• 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.

• 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.

• Proceedings of the Korean Society for Technology of Plasticity Conference
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• 2009.10a
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• pp.209-212
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• 2009

It has been widely reported that carbide-free bainitic steels or super-bainite WP (SB-TRIP) steels for the automotive industry are a new family of steels offering a unique combination of high strength and ductility. Hence, it is important to exactly evaluate the volume fraction of RA and to identify the 3-D morphology of constituent phases, because it plays a crucial role in mechanical properties. Recently, as electron back-scattered diffraction (EBSD) equipped with focused ion beam (FIB) has been developed, 3-D EBSD technique for materials science are used to these steels. Moreover, newly developed atom probe tomography (APT) technique can provide the exact distribution and chemical concentration of alloying elements in a sub-nm scale. The APT analysis results indicate exactly the distribution and composition of alloying elements in the austenite and bainite phases of SB-TRIP steels with the atomic-scale resolution. And thus, no partitioning of aluminum and manganese atoms was showed between the austenite containing $7.73{\pm}0.39$ at% C and the bainitic ferrite associated with $0.22{\pm}0.06$ at% C in the SB-TRIP steel.

• Transactions of Materials Processing
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• v.19 no.1
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• pp.44-49
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• 2010

It has been widely reported that carbide-free bainitic steels or super-bainite TRIP (SB-TRIP) steels for the automotive industry are a new family of steels offering a unique combination of high strength and ductility. Hence, it is important to exactly evaluate the volume fraction of RA and to identify the 3-D morphology of constituent phases, because it plays a crucial role in mechanical properties. Recently, as electron back-scattered diffraction (EBSD) equipped with focused ion beam (FIB) has been developed, 3-D EBSD technique for materials science are used to these steels. Moreover, newly developed atom probe tomography (APT) technique can provide the exact distribution and chemical concentration of alloying elements in a sub-nm scale. The APT analysis results indicate exactly the distribution and composition of alloying elements in the austenite and bainite phases of SB-TRIP steels with the atomic-scale resolution. And thus, no partitioning of aluminum and manganese atoms was showed between the austenite containing $7.73{\pm}0.39$ at% C and the bainitic ferrite associated with $0.22{\pm}0.06$ at% C in SB-TRIP steel.

• Korean Journal of Materials Research
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• v.26 no.5
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• pp.271-280
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• 2016

When a single inorganic precursor is used for the synthesis of a sol-gel coating, there is a problem of cracking on the surface of coating layer. In order to solve this problem of surface cracking, we synthesized inorganic-organic coatings that have hybrid properties of inorganic and organic materials. Sols of various ratios (1:0.07, 0.2, 0.41, 0.82, 1.64, 3.26, 6.54, 13.2) of an inorganic precursor of Tetrabutylorthotitanate ($Ti(OBu)_4$, TBOT) and an organic precursor of ${\gamma}$-Methacryloxy propyltrimethoxysilane (MAPTS) were prepared and coated on stainless steels (SUS316L) by dip coating method. The binding structure and the physical properties of the synthesized coatings were analyzed by FT-IR, FE-SEM, FIB (Focused Ion Beam), and a nano-indenter. Dynamic polarization testing and EIS (electrical impedance spectroscopy) were carried out to evaluate the micro-defects and the corrosion properties of the coatings. The prepared coatings show hybrid properties of inorganic oxides and organic materials. Crack free coatings were prepared when the MAPTS ratio was above a critical value. As the MAPTS ratio increased, the thickness and the corrosion resistance increased, and the hardness decreased.

• 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.

• 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.

• 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.

• Journal of Sensor Science and Technology
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• v.16 no.5
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• pp.377-383
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• 2007

We describe the fabrication and characterization of a doubly clamped multi-walled carbon nanotube (MWNT). The device was assembled by an application of electric field in solution. The MWNT was clamped on end of metal trench electrodes in solution and deposited with additional platinum (Pt) on edge of electrode for firmly suspending the MWNT by focused ion beam (FIB). The MWNTs range of diameter and length were 100 to 150 nm and 1.5 to $2{\mu}m$, respectively. Electrical characteristics of fabricated devices were measured by I-V curve and impedance analysis. The mechanical deformation was observed by resistivity in high air pressure. Resonant frequency around 6.8 MHz was detected and resistivity was linearly varied according to the magnitude of air pressure. This device could have potential applications in nanoelectronics and various sensors.