• Title/Summary/Keyword: FIB(Focused Ion Beam)

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Newly Developed BioDegradable Mg Alloys and Its Biomedical Applications

  • Seok, Hyeon-Gwang;Kim, Yu-Chan;Yang, Gui Fu;Cha, Pil-Ryeong;Jo, Seong-Yun;Yang, Seok-Jo
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2012.05a
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    • pp.55.2-55.2
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    • 2012
  • Intensive theoretical and experimental studies have been carried out at Korean Institute of Science and Technology (KIST) on controlling the bio absorbing rate of the Mg alloys with high mechanical strength through tailoring of electrochemical potential. Key technology for retarding the corrosion of the Mg alloys is to equalize the corrosion potentials of the constituent phases in the alloys, which prevented the formation of Galvanic circuit between the constituent phases resulting in remarkable reduction of corrosion rate. By thermodynamic consideration, the possible phases of a given alloy system were identified and their work functions, which are related to their corrosion potentials, were calculated by the first principle calculation. The designed alloys, of which the constituent phases have similar work function, were fabricated by clean melting and extrusion system. The newly developed Mg alloys named as KISTUI-MG showed much lower corrosion rate as well as higher strength than previously developed Mg alloys. Biocompatibility and feasibility of the Mg alloys as orthopedic implant materials were evaluated by in vitro cell viability test, in vitro degradation test of mechanical strength during bio-corrosion, in vivo implantation and continuous observation of the implant during in vivo absorbing procedures. Moreover, the cells attached on the Mg alloys was observed using cryo-FIB (focused ion beam) system without the distortion of cell morphology and its organ through the removal of drying steps essential for the preparation of normal SEM/TEM samples. Our Mg alloys showed excellent biocompatibility satisfying the regulations required for biomedical application without evident hydrogen evolution when it implanted into the muscle, inter spine disk, as well as condyle bone of rat and well contact interface with bone tissue when it was implanted into rat condyle.

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The Effect of Tool Geometry on the Mechanical Properties in a Friction Stir Welded Lap Joint between an Al Alloy and Zn-coated Steel (알루미늄 합금과 아연도금강판의 이종 겹치기 마찰교반접합에서 기계적성질에 미치는 Tool Geometry의 영향)

  • Kim, Nam-Kyu;Kim, Byung-Chul;Jung, Byung-Hoon;Song, Sang-Woo;Nakata, K.;Kang, Chung-Yun
    • Korean Journal of Metals and Materials
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    • v.48 no.6
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    • pp.533-542
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    • 2010
  • The specific motivation for joining an Al alloy and Zn-coated steel arises from the need to save fuel consumption by weight reduction and to enhance the durability of vehicle structures in the automobile industry. In this study, the lap joining A6K31 Al alloy (top) and SGARC340 Zn-coated steel (bottom) sheets with a thickness of 1.0 mm and 0.8 mm, respectively, was carried out using the friction stir weld (FSW) technique. The probe of a tool did not contact the surface of the lower Zn-coated steel sheet. The friction stir welding was carried out at rotation speeds of 1500 rpm and travel speeds of 80~200 mm/min. The effects of tool geometry and welding speed on the mechanical properties and the structure of a joint were investigated. The tensile properties for the joints welded with a larger tool were better than those for the joints done with a smaller tool. A good correlation between the tensile load and area of the welded region were observed. The bond strength using a larger tool (M4 and M3) decreased with an increase in welding speed. Most fractures occurred along the interface between the Zn-coated steel and the Al alloy. However, in certain conditions with a lower welding speed, fractures occurred at the A6K31 Al alloy.

Microstructural characteristics of a fresh U(Mo) monolithic mini-plate: Focus on the Zr coating deposited by PVD

  • Iltis, Xaviere;Drouan, Doris;Blay, Thierry;Zacharie, Isabelle;Sabathier, Catherine;Onofri, Claire;Steyer, Christian;Schwarz, Christian;Baumeister, Bruno;Allenou, Jerome;Stepnik, Bertrand;Petry, Winfried
    • 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.

Reliability of Sn-Ag-Cu Solder Joint on ENEPIG Surface Finish: 1. Effects of thickness and roughness of electroless Ni-P deposit (ENEPIG 표면처리에서의 Sn-Ag-Cu 솔더조인트 신뢰성: 1. 무전해 Ni-P도금의 두께와 표면거칠기의 영향)

  • Huh, Seok-Hwan;Lee, Ji-Hye;Ham, Suk-Jin
    • 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.

Hydrogen and Ethanol Gas Sensing Properties of Mesoporous P-Type CuO

  • Choi, Yun-Hyuk;Han, Hyun-Soo;Shin, Sun;Shin, Seong-Sik;Hong, Kug-Sun
    • 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.

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Contact Transfer Printing Using Bi-layer Functionalized Nanobio Interface for Flexible Plasmonic Sensing

  • Lee, Jihye;Park, Jiyun;Lee, Junyoung;Yeo, Jong-Souk
    • 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.

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Reliability of a Cobalt Silicide on Counter Electrodes for Dye Sensitized Solar Cells (코발트실리사이드를 이용한 염료감응형 태양전지 상대전극의 신뢰성 평가)

  • Kim, Kwangbae;Park, Taeyeul;Song, Ohsung
    • 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.