• 한국진공학회:학술대회논문집
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• 한국진공학회 2014년도 제46회 동계 정기학술대회 초록집
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• pp.244.2-244.2
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• 2014

금속, 플라스틱, 유리 등의 재료 표면에 다양한 색상을 표현하기 위해 일반적으로 습식 도금을 많이 적용하고 있다. 하지만 습식 도금은 공정 수가 많을 뿐만 아니라 위험물질 및 오염물질을 많이 사용하기 때문에 산업사고, 환경오염 등을 야기 시킨다. 따라서 본 연구에서는 친환경적 방법인 물리적기상증착(PVD ; Physical Vapor Deposition) 방식의 한 종류인 스퍼터링(Sputtering)으로 색상을 구현하였다. PVD 방식의 증착은 습식 도금 방식에 비해 친환경적이며, 전처리에서 후처리까지 한 공정으로 가능하다는 점이다. 스퍼터링은 PVD의 다른 방식인 E-beam 방식에 비해 대량생산을 할 수 있다는 장점이 있다. 양산형 스퍼터링 장비(${\Phi}1200mm{\times}H1400mm$)로 실험을 진행하였으며, 증착 물질은 Ti, Al, Cr 을 사용하였고, 반응성 가스(Reactive Gas) 로는 N2, C2H2 가스를 사용하였다. 전처리는 LIS (Linear Ion Source)로 식각(Etching) 하였고, 펄스직류전원공급장치(Pulsed DC Power Supply)를 사용하여 증착 하였으며, 증착시 기판에 bias (-100 V)를 인가 하였다. 그 결과 회색계열, 갈색계열 등 여러가지 색을 구현할 수 있었으며, 증착된 박막의 특성을 알아보기 위하여 색차계, 내마모 시험기, 연필경도 시험기를 사용하였다. 향후 후처리 공정으로 내지문(AF ; anti fingerprint coating) 박막 등과 같은 실용적인 박막을 증착할 계획이다.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2003년도 추계학술발표회초록집
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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.

• 한국결정성장학회지
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• 제22권5호
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• pp.227-232
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• 2012

차세대 원자력발전용 고온 열교환기 소재로 이용될 가능성이 높은 Ni-Cr계 고온합금인 Inconel 617과 Hastelloy X의 표면처리에 따른 FLiNaK(LiF-NaF-KF) 용융염 하에서의 고온물성에 대한 연구를 수행하였다. Inconel 617과 Hastelloy X기판 상에 각각 PVD인 arc discharge 및 sputtering법에 의해 TiAlN 및 $Al_2O_3$ 박막을 코팅 하였다. 이러한 표면처리가 이들 합금의 FLiNaK 용융염 하 고온 안정성에 미치는 영향에 대해 연구하였다. 용융염 하 Ni-Cr계 고온합금의 부식 원리를 이해하기 위해, 용융염 수송 loop에 사용 중 파단된 Inconel 파이프에 대한 미세구조 분석을 수행하였다. 표면처리 된 합금들을 $600^{\circ}C$ 용융염 내에서 열처리 하였으며, 열처리 전후 시편들에 대해 상형성, 미세구조 등 고온 물성 변화를 측정하였다. 연구결과 코팅되지 않은 경우 보다 TiAlN 및 $Al_2O_3$ 박막이 코팅된 소재에서 보다 우수한 고온 안정성을 보여주었다.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2001년도 춘계학술발표회 초록집
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• pp.14-14
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• 2001

Nitride films such as TiN, CrN etc. deposited on glass by PVD processes have been developed for many industrial applications. These nitride films deposited on glass were widely used for not only decorative and optical coatings but also wear and corrosion resistance coatings employed as dies and molds made of glass for the example of lens forming molds. However, the major problem of nitride coatings on glass by PVD process is non-uniform film owing to pin-hole and micro crack. It is estimated that nonuniform coating is influenced by a different surface energy between metal nitrides and glass due to binding states. In this work, therefore, for the evaluation of nucleation and growth mechanism of nitride films on glass TiN and CrN film were synthesized on glass with various nitrogen partial pressure by unbalanced magnetron sputtering. Prior to deposition, for the examination of relationship between surface energy and film microstructure plasma pre-treatment process was carried out with various argon to hydrogen flow rate and substrate bias voltage, duty cycle and frequency by using pulsed DC power supply. Surface energy owing to the different plasma pre-treatment was calculated by the measurement of wetting angle and surface conditions of glass were investigated by X-ray Photoelectron Spectroscopy(XPS) and Atomic Force Microscope(AFM). The microstructure change of nitride films on glass with increase of film thickness were analyzed by X-Ray Diffraction(XRD) and Scanning Electron Microscopy(SEM).

• 한국표면공학회지
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• 제28권6호
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• pp.368-375
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• 1995

Thermal CVD method is in general used for the fabrication of TiC/$Al_2O_3$-coated carbide tools. The growth of TiC layer and the coating morphology depended on the chemical composition of the hard metal substrate on which the tool properties were strongly influenced. TiC-coated layer was grown by the diffusion of carbon from the substrate, whereas the growth of $Al_2O_3$ layer was unrelated to the composition of substrate. In the nitride hard coatings of Zr, Nb and Mo metals deposited on high speed steel substrate by magnetron sputtering, the reactivity of the metal elements was decreased with increasing group number in one period of the periodic system. The hard material films exhibited the highest adhesion with the chemical composition of stoichiometry or substoichiometry. The critical load as a measure of adhesion was evaluated using scratch tester. The CVD tools indicated the values of 80 and 40N in the coated layers with proper bonding to the substrate and with $\eta$ phase of 1$\mu\textrm{m}$ in the interface respectively, but the nitride films prepared by sputtering of PVD showed only the values between 10 and 20N.

• 한국해양공학회지
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• 제30권5호
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• pp.356-360
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• 2016

Recently, the lifetime extension of nuclear power plants has been considered. Thus, it is necessary to consider facility safety management and economic management. However, when the bolts in nuclear power plants are replaced and the turbines of nuclear power plant are disassembled, numerous problems are found in relation to stuck bolts in clamping parts. In order to solve these problems, a hybrid vacuum chamber was first designed and manufactured. It can perform arc ion plating and sputtering, which were used to deposit Ti/TiN on an A913 B7 bolt. X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses were conducted to determine the composition and characteristics of the bolt, and tests were conducted to determine how long the bolt could endure under various conditions in a nuclear power plant. The SEM and XRD results clearly showed a continual and even coating layer. When this TiN-coated bolt is used in a nuclear power plant, the lifetime can be extended compared to a conventional bolt, but it is necessary to determine what additional properties are required.

• 한국진공학회:학술대회논문집
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• 한국진공학회 1999년도 제17회 학술발표회 논문개요집
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• pp.211-211
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• 1999

Titanium nitride (TiN) thin films have useful properties including high hardness, good electrical conductivity, high melting point, and chemical inertness. The applications have included wear-resistant hard coatings on machine tools and bearings, decorative coating making use of the golden color, thermal control coatings for widows, and erosion resistant coatings for spacecraft plasma probes. For all these applications as feature sizes shrink and aspect ratios grow, the issue of good step coverage becomes increasingly important. It is therefore essential to manufacture conformal coatings of TiN. The growth of TiN thin films by chemical vapor deposition (CVD) is of great interest for achieving conformal deposition. The most widely used precursor for TiN is TiCl4 and NH3. However, chlorine impurity in the as-grown films and relatively high deposition temperature (>$600^{\circ}C$) are considered major drawbacks from actual device fabrication. To overcome these problems, recently, MOCVD processes including plasma assisted have been suggested. In this study, therefore, we have doposited Ti(C, N) thin films on Si(100) and D2 steel substrates in the temperature range of 150-30$0^{\circ}C$ using tetrakis diethylamido titanium (TDEAT) and titanium isopropoxide (TIP) by pulsed DC plamsa enhanced metal-organic chemical vapor deposition (PEMOCVD) method. Polycrystalline Ti(C, N) thin films were successfully grown on either D2 steel or Si(100) surfaces at temperature as low as 15$0^{\circ}C$. Compositions of the as-grown films were determined with XPS and RBS. From XPS analysis, thin films of Ti(C, N) with low oxygen concentration were obtained. RBS data were also confirmed the changes of stoichiometry and microhardness of our films. Radical formation and ionization behaviors in plasma are analyzed by optical emission spectroscopy (OES) at various pulsed bias and gases conditions. H2 and He+H2 gases are used as carrier gases to compare plasma parameter and the effect of N2 and NH3 gases as reactive gas is also evaluated in reduction of C content of the films. In this study, we fond that He and H2 mixture gas is very effective in enhancing ionization of radicals, especially N resulting is high hardness. The higher hardness of film is obtained to be ca. 1700 HK 0.01 but it depends on gas species and bias voltage. The proper process is evident for H and N2 gas atmosphere and bias voltage of 600V. However, NH3 gas highly reduces formation of CN radical, thereby decreasing C content of Ti(C, N) thin films in a great deal. Compared to PVD TiN films, the Ti(C, N) film grown by PEMOCVD has very good conformability; the step coverage exceeds 85% with an aspect ratio of more than 3.

• Steel and Composite Structures
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• 제23권2호
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• pp.153-160
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• 2017

It is extremely important to be aware of the ballistic performances of engineering materials in order to be able to choose the lightest armor providing full ballistic protection in civil and military applications. Therefore, ballistic tests are an important part of armor design process. In this study, ballistic performance of plates made of carbon steel and cold worked tool steel against 7.62 mm AP (armor-piercing) bullets was examined experimentally and numerically in accordance with NIJ standards. Samples in different sizes were prepared to demonstrate the effect of target thickness on ballistic performance. Some of these samples were coated with titanium nitride using physical vapor deposition (PVD) method. After examining all successful and unsuccessful samples at macro and micro levels, factors affecting ballistic performance were determined. Explicit non-linear analyses were made using Ls-Dyna software in order to confirm physical ballistic test results. It was observed that the ballistic features of steel plates used in simulations comply with actual physical test results.

• 반도체디스플레이기술학회지
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• 제14권2호
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• pp.47-52
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• 2015

In this paper, the performance of uncoated- and Titanium nitride aluminium TiAlN-PVD coated- carbide twist drills were investigated when drilling aluminium alloy, Al 6061. This research focuses on the optimization of drilling parameters using the Taguchi technique to obtain minimum surface roughness and thrust force. A number of drilling experiments were conducted using the L9 orthogonal array on a CNC vertical machining center. The experiments were performed on Al 6061 material l blocks using uncoated and coated HSS twist drills under dry cutting conditions. Analysis of variance(ANOVA) was employed to determine the most significant control factors. The main objective is to find the important factors and combination of factors influence the machining process to achieve low surface roughness and low cutting thrust force. From the analysis of the Taguchi method indicates that among the all-significant parameters, feed rate are more significant influence on surface roughness and cutting thrust than spindle speed.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 1999년도 추계학술발표회 초록집
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• pp.3-4
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• 1999

최근 산업이 고속도화, 고능률화 및 고정멸화의 추세로 발전함에 따라 우수한 내마모성, 인성, 고온 안정성 및 내구성을 갖는 공구 및 금형을 요구하게 되었다. 그러나 이와같은 성질들은 어떤 단일 재료에서는 얻을 수 없으며 적당한 기판공구나 금혈위에 내마모성 보호피막을 coating함으로 비교적 저렴하게 얻을 수 있다. 화학증착법으로 TiC, TiN등을 증착시킬때에는 $1000^{\circ}C$정도의 반응온도가 필요하며 이러한 증착온도는 모재가 초경합금일때는 문제가 안되나 강재일 경우 모재의 연화와 칫수변화의 문제를 야기시킨다. 최근에는 플라즈마를 사용하여 증착반응온도를 $550^{\circ}C$ 이하로 낮추는 플라즈마 화학 증착볍(PACVD)이 대두되고 있다. 그러나 이 방법어서 는 뚱착하려는 금속원소가 TiCl4의 형태로 공급되고 있으므로 생성된 층이 염소를 포함하고 있다. 이 층에 잔존하는 염소는 층의 기계적 성질을 저하시키고 층내의 stress를 유발시킨다. 또한 HCI개스의 생성으로 인하여 펌프 및 장비의 부식이 촉진 된다 이러한 결점을 극복하기 위하여 금속유기화합물 전구체(metallo-organic precursor)로 $TiCl_4$를 대체하고자 하는 연구가 활발하게 진행되고 있으며 본 연구실에서 이에 대하여 연구한 결과를 소개하고자 한다. diethylamino titanium을 전구체로 사용하여 $H_2,\;N_2,\;Ar$분위기하에서 pulsed d.c.를 사용하는 MO-PACVD에 의하여 $150~250^{\circ}C$의 저온에서 Al 2024 기판에 TiCN층 형 성을 하였다. 전구체 증발온도는 $74~78^{\circ}C$의 온도범위어야 하며 고경도의 코탱층은 54% duty, 14.2kHz, 450V의 조건에서 얻어졌으며 duty, 주파수, 전압이 증가함에 따라 경도는 저하되었다. 이때의 표면 morphology를 SEM으로 조사한바 dome structure가 크게 발달되었음을 알 수 있었다. 본 실험의 온도 범위내에서 얻은 TiCN 증착반응의 활성화에너지는 7.5Kcal/mol이었다. 증착된 TiCN층은 우수한 내마모섣을 나타내었으며 스크래치테스트 결과 17N의 엄계하중을 나타내었다. 본 연구에서 변화 시킨 duty, 주파수, 전압의 범위에서는 층의 밀착력은 크게 변화하지 않았다. titanium isopropoxide를 전구체로 사용하여 Hz, Nz 분위기하에서 d.c.를 사용하는 MO-PACVD에 의하여 Ti(NCO) 코팅층을 SKDll, SKD61, SKH9 공구강에 형성시키는 공정을 개발하였다. 최적의 Ti(NCO) 코탱층을 얻기 위해 유입전구체 부피%의 양은 향착압력의 5%를 넘지 않아야 되고 수소와 젤소 가스비가 1:1일 때 가장 높은 코팅층의 경도값을 나타내었다. 수소와 질소 가스비가 3:7일 때 TiFeCr(NCO)의 복화합물 코팅층이 형성됨을 알 수 있었고 500t의 증착온도에서 얻은 Ti(NCO) 코팅층이 높은 경도값과 좋은 내식성을 나타내었다. 또한 이와같은 Ti(NCO) 코팅공정과 본 실험실에서 개발한 확산층만 형성시키는 plsma nitriding 공정을 결합하여 복합코탱층을 형성하였는데 이 복합코팅층은 고경도와 우수한 내마모성, 내식성 뿐만 아니라 10)N 이상의 뛰어난 밀착력을 나타내었다. 현재 많이 사용되고 있는 PVD법은 step coverage가 좋지 않은 점과 cost intensive p process라는 단점이 있다. MO-PACVD법은 이러한 문제를 해결할 수 있는 방법으로서 앞으로 지속적인 도전이 요구되는 분야이다.