• Title/Summary/Keyword: TEM microstructure

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Microscopic characterization of pretransition oxide formed on Zr-Nb-Sn alloy under various Zn and dissolved hydrogen concentrations

  • Kim, Sungyu;Kim, Taeho;Kim, Ji Hyun;Bahn, Chi Bum
    • Nuclear Engineering and Technology
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    • v.50 no.3
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    • pp.416-424
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    • 2018
  • Microstructure of oxide formed on Zr-Nb-Sn tube sample was intensively examined by scanning transmission electron microscopy after exposure to simulated primary water chemistry conditions of various concentrations of Zn (0 or 30 ppb) and dissolved hydrogen ($H_2$) (30 or 50 cc/kg) for various durations without applying desirable heat flux. Microstructural analysis indicated that there was no noticeable change in the microstructure of the oxide corresponding to water chemistry changes within the test duration of 100 days (pretransition stage) and no significant difference in the overall thickness of the oxide layer. Equiaxed grains with nano-size pores along the grain boundaries and microcracks were dominant near the water/oxide interface, regardless of water chemistry conditions. As the metal/oxide interface was approached, the number of pores tended to decrease. However, there was no significant effect of $H_2$ concentration between 30 cc/kg and 50 cc/kg on the corrosion of the oxide after free immersion in water at $360^{\circ}C$. The adsorption of Zn on the cladding surface was observed by X-ray photoelectron spectroscopy and detected as ZnO on the outer oxide surface. From the perspective of $OH^-$ ion diffusion and porosity formation, the absence of noticeable effects was discussed further.

Microstructural characteristics of a fresh U(Mo) monolithic mini-plate: Focus on the Zr coating deposited by PVD

  • Iltis, Xaviere;Drouan, Doris;Blay, Thierry;Zacharie, Isabelle;Sabathier, Catherine;Onofri, Claire;Steyer, Christian;Schwarz, Christian;Baumeister, Bruno;Allenou, Jerome;Stepnik, Bertrand;Petry, Winfried
    • Nuclear Engineering and Technology
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    • v.53 no.8
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    • pp.2629-2639
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    • 2021
  • Within the frame of the EMPIrE test, four monolithic mini-plates were irradiated in the ATR reactor. In two of them, the monolithic U(Mo) foil had been PVD-coated with Zr before the plate manufacturing. Extensive microstructural characterizations were performed on a fresh archive mini-plate, using Optical Microscopy (OM), Scanning Electron Microscopy (SEM) combined with Energy Dispersive Spectroscopy (EDS), Electron Backscattered Diffraction (EBSD) and Focused Ion Beam (FIB)/Transmission Electron Microscopy (TEM) with nano EDS. A particular attention was paid to the examination of the U(Mo) foil, the PVD coating, the cladding/Zr and Zr/U(Mo) interfaces. The Zr coating has a thickness around 15 ㎛. It has a columnar microstructure and appears dense. The cohesion of the cladding/Zr and Zr/U(Mo) interfaces seems to be satisfactory. An almost continuous layer with a thickness of the order of 100-300 nm is present at the cladding/Zr interface and corresponds to an oxidized part of the Zr coating. At the Zr/U(Mo) interface, a thin discontinuous layer is observed. It could correspond to locally oxidized U(Mo). This work provides a basis for interpreting the results of characterizations on EMPIrE irradiated plates.

A Study on Microstructure and Mechanical Properties of TiB2-steel Composite Fabricated by Gas Pressure Infiltration Process (가스압 함침 공정으로 제조된 TiB2-steel 금속복합재료의 미세조직 및 기계적 물성에 관한 연구)

  • Lee, Jihye;Lee, Donghyun;Cho, Seungchan;Kwon, Hansang;Lee, Sang-Kwan;Lee, Sang-Bok;Kim, Junghwan
    • Composites Research
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    • v.35 no.4
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    • pp.248-254
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    • 2022
  • In this study, TiB2-steel composite with high-fractional TiB2 reinforcement was fabricated by gas pressure infiltration process and the microstructure analysis and compressive strength and hardness were evaluated. To elucidate the correlation between microstructure and mechanical properties for fabricated composite, after the compression test of TiB2-steel composite, the fracture surface was analyzed and the fracture behavior on compression test was predicted. As a result of the compression fracture surface analysis, interfacial failure trace between the steel matrix and the reinforcement was observed, and the interface between the steel matrix and the reinforcement was analyzed using TEM. From the result of microstructure analysis on the fabricated composite, it was confirmed that, in addition to TiB2 reinforcement and steel matrix, TiC phase and coarse (Fe,M)2B (M=Cr,Mn) phase were formed. Throughout the thermodynamic calculation, it was confirmed that TiC and (Fe,M)2B can be formed as a stable phase under the process condition. The fabricated TiB2-steel composite had a significantly increased hardness, and the compressive strength and Young's modulus were improved by 3.07 times and 1.95 times, respectively, compared to steel matrix. It seems that the coarse (Fe,M)2B (M=Cr,Mn) phase formed throughout the composite causes the deterioration of mechanical properties, and by controlling the formation of the (Fe,M)2B (M=Cr,Mn) phase, it is judged that the mechanical properties of the TiB2-steel composite can be further improved.

A Study on the Electrochemical Properties of LiNi0.8Co0.2-xMxO2[M=Al] Cathode Materials Prepared by Sol-Gel Method (졸-겔법에 의해 제조된 정극 활물질 LiNi0.8Co0.2-xMxO2[M=Al]의 전기화학적 특성)

  • Han, Chang-Joo;Cho, Won-Il;Cho, Byung-Won;Yun, Kyung-Suk;Jang, Ho
    • Journal of the Korean Electrochemical Society
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    • v.6 no.4
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    • pp.266-270
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    • 2003
  • The $LiN_{0.8}Co_{0.2}O_2$ has shown outstanding electrochemical properties. The microstructure of $LiN_{0.8}Co_{0.2}O_2$ cathode was investigated by using TEM (transmission electron microscopy) and X-ray diffraction techniques. The $LiN_{0.8}Co_{0.2}O_2$ was produced by sol-gel method to synthesize fine particles less than $1{\mu}m$ in the average diameter. In this study, emphasis was given to the examination and interpretation of the microstructural change during charge-discharge cycling experiments, which appeared to be one of the main causes of early degradation of rechargeable batteries. Results showed that the $1{\mu}m$ cathode produced by sol-gel method had high reversible capacity and excellent cycling stability due to its homogeneous distribution of Ni and Co cations on u atomic scale. In particular, the $1{\mu}m$ cathode did not show severe strain induced structural defects or cubic spinel disordering during cycling experiments, which had been observed in the conventional $LiCoO_2$ cathode. The $LiNi_{0.8}Co_{0.2-x}M_x[M=Al]$ compounds show good reversibility but low discharge capacity.

Friction and Wear Properties of Plasma-sprayed Cr2O3-MoO3 Composite Coatings at High Temperature (MoO3가 첨가된 Cr2O3 플라즈마 용사코팅의 고온 마찰 마멸 특성)

  • Lyo, In-Woong;Ahn, Hyo-Sok;Lim, Dae-Soon
    • Journal of the Korean Ceramic Society
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    • v.39 no.9
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    • pp.851-856
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    • 2002
  • Tribological behavior of plasma-sprayed $Cr_2O_3$-based coatings containing $MoO_3$ at 450$^{\circ}C$ was investigated to understand the influence of $MoO_3$. A reciprocal disc-on-plate type tribo-tester was employed to examine fricition and wear behavior of the specimens. The microstructure and phase composition of the coating was characterized with Transmission Electron Microscopy(TEM). The TEM analysis indicated that $MoO_3$ was dispersed into the grain boundary, resulting in the increase of the hardness and density of the coating. Worn surfaces were investigated by scanning electron microscopy and chemistry of the worn surfaces was analyzed using a X-ray Photoelectron Spectrometer(XPS). The results showed that the friction coefficient of the $MoO_3$-added coatings was lower than that without $MoO_3$ addition. The larger protecting layers were observed at the worn surface of plasma spray coated specimens with $MoO_3$ composition in the protecting layer appears to be more favorable in reducing the friction.

Influences of the Irradiation of Intense Pulsed ion Beam (IPIB) on the Surface of Ni$_3$Al Base Alloy IC6

  • Le, X.Y.;Yan, S.;Zhao, W.J.;Han, B.H.;Wang, Y.G.;Xue, J.M.;Zhang, H.T.
    • Journal of Korean Vacuum Science & Technology
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    • v.6 no.2
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    • pp.92-96
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    • 2002
  • In this paper, we treated the Ni$_3$Al based alloy samples with intense pulsed ion beams (IPIB) at the beam parameters of 250KV acceleration voltage, 100 - 200 A/cm$^2$ current density and 60 u pulse duration. We simulated the thermal-mechanical process near the surface of Ni$_3$Al based alloy with our STEIPIB codes. The surface morphology and the cross-section microstructures of samples were observed with SEM, the composition of the sample surface layer was determined by X-ray Energy Dispersive Spectrometry (XEDS) and the microstructure on the surface was observed by Transmission Electron Microscope (TEM). The results show that heating rate increases with the current density of IPIB and cooling rate reached highest value less than 150 A/cm$^2$. The irradiation of IPIB induced the segregation of Mo and adequate beam parameter can improve anti-oxidation properly of IC6 alloy. Some craters come from extraneous debris and liquid droplets, and some maybe due to the melting of the intersection region of interphase. Increasing the pulse number enlarges average size of craters and decreases number density of craters.

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The Effects of Process Parameters on the Composition and Microstructure of Lead Titanate Thin Films deposited by ECR PECVD (ECR PECVD법으로 증착된 lead titanate박막의 조성과 미세구조에 대한 증착변수의 영향)

  • Chung, Su-Ock;Chung, Seong-Ung;Lee, Won-Jong
    • Korean Journal of Materials Research
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    • v.7 no.2
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    • pp.93-101
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    • 1997
  • Lead titanate박막을 $Pt/Ti/SiO_{2}/Si(Pt/Ti기판)와\;Pt/Ta/SiO_{2}/SiO_{2}$Si(Pt/Ta 기판) 위에서 전자 사이크로트론 공명플라즈마 화학증착법(ECR PECVD)으로 증착하였다. 증착온도, 산소유입량, MO source유입비등의 증착변수에 따른 lead titanate박막의 조성과 미세구조를 주사전자현미경(SEM), 투과전자현미경(TEM), X선 회절법(XRD)으로 조사하였다. 산소유입량이 적을 경우,Tisource와 Pb source의 산소화의 반응성 차이 때문에 Pb 농도가 부족한 화학양론비가 잘 맞는 박막이 증착되었다. Pt/ti기판은 lead titanate박막증착도중 기판의 Ti층과 Pt층의 확산으로 기판변형이 발생하는 반면, Pt/Ta기판은 기판변형이 일어나지 않았다. Pt/Ta기판에서 페롭스카이트 화학양론비를 갖는 매우 평탄한 lead titanate박막을 증착 하였는데, 산소유입량이 lead titanate박막의 결정성을 크게 지배하였다.

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Fabrication of Piezoelectric PZT Thick Film by Sol-gel Process (Sol-Gel 법에 의한 압전 PZT 후막의 제조)

  • Park, Jong-whan;Bang, Kook-soo;Park, Chan
    • Journal of Ocean Engineering and Technology
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    • v.29 no.1
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    • pp.94-99
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    • 2015
  • Lead zirconate titanate (PZT) thick films with thicknesses of ㎛ were fabricated on silicon substrates using an aerosol deposition method. A PZT powder solution was prepared using a sol-gel process. The average diameters (d50) obtained were 1.67, 1.98, and 2.40μm when the pyrolysis temperatures were 300℃, 350℃, and 450℃ respectively. The as-deposited film had a uniform microstructure without any cracks or pores. The as-deposited films on silicon were annealed at a temperature of 700℃. The 20-㎛-thick PZT film showed good adherence between the PZT film and substrate, with no tearing observed in the conventional solid phase process. This was probably because the presence of pores produced from organic residue during annealing relieved the residual stresses in the deposited film.

Photo-catalytic Properties of Nanotubes Synthesized using TiO2 Nanoparticles

  • Kim, Hyun;Kim, Dong Yun;Yang, Bee Lyong
    • Journal of the Korean Ceramic Society
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    • v.55 no.3
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    • pp.239-243
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    • 2018
  • Up to now, microstructure changes of photocatalysts have been studied to improve photocatalytic activity. Especially, to improve the adsorption of reactants and reactive sites, porous and fine crystal structures have received much attention because of their large specific surface area. In this study, $TiO_2$ nanotubes were synthesized by hydrothermal method using $TiO_2$ nanoparticles; nanotubes were evaluated by oxidized methylene blue reduction test. Using synthesized $TiO_2$ nanotubes, results of TEM showed that the $TiO_2$ nanoparticles were changed into folding sheets and nanotubes. XRD results showed that the peaks of the nanoparticles almost disappeared and only the rutile (110) and anatase (200) peaks were observed. Comparison of photocatalytic properties of nanoparticles and nanotube structures was performed by measuring the UV-vis absorbance with reducing oxidized methylene blue. As a result, the reduction rate of nanotubes was found to be $0.24{\mu}mol/s$, which was 2.6 times higher than the rate of reduction of nanoparticles.

Effects of Co-doping on Densification of Gd-doped CeO2 Ceramics and Adhesion Characteristics on a Yttrium Stabilized Zirconia Substrate

  • Lee, Ho-Young;Kang, Bo-Kyung;Lee, Ho-Chang;Heo, Young-Woo;Kim, Jeong-Joo;Lee, Joon-Hyung
    • Journal of the Korean Ceramic Society
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    • v.55 no.6
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    • pp.576-580
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    • 2018
  • In this study, a small amount of CoO was added to commercial Gd-doped $CeO_2$ (GDC) powder. The CoO addition greatly enhanced sinterability at low temperatures, i.e., more than 98% of relative density was achieved at $1,000^{\circ}C$. When GDC/8YSZ (8 mol% yttrium stabilized zirconia) bilayers were sintered, Co-doped GDC showed excellent adhesion to the YSZ electrolyte. Transmission electron microscope (TEM) analysis showed that there were no traces of liquid films at the grain boundaries of GDC, whereas liquid films were observed in the Co-doped GDC sample. Because liquid films facilitate particle rearrangement and migration during sintering, mechanical stresses at the interface of a bilayer, which are developed based on different densification rates between the layers, might be reduced. In spite of $Co^{2+}$ doping in GDC, the electrical conductivity was not significantly changed, relative to GDC.