• Title/Summary/Keyword: Field emission scanning electron microscopy

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Preparation and Characterization of Cellulose Nanofibril/Polyvinyl Alcohol Composite Nanofibers by Electrospinning

  • Park, Byung-Dae;Um, In Chul;Lee, Sun-Young;Dufresne, Alain
    • Journal of the Korean Wood Science and Technology
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    • v.42 no.2
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    • pp.119-129
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    • 2014
  • This work undertook to prepare nanofibers of cellulose nanofibrils (CNF)/polyvinyl alcohol (PVA) composite by electrospinning, and characterize the electrospun composite nanofibers. Different contents of CNFs isolated from hardwood bleached kraft pulp (HW-BKP) by 2,2,6,6-tetramethylpiperidine-1-oxy radical (TEMPO)-mediated oxidation were suspended in aqueous polyvinyl alcohol (PVA) solution, and then electrospun into CNF/PVA composite nanofibers. The morphology and dimension of CNFs were characterized by transmission electron microscopy (TEM), which revealed that CNFs were fibrillated form with the diameter of about $7.07{\pm}0.99$ nm. Morphology of the electrospun nanofiber observed by field-emission scanning electron microscopy (FE-SEM) showed that uniform CNF/PVA composite nanofibers were manufactured at 1~3% CNF contents while many beads were observed at 5% CNF level. Both the viscosity of CNF/PVA solution and diameter of the electrospun nanofiber decreased with an increase in CNF content. The diameter and its distribution of the electrospun nanofibers helped explain the differences observed in their morphology. These results show that the electrospinning method was successful in preparing uniform CNF/PVA nanofibers, indicating a great potential for manufacturing consistent and reliable cellulose-based nanofibrils for scaffolds in future applications.

Structural Variation of Diamond-like Carbon Thin Film According to the Annealing Temperature (열처리온도에 따른 다이아몬드상 카본박막의 구조적 특성변화)

  • Choi Won-Seok;Park Mun-Gi;Hong Byung-You
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.19 no.8
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    • pp.701-706
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    • 2006
  • In addition to its similarity to genuine diamond film, diamond-like carbon (DLC) film has many advantages, including its wide band gap and variable refractive index. In this study, DLC films were prepared by the RF PECVD (Plasma Enhanced Chemical Vapor Deposition) method on silicon substrates using methane $(CH_4)$ and hydrogen $(H_2)$ gas. We examined the effects of the post annealing temperature on the structural variation of the DLC films. The films were annealed at temperatures ranging from 300 to $900^{\circ}C$ in steps of $200^{\circ}C$ using RTA equipment in nitrogen ambient. The thickness of the film and interface between film and substrate were observed by surface profiler, field emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM), respectively. Raman and X-ray photoelectron spectroscopy (XPS) analysis showed that DLC films were graphitized ($I_D/I_G$, G-peak position and $sp^2/sp^3$ increased) ratio at higher annealing temperature. The variation of surface as a function of annealing treatment was verified by a AFM and contact angle method.

SUSCEPTIBILITY OF ALLOY 690 TO STRESS CORROSION CRACKING IN CAUSTIC AQUEOUS SOLUTIONS

  • Kim, Dong-Jin;Kim, Hong Pyo;Hwang, Seong Sik
    • Nuclear Engineering and Technology
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    • v.45 no.1
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    • pp.67-72
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    • 2013
  • Stress corrosion cracking (SCC) behaviors of Alloy 690 were studied in lead-containing aqueous alkaline solutions using the slow strain rate tension (SSRT) tests in 0.1M and 2.5M NaOH with and without PbO at $315^{\circ}C$. The side and fracture surfaces of the alloy were then examined using scanning electron microscopy after the SSRT test. Microstructure and composition of the surface oxide layer were analyzed by using a field emission transmission electron microscopy, equipped with an energy dispersive X-ray spectroscopy. Even though Alloy 690 was almost immune to SCC in 0.1M NaOH solution, irrespective of PbO addition, the SCC resistance of Alloy 690 decreased in a 2.5M NaOH solution and further decreased by the addition of PbO. Based on thermodynamic stability and solubility of oxide, high Cr of 30wt% in the Alloy 690 is favorable to SCC in mild alkaline and acidic solutions whereas the SCC resistance of high Cr Alloy 690 is weakened drastically in the strong alkaline solution where the oxide is not stable any longer and solubility is too high to form a passive oxide locally.

Glycothermal Synthesis and Characterization of 3Y-TZP Nanoparticles

  • Song, Jeong-Hwan;Lee, Ju-Hee
    • Korean Journal of Materials Research
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    • v.19 no.8
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    • pp.412-416
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    • 2009
  • In this study, 3 mol% yttria-tetragonal zirconia polycrystal (3Y-TZP) nanoparticles were synthesized by the glycothermal method under various reaction temperatures and times. The co-precipitated precursor of 3Y-TZP was prepared by adding $NH_4OH$ to starting solutions, and then the mixtures were placed in an autoclave reactor. Tetragonal yttria-doped zirconia nanoparticles were afforded through a glycothermal reaction at a temperature as low as $220^{\circ}C$, using co-precipitated gels of $ZrCl_4$ and $YCl_3{\cdot}6H_2O$ as precursors and 1,4-butanediol as the solvent. The synthesized 3Y-TZP particles were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and Raman spectroscopy. The 3Y-TZP particles have a stable tetragonal phase only at glycothermal temperatures above $200^{\circ}C$. To investigate phase transition, the 3Y-TZP particles were heat treated from 400 to $1400^{\circ}C$ for 2 h. Raman analysis indicated that, after heat treatment, the tetragonal phase of the 3Y-TZP particles remained stable. The results of this study, therefore, suggest that 3Y-TZP powders can be prepared by the glycothermal method.

Fabrication of Core-Shell Structured Ni-Based Alloy Nanopowder by Electrical Wire Explosion Method

  • Lee, A-Young;Lee, Gwang-Yeob;Oh, Hye-Ryeong;Kim, Hyeon-Ah;Kim, Song-Yi;Lee, Min-Ha
    • Journal of Powder Materials
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    • v.23 no.6
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    • pp.409-413
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    • 2016
  • Electrical wire explosion in liquid media is a promising method for producing metallic nanopowders. It is possible to obtain high-purity metallic nanoparticles and uniform-sized nanopowder with excellent dispersion stability using this electrical wire explosion method. In this study, Ni-Fe alloy nanopowders with core-shell structures are fabricated via the electrical explosion of Ni-Fe alloy wires 0.1 mm in diameter and 20 mm in length in de-ionized water. The size and shape of the powders are investigated by field-emission scanning electron microscopy, transmission electron microscopy, and laser particle size analysis. Phase analysis and grain size determination are conducted by X-ray diffraction. The result indicate that a core-shell structured Ni-Fe nanopowder is synthesized with an average particle size of approximately 28 nm, and nanosized Ni core particles are encapsulated by an Fe nanolayer.

Synthesis of TiO2 Nanowires by Thermal Oxidation of Titanium Alloy Powder (타이타늄 합금 분말의 열적산화를 통한 TiO2 나노와이어의 합성)

  • Kim, Yoo-Young;Cho, Kwon-Koo
    • Journal of Powder Materials
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    • v.25 no.1
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    • pp.48-53
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    • 2018
  • One-dimensional rutile $TiO_2$ is an important inorganic compound with applicability in sensors, solar cells, and Li-based batteries. However, conventional synthesis methods for $TiO_2$ nanowires are complicated and entail risks of environmental contamination. In this work, we report the growth of $TiO_2$ nanowires on a Ti alloy powder (Ti-6wt%Al-4wt%V, Ti64) using simple thermal oxidation under a limited supply of $O_2$. The optimum condition for $TiO_2$ nanowire synthesis is studied for variables including temperature, time, and pressure. $TiO_2$ nanowires of ${\sim}5{\mu}m$ in length and 100 nm in thickness are richly synthesized under the optimum condition with single-crystalline rutile phases. The formation of $TiO_2$ nanowires is greatly influenced by synthesis temperature and pressure. The synthesized $TiO_2$ nanowires are characterized using field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), and high-resolution transmission electron microscopy (HR-TEM).

Mesoporous Assembly of Layered Titanate with Well-Dispersed Pt Cocatalyst

  • Jung, Tae-Sung;Kim, Tae-Woo;Hwang, Seong-Ju
    • Bulletin of the Korean Chemical Society
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    • v.30 no.2
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    • pp.449-453
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    • 2009
  • A mesoporous assembly of layered titanate with well-dispersed Pt cocatalysts has been synthesized via a restacking of exfoliated titanate nanosheets and a simultaneous adsorption of Pt nanoparticles. According to powder X-ray diffraction analysis, the obtained mesoporous assembly shows amorphous structure corresponding to the disordered stacking of layered titanate crystallites. Field emission-scanning electron microscopy and $N_2$ adsorption-desorption isotherm measurement clearly demonstrate the formation of mesoporous structure with expanded surface area due to the house-of-cards type stacking of the titanate crystallites. From high resolution-transmission electron microscopy and elemental mapping analyses, it is found that Pt nanoparticles with the size of ~2.5 nm are homogeneously dispersed in the mesoporous assembly of layered titanate. In comparison with the protonated titanate, the present mesoporous assembly of layered titanate exhibits better photocatalytic activity for the photodegradation of organic molecules. This finding underscores that the restacking of exfoliated nanosheets is quite useful not only in creating mesoporous structure but also in improving the photocatalytic activity of titanium oxide.

Novel Fabrication of CdS Hollow Spheres Induced by Self-assembled Process

  • Choi, Kyoung-Hoon;Chae, Weon-Sik;Jung, Jin-Seung;Kim, Yong-Rok
    • Bulletin of the Korean Chemical Society
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    • v.30 no.5
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    • pp.1118-1120
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    • 2009
  • Micro-size CdS spheres of hollow shape were fabricated through the self-assembly of high density arrow-like nanorods. The synthesis of the CdS hollow spheres were accomplished in an aqueous solution of cadmium nitrate and triblock copolymer (Pluronic P123) at low temperature (80 ${^{\circ}C}$) through the slow release of S2- ions from thioacetamide. Morphology of the fabricated CdS hollow spheres was characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). The results indicate that the arrow-like CdS nanorods are simultaneously grown and attached each other to form the building units that become the spheres with hollow inside as a self-assembled process. The CdS spheres have a diameter of $2{\sim}3 {\mu}m$ and consist of the nanorods with a length of$\sim$800 nm. The nanocrystal building blocks have a hexagonal CdS structure.

γ-ray Radiation Induced Synthesis and Characterization of α-Cobalt Hydroxide Nanoparticles

  • Kim, Sang-Wook;Kwon, Bob-Jin;Park, Jeong-Hoon;Hur, Min-Goo;Yang, Seung-Dae;Jung, Hyun
    • Bulletin of the Korean Chemical Society
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    • v.31 no.4
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    • pp.910-914
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    • 2010
  • A novel synthetic route has been developed to prepare $\alpha$-cobalt hydroxide with intercalated nitrate anions. It was successfully synthesized by $\gamma$-ray irradiation under simple conditions, i.e., air atmosphere, without base. Under $\gamma$-ray irradiation, it leads to the formation of layered cobalt hydroxynitrate compounds which have small crystalline size and have the role of a generator of hydroxyl anion. Structural and morphological characterizations were performed by using power X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and high resolution transmission electron microscopy (HR-TEM). The component and thermal stability of the sample were respectively measured by Fourier transform infrared (FT-IR) spectroscopy, elemental analysis, and thermal analyses, including thermogravimetry (TG) and differential thermal analysis (DTA).

Synthesis of Mesoporous TiO2 and Its Application to Photocatalytic Activation of Methylene Blue and E. coli

  • Kim, Eun-Young;Kim, Dong-Suk;Ahn, Byung-Tae
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.193-196
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    • 2009
  • Mesoporous $TiO_2$ material was synthesized from diblock copolymers with ethylene oxide chains via a sol-gel process in aqueous solution. The properties of these materials were characterized with several analytical techniques including field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), wide angle X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) analysis, and Barrett-Joyner-Halenda (BJH) analysis. The mesoporous $TiO_2$ materials calcined at 400${^{\circ}C}$ were found to have specific surface areas 212 $m^2g^-1$, average pore sizes 6.2 nm, and their average crystal sizes were found to be 8.2 nm. The photocatalytic activity of mesoporous $TiO_2$ was characterized with UV-Vis spectroscopy, and it was found to be 5.8 times higher than that of Degussa P25 $TiO_2$ (P25). For deactivation of Escherichia coli, mesoporous $TiO_2$ also has high photocatalytic inactivity than that of P25. Such a high photocatalytic activity is explained with large surface area and small crystal size with wormhole-like mesoporous structure.