• Title/Summary/Keyword: field-emission scanning electron microscopy

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Development and Evaluation of Natural Hydroxyapatite Ceramics Produced by the Heat Treatment of Pig Bones

  • Lim, Ki-Taek;Kim, Jin-Woo;Kim, Jangho;Chung, Jong Hoon
    • Journal of Biosystems Engineering
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    • v.39 no.3
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    • pp.227-234
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    • 2014
  • Purpose: The aim of this research was to develop and evaluate natural hydroxyapatite (HA) ceramics produced from the heat treatment of pig bones. Methods: The properties of natural HA ceramics produced from pig bones were assessed in two parts. Firstly, the raw materials were characterized. A temperature of $1,200^{\circ}C$ was chosen as the calcination temperature. Fine bone powders (BPs) were produced via calcinations and a milling process. Sintered BPs were then characterized using field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), X-ray fluorescence spectroscopy (XRF), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared (FTIR) spectroscopy, and a 2-year in vitro degradability test. Secondly, an indirect cytotoxicity test was conducted on human osteoblast-like cells, MG63, treated with the BPs. Results: The average particle size of the BPs was $20{\pm}5{\mu}m$. FE-SEM showed a non-uniform distribution of the particle size. The phase obtained from XRD analysis confirmed the structure of HA. Elemental analysis using XRF detected phosphorus (P) and calcium (Ca) with the Ca/P ratio of 1.6. Functional groups examined by FTIR detected phosphate ($PO{_4}^{3-}$), hydroxyl ($OH^-$), and carbonate ($CO{_3}^{2-}$). The EDX, XRF, and FTIR analysis of BPs indicated the absence of organic compounds, which were completely removed after annealing at $1,200^{\circ}C$. The BPs were mostly stable in a simulated body fluid (SBF) solution for 2 years. An indirect cytotoxicity test on natural HA ceramics showed no threat to the cells. Conclusions: In conclusion, the sintering temperature of $1,200^{\circ}C$ affected the microstructure, phase, and biological characteristics of natural HA ceramics consisting of calcium phosphate. The Ca-P-based natural ceramics are bioactive materials with good biocompatibility; our results indicate that the prepared HA ceramics have great potential for agricultural and biological applications.

Pulsed DC $BCl_3/SF_6$ 플라즈마를 이용한 GaAs와 AlGaAs의 선택적 식각에 관한 연구

  • Choe, Gyeong-Hun;Kim, Jin-U;No, Gang-Hyeon;Sin, Ju-Yong;Park, Dong-Gyun;Song, Han-Jeong;Lee, Je-Won
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.02a
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    • pp.67-67
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    • 2011
  • Pulsed DC $BCl_3/SF_6$ 플라즈마를 사용하여 GaAs와 AlGaAs의 건식 식각을 연구하였다. 식각 공정 변수는 가스 유량 (50~100 % $BCl_3$ in $BCl_3/SF_6$), 펄스 파워 (450~600 V), 펄스 주파수 (100~250 KHz), 리버스 시간 (0.4~1.2 ${\mu}s$)이었다. 식각 공정 후 표면 단차 측정기 (Surface profiler)를 사용하여 표면의 단차와 거칠기를 분석하였다. 그 결과를 이용하여 식각률 (Etch rate), 표면거칠기 (Surface roughness), 식각 선택비 (Selectivity)와 같은 특성 평가를 하였다. 실험 후 주사 현미경 (FE-SEM, Field Emission Scanning Electron Microscopy)을 이용, 식각 후 시료의 단면과 표면을 관찰하였다. 실험 결과에 의하면 1) 18 sccm $BCl_3$ / 2 sccm $SF_6$, 500 V (Pulsed DC voltage), 0.7 ${\mu}s$ (Reverse time), 200 KHz (Pulsed DC frequency), 공정 압력이 100 mTorr인 조건에서 GaAs와 Al0.2Ga0.8As의 식각 선택비가 약 48:1로 우수한 결과를 나타내었다. 2) 펄스 파워 (Pulsed DC voltage), 리버스 시간(Reverse time), 펄스 주파수(Pulsed DC frequency)의 증가에 따라 각각 500~550 V, 0.7~1.0 ${\mu}s$, 그리고 200~250 KHz 구간에서 AlGaAs에 대한 GaAs의 선택비가 감소하게 되는 것을 알 수 있었다. 이는 척 (chuck)에 인가되는 전류와 파워를 증가시키고, 따라서 GaAs의 식각률이 크게 증가했지만 AlGaAs 또한 식각률이 증가하게 되면서 GaAs에 대한 식각 선택비가 감소한 것으로 생각된다. 3) 표면 단차 측정기와 주사전자현미경 사진 결과에서는 GaAs의 경우 10% $SF_6$ (18 sccm $BCl_3$ / 2 sccm $SF_6$)가 혼합된 조건에서 상당히 매끈한 표면 (RMS roughness < 1.0 nm)과 높은 식각률 (~0.35 ${\mu}m$/min), 수직의 식각 측벽 확보에서 매우 좋은 결과를 보여주었다. 또한 같은 공정 조건에서 AlGaAs는 식각이 거의 되지 않은 결과 (~0.03 ${\mu}m$/min)를 보여주었다. 위의 결과들을 종합해 볼 때 Pulsed DC $BCl_3/SF_6$ 플라즈마는 GaAs와 AlGaAs의 선택적 식각 공정에서 매우 우수한 공정 결과를 나타내었다.

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Fabrication and Mechanical Property of Fe-20Cu-1C Compacts by SPS process with Different Heating Rate (방전플라즈마소결법 적용 승온속도 변화에 따라 제조된 Fe-20Cu-1C 소결체 제조 및 특성평가)

  • Ryu, Jung-Han;Shin, Soo-Sik;Ryu, Byung-Rok;Kim, Kyung-Sik;Jang, Jun-Ho;Oh, Ik-Hyun;Kim, Kap-Tae;Park, Hyun-Kuk
    • Journal of Powder Materials
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    • v.24 no.4
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    • pp.302-307
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    • 2017
  • In this study, Fe-Cu-C alloy is sintered by spark plasma sintering (SPS). The sintering conditions are 60 MPa pressure with heating rates of 30, 60 and $9^{\circ}C/min$ to determine the influence of heating rate on the mechanical and microstructure properties of the sintered alloys. The microstructure and mechanical properties of the sintered Fe-Cu-C alloy is investigated by X-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM). The temperature of shrinkage displacement is changed at $450^{\circ}C$ with heating rates 30, 60, and $90^{\circ}C/min$. The temperature of the shrinkage displacement is finished at $650^{\circ}C$ when heating rate $30^{\circ}C/min$, at $700^{\circ}C$ when heating rate $60^{\circ}C/min$ and at $800^{\circ}C$ when heating rate $90^{\circ}C/min$. For the sintered alloy at heating rates of 30, 60, and $90^{\circ}C/min$, the apparent porosity is calculated to be 3.7%, 5.2%, and 7.7%, respectively. The hardness of the sintered alloys is investigated using Rockwell hardness measurements. The objective of this study is to investigate the densification behavior, porosity, and mechanical properties of the sintered Fe-Cu-C alloys depending on the heating rate.

A Study on the Self-cleaning Surface Finishing Using PFOA Free Fluoric Polymer and Silica Nano-sol (PFOA Free 불소 고분자 및 실리카 나노졸을 이용한 self cleaning 표면 가공에 관한 연구)

  • Park, Sung-Min;Kwon, Il-Jun;Kim, Ran;Yeum, Jeong-Hyun;Yoon, Nam-Sik;Lee, Kyeung-Nam
    • Textile Coloration and Finishing
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    • v.21 no.6
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    • pp.1-11
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    • 2009
  • Super-hydrophobic surface, with a water contact angle greater than $150^{\circ}$, has a self cleaning effect termed 'lotus effect'. We introduced super-hydrophobicity onto aramid/rayon mixture fabric with dual-scale structure by assembling silica nano-sol. Mixture fabric was treated with silica nano-sol, fluoric polymer using various parameters such as particle size, concentration. Silica nano-sol size were measured using particle size analyzer. Morphological changes by particle size were observed using field emission scanning electron microscopy(FE-SEM), contact angle measurement equipment. The contact angle of water was about $134.0^{\circ}$, $137.0^{\circ}$, $143.0^{\circ}$, $139.5^{\circ}$ and $139.0^{\circ}$ for mixture fabric coated with 100.2nm, 313.7nm, 558.2nm, 628.5nm and 965.4nm silica nano-sol, compared with about $120.0^{\circ}$ for mixture fabric coated with fluoric polymer. When we mixed particle sizes of 100.2nm and 558.2nm by 7:3 volume ratio, the contact angle of water was about $146.2^{\circ}$. And we mixed particle sizes of 313.7nm and 558.2nm by 7:3 volume ratio, the contact angle of water was about $141.8^{\circ}$. Also we mixed particle sizes of 558.2nm and 965.4nm by 7:3 volume ratio, the best super-hydrophobicity was obtained. In this paper, we fabricated the water-repellent surfaces with various surface structures by using four types of silica nano-sol, and we found that the dual-scale structure was very important for the super-hydrophobicity.

Preparation of Nickel Coated-carbon Nanotube/Zinc Oxide Nanocomposites and Their Antimicrobial and Mechanical Properties (니켈 코팅된 탄소나노튜브/산화아연 나노복합소재의 제조와 항균 및 기계적 특성 분석)

  • Kim, Hyeon-Hye;Han, Woong;An, Kay-Hyeok;Kim, Byung-Joo
    • Applied Chemistry for Engineering
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    • v.27 no.5
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    • pp.502-507
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    • 2016
  • This study was conducted to develop novel antimicrobial nano-composites, with the aim of fully utilizing antimicrobial properties of multi-walled carbon nanotubes (MWCNTs), nickel (Ni) and zinc oxide (ZnO). Ni coated-MWCNTs (Ni-CNT) were prepared and evaluated for their potential application as an antimicrobial material for inactivating bacteria. Field emission scanning electron microscopy (FE-SEM), and X-ray energy dispersive spectroscopy (EDS) were used to characterize the Ni coating and morphology of Ni-CNT. Staphylococcus aureus (S. aureus) and Escherichia coil (E. coil) were employed as the target bacterium on antimicrobial activities. Comparing with the nitric acid treated MWCNTs and Ni-CNT which have been previously reported to possess antimicrobial activity towards S. aureus and E. coil, Ni-CNT/ZnO exhibited a stronger antimicrobial ability. The nickel coating was confirmed to play an important role in the bactericidal action of Ni-CNTs/ZnO composites. Also, the addition of ZnO to the developed nanocomposite is suggested to improve the antimicrobial property.

MECHANICAL PROPERTIES OF TIN COATED FILM WITH VARIOUS COATING THICKNESS ON TITANIUM ALLOY (타이타늄 합금에 다양한 두께로 코팅된 TiN 피막의 기계적 성질)

  • Lee, Jae-Yun;Oh, Dong-Joon;Kim, Hee-Jung;Chung, Chae-Heon
    • The Journal of Korean Academy of Prosthodontics
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    • v.45 no.5
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    • pp.675-686
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    • 2007
  • Statement of problem: Titanium nitride(TiN) coatings are the most general and popular coating method and used to improve the properties of metallic surface for industrial purposes. When TiN coating applied to the abutment screw, frictional resistance would be reduced, as a results, the greater preload and prevention of the screw loosening could be expected. Purpose: The purpose of this study was to investigate mechanical properties of TiN coated film of various coating thickness on the titanium alloy surface and to evaluate proper coating thickness. Material and method: 95 Titanium alloy (Ti-6Al-4V) discs of 15 mm in diameter and 3 mm in thickness were prepared for TiN coating and divided into 7 groups in this study. Acceding to coating deposition time (CDT) with TiN by using Arc ion plating, were divided into 7 groups : Group A (CDT 30min), Group B (CDT 60min), Group C (CDT 90min), Group D (CDT 120min), Group E (CDT 150min), Group F(CDT 180min) and Group G (no CDT) as a control group. TiN coating surface was observed with Atomic Force Microscope(AFM), field emission scanning electron microscopy(FE-SEM) and examined with scratch tester, wear tester. Result: 1. Coating thickness fir each coated group was increased in proportion to coating deposition time. 2. Surface of all coated groups except Group A was homogeneous and smooth. However, surface of none coated Group G had scratch. 3. Adhesion strength for each coated group was increased in proportion to coating deposition time. 4. Wear resistance for each coated group was increased in proportion to coating deposition time. 5. Surface roughness in Group A, B, C was increased in proportion to coating deposition time. But, surface roughness in Group D, E, F was showed decreased tendency in proportion to coating deposition time. Conclusion: According to coating deposition time, mechanical properties of TiN coated film were changed. It was considered that 120 minutes coating deposition time ($1.32{\mu}m$ in coating thickness) is necessary.

Effect of Sputtering Powers on Mg and Ga Co-Doped ZnO Thin Films with Transparent Conducting Characteristics (RF 마그네트론 스퍼터를 이용하여 제작한 MGZO 박막의 구조적 및 전기적, 광학적 특성에 미치는 스퍼터링 전력의 영향)

  • Kim, In Young;Shin, Seung Wook;Kim, Min Sung;Yun, Jae Ho;Heo, Gi Seok;Jeong, Chae Hwan;Moon, Jong-Ha;Lee, Jeong Yong;Kim, Jin Hyoek
    • Korean Journal of Materials Research
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    • v.23 no.3
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    • pp.155-160
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    • 2013
  • ZnO thin films co-doped with Mg and Ga (MxGyZzO, x + y + z = 1, x = 0.05, y = 0.02 and z = 0.93) were prepared on glass substrates by RF magnetron sputtering with different sputtering powers ranging from 100W to 200W at a substrate temperature of $350^{\circ}C$. The effects of the sputtering power on the structural, morphological, electrical, and optical properties of MGZO thin films were investigated. The X-ray diffraction patterns showed that all the MGZO thin films were grown as a hexagonal wurtzite phase with the preferred orientation on the c-axis without secondary phases such as MgO, $Ga_2O_3$, or $ZnGa_2O_4$. The intensity of the diffraction peak from the (0002) plane of the MGZO thin films was enhanced as the sputtering power increased. The (0002) peak positions of the MGZO thin films was shifted toward, a high diffraction angle as the sputtering power increased. Cross-sectional field emission scanning electron microscopy images of the MGZO thin films showed that all of these films had a columnar structure and their thickness increased with an increase in the sputtering power. MGZO thin film deposited at the sputtering power of 200W showed the best electrical characteristics in terms of the carrier concentration ($4.71{\times}10^{20}cm^{-3}$), charge carrier mobility ($10.2cm^2V^{-1}s^{-1}$) and a minimum resistivity ($1.3{\times}10^{-3}{\Omega}cm$). A UV-visible spectroscopy assessment showed that the MGZO thin films had high transmittance of more than 80 % in the visible region and that the absorption edges of MGZO thin films were very sharp and shifted toward the higher wavelength side, from 270 nm to 340 nm, with an increase in the sputtering power. The band-gap energy of MGZO thin films was widened from 3.74 eV to 3.92 eV with the change in the sputtering power.

Capacitively Coupled Dry Etching of GaAs in BCl3/N2 Discharges at Low Vacuum Pressure (저진공 축전 결합형 BCl3/N2 플라즈마를 이용한 GaAs의 건식 식각)

  • Kim, Jae-Kwon;Park, Ju-Hong;Lee, Sung-Hyun;Noh, Ho-Seob;Joo, Young-Woo;Park, Yeon-Hyun;Kim, Tae-Jin;Lee, Je-Won
    • Korean Journal of Materials Research
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    • v.19 no.3
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    • pp.132-136
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    • 2009
  • This study investigates GaAs dry etching in capacitively coupled $BCl_3/N_2$ plasma at a low vacuum pressure (>100 mTorr). The applied etch process parameters were a RIE chuck power ranging from $100{\sim}200W$ on the electrodes and a $N_2$ composition ranging from $0{\sim}100%$ in $BCl_3/N_2$ plasma mixtures. After the etch process, the etch rates, RMS roughness and etch selectivity of the GaAs over a photoresist was investigated. Surface profilometry and field emission-scanning electron microscopy were used to analyze the etch characteristics of the GaAs substrate. It was found that the highest etch rate of GaAs was $0.4{\mu}m/min$ at a 20 % $N_2$ composition in $BCl_3/N_2$ (i.e., 16 sccm $BCl_3/4$ sccm $N_2$). It was also noted that the etch rate of GaAs was $0.22{\mu}m/min$ at 20 sccm $BCl_3$ (100 % $BCl_3$). Therefore, there was a clear catalytic effect of $N_2$ during the $BCl_3/N_2$ plasma etching process. The RMS roughness of GaAs after etching was very low (${\sim}3nm$) when the percentage of $N_2$ was 20 %. However, the surface roughness became rougher with higher percentages of $N_2$.

Enhanced Mechanical Properties and Thermal Stability of CrAlN Coatings by Interlayer Deposition (중간층 증착에 의한 CrAlN 코팅의 기계적 물성 및 내열성 향상에 관한 연구)

  • Kim, Hoe-Geun;Ra, Jeong-Hyeon;Song, Myeon-Gyu;Lee, Sang-Yul
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2016.11a
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    • pp.100-100
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    • 2016
  • 물리기상증착방법 (Physical vapor deposition)에 의하여 합성된 천이금속 질화물 박막은 경도, 내마모성 등 절삭공구의 성능을 향상시키며, Ti-Al-N, Ti-Zr-N, Zr-Al-N, Cr-Si-N 등의 3원계 경질 박막에 대한 연구가 지속적으로 이루어지고 있다. 이중에서도 CrAlN 코팅은 높은 경도, 낮은 표면 조도 등의 우수한 기계적 특성 이외에 고온에서 안정한 합금상 형성으로 인하여 우수한 내열성을 보유하여 공구 코팅으로의 적용 가능성이 크다. 그러나 최근 공구사용 환경의 가혹화로 인하여 코팅의 내마모성 및 내열성 등의 물성 향상을 통한 공구의 수명 향상이 필요시 되고 있으며, 코팅에 적합한 중간층을 합성함으로써 공구 코팅으로의 적용 가능성을 높이는 연구들이 진행되고 있다. 본 연구에서는 CrAlN 코팅의 물성을 향상시키기 위해 CrAlN 코팅과 WC-Co 6wt.% 모재 사이에 CrN, CrZrN, CrN/CrZrSiN 등의 다양한 중간층을 합성하였으며, 중간층을 포함한 모든 코팅의 두께는 $3{\mu}m$ 로 제어하였다. 합성된 코팅의 미세조직, 경도 및 탄성계수, 내모성을 분석하기 위해 field emission scanning electron microscopy(FE-SEM), nano-indentation, ball-on-disk 마모시험기 및 ${\alpha}-step$을 사용하였다. 코팅의 내열성을 확인하기 위해 코팅을 furnace에 넣어 공기중에서 500, 600, 700, 800, 900, $1,000^{\circ}C$로 30분 동안 annealing 한 후에 nano-indentation을 사용하여 경도를 측정하였다. CrAlN 코팅을 나노 인덴테이션으로 분석한 결과, 모든 코팅의 경도(35.5-36.2 GPa)와 탄성계수(424.3-429.2 GPa)는 중간층의 종류에 상관없이 비슷한 값을 보인 것으로 확인됐다. 그러나, 코팅의 마찰계수는 중간층의 종류에 따라 다른 값을 보였으며, CrN/CrZrSiN 중간층을 증착한 CrAlN 코팅의 마찰계수는 0.34로 CrZrN 중간층을 증착한 CrAlN 코팅의 마찰계수(0.41)에 비해 낮은 값을 보였다. 또한, 코팅의 마모율 및 마모폭도 비슷한 경향을 보인 것으로 보아, CrN/CrZrSiN 중간층을 합성한 CrAlN 코팅의 내마모성이 상대적으로 우수한 것으로 판단된다. 이것은 중간층의 H/E ratio가 코팅의 내마모성에 미치는 영향에 의한 결과로 사료된다. H/E ratio는 파단시의 최대 탄성 변형율로써, 모재/중간층/코팅의 H/E ratio 구배에 따라 코팅 내의 응력의 완화 정도가 변하게 된다. WC 모재 (H/E=0.040)와 CrAlN 코팅(H/E=0.089) 사이에서 CrN, CrZrSiN 중간층의 H/E ratio 는 각각 0.076, 0.083 으로 모재/중간층/코팅의 H/E ratio 구배가 점차 증가함을 확인 할 수 있었고, 일정 응력이 지속적으로 가해지면서 진행되는 마모시험중에 CrN과 CrZrSiN 중간층이 WC와 CrAlN 코팅 사이에서 코팅 내부의 응력구배를 완화시키는 역할을 함으로써 CrAlN 코팅의 내마모성이 향상된 것으로 판단된다. 모든 코팅을 열처리 후 경도 분석결과, CrN/CrZrSiN 중간층을 증착한 CrAlN 코팅은 $1,000^{\circ}C$까지 약 28GPa의 높은 경도를 유지한 것으로 확인 되었고, 이는 CrZrSiN 중간층 내에 존재하는 $SiN_x$ 비정질상의 우수한 내산화성에 의한 결과로 판단된다.

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Hot Corrosion Behavior of Plasma Sprayed 4 mol% Y2O3-ZrO2 Thermal Barrier Coatings with Volcanic Ash (플라즈마 용사법으로 제작된 4mol% Y2O3-ZrO2 열차폐코팅의 화산재에 의한 고온열화거동)

  • Lee, Won-Jun;Jang, Byung-Koog;Lim, Dae-Soon;Oh, Yoon-Suk;Kim, Seong-Won;Kim, Hyung-Tae;Araki, Hiroshi;Murakami, Hideyuki;Kuroda, Seiji
    • Journal of the Korean Ceramic Society
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    • v.50 no.6
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    • pp.353-358
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    • 2013
  • The hot corrosion behavior of plasma sprayed 4 mol% $Y_2O_3-ZrO_2$ (YSZ) thermal barrier coatings (TBCs) with volcanic ash is investigated. Volcanic ash that deposited on the TBCs in gas-turbine engines can attack the surface of TBCs itself as a form of corrosive melt. YSZ coating specimens with a thickness of 430-440 ${\mu}m$ are prepared using a plasma spray method. These specimens are subjected to hot corrosion environment at $1200^{\circ}C$ with five different duration time, from 10 mins to 100 h in the presence of corrosive melt from volcanic ash. The microstructure, composition, and phase analysis are performed using Field emission scanning electron microscopy, including Energy dispersive spectroscopy and X-ray diffraction. After the heat treatment, hematite ($Fe_2O_3-TiO_2$) and monoclinic YSZ phases are found in TBCs. Furthermore the interface area between the molten volcanic ash layers and YSZ coatings becomes porous with increases in the heat treatment time as the YSZ coatings dissolved into molten volcanic ash. The maximum thickness of this a porous reaction zone is 25 ${\mu}m$ after 100 h of heat treatment.