• Journal of the Korean institute of surface engineering
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• v.49 no.6
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• pp.580-586
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• 2016

Cr-Si-Al-N coating with different Si content were deposited by hybrid physical vapor deposition (PVD) method consisting of unbalanced magnetron (UBM) sputtering and arc ion plating (AIP). The deposition temperature was $300^{\circ}C$, and the gas ratio of $Ar/N_2$ were 9:1. The CrSi alloy and aluminum targets used for arc ion plating and sputtering process, respectively. Si content of the CrSi alloy targets were varied with 1 at%, 5 at%, and 10 at%. The phase analysis, composition and microstructural analysis performed using x-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) including energy dispersive spectroscopy (EDS), respectively. All of the coatings grown with textured CrN phase (200) plane. The thickness of the Cr-Si-Al-N films were measured about $2{\mu}m$. The friction coefficient and removal rate of films were measured by a ball-on-disk test under 20N load. The friction coefficient of all samples were 0.6 ~ 0.8. Among all of the samples, the removal rate of CrSiAlN (10 at% Si) film shows the lowest values, $4.827{\times}10^{-12}mm^3/Nm$. As increasing of Si contents of the CrSiAlN coatings, the hardness and elastic modulus of CrSiAlN coatings were increased. The morphology and composition of wear track of the films was examined by scanning electron microscopy (SEM) and energy dispersive spectroscopy, respectively. The surface energy of the films were obtained by measuring of contact angle of water drop. Among all of the samples, the CrSiAlN (10 at% Si) films shows the highest value of the surface energy, 41 N/m.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.104-104
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• 2016

음극아크증착과 스퍼터링을 동시에 사용한 하이브리드 공정으로 제조된 TiAlSiN 코팅층의 물성을 평가하였다. TiAlSiN 코팅층은 음극아크 소스에 Ti-Al 타겟을 장착하고 스퍼터링 소스에는 Si 타겟을 장착하여 아르곤과 질소 가스의 혼합가스 분위기에서 스테인리스(SUS304)와 초경(cemented carbide; WC-15wt.%Co) 기판 위에 제조되었다. 음극아크 소스에 인가되는 전류는 고정하고 스퍼터링 소스에 인가되는 전력을 조절하여 TiAlSiN 코팅층의 Si 함량을 제어하였다. TiAlSiN 코팅층의 Si 함량이 증가하면 코팅층의 구조가 주상정에서 비정질 구조로 변화한다. 이는 Si 함량이 증가하면 코팅층에 형성되는 알갱이 구조의 크기가 줄어들기 때문이다. X-선 회절 결과와 Scherrer's equation을 이용하여 Si 함량에 따른 알갱이 구조의 크기를 계산하면 Si이 없는 코팅층은 약 14 nm의 크기를 보이며 8 at.% 이상의 함량에서 약 2.5 nm로 포화된다. TiAlSiN 코팅층의 경도를 Si 함량에 따라 측정하면 Si 함량이 증가하면 경도도 증가하는 경향을 보이며 약 9 at.%의 Si 함량에서 3200 Hv로 최대가 되고 이후에는 감소한다. TiAlSiN이 코팅된 스테인리스 시편을 대기에서 열처리하고 시편 무게증가를 측정하여 코팅층의 내열성을 평가하였다. Si 함량이 증가하면 내열성도 향상되는데 14.4 at.%의 Si 함량에서 $700^{\circ}C$까지 무게 증가가 없으며 $900^{\circ}C$까지 0.43 mg의 증가를 보인다. 본 실험을 통해서 얻어진 TiAlSiN 코팅층은 비교적 높은 경도와 내열성을 확보하여 절상공구 보호막 코팅 소재 등으로 활용이 가능할 것으로 판단된다.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.29 no.10
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• pp.665-670
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• 2016

Prevailing dissemination of machine tools and cutting technology have caused drastic developments of high speed dry machining with work materials of high hardness, and demands on the high-hardness-materials with high efficiency have become increasingly important in terms of productivity, cost reduction, as well as environment-friendly issue. Addition of Si to TiAlN has been known to form nano-composite coating with higher hardness of over 30 GPa and oxidation temperature over $1,000^{\circ}C$. However, it is not easy to add Si to TiAlN by using conventional PVD technologies. Therefore, Ti-Al-Si-N have been prepared by hybrid process of PVD with multiple target sources or PVD combined with PECVD of Si source gas. In this study, a single composite target of Ti-Al-Si was prepared by powder metallurgy of MA (mechanical alloying) and SPS (spark plasma sintering). Properties of he resulting alloying targets were examined. They revealed a microstructure with micro-sized grain of about $1{\sim}5{\mu}m$, and all the elements were distributed homogeneously in the alloying target. Hardness of the Ti-Al-Si-N target was about 1,127 Hv. Thin films of Ti-Al-Si-N were prepared by unbalanced magnetron sputtering method by using the home-made Ti-Al-Si alloying target. Composition of the resulting thin film of Ti-Al-Si-N was almost the same with that of the target. The thin film of Ti-Al-Si-N showed a hardness of 35 GPa and friction coefficient of 0.66.

• Journal of the Korean Ceramic Society
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• v.42 no.2 s.273
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• pp.88-93
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• 2005

Ti-AI-Si-N coating layers were deposited on WC-Co substrates by a hybrid system of arc ion plating and sputtering techniques. The coatings were prepared with different Si contents to investigate the effect of Si content on their mechanical properties and microstructures. The dry sliding wear experiments were conducted on Ti-AI-Si-N coated WC-Co discs at constant load, 3N, and sliding speed, 0.1 m/s with two different counterpart materials such as steel ball and zirconia ball using a conventional ball-on-disc sliding wear apparatus. In the case of steel ball, the friction coefficient of Ti-AI-Si-N coating layers became lower than that of Ti-AI­N coating layers. The friction coefficient decreased with increasing of Si content due to adhesive wear behavior between coating layer and steel ball. On the contrary, in the case of zirconia ball, the friction coefficient increased with increasing of Si content, indicating that abrasive wear behavior was more dominant when the coating layers slid against zirconia ball.

• Journal of the Korean institute of surface engineering
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• v.50 no.5
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• pp.339-344
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• 2017

Highly corrosion resistance performance of CrAlSiN coatings were obtained by applying ultrathin $Al_2O_3$ thin films using atomic layer deposition (ALD) method. CrAlSiN coatings were prepared on Cr adhesion layer/SUS304 substrates by a hybrid coating system of arc ion plating and high power impulse magnetron sputtering (HiPIMS) method. And, ultrathin $Al_2O_3$ passivation layer was deposited on the CrAlSiN/Cr adhesion layer/SUS304 sample to protect CrAlSiN coatings by encapsulating the whole surface defects of coating using ALD. Here, the high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and energy dispersive X-ray spectrometry (EDX) analysis revealed that the ALD $Al_2O_3$ thin films uniformly covered the inner and outer surface of CrAlSiN coatings. Also, the potentiodynamic and potentiostatic polarization test revealed that the corrosion protection properties of CrAlSiN coatings/Cr/SUS304 sample was greatly improved by ALD encapsulation with 50 nm-thick $Al_2O_3$ thin films, which implies that ALD-$Al_2O_3$ passivation layer can be used as an effect barrier layer of corrosion.

• Composites Research
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• v.22 no.5
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• pp.15-23
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• 2009

The lubricant tribological characteristics of $Al_2O_3$ fiber and SiC particle hybrid metal matrix composites (MMCs) fabricated by squeeze casting method was investigated using a pin-on-disk wear tester. The wear tests of the MMCs were performed according to fiber/particle hybrid ratio in the planar-random (PR) and normal (N) orientations sliding against a counter steel disk at a fixed speed and $25\;kg_f$ loading under different sliding distances and temperatures. The test results showed that the wear behavior of MMCs varied with fiber orientation and hybrid ratio. At room temperature, the lubricant wear behavior of F20P0 unhybrid PR-MMCs was superior to that of N-MMCs while the hybrid composites exhibited the reverse lubricant wear behavior. It was also revealed that the wear resistance of PR-MMCs was superior to that of the N-MMCs due to the joint action of reinforcements and lubricant film between the friction surfaces at an elevated temperature of $100^{\circ}C$ for both fiber only and hybrid cases. In case of $150^{\circ}C$, although the trend of weight loss was similar to that of others, the wear resistance of PR-MMCs was better than that of N-MMCs for hybrid MMCs.

• Journal of Korea Foundry Society
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• v.23 no.1
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• pp.30-39
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• 2003

Porous hybrid preforms were fabricated by reactive sintering using the compacts consisting of SiC particles, Fe and Al powders. Squeeze casting processing was employed to produce the composite in which the matrix phase is Al-Si7Mg. The microstructural change and wear resistance of the composites were investigated in terms of an amount of SiC particles. The wear loss was increased with increasing the contact pressure in the alloy containing SiC particles coated with Cu. The most drastic change was found to the specimen tested at 2.5 MPa of contact pressure. Concerning the alloys containing SiC particles coated with Ni-P, a drastic increase in the wear loss exhibited at 2 MPa of contact pressure in those alloys containing 4 and 8 wt. % of SiC particles coated with Ni-P. In the alloy containing 16 wt. % a proportional increase in wear loss was observed to the change of contact pressure. With respecting to the sliding velocity, the wear loss of the alloy containing SiC particles coated with Cu increased at the initial stage of wear process and then decreased. Similar result was found in the alloys containing SiC particles coated with Ni-P. On the basis of the present results obtained, it was found that wear resistance of the alloys tested was improved to show in the order of the alloy reinforced by coated SiC particles > by uncoated SiC particles > by intermetallic compound without SiC particles.

• Korean Journal of Materials Research
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• v.15 no.3
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• pp.166-171
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• 2005

Fe-6Al-9Si(N) alloy powders were synthesized by hybrid process of chemical nitrification and mechanical milling. The nitriding treatment on Fe-6Al-9Si alloy powders formed $\gamma'-Fe_4N$ phase on the powders surface. The nitriding-treated powders were pulverized by horizontal high-energy ball milling machine. The longer ball milling time tended to reduce the size of alloy powders. In ball milling for 36h, extremely fine powders with about $7\~9wt\%$ nitrogen were obtained. Through X-ray diffraction analysis on the powders, it was found out that the longer milling time caused a disappearance of the crystallinity of $\alpha-Fe$ in the powders. TEM study confirmed that the powders is comprised of a few tens nano-meter sized crystals, including $\alpha-Fe$ phase with partially $\gamma'-Fe_4N$ phase. Hysteresis curves of the synthesized powders measured by VSM revealed lower saturation magnetization and higher coercivity, which seemed to be attributed to nitrogen-impregnation and severe residual stress developed during the high energy milling. Microstructure observation on the powder annealed at 873 K for 1 h showed 10 to 20 nm sized $\alpha-Fe$ crystal. Such a enhanced crystallinity significantly increased the magnetization and decreased the coercivity, which was attributed to not only the crystallinity but also residual stress relaxation.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.100-102
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• 2013

Magnetron-sputtering법을 사용하여 기존에 연구하였던 CrAlN (Cr 7：Al 3)박막에 Si를 첨가하여 Si의 함량 변화에 따라 미세구조와 화학적 결합상태, 온도저항계수(TCR) 및 산화저항의 영향과 기계적특성 개선을 통한 multi-functional heater resistor layer로써의 가능성을 연구하였다. CrAlSiN 박막의 Si 함량에 변화에 따라 온도저항계수 변화를 확인하였으며 X-선 회절 분석(XRD) 패턴 분석결과 CrAlSiN 박막의 결정구조가 Bl-NaCl 구조를 가지고 있는 것을 확인하였으며 SEM과 AFM을 통한 표면 및 미세구조 분석결과 Si의 함량이 증가할수록 입자가 조밀해짐을 알 수 있었다. 최근 digital priting technology의 핵심 기술로 부각되고 있는 inkjet priting technology는 널리 태양전지뿐만 아니라 thin film process, lithography와 같은 반도체 공정 기술에 활용 할 수 있기 때문에 반도체 제조장비에도 사용되고 있으며, 현재 thermal inkjet 방식을 사용하고 있다. Inkjet printing technology는 전기 에너지를 잉크를 배출하기 위해 열에너지로 변환하는 thermal inkjet 방식을 사용하고 있는데, 이러한 thermal inkjet 방식은 기본적으로 전기저항이 필요하지만 electrical resistor layer는 잉크를 높은 온도에서 순간적으로 가열하기 때문에 부식이나 산화 등의 문제가 발생할 수 있어 이에 대한 보호층을 필요로 한다. 하지만, 고해상도, 고속 잉크젯 프린터, 대형 인쇄 등을 요구되고 있어 저 전력 중심의 잉크젯 프린터의 열효율을 방해하는 보호층 제거에 필요성이 제기되고 있다. 본 연구는 magnetron-sputtering을 사용하여 기존의 CrAlN 박막에 Si를 합성하여 anti-oxidation, corrosion resistance 그리고 low temperature coefficient of resistance 값을 갖는 multi-functional heater resistor layer로써 CrAlSiN 박막의 Si 함량에 따른 효과에 초점을 두었다. 본 실험은 CrAlN 박막에 Si 함량을 4~11 at%까지 첨가시켜 함량의 변화에 따른 특성변화를 확인하였다. 함량이 증가할수록 amorphous silicon nitride phase의 영향으로 박막의 roughness는 감소하였으며 XRD 분석결과 (111) peak의 Intensity가 감소함을 확인하였으며 SEM 관찰시 모든 박막이 columnar structure를 나타내었으며 Si함량이 증가할수록 입자가 치밀해짐을 보여주었다.Si함량이 증가할수록 CrAlN 박막에 비하여 면저항은 증가하였으며 TCR 측정결과 Si함량이 6.5 at%일 때 가장 안정한 TCR값을 나타내었다. Multi-functional heater resistor layer 역할을 하기 위해서, CrAlSiN 박막의 원소 분포, 표면 거칠기, 미세조직, 전기적 특성 등을 조사하였다. CrAlN 박막의 Si의 첨가는 크게 XRD 분석결과 주상 성장을 억제 할 수 있으며 SEM 분석을 통하여 Si 함량이 증가할수록 Si3N4 형성이 감소하며 입자크기가 작아짐을 확인하였다. 면저항의 경우 Si 함량이 증가함에 따라 높은 면저항을 나타내었으며 Si함량이 6.5 at%일 때 가장 낮은 TCR 값인 3120.53 ppm/K값을 보였다. 이 값은 상용되고 있는 heater resistor보다 높지만, CrAlSiN 박막이 더 우수한 기계적 특성을 가지고 있기 때문에 hybrid heater resistor로 적용할 수 있을 것으로 기대된다.

• Steel and Composite Structures
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• v.21 no.6
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• pp.1327-1345
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• 2016

$Al_2O_3$/SiC particulate reinforced (Metal Matrix Composites) MMCs which were produced by using stir casting process, bending strength and hardening behaviour were obtained using an analysis of variance (ANOVA) technique that uses full factorial design. Factor variables and their ranges were: particle size $2-60{\mu}m$; the stirring speed 450 rpm, 500 rpm and the stirring temperature $620^{\circ}C$, $650^{\circ}C$. An empirical equation was derived from test results to describe the relationship between the test parameters. This model for the tensile strength of the hybrid composite materials with $R^2$ adj = 80% for the bending strength $R^2$ adj = 89% were generated from the data. The regression coefficients of this model quantify the tensile strength and bending strengths of the effects of each of the factors. The interactions of all three factors do not present significant percentage contributions on the tensile strength and bending strengths of hybrid composite materials. Analysis of the residuals versus was predicted the tensile strength and bending strengths show a normalized distribution and thereby confirms the suitability of this model. Particle size was found to have the strongest influence on the tensile strength and bending strength.