• Korean Journal of Materials Research
• /
• v.23 no.5
• /
• pp.260-265
• /
• 2013

Silicon nanoparticle is a promising material for electronic devices, photovoltaics, and biological applications. Here, we synthesize silicon nanoparticles via $CO_2$ laser pyrolysis and study the hydrogen flow effects on the characteristics of silicon nanoparticles using high resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), and UV-Vis-NIR spectrophotometry. In $CO_2$ laser pyrolysis, used to synthesize the silicon nanoparticles, the wavelength of the $CO_2$ laser matches the absorption cross section of silane. Silane absorbs the $CO_2$ laser energy at a wavelength of $10.6{\mu}m$. Therefore, the laser excites silane, dissociating it to Si radical. Finally, nucleation and growth of the Si radicals generates various silicon nanoparticle. In addition, researchers can introduce hydrogen gas into silane to control the characteristics of silicon nanoparticles. Changing the hydrogen flow rate affects the nanoparticle size and crystallinity of silicon nanoparticles. Specifically, a high hydrogen flow rate produces small silicon nanoparticles and induces low crystallinity. We attribute these characteristics to the low density of the Si precursor, high hydrogen passivation probability on the surface of the silicon nanoparticles, and low reaction temperature during the synthesis.

• Journal of Magnetics
• /
• v.13 no.4
• /
• pp.149-152
• /
• 2008

In this report, we present the results of a study on the effects of the particle size on the properties of the Prussian blue (PB) analog $Na_xMn_y[Fe(CN){_6}]$. A novel synthesis method of the $Na_xMn_y[Fe(CN){_6}]$ nano-particles using an organic solvent, formamide, is employed. The size of the PB particles is found to be 100-150 nm for the samples prepared in the formamide solvent, which is much smaller than that of the samples prepared using water only. The broadening of the X-ray diffraction peaks of the nano-sized PB samples is attributed to the lattice disorder and a dramatic reduction in the particle size. The compositions of the samples are confirmed by an energy-dispersive X-ray analysis (EDAX), and the result proves that the samples are actually $Na_xMn_y[Fe(CN){_6}]$ Prussian blue. The UV-vis spectra show a broad intervalence charge-transfer (CT) band in the visible region between 400 and 700 nm, and the absorption decreases abruptly in the green region for the nano-sized PB sample. A divergence between the field cooled (FC) and zero field cooled (ZFC) magnetization curves is observed for the nano-sized PB sample at 11 K, indicating that nanoparticles in the sample are single domain superparamagnets with a blocking temperature of 11 K. Our results reveal that the nano-sized PB samples show significantly different optical and magnetic properties than those of the bulk PB samples.

• Polymer(Korea)
• /
• v.38 no.5
• /
• pp.632-639
• /
• 2014

2,7-Dihydroxynaphthalene bis(trimellitate anhydride) (2,7-TA) was synthesized from trimellitic anhydride chloride and 2,7-dihydroxynaphthalene. Copolyimides (Co-PI) containing ester group were synthesized from 2,7-TA, pxylylenediamine, and 2,2'-bis(trifluoromethyl)benzidine (TFB). The Co-PI films were obtained from poly(amic acid) by solution casting through thermal imidization on a glass plate. The thermal property, gas permeation, and optical transparency of the Co-PI films with various TFB monomer contents were investigated. These Co-PIs could be solution-cast into a flexible and tough film. The cast Co-PI films exhibited high optical transparency with a cut-off wavelength of 370~395 nm in UV-vis. absorption and a low yellow index value of 3.55~7.63. The thermal property of Co-PI films increased linearly with increasing TFB content. However, the oxygen permeation and optical transparency of the Co-PI films was found to worsen with increasing TFB content.

• Bulletin of the Korean Chemical Society
• /
• v.35 no.4
• /
• pp.1182-1190
• /
• 2014

$Cd_{1-x}Zn_xS$-sensitized $K_4Nb_6O_{17}$ composite photocatalysts (designated $Cd_{1-x}Zn_xS/K_4Nb_6O_{17}$) were prepared via a simple deposition-precipitation method. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectrometry (EDS), $N_2$ sorption, ultraviolet-visible light diffuse reflectance spectroscopy (UV-Vis DRS), photoluminescence measurements (PL), and X-ray photoelectron spectroscopy (XPS). The $Cd_{0.8}Zn_{0.2}S$ particles were scattered on the surface of $K_4Nb_6O_{17}$, and had a relatively uniform size distribution around 50 nm. The absorption edge of $K_4Nb_6O_{17}$ was shifted to the visible light region and the recombination of photo-generated electrons and holes suppressed after $Cd_{0.8}Zn_{0.2}S$ loading. The $Cd_{0.8}Zn_{0.2}S$(25 wt %)/$K_4Nb_6O_{17}$ composite possessed the highest photocatalytic activity for hydrogen production under visible light irradiation, evolving 8.278 mmol/g in 3 h. Recyclability tests were performed, and the composite photocatalysts were found to be fairly stable. The mechanism of charge separation between the photogenerated electrons and holes at the $Cd_{0.8}Zn_{0.2}S/K_4Nb_6O_{17}$ composite was discussed.

• Bulletin of the Korean Chemical Society
• /
• v.28 no.1
• /
• pp.33-40
• /
• 2007

We have designed and synthesized three Zn(II)-porphyrin derivatives, such as Zn(II) porphyrin ([G-0]Zn-P1) and aryl ether-typed dendron substituted Zn(II)-porphyrin derivatives ([G-1]Zn-P1 and [G-1]Zn-P-CN1). Their chemical structures were characterized by 1H-NMR, FT-IR, UV-vis absorption, EI-mass, and MALDI-TOF mass spectroscopies. Their electrochemical properties were studied by cyclic voltammetry measurement. These Zn(II)-porphyrin derivatives have been used to fabricate dye-sensitized solar cells (DSSCs) based on solid polymeric electrolytes as dye sensitizers and their device performances were evaluated by comparing with that of a standard Ru(II) complex dye. [G-1]Zn-P-CN1 showed the enhanced power conversion efficiency than those of other porphyrin derivatives, as expected. Short-circuit photocurrent density (Jsc), open-circuit voltage (Voc), fill factor (FF), and power conversion efficiency (η) of solid-typed DSSC for [G-1]Zn-P-CN1 were evaluated to be Jsc = 11.67 mA/cm2, Voc = 0.51 V, FF = 0.46, and η = 2.76%, respectively.

• Bulletin of the Korean Chemical Society
• /
• v.30 no.3
• /
• pp.556-560
• /
• 2009

Aggregation behavior of three kinds of benzindocarbocyanine dyes in aqueous methanol solution was studied by UV-Vis absorption spectrum. The results indicated that the three dyes all existed monomer-dimer equilibrium in aqueous methanol solution (concentration range $10^{−5}\;to\;10^{−6}$ M) at 25.0$\sim$41.0 ${^{\circ}C}$ for Dye 1, 28.0$\sim$49.0 ${^{\circ}C}$ for Dye 2 and 26.0$\sim$47.0 ${^{\circ}C}$ for Dye 3. The fundamental property of the three dyes as the dimeric association constant KD, the dimeric free energy ${\Delta$}G_D, the dimeric entropy ${\Delta$}S_D, and the dimeric enthalpy ${\Delta$}H_D were determined. The ${\Delta$}H_D of three dyes: Dye 1, Dye 2 and Dye 3 was -42.5, -15.1 and -18.9 kJ/mol, respectively. The experimental observations were the subject of a theoretical study including the ground-state geometries which were fully optimized using DFT at B3LYP/6-31G level. The effect of dye molecule structure on ${\Delta$}H_D was discussed by theoretical calculations.

• Bulletin of the Korean Chemical Society
• /
• v.28 no.11
• /
• pp.1945-1950
• /
• 2007

Two fluorene-based conjugated copolymers containing hexyl-thiophene derivatives, PF-1T and PF-4T, were synthesized via the palladium-catalyzed Suzuki coupling reaction. The number-average molecular weights (Mn) of PF-1T and PF-4T were found to be 19,100 and 13,200, respectively. These polymers were soluble in common organic solvents such as chloroform, chlorobenzene, toluene, etc. The UV-vis absorption maximum peaks of PF-1T and PF-4T in the film state were found to be 410 nm and 431 nm, respectively. Electrochemical characterization revealed that these polymers have low highest occupied molecular orbital (HOMO) levels, indicating good resistance against oxidative doping. Thin film transistor devices were fabricated using the top contact geometry. PF-1T showed much better thin-film transistor performance than PF-4T. A thin film of PF- 1T gave a saturation mobility of 0.001-0.003 cm2 V?1 s?1, an on/off ratio of 1.0 × 105, and a small threshold voltage of ?8.3 V. To support TFT performance, we carried out DSC, AFM, and XRD measurements.

• KSBB Journal
• /
• v.26 no.5
• /
• pp.471-476
• /
• 2011

Nowadays biodiesel (fatty acid methyl ester, FAME) has been becoming an important issue as a desired alternative of energy products because of non-toxic, biodegradable properties, and lower exhaust emissions. During esterification of fatty acids or transesterification of oils and fats with short chain alcohols by the alkali-catalyzed methanolysis, FAME and unrefined glycerol are generated. Quantification of glycerol as a by-product is important because of a determinant of biodiesel quality. However, the glycerol analysis by gas chromatography (GC) method has laborious works with sample preparation, long time and cost of sample analysis. Thus, there is a need to analyze glycerol more simply. Herein we demonstrate that the colorimetric assay for glycerol analysis conducted by UV-vis spectrophotometer at the wavelength 617 nm whose peak is maximum intensity of malachite green, resulting in the red-shift occurred proportionally as a function of glycerol amount. Thus, it is considered the solvent media for malachite green fading for biodiesel production: (1) water, (2) MeOH, and (3) EtOH. The resulting findings show that the peak intensity at 617 nm in glycerol-malachite green mixture had a relationship between glycerol concentration and degree of peak shift as increase in pure glycerol concentration approximately at pH 7.0. However, when it was measured the unrefined glycerol concentration by diluting and adjusting with water to buffer (pH 7.0), it was not observed the absorption peak at 617 nm because of impurities and OH ions. In case of glycerol from biodiesel production factories, glycerol concentration could be successfully measured.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
• /
• 2003.05c
• /
• pp.154-157
• /
• 2003

$TiO_2$ thin films were fabricated by RF magnetron sputtering system at by controlling deposition times, ratios of $Ar:O_2$ partial presser ratio and substrate conditions. And the surface, cross-section morphology, microstructure, and composition ratio of the films were analyzed by FE-SEM, TEM and XPS. Besides, the optical absorption and transmittance of the $TiO_2$ films were measured by a UV-VIS-NIR Spectrophotometer, and photocatalytic properties were studied by G${\cdot}$C Analyzer & Data Analysis system. As the result, when $TiO_2$ thin film was made at deposition time of 120[min] and $Ar:O_2$ ratio of 60:40, the best structural and optical properties among many thin films could be accepted. The best results of properties were as follows: thickness; 360~370[nm), grain size; 40[nm], gap between two peak binding energy; $5.8{\pm}0.05[eV]$ ($2_{p3/2}$ peak and $2_{p1/2}$ peak of Ti was show at $458.3{\pm}0.05[eV]$ and $464.1{\pm}0.05[eV]$ respectively), binding energy; $530{\pm}0.05[eV]$, optical energy band gap; 3.4[eV].

• Proceedings of the Korean Vacuum Society Conference
• /
• 2013.08a
• /
• pp.142.2-142.2
• /
• 2013

The effect of substrate on catalytic activity of CO oxidation with transition metal Platinum nanoparticles on doped and undoped TiO2 was investigated. Titanium dioxide was doped chemically with non-metal anions including nitrogen and fluorine. Undoped TiO2 was synthesized via simple conventional sol-gel route. Thin films of titania were developed by spin coating technique and the characterization techniques SEM, XRD, UV-Vis Absorption Spectroscopy and XPS were carried out to examine the morphology of films, crystal phase, crystallites, optical properties and elemental composition respectively. XPS analysis from doped TiO2 confirmed that the nitrogen site were interstitial whereas fluorine was doped into TiO2 lattice substitutionally. Catalytic activity systems of Pt/doped-TiO2 and Pt/undoped-TiO2 were fabricated to reveal the strong metal-support interaction effect during catalytic activity of CO oxidation reactions. By arc plasma deposition technique, platinum nanoparticles with mean size of 2.7 nm were deposited on the thin films of doped and undoped titanium dioxide. The CO oxidation was performed with 40 Torr CO and 100 Torr O2 with 620 Torr He carrier gas. Turn over frequency was observed two to three folds enhancement in case of Pt/doped TiO2 as compared to Pt/TiO2. The electronic excitation and the oxygen vacancies that were formed with the doping process were the plausible reasons for the enhancement of catalytic activity.