• 제목/요약/키워드: in-situ scanning electron microscopy

검색결과 103건 처리시간 0.025초

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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    • 제28권7호
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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.

Surface Coating and Electrochemical Properties of LiNi0.8Co0.15Al0.05O2 Polyaniline Composites as an Electrode for Li-ion Batteries

  • Chung, Young-Min;Ryu, Kwang-Sun
    • Bulletin of the Korean Chemical Society
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    • 제30권8호
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    • pp.1733-1737
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    • 2009
  • A new cathode material based on Li$Ni_{0.8}Co_{0.15}Al_{0.05}O_2$ (LNCA)/polyaniline (Pani) composite was prepared by in situ self-stabilized dispersion polymerization in the presence of LNCA. The materials were characterized by fourier transform infrared spectroscopy (FT-IR), ultraviolet-visible spectroscopy (UV-Vis), X-ray diffraction (XRD), and scanning electron microscopy (SEM). Electrochemical properties including galvanostatic charge-discharge ability, cyclic voltammetry (CV), capacity, cycling performance, and AC impedance were measured. The synthesized LNCA/Pani had a similar particle size to LNCA and exhibited good electrochemical properties at a high C rate. Pani (the emeraldine salt form) interacts with metal-oxide particles to generate good connectivity. This material shows good reversibility for Li insertion in discharge cycles when used as the electrode of lithium ion batteries. Therefore, the Pani coating is beneficial for stabilizing the structure and reducing the resistance of the LNCA. In particular, the LNCA/Pani material has advantageous electrochemical properties.

Fabrication of Fe-TiB2 Composite Powder by High-Energy Milling and Subsequent Reaction Synthesis

  • Khoa, H.X.;Tuan, N.Q.;Lee, Y.H.;Lee, B.H.;Viet, N.H.;Kim, J.S.
    • 한국분말재료학회지
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    • 제20권3호
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    • pp.221-227
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    • 2013
  • $TiB_2$-reinforced iron matrix composite (Fe-$TiB_2$) powder was in-situ fabricated from titanium hydride ($TiH_2$) and iron boride (FeB) powders by the mechanical activation and a subsequent reaction. Phase formation of the composite powder was identified by X-ray diffraction (XRD). The morphology and phase composition were observed and measured by field emission-scanning electron microscopy (FE-SEM) and energy-dispersive X-ray spectroscopy (EDS), respectively. The results showed that $TiB_2$ particles formed in nanoscale were uniformly distributed in Fe matrix. $Fe_2B$ phase existed due to an incomplete reaction of Ti and FeB. Effect of milling process and synthesis temperature on the formation of composite were discussed.

Low temperature wet-chemical synthesis of spherical hydroxyapatite nanoparticles and their in situ cytotoxicity study

  • Mondal, Sudip;Dey, Apurba;Pal, Umapada
    • Advances in nano research
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    • 제4권4호
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    • pp.295-307
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    • 2016
  • The present research work reports a low temperature ($40^{\circ}C$) chemical precipitation technique for synthesizing hydroxyapatite (HAp) nanoparticles of spherical morphology through a simple reaction of calcium nitrate tetrahydrate and di-ammonium hydrogen phosphate at pH 11. The crystallinity of the single-phase nanoparticles could be improved by calcinating at $600^{\circ}C$ in air. Thermogravimetric and differential thermal analysis (TG-DTA) revealed the synthesized HAp is stable up to $1200^{\circ}C$. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) studies confirmed the formation of spherical nanoparticles with average size of $23.15{\pm}2.56nm$ and Ca/P ratio of 1.70. Brunauer-Emmett-Teller (BET) isotherm of the nanoparticles revealed their porous structure with average pore size of about 24.47 nm and average surface area of $78.4m2g^{-1}$. Fourier transform infrared spectroscopy (FTIR) was used to confirm the formation of P-O, OH, C-O chemical bonds. Cytotoxicity and MTT assay on MG63 osteogenic cell lines revealed nontoxic bioactive nature of the synthesized HAp nanoparticles.

Addition of Various Cellulosic Components to Bacterial Nanocellulose: A Comparison of Surface Qualities and Crystalline Properties

  • Bang, Won Yeong;Kim, Dong Hyun;Kang, Mi Dan;Yang, Jungwoo;Huh, Taelin;Lim, Young Woon;Jung, Young Hoon
    • Journal of Microbiology and Biotechnology
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    • 제31권10호
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    • pp.1366-1372
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    • 2021
  • Bacterial nanocellulose (BNC) is a biocompatible material with a lot of potential. To make BNC commercially feasible, improvements in its production and surface qualities must be made. Here, we investigated the in situ fermentation and generation of BNC by addition of different cellulosic substrates such as Avicel and carboxymethylcellulose (CMC) and using Komagataeibacter sp. SFCB22-18. The addition of cellulosic substrates improved BNC production by a maximum of about 5 times and slightly modified its structural properties. The morphological and structural properties of BNC were investigated by using Fourier transform-infrared spectroscopy (FT-IR), scanning electron microscopy and X-ray diffraction. Furthermore, a type-A cellulose-binding protein derived from Clostridium thermocellum, CtCBD3, was used in a novel biological analytic approach to measure the surface crystallinity of the BNC. Because Avicel and CMC may adhere to microfibrils during BNC synthesis or crystallization, cellulose-binding protein could be a useful tool for identifying the crystalline properties of BNC with high sensitivity.

Growth of superconducting $MgB_2$ fibers for wire applications

  • Kim J. H.;Yoon H. R.;Jo W.
    • 한국초전도ㆍ저온공학회논문지
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    • 제7권4호
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    • pp.1-3
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    • 2005
  • Superconducting $MgB_2$ fibers are in-situ grown by a diffusion method. The fibers are prepared by exposing B filaments to Mg vapor inside a folded Ta foil over a wide range of temperature and growth time. The materials are sealed inside a quartz tube by gas welding. The as - grown fibers are characterized by scanning electron microscopy and energy dispersive x - ray analysis. The fibers have a diameter of about $110{\mu}m$. Surface morphology of the fibers looks dependent on growth temperature and mixing ratio of Mg and B. Radial distribution of Mg ions into B is observed and analyzed over the cross - sectional area. Transport properties of the $MgB_2$ fibers are examined by a physical property measurement system. The $MgB_2$ fibers grown at $900^{\circ}C$ for 2 hours show a superconducting transition at 39.8K with ${\Delta}T_c<$ 2.0 K. Resistance at room temperature $MgB_2$ is 3.745 $\Omega$ and residual resistivity ratio (RRR) is estimated as 4.723.

아크 방전법으로 성장된 대면적 단일벽 탄소나노튜브 필름 (Single Wall Carbon Nanotube Films Produced by Arc Discharge)

  • 강영진;오동훈;송혜진;정진연;정혁;조유석;김도진
    • 한국재료학회지
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    • 제18권5호
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    • pp.253-258
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    • 2008
  • A simple method to deposit carbon nanotube films uniformly on large area substrates using an arc discharge method is reported in this paper. The arc discharge method was modified to deposit carbon nanotube films in situ on the substrates. The substrates were scanned several times over the arcing point for a uniform film thickness. Deposition was carried out under variable dc bias conditions at 600 torr of $H_2$ gas. The thickness uniformity of the single-wall carbon nanotube films as characterized by a four-point probe was within 30% deviation. The morphology and crystal quality of the single-wall carbon nanotube film were also characterized by field emission scanning electron microscopy and Raman spectroscopy.

Effects of Sputter Parameters on Electrochromic Properties of Tungsten Oxide Thin Films Grown by RF Sputtering

  • Nah, Yoon-Chae
    • 한국재료학회지
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    • 제21권12호
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    • pp.703-707
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    • 2011
  • The electrochromic properties of tungsten oxide films grown by RF sputtering were investigated. Among the sputter parameters, first the $Ar:O_2$ ratios were controlled with division into only an $O_2$ environment, 1:1 and 4:1. The structure of each film prepared by these conditions was studied by X-ray diffraction, X-ray photoelectron spectroscopy and Rutherford backscattering spectroscopy. The sputter-deposited tungsten oxide films had an amorphous structure regardless of the $Ar:O_2$ ratios. The chemical compositions, however, were different from each other. The stoichiometric structure and low-density film was obtained at higher $O_2$ contents. Electrochemical tests were performed by cyclic voltammetry and chronoamperometry at 0.05 M $H_2SO_4$ solutions. The current density and charge ratio was estimated during the continuous potential and pulse potential cycling at -0.5 V and 1.8 V, respectively. The film grown in a higher oxygen environment had a higher current density and a reversible charge reaction during intercalation and deintercalation. The in-situ transmittance tests were performed by He-Ne laser (633 nm). At higher oxygen contents, a big transmittance difference was observed but the response speed was too slow. This was likely caused by higher film resistivity. Furthermore, the effect of sputtering pressure was also investigated. The structure and surface morphology of each film was observed by X-ray diffraction and scanning electron microscopy. A rough surface was observed at higher sputtering pressure, and this affected the higher transmittance difference and coloration efficiency.

Effects of Micronization on the In situ and In vitro Digestion of Cereal Grains

  • McAllister, T.A.;Sultana, H.
    • Asian-Australasian Journal of Animal Sciences
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    • 제24권7호
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    • pp.929-939
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    • 2011
  • The effects of micronization on in situ and in vitro nutrient disappearances of wheat, barley and corn were investigated in a series of experiments. In Experiment 1, chemical composition and in situ dry matter disappearance (DMD) of six varieties of wheat were determined. In addition, an in vitro study was completed using ground micronized and unmicronized wheat (var. Kansas). In Experiment 2, three varieties of wheat (Kansas, Sceptre and Laura) and in Experiment 3, three cereal grains (wheat, barley and corn) were either micronized for 1 min to attain internal kernel temperatures of 90-100$^{\circ}C$ or not (controls), and DM, protein and starch disappearances were estimated. In Experiment 2, an in vitro study was also completed using ground micronized and unmicronized wheat (var. Kansas). Wheat samples varied with respect to crude protein (10.0-21.2%), starch (61.6-73.9%), NDF (8.5-11.8%), volume weight (753-842 g/L) and kernel hardness (0.0-32.0). Rate (p = 0.003) and extent (p = 0.001) of in situ DMD differed among wheat varieties. Correlations between in situ kinetics, and chemical and physical properties of wheat varieties showed that protein content was negatively correlated with the rate of disappearance ($r^2$ = -0.77). Micronization of all grains markedly reduced (p = 0.001) the rate and extent of DM, and protein disappearances as compared to control samples. Micronization increased (p<0.05) the digestion of starch in wheat. However, release of ammonia into the incubation medium was markedly reduced (p<0.05), suggesting that micronization increased the resistance of protein to microbial digestion. Disappearances of DM, protein and starch differed (p = 0.001) among cereal grains with wheat>barley>corn. Micronization reduced the rate of DM disappearance (p = 0.011) and slowly degradable protein fractions (p = 0.03), however, increased (p = 0.004) slowly degradable starch fractions of all three cereals. Examination of in situ samples by scanning electron microscopy confirmed that microbial colonization focused on starch granules in micronized grains, and that the protein matrix exhibited resistance to microbial colonization. These results suggest that micronization may be used to increase the ruminal escape value of protein in cereal grains, but may lead to increased starch digestion if grains are finely ground.

R.F Magnetron Sputtering법으로 제조한 TiO2 박막의 특성 (Characteristics of TiO2 Thin Films Fabricated by R.E, Magnetron Sputtering)

  • 추용호;최대규
    • 한국재료학회지
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    • 제14권11호
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    • pp.821-827
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    • 2004
  • Titanium oxide thin films were prepared on Si(100) substrates by R.F. magnetron reactive sputtering at $30\sim200watt$ R.F power range, and annealed at $600^{\circ}C\sim800^{\circ}C$ for 1 hour. The properties of $TiO_2$ thin films were analyzed using x-ray, ${\alpha}-step$, ellipsometer, scanning electron microscopy, and FT-IR spectrometer. Upon in-situ depositions, the initial phase of $TiO_2$ thin film showed non-crystalline phase at R.F. power $30\sim100$ watt. The crosssection of $TiO_2$ thin films were sbserved to be the columnar structure. With the increasing R.F power and annealing temperature, the grain size, crystallinity, refractive index, and void size of titanium oxides showed a tended to increase. The FT-IR transmittance spectra of titanium oxide thin films have the obsorption band of Ti-O bond, Si-O bond, Si-O-Ti bond and O-H bond. With the increase of R.F. power and annealing temperature, these films have the stronger bond structures. It is considered that such a phenomena is due to phase transition and good crystallinity