• Title/Summary/Keyword: Micro-columnar

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Transmission Electron Microscopy Characterization of Early Pre-Transition Oxides Formed on ZIRLOTM

  • Bae, Hoyeon;Kim, Taeho;Kim, Ji Hyun;Bahn, Chi Bum
    • Corrosion Science and Technology
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    • v.14 no.6
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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.

Oxidation of CrAlN and CrZrN Films (CrAlN과 CrZrN의 산화)

  • Kim, Min-Jeong;Kim, Seul-Gi;Lee, Sang-Yul;Lee, Dong-Bok
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2011.05a
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    • pp.33-35
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    • 2011
  • Films of CrAlN and CrZrN were deposited on a steel substrate by closed field unbalanced magnetron sputtering, and their oxidation behaviors were investigated. CrAlN films consisted of dense, polycrystalline CrN and AlN fine columns. The formed oxides consisted primarily of crystalline $Cr_2O_3$ incorporated with $Al_2O_3$. The oxide layers were thin and compact so as to make CrAlN films more protective than CrN films. In case of CrZrN films, Zr atoms were dissolved in the CrN phase. Zr atoms advantageously refined the columnar structure, reduced the surface roughness, and increased the micro-hardness. However, the addition of Zr did not increased oxidation resistance, mainly because Zr was not a protective element. All the deposited films displayed relatively good oxidation resistance, owing to the formation of the highly protective $Cr_2O_3$ on their surface. The $Cr_{40}Zr_9N$ and $Cr_{31}Zr_{16}N$ films oxidized to $Cr_2O_3$ as the major phase and ${\alpha}-ZrO_2$ as the minor one, whereas the CrN film oxidized to $Cr_2O_3$.

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Mineralogical Characteristics of Naturally Occurring Asbestos (NOA) at Daero-ri, Seosan, Chungnam, Korea (충남 서산 대로리 일대 자연발생석면의 광물학적 특성)

  • Jung, Haemin;Shin, Joodo;Kim, Yumi;Park, Jaebong;Roh, Yul
    • Economic and Environmental Geology
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    • v.47 no.5
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    • pp.467-477
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    • 2014
  • Naturally occurring asbestos (NOA) occurs in rocks and soils as a result of natural weathering and human activities. The asbestos have been associated with ultramafic and mafic rocks, and carbonate rock. The previous studies on NOA were mainly limited to ultramafic and mafic rock-hosted asbestos in Korea. But, studies on carbonatehosted asbestos are relatively rare. Therefore, the purposes of this study were to investigate mineralogical characteristics of carbonate-hosted and metapelite-hosted NOA and to examine genesis of NOA occurred in the both rocks. The study area was Daerori, Seosan, Chungnam Province, Korea. The major rock formation consisted of limestone and schist which have been known to contain asbestos. Sampling was performed at outcrop which contained carbonate rock showing acicular asbestos crystals as well as pegmatitic intrusion that contacted with carbonate rock. PLM, XRD, EPMA, and EDS analyses were used to characterize mineral assemblages, mineralogical characteristics, and crystal habits of amphiboles and other minerals. BSEM images were also used to examine the genesis of asbestos minerals. The amphibole group was observed in all of the carbonate rocks, and actinolite and tremolite were identified in all rocks. These mineral habits were mainly micro-acicular crystals or secondary asbestiform minerals on the surface of non-asbestiform minerals appearing split end of columnar crystals produced by weathering. BSEM images showed residual textures of samples. The residual textures of carbonate rocks showed dolomite-tremolite-diopside mineral assemblages that formed during prograde metasomatism stage. Some carbonate rock also showed diopside-tremolite-talc mineral assemblages which were formed during retrograde metasomatism stage, as the residual textures. In result the presence of asbestos actinolite-tremolite in the carbonate rocks were confirmed in the areas where actinolite-tremolite asbestos was influenced by low temperature hydrothermal solution during metasomatism stage. These asbestos minerals showed the acicular asbestiform minerals, but even non-asbestiform minerals, a bundle or columnar shape, could transform to asbestiform minerals as potential NOA by weathering because the end of columnar shape of non-asbestiform minerals appeared as multiple acicular shaped fibers.

Effect of the Coating Structure on the Corrosion Resistance of Al-Mg Coated Steel (Al-Mg 코팅층의 구조가 강판 내식성에 미치는 영향)

  • Jung, Jae-Hun;Yang, Ji-Hoon;Kim, Sung-Hwan;Byeon, In-Seop;Jeong, Jae-In;Lee, Myeong-Hoon
    • Journal of the Korean institute of surface engineering
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    • v.49 no.5
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    • pp.454-460
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    • 2016
  • Double-layered Al-Mg films have been deposited by using an e-beam deposition method on a cold-rolled steel sheet(CR), which the structure of the film was Al/Mg/CR. The micro-structure, alloy phase, and corrosion resistance of the Al-Mg coated CR were investigated before and after heat treatment at $400^{\circ}C$ for 2, 3, and 10 min in a nitrogen atmosphere. Total thickness of Al-Mg films was fixed at $3{\mu}m$ and the thickness ratio of Al and Mg layers(Al:Mg) has been changed from 5:1 to 1:5. The cross-sectional morphology of the films, which had the thickness ratio of 2:1(Al:Mg), 1:1, and 1:2, was changed after heat treatment from columnar to featureless structure. The x-ray diffraction data for as-deposited films showed only pure Al and Mg peaks. Al-Mg alloy peaks such as $Al_3Mg_2$ and $Al_{12}Mg_{17}$ phase appeared after the heat treatment. The Al-Mg coating with the thickness ratio of 1:1(Al:Mg) showed the best corrosion resistance of up to 500 hours by salt spray test.

Microstructures and Electrical Properties of Thick PZT Films with Thickness Variation Fabricated by Multi-coating Method (Multi-coating법으로 제조된 두꺼운 PZT막의 두께 변화에 따른 미세구조 및 전기적 특성)

  • Park, Jun-Sik;Jang, Yeon-Tae;Park, Hyo-Deok;Choe, Seung-Cheol;Gang, Seong-Gun
    • Korean Journal of Materials Research
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    • v.12 no.3
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    • pp.211-214
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    • 2002
  • Properties of 52/48 PZT films with various thicknesses for piezoelectric micro-electro mechanical systems (MEMS) devices fabricated by multi-coating method on $Pt(3500{\AA})/Ti(400{\AA})/SiO_2(3000{\AA})/Si$(525$\mu\textrm{m}$) substrates were investigated. PZT films were deposited by spin-coating process at 3500 rpm for 30 sec, followed by pyrolysis at 45$0^{\circ}C$ for 10 min producing the thickness of about 120nm. These processes were repeated 4, 8, 12, 16 and 20 times in order to have various thicknesses, respectively. Finally, they were crystallized at $650^{\circ}C$ for 30 min. All thick PZT films showed dense and homogeneous surface microstructures. Thick PZT films showed crystalline structures of random orientations with increasing thickness. Dielectric constants of thick PZT films were increased with increasing film thickness and reached 800 at 100kHz for 2.3$\mu\textrm{m}$ thick PZT film. $P_r\; and\; E_c$ of 2.3$\mu\textrm{m}$ thick PZT films were about 20$\mu$C/$\textrm{cm}^2$ and 63kV/cm. Depth profile analysis by Auger Electron Spectroscopy (AES) of 4800 $\AA$ thick PZT film showed the formation of the perovskite phase on Pt layer by Pb diffusion behavior. It was considered that Pb-Pt intermediate layer promoted PZT (111) columnar structures.

Effects of Sputtering Ar Pressure on Magnetic and Magneto-optical Propwrties in Compositionally Modulated Co/Pd Supwrlattice Thin Films (조성변조 Co/Pd 초격자 박막의 Ar가스 압력변화에 따른 자기 및 자기광학적 특성)

  • 김진홍;신성철
    • Journal of the Korean Magnetics Society
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    • v.2 no.2
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    • pp.119-124
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    • 1992
  • We have investigated the effects of sputtering Ar gas pressure on magnetic and magneto-optical properties in compositionally modulated Co/Pd superlattice thin films. The samples were prepared by dc magnetron sputtering from 2-in.-diam Co and Pd targets by alternately exposing the substrates to targets. Sputtering Ar gas pressure was varied from 2 to 30 mTorr. All samples had same bilayer thicknesses composed of 2-$\AA$-thick Co and 9-$\AA$-thick Pd sublayers. It was observed that the colum-nar structure was more distinctively developed with increasing Ar gas pressure. We observed that the intrinsic uniaxial anisotropy energy, magnetization and polar Kerr rotation were decreased with increasing Ar gas pressures. Large coercivity and perfect squareness were attained by the deposition at the high Ar gas pressure. We believe that the results are mainly ascribed the variation of micro-structure with sputtering Ar gas pressure.

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Characteristics of TiAlN Film on Different Buffer Layer by D.C Magnetron Sputter (D.C magnetron sputter법으로 증착된 TiAlN의 중간층에 따른 특성연구)

  • Kim, Myoung-Ho;Lee, Doh-Jae;Lee, Kwang-Min;Kim, Woon-Sub;Kim, Min-Ki;Park, Burm-Su;Yang, Kook-Hyun
    • Korean Journal of Materials Research
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    • v.18 no.10
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    • pp.558-563
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    • 2008
  • TiAlN films were deposited on WC-5Co substrates with different buffer layers by D.C. magnetron sputtering. The films were evaluated by microstructural observations and measuring of preferred orientation, hardness value, and adhesion force. As a process variable, various buffer layers were used such as TiAlN single layer, TiAlN/TiAl, TiAlN/TiN and TiAlN/CrN. TiAlN coating layer showed columnar structures which grew up at a right angle to the substrates. The thickness of the TiAlN coating layer was about $1.8{\mu}m$, which was formed for 200 minutes at $300^{\circ}$. XRD analysis showed that the preferred orientation of TiAlN layer with TiN buffer layer was (111) and (200), and the specimens of TiAlN/TiAl, TiAlN/CrN, TiAlN single layer have preferred orientation of (111), respectively. TiAlN single layer and TiAlN/TiAl showed good adhesion properties, showing an over 80N adhesion force, while TiAlN/TiN film showed approximately 13N and the TiAlN/CrN was the worst case, in which the layer was destroyed because of high internal residual stress. The value of micro vickers hardness of the TiAlN single layer, TiAlN/TiAl and TiAlN/TiN layers were 2711, 2548 and 2461 Hv, respectively.

Residual Stress and Elastic Modulus of Y2O3 Coating Deposited by EB-PVD and its Effects on Surface Crack Formation

  • Kim, Dae-Min;Han, Yoon-Soo;Kim, Seongwon;Oh, Yoon-Suk;Lim, Dae-Soon;Kim, Hyung-Tae;Lee, Sung-Min
    • Journal of the Korean Ceramic Society
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    • v.52 no.6
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    • pp.410-416
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    • 2015
  • Recently, a new $Y_2O_3$ coating deposited using the EB-PVD method has been developed for erosion resistant applications in fluorocarbon plasma environments. In this study, surface crack formation in the $Y_2O_3$ coating has been analyzed in terms of residual stress and elastic modulus. The coating, deposited on silicon substrate at temperatures higher than $600^{\circ}C$, showed itself to be sound, without surface cracks. When the residual stress of the coating was measured using the Stoney formula, it was found to be considerably lower than the value calculated using the elastic modulus and thermal expansion coefficient of bulk $Y_2O_3$. In addition, amorphous $SiO_2$ and crystalline $Al_2O_3$ coatings were similarly prepared and their residual stresses were compared to the calculated values. From nano-indentation measurement, the elastic modulus of the $Y_2O_3$ coating in the direction parallel to the coating surface was found to be lower than that in the normal direction. The lower modulus in the parallel direction was confirmed independently using the load-deflection curves of a micro-cantilever made of $Y_2O_3$ coating and from the average residual stress-temperature curve of the coated sample. The elastic modulus in these experiments was around 33 ~ 35 GPa, which is much lower than that of a sintered bulk sample. Thus, this low elastic modulus, which may come from the columnar feather-like structure of the coating, contributed to decreasing the average residual tensile stress. Finally, in terms of toughness and thermal cycling stability, the implications of the lowered elastic modulus are discussed.

Corrosion behaviors of Cp-Ti and Ti-6Al-4V alloys by TiN coating (TiN 코팅된 Ti 및 Ti-6Al-4V합금의 부식거동)

  • Lee, Soon-Hyun;Jung, Yoong-Hun;Choi, Han-Chul;Ko, Yeong-Mu
    • Journal of Technologic Dentistry
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    • v.30 no.1
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    • pp.25-31
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    • 2008
  • Cp-Ti and Ti-6Al-4V alloys commonly used dental implant materials, particularly for orthopaedic and osteosynthesis because of its suitable mechanical properties and excellent biocompatibility. This alloys have excellent corrosion behavior in the clinical environment. The first factor to decide the success of dental implantation is sufficient osseointegration and high corrosion resistance between on implant fixture and its surrounding bone tissue. In this study, in order to increase corrosion resistance and biocompatibility of Cp-Ti and Ti-6Al-4V alloy that surface of manufactured alloy was coated with TiN by RF-magnetron sputtering method. The electrochemical behavior of TiN coated Cp-Ti and Ti-6Al-4V alloy were investigated using potentiodynamic (EG&G Co, PARSTAT 2273. USA) and potentiostatic test (250mV) in 0.9% NaCl solution at 36.5 $\pm$ 1$^{\circ}C$. These results are as follows : 1. From the microstructure analysis, Cp-Ti showed the acicular structure of $\alpha$-phase and Ti-6Al-4V showed the micro-acicular structure of ${\alpha}+{\beta}$ phase. 2. From the potentiodynamic test, Ecorr value of Cp-Ti and Ti-6Al-4V alloys showed -702.48mV and -319.87mV, respectively. Ti-6Al-4V alloy value was higher than Cp-Ti alloy. 3. From the analysis of TiN and coated layer, TIN coated surface showed columnar structure with 800 nm thickness. 4. The corrosion resistance of TiN coated Cp-Ti and Ti-6Al-4V alloys were higher than those of the non-coated Ti alloys in 0.9% NaCl solution from potentiodynamic test, indicating better protective effect. 5. The passivation current density of TiN coated Cp-Ti and Ti-6Al-4V alloys were smaller than that of the noncoated implant fixture in 0.9% NaCl solution, indicating the good protective effect resulting from more compact and homogeneous layer formation.

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