• Title/Summary/Keyword: $Cl_2$/Ar

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Electrochemical Characteristics of Nanotubular Ti-25Nb-xZr Ternary Alloys for Dental Implant Materials

  • Byeon, In-Seop;Park, Seon-Young;Choe, Han-Cheol
    • Journal of Korean Dental Science
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    • v.10 no.1
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    • pp.10-21
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    • 2017
  • Purpose: The purpose of this study was to investigate the electrochemical characteristics of nanotubular Ti-25Nb-xZr ternary alloys for dental implant materials. Materials and Methods: Ti-25Nb-xZr alloys with different Zr contents (0, 3, 7, and 15 wt.%) were manufactured using commercially pure titanium (CP-Ti), niobium (Nb), and zirconium (Zr) (99.95 wt.% purity). The alloys were prepared by arc melting in argon (Ar) atmosphere. The Ti-25Nb-xZr alloys were homogenized in Ar atmosphere at $1,000^{\circ}C$ for 12 hours followed by quenching into ice water. The microstructure of the Ti-25Nb-xZr alloys was examined by a field emission scanning electron microscope. The phases in the alloys were identified by an X-ray diffractometer. The chemical composition of the nanotube-formed surfaces was determined by energy-dispersive X-ray spectroscopy. Self-organized $TiO_2$ was prepared by electrochemical oxidation of the samples in a $1.0M\;H_3PO_4+0.8wt.%$ NaF electrolyte. The anodization potential was 30 V and time was 1 hour by DC supplier. Surface wettability was evaluated for both the metallographically polished and nanotube-formed surfaces using a contact-angle goniometer. The corrosion properties of the specimens were investigated using a 0.9 wt.% aqueous solution of NaCl at $36^{\circ}C{\pm}5^{\circ}C$ using a potentiodynamic polarization test. Result: Needle-like structure of Ti-25Nb-xZr alloys was transform to equiaxed structure as Zr content increased. Nanotube formed on Ti-25Nb-xZr alloys show two sizes of nanotube structure. The diameters of the large tubes decreased and small tubes increased as Zr content increased. The lower contact angles for nanotube formed Ti-25NbxZr alloys surfaces showed compare to non-nanotube formed surface. The corrosion resistance of alloy increased as Zr content increased, and nanotube formed surface showed longer the passive regions compared to non-treatment surface. Conclusion: It is confirmed that corrosion resistance of alloy increased as Zr content increased, and nanotube formed surface has longer passive region compared to without treatment surface.

Mineralogy and Geochemistry of the Jeonheung and Oksan Pb-Zn-Cu Deposits, Euiseong Area (의성(義城)지역 전흥(田興) 및 옥산(玉山) 열수(熱水) 연(鉛)-아연(亞鉛)-동(銅) 광상(鑛床)에 관한 광물학적(鑛物學的)·지화학적(地化學的) 연구(硏究))

  • Choi, Seon-Gyu;Lee, Jae-Ho;Yun, Seong-Taek;So, Chil-Sup
    • Economic and Environmental Geology
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    • v.25 no.4
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    • pp.417-433
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    • 1992
  • Lead-zinc-copper deposits of the Jeonheung and the Oksan mines around Euiseong area occur as hydrothermal quartz and calcite veins that crosscut Cretaceous sedimentary rocks of the Gyeongsang Basin. The mineralization occurred in three distinct stages (I, II, and III): (I) quartz-sulfides-sulfosalts-hematite mineralization stage; (II) barren quartz-fluorite stage; and (III) barren calcite stage. Stage I ore minerals comprise pyrite, chalcopyrite, sphalerite, galena and Pb-Ag-Bi-Sb sulfosalts. Mineralogies of the two mines are different, and arsenopyrite, pyrrhotite, tetrahedrite and iron-rich (up to 21 mole % FeS) sphalerite are restricted to the Oksan mine. A K-Ar radiometric dating for sericite indicates that the Pb-Zn-Cu deposits of the Euiseong area were formed during late Cretaceous age ($62.3{\pm}2.8Ma$), likely associated with a subvolcanic activity related to the volcanic complex in the nearby Geumseongsan Caldera and the ubiquitous felsite dykes. Stage I mineralization occurred at temperatures between > $380^{\circ}C$ and $240^{\circ}C$ from fluids with salinities between 6.3 and 0.7 equiv. wt. % NaCl. The chalcopyrite deposition occurred mostly at higher temperatures of > $300^{\circ}C$. Fluid inclusion data indicate that the Pb-Zn-Cu ore mineralization resulted from a complex history of boiling, cooling and dilution of ore fluids. The mineralization at Jeonheung resulted mainly from cooling and dilution by an influx of cooler meteoric waters, whereas the mineralization at Oksan was largely due to fluid boiling. Evidence of fluid boiling suggests that pressures decreased from about 210 bars to 80 bars. This corresponds to a depth of about 900 m in a hydrothermal system that changed from lithostatic (closed) toward hydrostatic (open) conditions. Sulfur isotope compositions of sulfide minerals (${\delta}^{34}S=2.9{\sim}9.6$ per mil) indicate that the ${\delta}^{34}S_{{\Sigma}S}$ value of ore fluids was ${\approx}8.6$ per mil. This ${\delta}^{34}S_{{\Sigma}S}$ value is likely consistent with an igneous sulfur mixed with sulfates (?) in surrounding sedimentary rocks. Measured and calculated hydrogen and oxygen isotope values of ore-forming fluids suggest meteoric water dominance, approaching unexchanged meteoric water values. Equilibrium thermodynamic interpretation indicates that the temperature versus $fs_2$ variation of stage I ore fluids differed between the two mines as follows: the $fs_2$ of ore fluids at Jeonheung changed with decreasing temperature constantly near the pyrite-hematite-magnetite sulfidation curve, whereas those at Oksan changed from the pyrite-pyrrhotite sulfidation state towards the pyrite-hematite-magnetite state. The shift in minerals precipitated during stage I also reflects a concomitant $fo_2$ increase, probably due to mixing of ore fluids with cooler, more oxidizing meteoric waters. Thermodynamic consideration of copper solubility suggests that the ore-forming fluids cooled through boiling at Oksan and mixing with less-evolved meteoric waters at Jeonheung, and that this cooling was the main cause of copper deposition through destabilization of copper chloride complexes.

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DC 반응성 스퍼터링법으로 증착한 TiN/Al, TiCN/Al 박막의 전기적.기계적 특성 및 내부식성 평가

  • Lee, Hyeon-Jun;Song, Pung-Geun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.346-347
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    • 2012
  • 최근 화석연료 대체 에너지원으로서 자동차용으로 연구 개발 및 응용되고 있는 고분자 전해질 연료전지(PEMFC: Proton exchange membrane fuel cells)에서 분리판(Bipolar Plate)은 스택 전체 무게의 80%, 스택 가격의 60% 정도로 가장 높은 비중을 차지한다. 분리판은 연료와 산화제를 공급해주는 통로 및 전지 운전 중에 생성된 물을 제거하는 통로 역할과 anode, cathode로서 전극 역할을 통해 스택 전력을 형성하는 핵심 기능과 전지와 전지 사이의 지지대 역할을 한다. 따라서 분리판은 전기전도성, 내부식성 및 기계적 특성이 우수해야함은 물론이고, 얇고 가벼우며 가공성이 뛰어나야 한다. 현재 가장 많이 사용되고 있는 금속 분리판 소재 중 스테인리스 스틸은 전기적, 기계적 특성 및 내부식성이 우수한 반면, 가격이 비싸고, 중량이 무거운 단점이 있다. 따라서 본 연구에서는 DC 반응성 마그네트론 스퍼터링법으로 전기적, 기계적 특성 및 내부 식성이 우수한 TiN, TiCN 박막을 스테인리스에 비해 중량이 1/3, 소재 단가가 1/4인 알루미늄 기판 위에 증착하여 박막 물성을 평가하였다. DC Power는 400 W, 기판과 타겟 사이의 거리는100 mm, 공정 압력은 0.5 Pa로 고정하였고, 3 inch의 지름과 순도 99.95%를 갖는 티타늄 타겟을 사용하였다. 공정 가스는 Ar을 주입하였으며, 질소와 탄소의 공급원으로는 질소($N_2$)와 메탄($CH_4$) 가스를 사용하여 챔버 내 주입혼합가스의 전체 유량을 50 sccm으로 고정시켰다. 증착된 박막의 전기적, 기계적 특성을 측정하였고, X-ray diffraction (XRD), Scanning electron microscope (SEM)을 이용하여 박막의 미세구조 및 표면 상태를 확인하였다. 또한, 내부식 특성을 평가하기 위해 potentiostatic, potentiodynamic 법을 이용하여 박막의 부식저항을 측정하였다. 증착된 TiN 박막의 경우 질소 함량의 증가에 따라 박막 증착속도는 감소하는 경향을 보였다. 이는 타겟 부근의 질소 라디칼 비율이 증가함에 따라 질화반응이 촉진된 것으로 생각된다. 또한, 증착된 TiN과 TiCN 박막은 반응성 질소 유량과 탄소 유량에 따라 각각 다른 미세구조를 가지는 것을 확인하였다. TiN과 TiCN은 NaCl형의 면심입방격자(FCC)로 같은 구조이며, 격자상수가 비슷하여 전율고용되어 TiCN을 형성하고, 탄소와 질소의 비에 따라 전기적 기계적 특성이 달라짐을 확인하였다.

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Properties Investigation of Corrosion Monitoring for Pure Mg Thin Films under Wet-Dry Cyclic Conditions by Using Electrochemical Impedance Spectroscopy Method (건습환경중 순 Mg박막의 EIS부식 모니터링 특성 관찰)

  • Bae, I.Y.;Lee, K.H.;Kim, K.J.;Moon, K.M.;Lee, M.H.
    • Proceedings of the Korean Society of Marine Engineers Conference
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    • 2005.11a
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    • pp.192-193
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    • 2005
  • Magnesium thin films were prepared on cold-rolled steel substrates by RF(Radio Frequency) magnetron sputtering technique.$^{1)}$ The crystal orientation and monitoring of the deposited films were investigated by using XRD(X-ray Diffraction) and EIS(Electrochemical Impedance Spectroscopy), respectively. The corrosion rates of Mg thin films deposited with different argon gas pressure and substrate bias voltage were monitored by AC impedance method under a cyclic wet-dry condition, which was conducted by exposure to alternate conditions of 1h immersion in 3%NaCl solution and 5h drying at 60% RH and 25$^{\circ}C$. The result of corrosion rate of Mg thin films deposited at various Ar gas pressures and substrate bias voltage under wet-dry cyclic exposure in chloride-containing solutions was showed the following conclusions. At the region I during the onset of the wet cycle, corrosion rate showed relatively low value. The increase in the Corrosion rate of region II is due to the increase in the chloride concentration. Corrosion rate of region III during the onset of the cycle zero and salt crystals remain on the metal surface.$^{2)}$

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COMMISSIONING RESULT OF THE KSTAR HELIUM REFRIGERATION SYSTEM

  • Park, Dong-Seong;Chang, Hyun-Sik;Joo, Jae-Joon;Moon, Kyung-Mo;Cho, Kwang-Woon;Kim, Yang-Soo;Bak, Joo-Shik;Cho, Myeon-Chul;Kwon, Il-Keun;Andrieu, Frederic;Beauvisage, Jerome;Desambrois, Stephane;Fauve, Eric
    • Nuclear Engineering and Technology
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    • v.40 no.6
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    • pp.467-476
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    • 2008
  • To keep the superconducting (SC) magnet coils of KSTAR at proper operating conditions, not only the coils but also other cold components, such as thermal shields (TS), magnet structures, SC bus-lines (BL), and current leads (CL) must be maintained at their respective cryogenic temperatures. A helium refrigeration system (RRS) with an exergetic equivalent cooling power of 9 kW at 4.5 K without liquid nitrogen ($LN_2$) pre-cooling has been manufactured and installed. The main components of the KST AR helium refrigeration system (HRS) can be classified into the warm compression system (WCS) and the cryogenic devices according to the operating temperature levels. The process helium is compressed from 1 bar to 22 bar passing through the WCS and is supplied to cryogenic devices. The main components of cryogenic devices are consist of cold box (C/B) and distribution box (D/B). The C/B cool-down and make the various cryogenic helium for the KSTAR Tokamak and the various cryogenic helium is distributed by the D/B as per the KSTAR requirement. In this proceeding, we will present the commissioning results of the KSTAR HRS. Circuits which can simulate the thermal loads and pressure drops corresponding to the cooling channels of each cold component of KSTAR have been integrated into the helium distribution system of the HRS. Using those circuits, the performance and the capability of the HRS, to fulfill the mission of establishing the appropriate operating condition for the KSTAR SC magnet coils, have been successfully demonstrated.

Etching of Pt Thin Film for SAW Filter Fabrication (표면탄성파 필터 제작을 위한 Pt 박막 식각)

  • Choi, Yong-Hee;Song, Ho-Young;Park, Se-Geun;Lee, Taek-Joo;O, Beom-Hoan;Lee, Seung-Gol;Lee, El-Hang
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2003.11a
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    • pp.103-107
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    • 2003
  • The inductively coupled plasma(ICP) etching process was selected to fabricate RF Surface Acoustic Wave(SAW) filters and a Pt thin film was sputtered on a $LiTaO_3$ substrate applied to electrode materials to reduce the spurious response and improve the power durability. Steep sidewall pattern was achieved employing $C_4F_8/Ar/Cl_2$ gas chemistry. We investigated an etching mechanism and parameter dependence of the Pt thin film about $C_4F_8$ addition. Sidewall etch angle was about $80^{\circ}$ at the $C_4F_8$ 20% mixing ratio. Fabricated SAW filter is consists of some series and parallel arm SAW resonators which work as impedance elements and show capacitance characteristics at out of the passband. It can be modified for $800{\sim}900\;MHz$ RF filters. External matching circuits were unnecessary.

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Selective Etching of Magnetic Layer Using CO/$NH_3$ in an ICP Etching System

  • Park, J.Y.;Kang, S.K.;Jeon, M.H.;Yeom, G.Y.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.448-448
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    • 2010
  • Magnetic random access memory (MRAM) has made a prominent progress in memory performance and has brought a bright prospect for the next generation nonvolatile memory technologies due to its excellent advantages. Dry etching process of magnetic thin films is one of the important issues for the magnetic devices such as magnetic tunneling junctions (MTJs) based MRAM. CoFeB is a well-known soft ferromagnetic material, of particular interest for magnetic tunnel junctions (MTJs) and other devices based on tunneling magneto-resistance (TMR), such as spin-transfer-torque MRAM. One particular example is the CoFeB - MgO - CoFeB system, which has already been integrated in MRAM. In all of these applications, knowledge of control over the etching properties of CoFeB is crucial. Recently, transferring the pattern by using milling is a commonly used, although the redeposition of back-sputtered etch products on the sidewalls and the low etch rate of this method are main disadvantages. So the other method which has reported about much higher etch rates of >$50{\AA}/s$ for magnetic multi-layer structures using $Cl_2$/Ar plasmas is proposed. However, the chlorinated etch residues on the sidewalls of the etched features tend to severely corrode the magnetic material. Besides avoiding corrosion, during etching facets format the sidewalls of the mask due to physical sputtering of the mask material. Therefore, in this work, magnetic material such as CoFeB was etched in an ICP etching system using the gases which can be expected to form volatile metallo-organic compounds. As the gases, carbon monoxide (CO) and ammonia ($NH_3$) were used as etching gases to form carbonyl volatiles, and the etched features of CoFeB thin films under by Ta masking material were observed with electron microscopy to confirm etched resolution. And the etch conditions such as bias power, gas combination flow, process pressure, and source power were varied to find out and control the properties of magnetic layer during the process.

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A Study on the Properties of $Al_2$ $O_3$ and $Al_2$ $O_3$/( $Ti_{0.5}$ $Al_{0.5}$)N Coatings Produced by Plasma Enhanced Chemical Vapor Deposition (플라즈마 화학 증착법에 의한 $Al_2$ $O_3$ 단층피막과 $Al_2$ $O_3$/( $Ti_{0.5}$ $Al_{0.5}$)N 이중피막의 제조 및 특성에 관한 연구)

  • 손경석;이승훈;이동각;임주완;이후철;이정중
    • Journal of the Korean institute of surface engineering
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    • v.34 no.2
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    • pp.105-114
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    • 2001
  • $Al_2$$O_3$ coatings were deposited on M2 high speed steels by the plasma enhanced chemical vapor deposition (PECVD) process, using a gas mixture of AlC1$_3$, $H_2$, $CO_2$ and Ar $Al_2$$O_3$ coatings had interference color and showed amorphous phase. $A1_2$X$A1_3$/($Ti_{0.5}$ /$Al_{0.5}$ )N double layer coatings were produced in the sequence of substrate $NH_3$ plasma pretreatment, ($Ti_{0.5}$$Al_{0.5}$)N depoition process, $Al_2$$O_3$ deposition process. $Al_2$ $O_3$/( $Ti_{0.5}$A $l_{0.5}$)N double layer coatings showed NaCl structure in ( $Ti_{0.5}$A $l_{0.5}$)N layer and amorphous phase in A1$_2$ $O_3$ layer. It was shown that $Al_2$ $O_3$ columns continuously grew onto ( $Ti_{0.5}$A $l_{0.5}$)N columns. ( $Ti_{0.5}$A $l_{0.5}$)N single coating and $Al_2$ $O_3$/( $Ti_{0.5}$A $l_{0.5}$)N double layer coating were oxidized at $700^{\circ}C$, 80$0^{\circ}C$, 90$0^{\circ}C$ for 1hr, 3hr in atmosphere. At 80$0^{\circ}C$, single layer coatings were oxidized, which were examined substrate oxide particle. But $Al_2$ $O_3$/ ( $Ti_{0.5}$A $l_{0.5}$)N double layer coatings maintained the asdeposited state. Therefore, $Al_2$ $O_3$/ ( $Ti_{0.5}$A $l_{0.5}$)N double layer coatings have moreexcellent oxidation resistance than ( $Ti_{0.5}$A $l_{0.5}$)N single layer coatings.X> 0.5/)N single layer coatings.s.

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Mesothermal Gold-Silver Mineralization at the Bodeok Mine, Boseong Area : A Fluid Inclusion and Stable Isotope Study (전남(全南) 보성지역(寶城地域) 보덕광산(寶德鑛山)의 심부(深部) 중온형(中溫型) 금(金)-은(銀) 광화작용(鑛化作用): 유체포유물(流體包有物) 및 안정동위원소(安定同位元素) 연구(硏究))

  • So, Chil-Sup;Yun, Seong-Taek;Kim, Se-Hyun;Youm, Seung-Jun;Heo, Chul-Ho;Choi, Seon-Gyu
    • Economic and Environmental Geology
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    • v.26 no.4
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    • pp.433-444
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    • 1993
  • Electrum (32~73 atom. % Ag)-sulfide mineralization of the Bodeok mine in the Boseong area was deposited in two stages of mineralogically simple, massive quartz veins that fill the fractures along fault shear zones in Precambrian gneiss. Radiometric dating indicates that mineralization is Late Jurassic age ($155.9{\pm}2.3$ Ma). Fluid inclusion data show that ore mineralization was formed from $H_2O-CO_2$ fluids with variable $CO_2$ contents ($X_{CO_2}=0.0$ to 0.7) and low salinities (0.0 to 7.4 wt. % eq. NaCl) at temperatures between $200^{\circ}$ and $370^{\circ}C$. Evidence of fluid unmixing ($CO_2$ effervescence) indicates pressures up to 1 kbar. Gold-silver deposition occurred later than base-metal sulfide deposition, at temperatures near $250^{\circ}C$ and was probably a result of cooling and decreasing sulfur activity caused by sulfide precipitation and/or $H_2S$ loss (through fluid unmixing). Calculated sulfur isotope compositions of ore fluids (${\delta}^{34}S_{{\Sigma}S}=1.7$ to 3.3‰) indicate an igneous source of sulfur in hydrothermal fluids. Measured and calculated O and H isotope compositions of ore fluids (${\delta}^{18}O_{water}=4.8$ to 7.2‰, ${\delta}D_{water}=-73$ to -76‰) indicate that mesothermal auriferous fluids at Bodeok were likely mixtures of $H_2O-rich$, isotopically evolved meteoric waters and magmatic $H_2O-CO_2$ fluids.

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A Study on the Characteristics of $(Ti_{1-x}Al_x)N$ Coatings Deposited by Plasma Enhanced Chemical Vapor Deposition after Heat Treatment (플라즈마 화학 증착법으로 제조된 $(Ti_{1-x}Al_x)N$ 박막의 열처리에 따른 특성 평가)

  • 이승훈;임주완
    • 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.

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