• Title/Summary/Keyword: in-situ SEM

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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.

Preparation of Pore-filled Anion-exchange Membrane with PVDF and Poly(vinylbenzylchloride)

  • Park, Byungkyu;Byungpyo Hong;Kwangsoo Yu;Hongsik Byun
    • Proceedings of the Membrane Society of Korea Conference
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    • 2004.05a
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    • pp.207-210
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    • 2004
  • The pore-filled anion-exchange membranes were prepared in this study with an asymmetric poly(vinylidene fluoride)(PVDF) membrane as a nascent membrane and poly(vinylbenzyl chloride)(PVBCl) as a polyelectrolyte. The solution of PVBCI having the chloromethylate aryl ring of 80 percents and 1,4-diaminobicyclo [2,2,2]octane(DABCO) was made with the solvent of tetrahydrofuran(THF) and N,N-Dimethylformamide(DMF), which is in the rotio of 8:2. A new preparation method in this study, i.e. in-situ crosslinking, enabled us to produce the pore-filled membranes without change of size, and to control the properties of final membrane with various degree of cross-linking. From the result of surface morphologies of SEM and AFM the polyelectrolyte exists in the pores of nascent membrane as a certain configuration. From the investigation of the solvent affecting much to the permeability and rejection, it was found. that the membranes using DMF and THF showed better performances than the membranes produced by THF only. The water permeability of the final membrane at low pressure(100㎪) showed a typical ultrafiltation membrane's permeability (8-10kg/㎡hr) and good values of rejection(55∼60 percent).

Electrochemical and surface investigations of copper corrosion in dilute oxychloride solution

  • Gha-Young Kim ;Junhyuk Jang;Jeong-Hyun Woo;Seok Yoon;Jin-Seop Kim
    • Nuclear Engineering and Technology
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    • v.55 no.8
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    • pp.2742-2746
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    • 2023
  • The corrosion behavior of copper immersed in dilute oxychloride solution (100 mM) was studied through surface investigation and in-situ monitoring of open-circuit potential. The copper corrosion was initiated with copper dissolution into a form of CuCl-2, resulting in mass decrease within the first 40 h of immersion. This was followed by a hydrolysis reaction initiated by the CuCl-2 at the copper surface, after which oxide products were formed and deposited on the surface, resulting in a mass increase. The formation of nucleation sites for copper oxide and its lateral extension during the corrosion process were examined using focused ion beam (FIB)-scanning electron microscopy (SEM). The presence of metastable compounds such as atacamite (CuCl2·3Cu(OH)2) on the corroded copper surface was revealed by X-ray photoelectron spectra (XPS) and transmission electron microscopy (TEM)-energy dispersive spectrometry (EDS) analysis.

Preparation and characterization of nanoflake composite multi core-shell SrFe12O19/Fe3O4/PEG/PPy

  • Hosseini, Seyed Hossein;Majidpour diz, Mohammad
    • Advances in materials Research
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    • v.1 no.2
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    • pp.161-168
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    • 2012
  • Nanoflake composite multi core-shell $SrFe_{12}O_{19}/Fe_3O_4$/PEG/Polypyrrole was synthesized by in situ polymerization method. In this paper, the fabrication of $SrFe_{12}O_{19}$ nanoflake is as first core by solgel method. Then fabricated a shell layer from magnetic nanoparticles of $Fe_3O_4$, which synthesized by coprecipitation technique, onto the $SrFe_{12}O_{19}$ nanoflake. Polyethylene glycol (PEG) as a polymer layer and as second shell was coated onto the before core-shell. Than core-shell $SrFe_{12}O_{19}/Fe_3O_4$/PEG was used as template for the preparation of $SrFe_{12}O_{19}/Fe_3O_4$/PEG/Polypyrrole composite. Final composite has a conductive property among $4.23{\times}10^{-2}Scm^{-1}$ and magnetic property about $M_s$=2.99 emu/g. Also final composite in soluble at organic solvent such as DMF and DMSO and has a flake structure. Conductivity and magnetic property respectively determine by four-probe instrument and vibrant sample magnetometer (VSM), morphology and article size determined by FE-SEM, TEM and XRD.

Electrorheology of conducting polyaniline-$BaTiO_3$ composite

  • Kim Ji-Hye;Fang Fei Fei;Lee Ki-Bo;Choi Hyoung-Jin
    • Korea-Australia Rheology Journal
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    • v.18 no.2
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    • pp.103-107
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    • 2006
  • Organic-inorganic composite of polyaniline and barium titanate (PANI-$BaTiO_3$) was synthesized via an in-situ oxidation polymerization of aniline in the presence of barium titanate ($BaTiO_3$) nanoparticles dispersed in an acidic medium. Barium titanate has large electric resistance and relatively high dielectric constant which is one of the essential properties for its electrorheological (ER) applications. The microstructure and composition of the obtained PANI/$BaTiO_3$ composite were characterized by SEM, FT-IR and XRD. In addition, we also employed a rotational rheometer to investigate the rheological performance of the ER fluids based on both pure PANI particle and PANI/$BaTiO_3$ composite. It was found that the composite materials possess much higher yield stresses than the pristine PANI due to unique dielectric properties of the inorganic $BaTiO_3$ particles. Finally, we also examined dynamic yield stress by analyzing its extrapolated yield stress data as a function of electric field strengths. Using the critical electric field strengths deduced, we further found that the universal yield stress equation collapses their data onto a single curve.

Effect of Oxygen Annealing on the Structural and Optical Properties of Sputter-deposited Vanadium Oxide Thin Films (스퍼터링으로 퇴적시킨 바나듐 산화막의 구조적, 광학적 특성에 미치는 산소 어닐링의 효과)

  • 최복길;최창규;김성진
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.13 no.12
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    • pp.1003-1010
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    • 2000
  • Thin films of vanadium oxide(VOx) have been deposited by r.f. magnetron sputtering from V$_2$O$\_$5/ target in gas mixture of argon and oxygen. Crystal structure, surface morphology, chemical composition, molecular structure and optical properites of films in-situ annealed in O$_2$ambient with various heat-treatment conditions are characterized through XRD, SEM, AES, RBS, RTIR and optical absorption measurements. The films annealed below 200$\^{C}$ are amorphous, and those annealed above 300$\^{C}$ are polycrystalline. The growth of grains and the transition of vanadium oxide into the higher oxide have been observed with increasing the annealing temperature and time. The increase of O/V ratio with increasing the annealing temperature and time is attributed to the diffusion of oxygen and the partial filling of oxygen vacancies. It is observed that the oxygen atoms located on the V-O plane of V$_2$O$\_$5/ layer participate more readily in the oxidation process. Also indirect and direct optical band gaps were increased with increasing the annealing temperature and time.

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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.

Preparation, Characterization and Low Frequency a.c. Conduction of Polypyrrole-Lead Titanate Composites

  • Basavaraja, C.;Choi, Young-Min;Park, Hyun-Tae;Huh, Do-Sung;Lee, Jae-Wook;Revanasiddappa, M.;Raghavendra, S.C.;Khasim, S.;Vishnuvardhan, T.K.
    • Bulletin of the Korean Chemical Society
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    • v.28 no.7
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    • pp.1104-1108
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    • 2007
  • Conducting Polypyrrole-lead titanate (PPy/PbTiO3) composites have been prepared by in situ deposition technique by placing different wt.% of fine grade powder of PbTiO3 (10, 20, 30, 40, and 50%) during polymerization of pyrrole. The composites formed were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA), and these data indicate that PbTiO3 particles are dominating with an increase in crystallinity as well as thermal stability of the composites. The results on the low frequency dielectric studies which are obtained in the form of pressed pellet state are interpreted in terms of Maxwell Wagner polarization, which are responsible for the dielectric relaxation mechanism and frequency dependence of conductivity.

High Electrical Current Stressing Effects on the Failure Mechanisms of Austudbumps/ACFFlip Chip Joints (고전류 스트레싱이 금스터드 범프를 이용한 ACF 플립칩 파괴 기구에 미치는 영향)

  • Kim Hyeong Jun;Gwon Un Seong;Baek Gyeong Uk
    • Proceedings of the International Microelectronics And Packaging Society Conference
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    • 2003.11a
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    • pp.195-202
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    • 2003
  • In this study, failure mechanisms of Au stud bumps/ACF flip chip joints were investigated underhigh current stressing condition. For the determination of allowable currents, I-V tests were performed on flip chip joints, and applied currents were measured as high as almost 4.2Amps $(4.42\times10^4\;Amp/cm^2)$. Degradation of flip chip joints was observed by in-situ monitoring of Au stud bumps-Al pads contact resistance. All failures, defined at infinite resistance, occurred at upward electron flow (from PCB pads to chip pads) applied bumps (UEB). However, failure did not occur at downward electron flow applied bumps (DEB). Only several $m\Omega$ contact resistance increased because of Au-Al intermetallic compound (IMC) growth. This polarity effect of Au stud bumps was different from that of solder bumps, and the mechanism was investigated by the calculation of chemical and electrical atomic flux. According to SEM and EDS results, major IMC phase was $Au_5Al_2$, and crack propagated along the interface between Au stud bump and IMC resulting in electrical failures at UEB. Therefore. failure mechanisms at Au stud bump/ACF flip chip Joint undo high current density condition are: 1) crack propagation, accompanied with Au-Al IMC growth. reduces contact area resulting in contact resistance increase; and 2) the polarity effect, depending on the direction of electrons. induces and accelerates the interfacial failure at UEBs.

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Influence of in-situ remote plasma treatment on characteristics of amorphous indium gallium zinc oxide thin film-based transistors

  • Gang, Tae-Seong;Gu, Ja-Hyeon;Hong, Jin-Pyo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.02a
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    • pp.257-257
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    • 2011
  • The amorphous indium-gallium-zinc-oxide (a-IGZO) materials for use in high performance display research fields are strongly investigated due to its good performance, such as high mobility and better transparency. However, the stability of a-IGZO materials is increasingly becoming one of critical issues due to the sub-gap electron trap sites induced by rough interfaces during deposition processing. It is well-known that the threshold voltage shift is related to interface roughness and oxygen vacancy formed by breaking weak chemical bonds. Here, we report the better properties of transparent oxide transistors by reducing the threshold voltage shift with an external rf plasma supported magnetron sputtering system. Mainly, our sputtering method causes the surface of sample to be sleek, so that it prevents the formation of various defects, such as shallow electron trap sites in the interface. External rf power was applied from 0 to 50W during RF sputtering process to enhance the stability of our oxide transistor without having a large voltage shift. To observe the effects of external rf-plasma source on the properties of our devices, Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), Transmission Electron Microscopy (TEM) are carried out to observe surface roughness and morphology of sputtered thin film. In addition, typical electrical properties, such as I-V characteristics are analyzed.

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