• Title/Summary/Keyword: in-situ scanning electron microscopy

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Comparison study of the effect of blending method on PVDF/PPTA blend membrane structure and performance

  • Li, Hongbin;Shi, Wenying;Zhang, Yufeng;Zhou, Rong
    • Membrane and Water Treatment
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    • v.6 no.3
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    • pp.205-224
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    • 2015
  • A novel hydrophilic poly (vinylidene fluoride)/poly (p-phenylene terephthalamide) (PVDF/PPTA) blend membrane was prepared by in situ polycondensation of p-phenylene diamine (PPD) and terephthaloyl chloride (TPC) in PVDF solution with subsequent nonsolvent induced phase separation (NIPS) process. For comparison, conventional solution blend membrane was prepared directly by adding PVDF powder into PPTA polycondensation solution. Blend membranes were characterized by means of viscometry, X-ray photoelectron spectroscopy (XPS), Field Emission Scanning Electron Microscopy (FESEM). The effects of different blending methods on membrane performance including water contact angle (WCA), mechanical strength, anti-fouling and anti-compression properties were investigated and compared. Stronger interactions between PVDF and PPTA in in situ blend membranes were verified by viscosity and XPS analysis. The incorporation of PPTA accelerated the demixing rate and caused the formation of a more porous structure in blend membranes. In situ blend membranes exhibited better hydrophilicity and higher tensile strength. The optimal values of WCA and tensile strength were $65^{\circ}$ and 34.1 MPa, which were reduced by 26.1% and increased by 26.3% compared with pure PVDF membrane. Additionally, antifouling properties of in situ blend membranes were greatly improved than pure PVDF membrane with an increasing of flux recovery ratio by 25%. Excellent anti-compression properties were obtained in in situ blend membranes with a stable pore morphology. The correlations among membrane formation mechanism, structure and performance were also discussed.

Structural Analysis of Low Temperature Processed Schottky Contacts to n-InGaAs (저온공정 n-InGaAs Schottky 접합의 구조적 특성)

  • 이홍주
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.14 no.7
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    • pp.533-538
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    • 2001
  • The barrier height is found to increase from 0.25 to 0.690 eV for Schottky contacts on n-InGaAs using deposition of Ag on a substrate cooled to 77K(LT). Surface analysis leads to an interface model for the LT diode in which there are oxide compounds of In:O and As:O between the metal and semiconductor, leading to behavior as a metal-insulator-semiconductor diode. The metal film deposited t LT has a finer and more uniform structure, as revealed by scanning electron microscopy and in situ metal layer resistance measurement. This increased uniformity is an additional reason for the barrier height improvement. In contrast, the diodes formed at room temperature exhibit poorer performance due to an unpassivated surface and non-uniform metal coverage on a microscopic level.

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A Study on the Aging Behavior of a Mg-8.5Li-4.5Al alloy by Differential Scanning Calorimetry (열분석법에 의한 Mg-8.5Li-4.5Al합금의 시효거동 연구)

  • Kim, Y.W.;Hwang, Y.H.;Park, T.W.;Kim, D.H.;Hong, C.P.
    • Journal of the Korean Society for Heat Treatment
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    • v.10 no.4
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    • pp.255-265
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    • 1997
  • Precipitation and strengthening mechanisms in squeeze cast Mg-8.5wt%Li-4.5wt%Al have been investigated by differential scanning calorimetry(DSC), scanning electron microscopy(SEM), in-situ and ex-situ X-ray diffraction analysis and hardness measurement. Special emphasis was placed on the investigation of the precipitation behavior by the DSC technique. Microstructural and calorimetric analysis showed that ${\theta}$ and ${\delta}$ precipitates in the b.c.c. ${\beta}$ phase matrix, forming two exothermic peaks at the temperature ranges of $130^{\circ}C{\sim}180^{\circ}C$ and $236^{\circ}C{\sim}280^{\circ}C$. ${\theta}$ and ${\delta}$ dissolve into the matrix forming an endothermic peak at the temperature range of $280^{\circ}C{\sim}352^{\circ}C$. The as-cast microstructure consists of ${\alpha}$, ${\beta}$ and ${\delta}$. Peak strength was obtained after aging for 1 hour at $50^{\circ}C$. The aging time required for the peak strength decreased as the aging temperature increases. The hardness decrease during overaging was due to the coarsening of ${\theta}$ precipitates. Microhardness measurement showed that variation of the hardness of ${\beta}$ matrix was more pronounced than that of the ${\alpha}$ phase, indicating that the ${\beta}$ phase is more responsible for the strengthening of the Mg-8.5wt%Li-4.5wt%Al alloy.

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Mechanical Properties of Styrene-Butadiene Rubber Reinforced with Silica by in situ Tetraethoxysilane Hydrolysis over Acid Catalyst

  • Li, Qingyuan;Li, Xiangxu;Cho, Ur Ryong
    • Elastomers and Composites
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    • v.53 no.2
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    • pp.57-66
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    • 2018
  • Styrene-butadiene rubber (SBR), reinforced with different contents of silica (with or without modification using silane coupling agents), was prepared by a modified sol-gel method involving hydrolyzation of tetraethoxysilane over an acid catalyst. The structures of the as-prepared samples were characterized using various techniques, such as scanning electron microscopy, X-ray photoelectron spectroscopy, Fourier-transform infrared spectroscopy, and thermogravimetric analysis. The mechanical properties of the as-prepared samples were discussed in detail. The results revealed an increasing of the storage modulus (G') with increase in the silica content without modification. In contrast, G' decreased after modification using silane coupling agents, indicating a reduction in the silica-silica interaction and improved dispersion of silica in the SBR matrix. Both tensile stress and hardness increased with increase in the silica content (with modification) in the SBR matrix, albeit with low values compared to the samples with un-modified silica, except for the case of silica modified using (3-glycidyloxypropyl) trimethoxysilane (GPTS). The latter observation can be attributed to the special structure of GPTS and the effort of oxygen atom lone-pair.

Self-Organized Synthesis and Mechanism of SnO2@Carbon Tube-Core Nanowire

  • Luo, Minting;Ma, Yong-Jun;Pei, Chonghua;Xing, Yujing;Wen, Lixia;Zhang, Li
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2535-2538
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    • 2012
  • $SnO_2@carbon$ tube-core nanowire was synthesized via a facile self-organized method, which was in situ by one step via Chemical Vapor Deposition. The resulting composite was characterized by scanning electron microscopy, X-ray diffraction and transmission electron microscope. The diameter of the single nanowire is between 5 nm and 60 nm, while the length would be several tens to hundreds of micrometers. Then X-ray diffraction pattern shows that the composition is amorphous carbon and tin dioxide. Transmission electron microscope images indicate that the nanowire consists of two parts, the outer carbon tube and the inner tin dioxide core. Meanwhile, the possible growth mechanism of $SnO_2@carbon$ tube-core nanowire is also discussed.

Synthesis and Characterization of Tungsten Trioxide Films Prepared by a Sol-Gel Method for Electrochromic Applications

  • Kim, Tae-Ho;Nah, Yoon-Chae
    • Journal of Powder Materials
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    • v.22 no.5
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    • pp.309-314
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    • 2015
  • Tungsten trioxide thin films are successfully synthesized by a sol-gel method using tungsten hexachloride as precursors. The structural, chemical, and optical properties of the prepared films are characterized by scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and UV-Vis spectrophotometry. The electrochemical and electrochromic properties of the films before and after heat treatment are also investigated by cyclic voltammetry, chronoamperometry, and in situ transmittance measurement system. Compared to as-prepared films, heat-treated tungsten trioxide thin films exhibit a higher electrochemical reversibility of 0.81 and superior coloration efficiency of $65.7cm^2/C$, which implies that heat treatment at an appropriate temperature is a crucial process in a sol-gel method for having a better electrochromic performance.

Preparation of Poly(methyl methacrylate)/Na-MMT Nanocomposites via in-Situ Polymerization with Macroazoinitiator

  • Jeong Han Mo;Ahn Young Tae
    • Macromolecular Research
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    • v.13 no.2
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    • pp.102-106
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    • 2005
  • Poly(methyl methacrylate) (PMMA)/sodium montmorillonite (Na-MMT) nanocomposites were prepared with a novel method utilizing a macroazoinitiator (MAI). To induce the intergallery polymerization of methyl methacrylate (MMA), the MAI containing a po1y(ethylene glycol) (PEG) segment was intercalated between the lamellae of Na-MMT and swelled with water to enhance the diffusion of MMA into the gallery. The structure of the nanocomposite was examined using X-ray diffraction and transmission electron microscopy, and the thermal properties were examined using differential scanning calorimetry and thermogravimetry. The PMMA/Na-MMT nanocomposite prepared by intergallery polymerization showed a distinct enhancement of its thermal properties; an approximately $30^{\circ}C$ increase in its glass transition temperature and an $80\sim100^{\circ}C$ increase in its thermal decomposition temperature for a $10\%$ weight loss.

Long-term Testing and Analysis of a ScSZ/LaSrCuFe Cell

  • Wackerl, Jurgen;Peck, Dong-Hyun;Markus, Torsten
    • Journal of the Korean Ceramic Society
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    • v.45 no.12
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    • pp.788-795
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    • 2008
  • An electrolyte supported SOFC cell was tested at $800^{\circ}C$ in air for 3600 h with an applied current density of $200\;mA/cm^2$ to examine possible cathode degradation issues. A scandium- stabilized zirconia (ScSZ) with additional manganese doping (ScSZ: Mn) was used as electrolyte. A strontium and copper-doped lanthanum ferrite (LaSrCuFe) and platinum were used as cathode and quasi-anode material, respectively. The DC resistance was logged over the complete testing period. Additionally, impedance spectroscopy was used from time to time to track changes of the cell in-situ. Post-test analysis of the cell using methods like scanning electron microscopy imaging and other electrochemical testing methods allow the identification of different degradation sources. The results indicate a promising combination of electrolyte and cathode material in terms of chemical compatibility and electrical performance.

Effect of Na3PO4 Concentration on The Formation Behavior of PEO films on AZ31 Mg Alloy (AZ31 Mg합금의 PEO피막 형성거동에 미치는 인산나트륨 농도의 영향)

  • Moon, Sungmo;Kim, Juseok
    • Journal of the Korean institute of surface engineering
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    • v.52 no.5
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    • pp.265-274
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    • 2019
  • Formation behavior of PEO (Plasma Electrolytic Oxidation) films on AZ31 Mg alloy was investigated under application of 310 Hz AC as a function of $Na_3PO_4$ concentration from 0.02 M to 0.2 M. Film formation voltage and in-situ observation of arcs generated on the specimen surface were recorded with time, and surface morphologies of the PEO films were investigated using optical microscopy, confocal scanning laser microscopy and scanning electron microscopy. PEO film formation voltage decreased linearly with increasing $Na_3PO_4$ concentration which is attributed to the increase of solution pH. PEO films were grown uniformly over the entire surface in $Na_3PO_4$ solutions between 0.05 M and 0.1 M. However, non-uniform PEO films with white spots were formed in $Na_3PO_4$ solutions containing more than 0.1 M. Thickness and roughness of PEO films on AZ31 Mg alloy increased linearly with increasing $Na_3PO_4$ concentration and their increasing rates appeared to be much higher under 1 M than above 1 M. The experimental results suggest that phosphate ions can contribute to the formation of PEO films but higher $Na_3PO_4$ concentration more than 1 M results in local damages of PEO films due to repeated generation of white arcs at the same surface site of AZ31 Mg alloy.

Endurance in Al Alloy Melts and Wear Resistance of Titanium Matrix Composite Shot-Sleeve for Aluminum Alloy Die-casting (Al 합금 다이캐스팅 용 타이타늄 기지 복합재료 슬리브의 내용손성 및 내마모성 평가)

  • Choi, Bong-Jae;Sung, Si-Young;Kim, Young-Jig
    • Korean Journal of Metals and Materials
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    • v.50 no.2
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    • pp.176-182
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    • 2012
  • The main purpose of this study was to evaluate the endurance against Al alloy melts and wear resistance of an in-situ synthesized titanium matrix composite (TMC) sleeve for aluminum alloy die-casting. The conventional die-casting shot sleeve material was STD61 tool steel. TMCs have great thermal stability, wear and oxidation resistance. The in-situ reaction between Ti and $B_4C$ leads to two kinds of thermodynamically stable reinforcements, such as TiBw and TiCp. To evaluate the feasibility of the application to a TMCs diecasting shot sleeve, the interfacial reaction behavior was examined between Al alloys melts with TMCs and STD61 tool steel. The pin-on-disk type dry sliding wear test was also investigated for TMCs and STD61 tool steel.