• Bulletin of the Korean Chemical Society
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• v.35 no.2
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• pp.431-435
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• 2014

Zinc peroxide nanoparticles ($ZnO_2$ NPs) were prepared by reacting zinc(II) isobutylcarbamate, as an organometallic precursor, with hydrogen peroxide ($H_2O_2$) at $60^{\circ}C$. Polyethylene glycol and polyvinylpyrrolidone were used as stabilizers, which suppressed aggregation of the $ZnO_2$ NPs. Conditions such as concentrations of $H_2O_2$ and the stabilizer were systemically controlled to determine their effect on the formation of nano-sized $ZnO_2$ NPs. The formation of stable $ZnO_2$ NPs was confirmed by UV-vis, Raman spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray diffraction. The TEM images revealed that polyvinylpyrrolidone-stabilized $ZnO_2$ NPs (diameter, 10-30 nm) were well dispersed in the organic solvent. Quite pure ZnO NPs were obtained from the peroxide powder by simple heat treatment of $ZnO_2$. The transition temperature of $170^{\circ}C$ was determined by differential scanning calorimetry.

• Progress in Superconductivity and Cryogenics
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• v.21 no.3
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• pp.27-31
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• 2019

Large grain YBCO bulk superconductors are fabricated by the top-seeded melt growth (TSMG) or top-seeded infiltration growth (TSIG) method. Both growth methods use at least one of $YBa_2Cu_3O_{7-{\delta}}$, $Y_2BaCuO_5$, $BaCuO_3$ pre-reacted precursor powders. However, the synthesis of the pre-reacted powders includes multiple calcination runs which are cost-bearing and time-consuming. In this work, we report the successful growth of single-domain YBCO bulk superconductors directly by using the powder compact that has been pressed from the mixture of $Y_2O_3$, $BaCuO_3$ and CuO powders without any intermediate grinding step. Single-domain YBCO bulk superconductor has been also prepared by using $Y_2O_3$, $BaO_2$ and CuO powders without intermediate grinding step. Investigations on the trapped magnetic field and microstructure of the melt-processed specimen show that the elimination of the repeated processes of calcinations and pulverization has hardly affected on the crystal growth and the magnetic properties of the grown YBCO bulk superconductors. However, it is thought that the presence of residual carbon affects on the size of Y211 particles in melt-processed YBCO bulk superconductor.

• Journal of Ceramic Processing Research
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• v.20 no.6
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• pp.655-659
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• 2019

Calcium phosphates such as HA (hydroxyapatite), β-TCP (tricalcium phosphate) and biphasic HA/β-TCP, were synthesized by wet chemical precipitation in aqueous solution combined with ball milling process. Nanosize powders of the calcium phosphates were synthesized using Ca(OH)2 and H3PO4. The effects of initial precursor Ca/P ratio (1.30, 1.50 and 1.67), ball milling process and post heat-treatment on the phase evolution behavior of the powders were investigated. The phase of resulting powder was controllable by adjusting the initial Ca/P ratio. HA was the only phase for as-prepared powders in both cases of Ca/P ratios of 1.50 and 1.67. The single HA phase without any noticeable second phase was obtained for the initial Ca/P ratio of 1.67 in the overall heat-treatment range. Pure β-TCP and biphasic calcium phosphate (HA/β-TCP) were synthesized from precursor solutions having Ca/P molar ratios of 1.30 and 1.50, respectively, after having been heat-treated above 700 ℃. The β-TCP phase has appeared on the pre-existing DCPD (dicalcium phosphate dihydrate) and/or HA phase. Dense ceramics having translucency were obtained at a considerably lower sintering temperature. The modified process offered a fast, convenient and economical route for the synthesis of calcium phosphates.

• Current Photovoltaic Research
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• v.2 no.4
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• pp.177-181
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• 2014

$Cu_2ZnSn(S_xSe_{1-x})_4$ (CZTSSe) absorber thin films were prepared on Mo coated soda lime glass substrates by sulfo-selenization of sputtered stacked Zn-Sn-Cu precursor thin films. The Zn-Sn-Cu precursor thin films were sulfo-selenized inside a graphite box containing S and Se powder using rapid thermal processing furnace at $540^{\circ}C$ in Ar atmosphere with pre-treatment at $300^{\circ}C$. The effect of different S/Se ratio on the structural, compositional, morphological and electrical properties of the CZTSSe thin films were studied using XRD (X-ray diffraction), XRF (X-ray fluorescence analysis), FE-SEM (field-emission scanning electron microscopy), respectively. The XRD, FE-SEM, XRF results indicated that the properties of sulfo-selenized CZTSSe thin films were strongly related to the S/Se composition ratio. In particular, the CZTS thin film solar cells with S/(S+Se)=0.25 shows best conversion efficiency of 4.6% ($V_{oc}$ : 348 mV, $J_{sc}$ : $26.71mA/cm^2$, FF : 50%, and active area : $0.31cm^2$). Further detailed analysis and discussion for effect of S/Se composition ratio on the properties CZTSSe thin films will be discussed.

• Proceedings of the IEEK Conference
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• 2001.10a
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• pp.240-244
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• 2001

Recycling process involving mechanical, thermal, hydrometallurgical, and sol-gel step has been applied to recover cobalt and lithium from spent lithium ion batteries and to synthesize LiCoO$_2$from leach liquor as cathodic active materials. Electrode materials containing lithium and cobalt could be concentrated with 2-step thermal and mechanical treatment. Leaching behaviors of the lithium and cobalt in nitric acid media was investigated in terms of reaction variables. Hydrogen peroxide in 1 M HNO$_3$solution turned out to be an effective reducing agent by enhancing the leaching efficiency. O f many possible processes to produce LiCoO$_2$, the amorphous citrate precursor process (ACP) has been applied to synthesize powders with a large specific surface area and an exact stoichiometry. After leaching used LiCoO$_2$with nitric acid, the molar ratio of Li/Co in the leach liquor was adjusted at 1.1 by adding a fresh LiNO$_3$solution. Then, 1 M citric acid solution at a 100% stoichiometry was also added to prepare a gelatinous precursor. When the precursor was calcined at 95$0^{\circ}C$ for 24 hr, purely crystalline LiCoO$_2$was successfully obtained. The particle size and specific surface area of the resulting crystalline powders were 20 пm and 30 $\textrm{cm}^2$/g, respectively The LiCoO$_2$powder was proved to have good characteristics as cathode active materials in charge/discharge capacity and cyclic performance.

• 한국신재생에너지학회:학술대회논문집
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• 2007.11a
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• pp.17-18
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• 2007

Solid oxide fuel cells are clean, pollution-free technology for the electrochemical generation of electricity at high efficiency. Specially, the polarization resistance between electrolyte and electrode of SOFC unit cell is of importance, because it is desirable to develop SOFC operating at intermediate temperature below $800^{\circ}C$. The LSCF cathode prepared using modified oxalate method was investigated with different electrolyte. A precursor was prepared with oxalic acid, ethanol and $NH_4OH$ solution. The LSCF precursor was prepared at $80^{\circ}C$, and pH control was 2, 6, 8, 9 and 10. The precursor powder was calcined at $800^{\circ}C$, $1000^{\circ}C$ and $1200^{\circ}C$ for 4hrs. The crystal of LSCF powders show single phase at pH 2, 6, 8 and 9, and the average particle size was about $3{\mu}m$. The LSCF cathode with heat treatment at $1200^{\circ}C$ showed a plot of electric conductivity versus temperature. Unit cell prepared from the LSCF cathode, buffer layer between cathode and electrolyte and the LSGM, YSZ, ScSZ and CeSZ electrolyte. Also interface reaction between LSCF, buffer layer and electrolyte were measured by EPMA and the polarization resistance for unit cell with cycle measure using a Solatron 1260 analyzer.

• Resources Recycling
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• v.16 no.5
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• pp.41-45
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• 2007

Tetramethylorthosilicate (TMOS) and silica nanopowder were synthesized from the waste silicon sludge containing 15% weight of silicon powder. TMOS, a precursor of silica nanopowder, was firstly prepared from the waste silicon sludge by catalytic chemical reaction. The maximum recovery of the TMOS was 100% after 5 hrs regardless of reaction temperature above $130^{\circ}C$. But the initial reaction rate became faster while the reaction temperature was higher than $150^{\circ}C$. As the methanol feedrate Increased from 0.8 ml/min to 1.4 ml/min, the yield of reaction was not varied after 3 hrs. Then, silica nanopowder was synthesized from the synthesized TMOS by flame spray pyrolysis. The morphology of as-prepared silica nanopowder was spherical and non-aggregated. The average particle diameters ranged from 9 nm to 30 nm and were in proportional to the precursor feed rate, and precursor concentration.

• Korean Journal of Materials Research
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• v.20 no.3
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• pp.142-147
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• 2010

Nano-sized $BaNd_2Ti_5O_{14}$ powders were prepared by the spray pyrolysis process. Sucrose used as the organic additive enabled the formation of nano-sized $BaNd_2Ti_5O_{14}$ powders. The powders prepared from the spray solution without sucrose had a spherical shape, dense structure and micron size before and after calcination. However, the precursor powders prepared from the spray solution with sucrose had a large size, and hollow and porous morphology. The precursor powders had an amorphous crystal structure because of the short residence time of the powders inside the hot wall reactor. The complete decomposition of sucrose did not occur inside the hot wall reactor. Therefore, the precursor powders obtained from the spray solution with sucrose of 0.5M had a carbon content of 39.2wt.%. The powders obtained from the spray solution with sucrose of 0.5M had a slightly aggregated structure of nano-sized primary powders of $BaNd_2Ti_5O_{14}$ crystalline phase after calcination at $1000^{\circ}C$. The calcined powders turned into nano-sized $BaNd_2Ti_5O_{14}$ powders after milling. The mean size of the $BaNd_2Ti_5O_{14}$ powders was 125 nm.

• YAKHAK HOEJI
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• v.53 no.5
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• pp.293-297
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• 2009

The abuse of methamphetamine (MA) is one of the most serious drug abuses in Asia. And, the prevention of precursor production for abuse drug is one of the most effective drug control system. Isotope ratio analysis at natural abundance levels have been used to establish the environmental source or the geographic origin of various biological and nonbiological materials. Ephedrine, the precursor of MA, is produced by one of three methods; extraction from Ephedra plants, full chemical synthesis or via a semi-synthetic process involving the fermentation of sugar, followed by amination. We investigated the origin of ephedrine and pseudoephedrine based on the carbon and nitrogen values for nineteen pharmaceutical powder materials (PPMs) obtained from pharmaceutical company in Korea by stable isotope ratio mass spectrometry coupled to an elemental analyser (EA-IRMS). The carbon delta values for the ephedrine and pseudoephedrine were -24.21~-22.72 (mean=-23.72) $^{\cir}/_{\circ\circ}$ and -23.79~-22.71 (mean=-23.48) $^{\cir}/_{\circ\circ}$. The nitrogen delta values were 3.51~5.55 (4.43) $^{\cir}/_{\circ\circ}$ and 2.24~8.22 (5.42) $^{\cir}/_{\circ\circ}$. These results indicate that PPMs are semi-synthetic products. Therefore the origins of ephedrine(natural, semi-synthetic or synthetic) could be discriminated by using carbon and nitrogen stable isotope ratios. we are sure tat this stable isotope ratio analysis can discriminate the origins of precursors of methamphetamine.

• Bulletin of the Korean Chemical Society
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• v.21 no.11
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• pp.1125-1132
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• 2000

The pH effect of the precursor solution on the preparation of $LiCoO_2$ by a solution phase reaction containing malonic acid was carried out. Layered $LiCoO_2$ powders were obtained with the precursors prepared at the different pHs (4, 7, and 9) and heat-treated at $700^{\circ}C(LiCoO_2-700)$ or $850^{\circ}C(LiCoO_2-850)$ in air. pHs of the media for precursor synthesis affects the charge/discharge and electrochemical properties of the $LiCoO_2electrodes.$ Upon irrespective of pH of the precursor media, X-ray diffraction spectra recorded for $LiCoO_2-850$ powder showed higher peak intensity ratio of I(003)/I(104) than that of $LiCoO_2-700$, since the better crystallization of the former crystallized better. However, $LiCoO_2$ synthesized at pH 4 displayed an abnormal higher intensity ratio of I(003)/I(104) than those synthesized at pH 7 and 9. The surface morphology of the $LiCoO_2-850$ powders was rougher and more irregular than that of $LiCoO_2-700$ made from the precursor synthesized at pH 7 and 9. The $LiCoO_2electrodes$ prepared with the precursors synthesized at pH 7 and 9 showed a better electrochemical and charge/discharge characteristics. From the AC impedance spectroscopic experiments for the electrode made from the precursor prepared in pH 7, the chemical diffusivity of Li ions (DLi+) in $Li0.58CoO_2determined$ was 2.7 ${\times}$10-8 $cm^2s-1$. A cell composed of the $LiCoO_2-700$ cathode prepared in pH 7 with Lithium metal anode reveals an initial discharge specific capacity of 119.8 mAhg-1 at a current density of 10.0 mAg-1 between 3.5 V and 4.3 V. The full-cell composed with $LiCoO_2-700$ cathode prepared in pH 7 and the Mesocarbon Pitch-based Carbon Fiber (MPCF) anode separated by a Cellgard 2400 membrane showed a good cycleability. In addition, it was operated over 100 charge/discharge cycles and displayed an average reversible capacity of nearly 130 mAhg-1.