• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2003.10a
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• pp.134-135
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• 2003

The dental implant materials required good mechanical properties, such as fatigue strength, combined with a high resistance to corrosion. For increasing fatigue resistance and delaying onset of stress corrosion cracking, shot peening has been used for > 50 years to extend service life of metal components. However, there is no information on the electrochemical behavior of shot peened and hydroxyapatite(HA) coated Ti-6Al-4V alloys. To increase fatigue strength, good corrosion resistance, and biocompatibility, the electrochemical characteristics of Ti/TiN/HA coated and shot peened Ti-6Al-4V alloys by electron beam physical vapor deposition(EB-PVD) have been researched by various electrochemical method in 0.9%NaCl. Ti-6Al-4V alloys were prepared under the condition of hydrogen and vacuum arc furnace. The produced materials were quenched at 1000$^{\circ}C$ under high purity dried Ar atmosphere and were hold at 500$^{\circ}C$ for 2 hrs to achieve the fatigue strength(1140㎫) of materials. Ti-6Al-4V alloys were prepared under the condition of hydrogen and vacuum arc furnace. Shot peening(SP) and sand blasting treatment was carried out for 1, 5, and 10min. On the surface of Ti-6Al-4V alloys using the steel balls of 0.5mm and alumina sand of 40$\mu\textrm{m}$ size. Ti/TiN/HA multilayer coatings were carried out by using electron-beam deposition method(EB-PVD) as shown Fig. 1. Bulk Ti, powder TiN and hydroxyapatite were used as the source of the deposition materials. Electrons were accelerated by high voltage of 4.2kV with 80 - 120mA on the deposition materials at 350$^{\circ}C$ in 2.0 X 10-6 torr vacuum. Ti/TiN/HA multilayer coated surfaces and layers were investigated by SEM and XRD. A saturated calomel electrode as a reference electrode, and high density carbon electrode as a counter electrode, were set according to ASTM GS-87. The potentials were controlled at a scan rate of 100 mV/min. by a potentiostat (EG&G Co.273A) connected to a computer system. Electrochemical tests were used to investigate the electrochemical characteristics of Ti/TiN/HA coated and shot peened materials in 0.9% NaCl solution at 36.5$^{\circ}C$. After each electrochemical measurement, the corrosion surface of each sample was investigated by SEM.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2001.11a
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• pp.28-28
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• 2001

$TiCl_44,{\;}AICl_3,{\;}H_2,{\;}Ar,{\;}NH_3$ 기체를 사용하여 플라즈마 화학 증착법으로 $(Ti_{1-x}AI_x)N$ 피막을 증착한 후 진공열처리 실험을 통해 열처리 전후에 나타나는 피막의 가계적 특성 변화 및 상변화 양상에 대해 연구하였다. 기판으로는 M2 고속도강과 알루미나(${\alpha}-Al_2O_3$)를 사용하였으며, 열처리 실험은 진공 열처리로를 이용하여 $800$ ~ $1100^{\circ}C$ 에서 진행하였다. M2 고속도강 위에 증착한 $(Ti_{1-x}AI_x)N$ 피막은 모두 (200) 우선 방위를 갖고 있었으며, AI의 함량이 높아짐에 따라 입자의 크기가 미세해져 $(Ti_{0.2}AI_{0.8})N$ 의 경우 수 nm의 업자들로 이루어져 있었다. 열처리 시간을 일정하게 하고, 그 온도를 증가시킬 경우 비교적 낮은 온도 영역($~900^{\circ}C$)에서는 경도 증가를 나타내지만, 열처리가 더욱 진행됨에 따라 다시 경도가 감소하는 양상을 나타내었으며, 열처리 온도를 일정하게 하고 열처리 시간을 변화 시킬 경우에도 초기에 경도가 증가하다가 열처리가 진행됨에 따라 경도가 다시 감소하는 현상을 관찰 하였다. 이때 경도증가 정도는 Al 함량이 높을 수록 뚜렷하고 오래 지속되었으며, $(Ti_{0.2}AI_{0.8})N$ 피막의 경우 열처리 전 $2000HK_{0.01}$에서 열처리 후 $4500HK_{0.01}$로, 매우 큰 경도 증가를 나타내었다. 이와 같은 열처리 전후의 기계적 특성 변화는 준 안정상의 $(Ti_{1-x}AI_{x})N$ 피막에서, 열처리가 진행됨에 따라 미세한 AlN 업자가 석출되면서 나타나는 현상으로, 고분해능 전자현미경(HRTEM) 분석을 통해 경도가 증가한 시편의 경우 석출상의 크기가 5nm 이하로 매우 작고 대체로 기지와 연속적인 계면을 형성하나, 열처리가 진행될수록 석 출상의 크기가 커지고 임계크기 이상에 이르면 연속적인 계면은 거의 발견되지 않고, 대부 분 불연속적이고 확연한 계면을 형성함을 관찰 할 수 있었다. 알루미나(${\alpha}-Al_2O_3$) 기판 위에 증착한 $(Ti_{1-x}AI_{x})N$ 피막은 마찬가지로 (200) 우선 방위를 나타내었으나, 그 입자의 크기가 수십 nm로 고속도강위에 증착한 피막에 비해 상당히 크게 형성되었다. 또한 열처리 후에 AIN의 석출이 진행됨에도 불구하고 경도 증가는 나타나지 않고, 열처리가 진행됨에 따라 경도가 감소하는 양상만을 나타내었다. 결국 $(Ti_{1-x}AI_{x})N$ 피막이 열처리 전후에 보아는 기계적 특성의 변화 양상은 열역학적으로 안정한 Wurzite-AlN의 석출에 따른 것으로 AlN 석출상의 크기에 의존하며, 또한 이러한 영향은 $(Ti_{1-x}AI_{x})N$ 피막에 존재하는 AI의 함량이 높고, 초기에 증착된 막의 업자 크기가 작을 수록 클 것으로 여겨진다.

• Journal of the Korean Society for Heat Treatment
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• v.18 no.3
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• pp.183-189
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• 2005

The effects of duplex-treatment of plasma carburization and CrN coating onto Ti-6Al-4V alloy on its creep properties were investigated by means of a constant stress creep tester. Applying duplex-treatment, specimens having an inner carburized layer of about $150{\mu}m$ in depth and outer CrN layer of about $7.5{\mu}m$ in thickness were prepared. The hardness of duplex-treatment surface was about 1,960 VHN. It also appeared that the duplex-treatment improved the roughness of the surface significantly; $Ra=0.045{\mu}m$ for treated alloy while $Ra=0.321{\mu}m$ for untreated alloy. The steady-state creep behaviors were investigated in a temperature range of $510{\sim}550^{\circ}C$ ($0.42{\sim}0.44T_m$) under an applied stress range of 200~275 MPa. The stress exponent, n, was derived assuming the power law creep behavior. The surface treatment showed a decrease in a value from 9.32 (untreated) to 8.79 (treated). Also the activation energy obtained from an Arrhenius plot increased from 238 to 257 kJ/mol.

• Journal of the Korean institute of surface engineering
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• v.37 no.5
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• pp.249-252
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• 2004

Effects of HA and TiN coating on the electrochemical characteristics of Ti-6AI-4V alloys for bone plates were investigated using various test methods. Ti-6AI-4V alloys were fabricated by using a vacuum induction furnace and bone plates were made by laser cutting and polishing. HA was made of extracted tooth sintered and then tooth ash was used as HA coating target. The TiN and HA film coating on the surface were carried on using electron-beam physical vapor deposition (EB-PVD) method. The corrosion behaviors of the samples were examined through potentiodynamic method in 0.9% NaCI solutions at $36.5\pm$$1^{\circ}C$ and corrosion surface was observed using SEM and XPS. The surface roughness of TiN coated bone plates was lower than that of tooth ash coated plates. The structure of TiN coated layer showed the columnar structure and tooth ash coated layer showed equiaxed and anisotrophic structure. The corrosion potential of the TiN coated specimen is comparatively high. The active current density of TiN and tooth ash coated alloy showed the range of about $1.0xl0^{-5}$ $A\textrm{cm}^2$, whereas that of the non-coated alloy was$ 1.0xl0^{-4}$ $A\textrm{cm}^2$. The active current densities of HA and TiN coated bone plates were smaller than that of non-coated bone plates in 0.9% NaCl solution. The pitting potential of TiN and HA coated alloy is more drastically increased than that of the non-coated alloy. The pit number and pit size of TiN and HA coated alloy decreased in compared with those of non-coated alloy. For the coated samples, corrosion resistance increased in the order of TiN coated, tooth ash coated, and non-coated alloy.

• Proceedings of the Korean Vacuum Society Conference
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• 2016.02a
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• pp.132-132
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• 2016

기계 가공품의 정밀화, 경량화 요구로 난색재로 분류되는 비철분야 및 복합재 가공용 공구개발에 대한 수요가 급증하고 있으나, 기존 난삭재 가공 시 절삭공구의 마모가 빠르고, 상대재의 융착 불량 등이 공구 수명 감소의 주요 영향으로 보고된다. 상기문제를 해결하기 위해 절삭가공 공정 중 과다한 절삭유의 사용에 따른 가공비용, 에너지소모 증가, 환경오염 등으로 절삭유의 최소화 또는 절삭유를 사용하지 않는 표면처리기술등의 친환경 가공기술의 개발이 필요하다. 내융착 및 내마모 특성 향상을 위한 표면코팅 방법으로 수소가 포함되지 않은 고경도 비정질 카본 (ta-C)이 있으나, ta-C 코팅 막은 경도 30 - 80 GPa, 잔류응력 3 - 10 GPa 범위로 일반 경질 코팅 막 (AlTiN, TiSiCrN : 평균 3 GPa)에 비해 높고 산업적 활용이 가능한 0.5 - 1.5 um 두께 수준의 후막화가 힘들어 매우 우수한 절삭공구용 코팅 막 특성에도 불구하고 적용사례가 매우 적다. 따라서, 본 연구에서는 아크플라즈마 방식 (Filtered Cathode Vacuum Arc Plasma, FCVA)을 활용한 고경도/무수소 카본 코팅 막을 후막형태로 증착하여 비철금속가공용 절삭 공구류의 수명향상 기법을 제시하고자 한다. ta-C 코팅 막의 기초 공정개발 단계에서는 바이어스 전압, 공정시간을 달리하여 ta-C 코팅 막의 기계적 물성(경도: $50{\pm}3GPa$, 잔류응력: $6{\pm}1GPa$, 밀착력: 30N 이상 및 트라이볼로지 특성: 마찰계수 0.1 이하, 마멸량: $1.85{\times}10-14mm^3$)을 확보하여 절삭공구로의 공정실용화 적용검토를 실시하였다. ta-C 코팅 막은 (1) WC 공구 및 기존 상용품인 (2) TiAlN/TiN/WC 구조에 대해 증착을 실시하였으며 코팅 막의 두께 변화에 따른 실제 절삭환경에서의 내수명 관측을 진행하였다. 시험결과, ta-C/WC의 단일막 구조인 절삭공구의 경우, 실제 절삭환경에서 쉽게 박리가 발생하여 코팅 막으로서의 효과를 나타내지 못하였다. 이는, 기초 공정개발 단계에서의 밀착력 기준이 실제 환경과 부합하지 않는 것을 의미하며 추후 공정개선을 통해 극복하고자 한다. 반면에, 상용품인 (2) TiAlN/TiN/WC 구조의 절삭공구 대비 ta-C/TiAlN/TiN/WC 구조에서 내수명 증가는 약 2.5배 (기존 300회, 코팅 후 800회)로 증가하였으며 ta-C 코팅 막의 두께가 $0.6-0.8{\mu}m$일 때 최대치를 취한 후 감소하였다. 이를 통해, 절삭공구로의 ta-C 코팅 막 효과는 최외각 층의 두께 범위와 모재 강도보강을 할 수 있는 적절한 중간층 막 (TiN/TiAlN 층)이 혼합되어 나타난 것으로 사료되며 현재 산업계로의 적용을 위한 대량생산용 코팅장비의 개발 및 비용절감을 위한 공정개발이 진행 중이다.

• Proceedings of the KIEE Conference
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• 1995.11a
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• pp.364-366
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• 1995

We investigated the Electromigration characteristics in Cu alloyed Al line and the effect of Ti/TiN barrier layer on the characteristics. Test structures were fabricated by wafer level and 50% failure times were tested in the condition of j= 2 MA/$cm^3$, T= 300$^{\circ}C$. The reliability of Al line was improved which was 0.5%Cu Alloyed, but Ti/TiN under layer deteriorated the reliability while TiN over layer improved the characteristics.

• Journal of the Korean Ceramic Society
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• v.32 no.9
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• pp.977-988
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• 1995

Several oxide (ZrO2, Al2TiO5, reactive Al2O3) and nonoxide (SiC, Si3N4, "ALON" (5AlN.9Al2O3)) additives were used as a microfiller for alumina based LCC (Low-Cement-Castable). High temperature prooperties (HMOR, softening under load) and the phase changes of developed LCC on various sintering temperatures were examined. In addition, thermal shock test and corrosion test were accomplished. Based on these data the effects of each microfiller on the properties of LCC were established comparing to those of the commercial LCC with amorphous silica as a microfiller. The castables, containing reactive alumina, ZrO2 and "ALON" (5AlN.9Al2O3) as a first portion, exhibited considerably higher HMOR-values over 100$0^{\circ}C$, better creep behavior, and thermal shock resistance than those of castables with amorphous silica. The LCC with 5% Al2TiO5 showed no corrosion against molten aluminum.nst molten aluminum.

• Korean Journal of Metals and Materials
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• v.47 no.8
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• pp.488-493
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• 2009

Direct syntheses of bulk $Ti_3Al$ via electro-discharge-sintering (EDS) of a stoichiometric elemental powder mixture were investigated. A capacitor bank of $450{\mu}F$ was charged with three input energies, 0.5, 1.0, and 1.5 kJ. The charged capacitor bank was then instantaneously discharged through 0.3 g of a Ti-25.0 at.%Al powder mixture for consolidation. Complete phase transformation occurred in less than $200{\mu}sec$ by the discharge and a bulk $Ti_3Al$ compact was obtained. Compared with consolidated samples fabricated by conventional methods such as high vacuum sintering and casting, the electro-discharge-sintered $Ti_3Al$ compact shows a very fine microstructure with a hardness value of 425 Hv. Electro-discharge-sintering under a $N_2$ atmosphere successfully modified the surface Ti oxide of the $Ti_3Al$ compact into Ti nitride, which concurred with the synthesis and consolidation of $Ti_3Al$. Complete conversion yielding a single phase $Ti_3Al$ is primarily dominated by the fast solid state diffusion reaction.

• Journal of the Korean institute of surface engineering
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• v.36 no.6
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• pp.480-490
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• 2003

Effects of plasma-nitriding on the pitting corrosion of Fe-30at%Al-5at%Cr alloy containing Ti, Hf, and Zr were investigated using potentiostat in 0.1M HCl. The specimen was casted by the vacuum arc melting. The subsequent homogenization was carried out in Ar gas atmosphere at $1000^{\circ}C$ for 7days and phase stabilizing heat treatment was carried out in Ar gas atmosphere at $500^{\circ}C$ for 5 days. The specimen was nitrided in the $N_2$, and $H_2$, (1:1) mixed gas of $10^{-4}$ torr at $480^{\circ}C$ for 10 hrs. After the corrosion tests, the surface of the tested specimens were observed by the optical microscopy and scanning electron microscopy(SEM). For Fe-30at%Al-5Cr alloy, the addition of Hf has equi-axied structure and addition of Zr showed dendritic structure. For Fe-30at%Al-5Cr alloy containing Ti, plasma nitriding proved beneficial to decrease the pitting corrosion attack by increasing pitting potential due to formation of TiN film. Addition of Hf and Zr resulted in a higher activation current density and also a lower pitting potential. These results indicated the role of dendritic structure in decreasing the pitting corrosion resistance of Fe-30Al-5Cr alloy. Ti addition to Fe-30Al-5Cr decreased the number and size of pits. In the case of Zr and Hf addition, the pits nucleated remarkably at dendritic branches.

• Journal of the Microelectronics and Packaging Society
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• v.5 no.1
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• pp.7-18
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• 1998

In the flip chip interconnection on organic substrates using eutectic Pb/Sn solder bumps highly reliable Under Bump Metallurgy (UBM) is required to maintain adhesion and solder wettability. Various UBM systems such as 1$\mu$m Al/0.2$\mu$m Pd/1$\mu$m Cu, laid under eutectic Pb/Sn solder were investigated with regard to their interfacial reactions and adhesion proper-ties. The effects of numbers of solder reflow and aging time on the growth of intermetallic compounds (IMCs) and on the solder ball shear strength were investigated. Good ball shear strength was obtained with 1$\mu$m Al/0.2$\mu$m Ti/5$\mu$m Cu and 1$\mu$m Al/0.2$\mu$m ni/1$\mu$m Cu even after 4 solder reflows or 7 day aging at 15$0^{\circ}C$. In contrast 1$\mu$m Al/0.2$\mu$m Ti/1$\mu$m Cu and 1$\mu$mAl/0.2$\mu$m Pd/1$\mu$m 쳐 show poor ball shear strength. The decrease of the shear strength was mainly due to the direct contact between solder and nonwettable metal such as Ti and Al resulting in a delamination. In this case thin 1$\mu$m Cu and 0.2$\mu$m Pd diffusion barrier layer were completely consumed by Cu-Sn and pd-Sn reaction.