• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2017년도 춘계학술대회 논문집
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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.

• 한국분말재료학회지
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• 제16권2호
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• pp.138-145
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• 2009

FIB와 나노메니퓰레이터를 이용한 다양한 nano manufacturing을 통해 단일 나노선 소자제작 및 평가가 가능하였으며 또한 나노물질 자체의 전기적, 기계적 특성 평가를 수행할 수 있었다. 나노메니퓰레이터를 나노선에 직접 접촉시켜 전기적 특성을 평가하는 기술은 STA 등과 함께 사용될 때 높은 신뢰도를 갖는 신호를 얻을 수 있었다. 특히, 이를 이용한 나노 소재 특성 평가기술은 소자제작 시간을 단축시킬 수 있고 패턴닝으로부터 화학적 오염을 줄일 수 있는 장점을 갖고 있었다. 또한 FIB와 나노메니퓰레이터를 적절히 이용하면 나노인장시험기로서 활용이 가능하였으며 나노선의 기계적 특성을 본격적으로 평가할 수 있었다. 본 연구의 나노인장시험으로부터 얻은 인장실험 및 TEM분석으로부터 Au 및 Pd 나노선의 인장 및 파괴거동을 직접적으로 관찰할 수 있었다. Au 나노선은 인장초기에 {111}<112> 쌍정이 생성되고 나노선의 직경이 감소하다가 더 이상 인장응력을 수용할 수 없게되면 <110> 축으로부터 <002> 방향으로 재배열하는 방식으로 네킹이 형성되며 최종적으로 결정축 재배열 이후에는 슬립에 의한 파괴가 진행된다. Pd 나노선의 경우에는 Au와는 전혀 다른 파괴거동을 보였다. 먼저 네킹없이 <002> 축으로의 재배열 현상이 관찰되며 이후 cross-slip에 의한 변형을 하였다. 두 나노선 모두 인장 응력이 가해지면 네킹 부분을 중심으로 한 부분에서만 변형이 일어나며 다른 부분에서는 아무런 변형을 찾아 볼 수 없었다.

• Corrosion Science and Technology
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• 제14권2호
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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.

• 한국소성가공학회:학술대회논문집
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• 한국소성가공학회 2009년도 추계학술대회 논문집
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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.

• 소성∙가공
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• 제19권1호
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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.

• 한국재료학회지
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• 제26권5호
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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.

• 마이크로전자및패키징학회지
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• 제21권4호
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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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• 제14권6호
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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.

• 한국재료학회지
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• 제20권12호
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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.

• 센서학회지
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• 제16권5호
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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.