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

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Comparison of microstructures in T1-1223/Ag tapes with different chemical compositions and J$_c$'s

  • Jeong, D.Y.;Kim, H.K.;Lee, H.Y.;Cha, M.K.;Ha, H.S.;Oh, S.S.;Tsuruta, T.;Horiuchi, S.
    • 한국초전도학회:학술대회논문집
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    • v.9
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    • pp.280-290
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    • 1999
  • The microstructures of a Tl$_{0.8}Pb_{0.2}Bi_{0.2}Sr_{1.6}Ca_2Cu_3O_{9+{\delta}}$/Ag tape (tape I ) with J$_c$ of 17,600 A/cm$^2$ at 77 K and 0 T and three Tl$_{0.8}Pb_{0.2}Bi_{0.2}Sr_{1.8}Ba_{0.2}Ca_{2.2}Cu_3O_{9+{\delta}}$/Ag tapes with J$_c$'s of 9,300 (tape II), 16,700 (tape III) and 25,200 A/cm$^2$ (tape IV)prepared using the powder-in-tube method and an in-situ reaction method, were investigated using scanning electron microscopy and high-resolution transmission electron microscopy, and compared each other. ln the tape preparation, an intermediate rolling process was incorporated during final heat-treatment for the last tape, but not for the rest of the tapes. The microstructural analysis revealed clear differences in grain-texturing, crystallographic defects and impurity phases, depending on the chemical composition of the tape. Tendency of directional grain-alignment increased in an order of tapes I, II III and IV. In tape IV, T1-1223 grains are textured, at least in local regions. In crystallographic defects, while stacking faults were prevalent in the former composition, dislocations and voids were frequently observed in the latter. Also impurity phases were appeared to be more abundant in the former than in the latter. The relationship between 1,and the microstructure in the tapes was attempted to explain in a term of grain-linking.

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Experimental study on nano silica modified cement base grouting reinforcement materials

  • Zhou, Fei;Sun, Wenbin;Shao, Jianli;Kong, Lingjun;Geng, Xueyu
    • Geomechanics and Engineering
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    • v.20 no.1
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    • pp.67-73
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    • 2020
  • With the increasing number of underground projects, the problem of rock-water coupling catastrophe has increasingly become the focus of safety. Grouting reinforcement is gradually applied in subway, tunnel, bridge reinforcement, coal mine floor and other construction projects. At present, cement-based grouting materials are easy to shrink and have low strength after solidification. In order to overcome the special problems of high water pressure and high in-situ stress in deep part and improve the reinforcement effect. In view of the mining conditions of deep surrounding rock, a new type of cement-based reinforcement material was developed. We analyses the principle and main indexes of floor strengthening, and tests and optimizes the indexes and proportions of the two materials through laboratory tests. Then, observes and compares the microstructures of the optimized floor strengthening materials with those of the traditional strengthening materials through scanning electron microscopy. The test results show that 42.5 Portland cement-based grouting reinforcement material has the advantages of slight expansion, anti-dry-shrinkage, high compressive strength and high density when the water-cement ratio is 0.4, the content of bentonite is 4%, and the content of Nano Silica is 2.5%. The reinforcement effect is better than other traditional grouting reinforcement materials.

Facile in situ Formation of CuO/ZnO p-n Heterojunction for Improved H2S-sensing Applications

  • Shanmugasundaram, Arunkumar;Kim, Dong-Su;Hou, Tian Feng;Lee, Dong Weon
    • Journal of Sensor Science and Technology
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    • v.29 no.3
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    • pp.156-161
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    • 2020
  • In this study, hierarchical mesoporous CuO spheres, ZnO flowers, and heterojunction CuO/ZnO nanostructures were fabricated via a facile hydrothermal method. The as-prepared materials were characterized in detail using various analytical methods such as powder X-ray diffraction, micro Raman spectroscopy, X-ray photoelectron spectroscopy, field-emission scanning electron microscopy, and transmission electron microscopy. The obtained results are consistent with each other. The H2S-sensing characteristics of the sensors fabricated based on the CuO spheres, ZnO flowers, and CuO/ZnO heterojunction were investigated at different temperatures and gas concentrations. The sensor based on ZnO flowers showed a maximum response of ~141 at 225 ℃. The sensor based on CuO spheres exhibited a maximum response of 218 at 175 ℃, whereas the sensor based on the CuO/ZnO nano-heterostructure composite showed a maximum response of 344 at 150 ℃. The detection limit (DL) of the sensor based on the CuO/ZnO heterojunction was ~120 ppb at 150 ℃. The CuO/ZnO sensor showed the maximum response to H2S compared with other interfering gases such as ethanol, methanol, and CO, indicating its high selectivity.

Maximizing TPBs through Ni-self-exsolution on GDC based composite anode in solid oxide fuel cells

  • Tan, Je-Wan;Lee, Dae-Hui;Kim, Bo-Gyeong;Kim, Ju-Seon;Mun, Ju-Ho
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.402.1-402.1
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    • 2016
  • The performance of solid oxide fuel cells (SOFCs) is directly related to the electrocatalytic activity of composite electrodes in which triple phase boundaries (TPBs) of metallic catalyst, oxygen ion conducting support, and gas should be three-dimensionally maximized. The distribution morphology of catalytic nanoparticle dispersed on external surfaces is of key importance for maximized TPBs. Herein in situ grown nickel nanoparticle onto the surface of fluorite oxide is demonstrated employing gadolium-nickel co-doped ceria ($Gd0.2-xNixCe0.8O2-{\delta}$, GNDC) by reductive annealing. GNDC powders were synthesized via a Pechini-type sol-gel process while maximum doping ratio of Ni into the cerium oxide was defined by X-ray diffraction. Subsequently, NiO-GNDC composite were screen printed on the both sides of yttrium-stabilized zirconia (YSZ) pellet to fabricate the symmetrical half cells. Electrochemical impedance spectroscopy (EIS) showed that the polarization resistance was decreased when it was compared to conventional Ni-GDC anode and this effect became greater at lower temperature. Ex situ microstructural analysis using scanning electron microscopy after the reductive annealing exhibited the exsolution of Ni nanoparticles on the fluorite phases. The influence of Ni contents in GNDC on polarization characteristics of anodes were examined by EIS under H2/H2O atmosphere. Finally, the addition of optimized GNDC into the anode functional layer (AFL) dramatically enhanced cell performance of anode-supported coin cells.

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Granulation and Characteristics of Sludges in the Combined SHARON/ANAMMOX Processes (SHARON/ANAMMOX 결합공정에서 슬러지의 입상화와 특성)

  • Hwang, In-Su;Min, Kyung-Sok
    • Journal of Korean Society on Water Environment
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    • v.22 no.2
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    • pp.300-307
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    • 2006
  • The combined SHARON (Single reactor system for High ammonium Removal Over Nitrite)-ANAMMOX (Anaerobic ammonium oxidation) reactor were operated in mesophilic condition ($35^{\circ}C$). In this study, microbial granulation and characteristics of SHARON and ANAMMOX sludges were investigated using settling test, Scanning Electron Microscopy (SEM) and Fluorescence In Situ Hybridization (FISH). In SHARON reactor, Aerobic granulation with diameter of 1.5~2.5 mm was accomplished but aerobic granulation was weaker than anaerobic granular sludge. Initial seed sludge of ANAMMOX reactor was used as attached media for biofilm growth. ANAMMOX sludge was more compact and rounder rather than seed sludge. Though ANAMMOX sludge has high activity, it has lower settling ability than the seed granule. The color of ANAMMOX sludge was changed from dark to redish brown granular with diameter of 1~2 mm. In FISH of ANAMMOX sludge, high fraction of Candidatus B. stuttgartiensis which paid great role of nitrogen conversion was detected. Also, FISH results reveals that ANAMMOX bacteria inhabit at inner parts near surface, having advantages in utilization of substrates and protection from oxygen inhibition.

Interaction of Mechanics and Electrochemistry for Magnesium Alloys

  • Han, En-Hou;Wang, JianQiu;Ke, Wei
    • Corrosion Science and Technology
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    • v.7 no.5
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    • pp.243-251
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    • 2008
  • Magnesium alloys become popular research topic in last decade due to its light weight and relatively high strength-to-weight ratio in the energy aspiration age. Almost all structure materials are supposed to suspend stress. Magnesium is quite sensitive to corrosive environment, and also sensitive to environmental assisted cracking. However, so far we have the limited knowledge about the environmental sensitive cracking of magnesium alloys. The corrosion fatigue (CF) test was conducted. Many factors' effects, like grain size, texture, heat treatment, loading frequency, stress ratio, strain rate, chemical composition of environment, pH value, relative humidity were investigated. The results showed that all these factors had obvious influence on the crack initiation and propagation. Especially the dependence of CF life on pH value and frequency is quite different to the other traditional structural metallic materials. In order to interpret the results, the electrochemistry tests by polarization dynamic curve and electrochemical impedance spectroscopy were conducted with and without stress. The corrosion of magnesium alloys was also studied by in-situ observation in environmental scanning electron microscopy (ESEM). The corrosion rate changed with the wetting time during the initial corrosion process. The pre-charging of hydrogen caused crack initiated at $\beta$ phase, and with the increase of wetting time the crack propagated, implying that hydrogen produced by corrosion reaction participated in the process.

Preparation of Honeycomb-patterned Polyaniline-MWCNT/Polystyrene Composite Film and Studies on DC Conductivity

  • Kim, Won-Jung;Huh, Do-Sung
    • Bulletin of the Korean Chemical Society
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    • v.33 no.7
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    • pp.2345-2351
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    • 2012
  • Conductive honeycomb-patterned polystyrene (PS) thin films were prepared by the formation of a polyaniline (PANI) thin layer on the surface of the patterned PS thin films using simple one-step chemical oxidative polymerization of aniline. The in situ chemical oxidation polymerization of aniline hydrochloride solution on the patterned structure of the PS films was conducted in the presence of multiwalled carbon nanotubes (MWCNT) to prepare the PANI-MWCNT/PS composite film. The concentration (wt %) of MWCNT was varied in the range of 1%-3% by weight. The dependence of surface morphology of the PANI/PS and PANI-MWCNT/PS composite film to the polymerization time was observed by scanning electron microscopy. The room temperature DC conductivity was obtained by the four-probe technique. The conductivity of the PANI-MWCNT/PS composite film was affected both by the MWCNT concentration and polymerization time. In addition, DC electrical field was loaded during the oxidative polymerization to affect the distribution of the MWCNT included in the composite film, varying the loading voltage in the range of 0.1-3.0 V. The conductivity of the PANI-MWCNT/PS composite film was increased as loading voltage rose. However, this increase stops at a voltage higher than the critical value.

Incorporation of Montmorillonite/Silica Composite for the Corrosion Protection of an Epoxy Coating on a 2024 Aluminum Alloy Substrate

  • Thai Thu Thuy;Trinh Anh Truc;Pham Gia Vu
    • Corrosion Science and Technology
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    • v.22 no.2
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    • pp.99-107
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    • 2023
  • Layered silicate clay montmorillonite (MMT) has been used in nanocomposite coating to improve corrosion protection by reinforcing the barrier property. The better dispersion of MMT in the coating produces a higher barrier effect. Pretreatment with MMT could favor the delamination of clay platelets, facilitating MMT dispersion in the coating. In the present work, a montmorillonite/silica (MMT/Si) composite was prepared by the in situ sol-gel method. x-ray diffraction measurements and field-emission scanning electron microscopy observations showed silica crystal formation and increased basal spacing between the MMT platelets. Composite MMT/Si particles were introduced in an epoxy resin to reinforce the corrosion protection of the coating applied on the AA2024 surface. Electrochemical impedance spectroscopy (EIS) was performed to characterize the protective property of the coating. The results demonstrated the high barrier effect of the coating containing 5 wt% of MMT/Si. Adhesion evaluation after a salt spray test exhibited a high adherence to the epoxy coating containing MMT/Si.

Synthesis and Properties of Partially Hydrolyzed Acrylonitrile-co-Acrylamide Superabsorbent Hydrogel

  • Pourjavadi, Ali;Hosseinzadeh, Hossein
    • Bulletin of the Korean Chemical Society
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    • v.31 no.11
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    • pp.3163-3172
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    • 2010
  • In this work, a novel method to synthesis of an acrylic superabsorbent hydrogel was reported. In the two stage hydrogel synthesis, first copolymerization reaction of acrylonitrile (AN) and acrylamide (AM) monomers using ammonium persulfate (APS) as a free radical initiator was performed. In the second stage, the resulted copolymer was hydrolyzed to produce carboxamide and carboxylate groups followed by in situ crosslinking of the polyacrylonitrile chains. The results from FTIR spectroscopy and the dark red-yellow color change show that the copolymerization, alkaline hydrolysis and crosslinking reactions have been do take place. Scanning electron microscopy (SEM) verifies that the synthesized hydrogels have a porous structure. The results of Brunauer-Emmett-Teller (BET) analysis showed that the average pore diameter of the synthesized hydrogel was 13.9 nm. The synthetic parameters affecting on swelling capacity of the hydrogel, such as AM/AN weight ratio and hydrolysis time and temperature, were systematically optimized to achieve maximum swelling capacity (330 g/g). The swollen gel strength of the synthesized hydrogels was evaluated via viscoelastic measurements. The results indicated that superabsorbent polymers with high water absorbency were accompanied by low gel strength. The swelling of superabsorbent hydrogels was also measured in various solutions with pH values ranging from 1 to 13. Also, the pH reversibility and on-off switching behavior makes the hydrogel as a good candidate for controlled delivery of bioactive agents. Finally, the swelling of synthesized hydrogels with various particle sizes obey second order kinetics.

Novel Composite Membranes Comprising Silver Salts Physically Dispersed in Poly(ethylene-co-propylene) for the Separation of Propylene/Propane

  • Kim, Jong-Hak;Min, Byoung-Ryul;Kim, Yong-Woo;Kang, Sang-Wook;Won, Jong-Ok;Kang, Yong-Soo
    • Macromolecular Research
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    • v.15 no.4
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    • pp.343-347
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    • 2007
  • Novel composite membranes, which delivered high separation performance for propylene/propane mixtures, were developed by coating inert poly(ethylene-co-propylene) rubber (EPR) onto a porous polyester substrate, followed by the physical distribution of $AgBF_4$. Scanning electron microscopy-wavelength dispersive spectrometer (SEM-WDS) revealed that silver salts were uniformly distributed in the EPR layer. The physical dispersion of the silver salts in the inert polymer matrix, without specific interaction, was characterized by FT-IR and FT-Raman spectroscopy. The high separation performance was presumed to stem from the in-situ dissolution of crystalline silver ionic aggregates into free silver ions, which acted as an active propylene carrier within a propylene environment, leading to facilitated propylene transport through the membranes. The membranes were functional at all silver loading levels, exhibiting an unusually low threshold carrier concentration (less than 0.06 of silver weight fraction). The separation properties of these membranes, i.e. the mixed gas selectivity of propylene/propane ${\sim}55$ and mixed gas permeance ${\sim}7$ GPU, were stable for several days.