counter electrode in order to confirm its reliability in dye-sensitized solar cell (DSSC) devices. 100 nm-Co/300 nm-Si/quartz was formed by an evaporator and cobalt silicide was formed by vacuum heat treatment at $700^{\circ}C$ for 60 min to form approximately 350 nm-CoSi. This process was followed by etching in $80^{\circ}C$-30% $H_2SO_4$ to remove the cobalt residue on the cobalt silicide surface. Also, for the comparison against Pt, we prepared a 100 nm-Pt/glass counter electrode. Cobalt silicide was used for the counter electrode in order to confirm its reliability in DSSC devices and maintained for 0, 168, 336, 504, 672, and 840 hours at $80^{\circ}C$. The photovoltaic properties of the DSSCs employing cobalt silicide were confirmed by using a simulator and potentiostat. Cyclic-voltammetry, field emission scanning electron microscopy, focused ion beam scanning electron microscopy, and energy dispersive spectrometry analyses were used to confirm the catalytic activity, microstructure, and composition, respectively. The energy conversion efficiency (ECE) as a function of time and ECE of the DSSC with Pt and CoSi counter electrodes were maintained for 504 hours. However, after 672 hours, the ECEs decreased to a half of their initial values. The results of the catalytic activity analysis showed that the catalytic activities of the Pt and CoSi counter electrodes decreased to 64% and 57% of their initial values, respectively(after 840 hours). The microstructure analysis showed that the CoSi layer improved the durability in the electrolyte, but because the stress concentrates on the contact surface between the lower quartz substrate and the CoSi layer, cracks are formed locally and flaking occurs. Thus, deterioration occurs due to the residual stress built up during the silicidation of the CoSi counter electrode, so it is necessary to take measures against these residual stresses, in order to ensure the reliability of the electrode.