• Journal of the Korean Chemical Society
• /
• v.38 no.2
• /
• pp.160-168
• /
• 1994

Pentadentate Schiff base molybdenum(Ⅴ) complexes such as [Mo(Ⅴ)O(Sal-DET)(NCS)] and [Mo(Ⅴ)O(Sal-DPT)(NCS)] were synthesized by Sabat method. The structure of these complexes were identified by elemental analysis, spectroscopy, and thermogravimetric analysis(T.G.A.). It was found that the mole ratio of Schiff base ligand to the complexes was found to be 1 : 1. The redox processes of the complexes were investigated by cyclic voltammetric and differential pulse polarographic technique in nonaqueous solvent containing 0. 1 M tetraethyl ammonium perchlorate(TEAP) as supporting electrolyte at glassy carbon electrode. It was found that diffusion controlled reduction processes of four steps with one electron were 2Mo(Ⅴ)$\rightleftarrow^{e-}$ Mo(Ⅴ)Mo(Ⅳ) $\longrightarrow^{e-}$ 2Mo(Ⅳ), Mo(Ⅳ) $\longrightarrow^{e-}$ Mo(Ⅲ) $\longrightarrow^{e-}$ Mo(Ⅱ)

• Journal of the Korean Electrochemical Society
• /
• v.24 no.3
• /
• pp.35-41
• /
• 2021

In this study, the effect of zwitterionic surfactant on Cu electrodeposition was investigated through cyclic voltammetry. With the addition of (dodecyldimethylammonio)propanesulfonate (DDAPS) as a representative zwitterionic surfactant in the electrolyte for Cu electrodeposition, the electrochemical Cu²⁺ reduction was inhibited on Cu and glassy carbon electrodes. Its inhibition effect was similar to that of cationic surfactant rather than anionic surfactant. Moreover, DDAPS interacted with chloride ion and exhibited the mass transfer-dependent inhibition behavior, which indicates that its inhibition function is associated with the formation of its surface aggregates on anion-covered Cu surface. In addition, adsorbed DDAPS slightly reduced the surface roughness of Cu electrodeposits. These characteristics were similar to those of cationic surfactant, but less obvious. It means the effect of DDAPS on Cu electrodeposition originates from the cationic head group which is shield by anionic head group.

• Journal of Electrochemical Science and Technology
• /
• v.13 no.4
• /
• pp.497-503
• /
• 2022

Spinel ferrites (Ni_xFe_3-xO₄; x = 0.25, 0.5, 0.75 and 1.0) have been prepared at 550℃ by egg white auto-combustion route using egg white at 550℃ and characterized by physicochemical (TGA, IR, XRD, and SEM) and electrochemical (CV and Tafel polarization) techniques. The presence of characteristic vibration peaks in FT-IR and reflection planes in XRD spectra confirmed the formation of spinel ferrites. The prepared oxides were transformed into oxide film on glassy carbon electrodes by coating oxide powder ink using the nafion solution and investigated their electrocatalytic performance for OER in an alkaline solution. The cyclic voltammograms of the oxide electrode did not show any redox peaks in oxygen overpotential regions. The iR-free Tafel polarization curves exhibited two Tafel slopes (b₁ = 59-90 mV decade^-1 and b₂ = 92-124 mV decade^-1) in lower and higher over potential regions, respectively. Ni-substitution in oxide matrix significantly improved the electrocatalytic activity for oxygen evolution reaction. Based on the current density for OER, the 0.75 mol Ni-substituted oxide electrode was found to be the most active electrode among the prepared oxides and showed the highest value of apparent current density (~9 mA cm^-2 at 0.85 V) and lowest Tafel slope (59 mV decade^-1). The OER on oxide electrodes occurred via the formation of chemisorbed intermediate on the active sites of the oxide electrode and follow the second-order mechanism.

• Korean Journal of Heritage: History & Science
• /
• v.48 no.4
• /
• pp.138-153
• /
• 2015

A Jincheon Seokjangri B23 furnace was reconstructed and iron smelting experiment was performed to investigate an ancient Baekjae iron production process. The work mainly described in this paper is the $1^{st}$ and $2^{nd}$ experiments among the several experiments carried out at Jungwon National Research Institute of Cultural Heritage. Iron ore(magnetite) and oak charcoal were used as a source and a foot bellow was used for air supply. Common results of the experiments are masses of iron, slag and charcoal formed in the furnace. Most iron lumps were formed nearby the tuyere rather than the area of tapping hole. Metallographic and chemical analysis shows that the iron lumps can be used for either forge or cast depending on their carbon content. Low Fe content and glassy texture of the inner slags suggest that the operation environment was quite reducing. Based on the results of the iron smelting experiments, measurements and analysis, various information was obtained regarding physical-chemical and metallurgical processes of the ancient iron smelting process. It is firmly believed that its undisclosed contents can be revealed more in depth with continual reconstitution experiments.

• Journal of the Korean Chemical Society
• /
• v.33 no.2
• /
• pp.192-202
• /
• 1989

Tetradentate schiff bases cabalt (II) complexes; Co(SED) and Co(ο-BSDT) were synthesized and these complexes allowed to reaction with dry oxygen to form oxygen adduct cobalt(III) complexes such as $[Co(o-BSDT)(DMSO)]_2O_2,\;[Co(SED)(Py)]_2O_2\;and\;[Co(o-BSDT)(Py)]_2O_2$ in DMSO and pyridine solutions. It has been found that the oxygen adduct cobalt(III) complexes have hexacoordinated octahedral configuration with tetradentate schiff base cobalt(II), DMSO or pyridine and oxygen, and the mole ratio of oxygen to cobalt(II) complexes are 1:2. The redox processes, were investigated for Co(SEDT) and Co(ο-BSD) complexes in 0.1M TEAP-DMSO and 0.1M TEAP-pyridine by cyclic voltammetry with glassy carbon electrode. As a result the redox processes of Co(II)/Co(III) and Co(II)/Co(I) found to be reversible or quasi-reversible for non uptake oxygen complexes but oxygen adduct complexes found to be irreversible processes and reaction processes of oxygen for oxygen adduct complexes are quasi-reversible process, the potential range was $E_{pc}=-0.85{\sim}-1.19V\;and\;E_{pa}=-0.74{\sim}-0.89V$.

• Resources Recycling
• /
• v.23 no.6
• /
• pp.3-11
• /
• 2014

Bottom ash from coal fired power plants is not widely used due to a broad range of particle sizes and a high carbon content for producing geopolymers. The effect of mechanical activation on compressive strength of bottom ash- based geopolymers was examined by rod and planetary-ball milling to encourage full-fledged recycling of bottom ash, the main component of pond ash. The amount of amorphous component in the milled ash samples did not change significantly after the mechanical activation. It is presumably because needle-shaped mullite crystals, which is a major crystalline phase and grown in a glassy matrix, possess high strength and toughness, and therefore, they could endure external shocks and remain almost intact. Milling operation, however, decreased the particle size and improved the homogeneity of ash, thereby leading to increase reactivity of milled ash with alkali activators. Rod milling produced a relatively narrow particle size distribution of the milled ash particles; however, it was less effective in reducing the particle size. Nevertheless, it was interesting to observe that rod milling had equal effect on improving the compressive strength of geopolymers up to about 37%, as that of planetary ball milling. Rod milling is believed to be suitable process for enhancing the reactivity of bottom ash for large-scale recycling of bottom ash and producing geopolymers.

• Analytical Science and Technology
• /
• v.11 no.5
• /
• pp.332-340
• /
• 1998

Tridentate Schiff base ligands, $SIPH_2$, $SIPCH_2$, $HNIPH_2$, and $HNIPCH_2$ were prepared by the reactions of salicylaldehyde and 2-hydroxy-1-naphthaldehyde with 2-aminophenol and 2-amino-p-cresol. Ni(II) complexes of those ligands were synthesized. The structures and properties of ligands and their complexes were studied by elemental analysis, $^1H$-NMR, IR, UV-visible spectra, and thermogravimetric analysis. The mole ratio of Schiff base to the metal of complexes was found to be 1:1. Ni(II) complexes were contemplated to be hexa-coordinated octahedral configuration containing three water molecules. The redox process of ligands and complexes in DMSO solution containing 0.1 M TBAP as supporting electrolyte was investigated by cyclic voltammetry and differential pulse voltammetry with glassy carbon electrode. The redox process of the tridentate Schiff base ligands was totally irreversible. The redox process of Ni(II) complexes were quasi-reversible and diffusion-controlled as one electron by one step process Ni(II)/Ni(I). The reduction potentials of the Ni(II) complexes shifted in the positive direction in the order [$Ni(II)(HNIP)(H_2O)_3$]>[$Ni(II)(SIP)(H_2O)_3$]>[$Ni(II)(SIPC)(H_2O)_3$]>[$Ni(II)(HNIPC)(H_2O)_3$] and their dependence on ligands were not so high. Consequently the [$Ni(II)(HNIPC)(H_2O)_3$] complex among the synthesized Ni(II) complexes was found to be most stable in the DMSO solution.

• Journal of the Korean Chemical Society
• /
• v.35 no.6
• /
• pp.689-698
• /
• 1991

Activated oxidation catalysts are generated by the treatment of pentadentate Schiff base cobalt(Ⅱ) complexes with the oxygen saturated DMF solution. Oxidation of 2,6-di-tert-butylphenol by homogeneous oxidation catalysts of superoxo type pentadentate schiff base cobalt(Ⅲ) complexes yields 2,6-di-tert-butylbenzoquinone(BQ) as a major product. And $O_2$/Co mole ratio of homogeneous oxidative catalysts such as [Co(Ⅲ)(sal-DET)]$O_2$ and [Co(Ⅲ)(sal-DPT)]$O_2$by PVT method of the oxygen absorption in DMSO and pyridine solution was 1:1, 1:1.52 in DMF solution and ${\mu}$-peroxo type cobalt(Ⅲ) complexes formed at solid state. The redox reaction processes of superoxo type cobalt(Ⅲ) complexes as homogeneous oxidation catalysts were investigated by cyclic voltammetry and DPP method at a glassy carbon electrode. As a result of electrochemical measurements the reduction processes of oxygen adducted superoxo type cobalt(Ⅲ) complexes occurred to four steps including prewave of $O_2$-in 0.1M TEAP-DMSO and 0.1 M TEAP-Pyridine as supporting electrolyte solution.

• Journal of Energy Engineering
• /
• v.7 no.1
• /
• pp.146-156
• /
• 1998

Fly ash produced in coal combustion is a fine-grained material consisting mostly of spherical, glassy, and porous particles. A physical, morphological, and chemical characteristic of fly ash has been analyzed. This study may contribute to the data base of domestic fly ash, the improvement of combustion efficiency, ash recycling and ash collection in the electrostatic precipitator. The physical property of fly ash is determined using a particle counter for the measurement of ash size distribution and gravimeter. Morphological characteristic of fly ash is performed using a scanning electron micrograph and an optical microscope. The chemical components of fly ash are determined using an inductively coupled plasma emission spectrometry (ICP). The distribution of fly ash size was ranged from 15 to 25 $\mu$m in mass median diameter. Exposure conditions of flue gas temperature and duration within the combustion zone of the boiler played an important role on the morphological properties of the fly ash such as shape, relative opacity, coloration, cenosphere and plerosphere. The spherical fly ash might be generated at the condition of complete combustion. The size of fly ash was found to be increased the with particle-particle interaction of agglomeration and coagulation. Fly ash consisted of $SiO_2\;Al_2O_3\;and\;Fe_2O_3$ with 85% and carbon with 3~10% of total mass.

• Polymer(Korea)
• /
• v.25 no.1
• /
• pp.6-14
• /
• 2001

The monomer N,N'-bis(3-pyrrol-1-yl-propyl)-4,4'-bipyridinium$(PF_6)_2$ was electrochemically polymerized on glassy carbon electrode surface. This polymer film electrode has electroactive sites on its bipyridinium ions distributed at the polymer strands. The formal potentials of the electrodes were -0.41V and -0.81V(vs. SSCE) for each step at phosphate buffer(pH=5.70). The diffusion coefficients of the dopants ions into the polymer matrix were $1.57{\times}10^{-4}$ and $4.35{\times}10^{-5}cm^2s^{-1}$ for first and second redox couple, respectively. The rate constants of electron transfer at $V^{2+/+}$ of the first step was a $57.53s^{-1}$, which was 22 times higher than $V^{+/0}$ one having $2.63s^{-1}$ in the solution. The charge transfer resistance of the polymer film was influenced by the dopant ion of the electrolyte. Thus the resistances were 22.63, 16.81, 12.44 and $11.36k{\Omega}$ for $LiClO_4,\;NaClO_4,\;KClO_4$, and phosphate buffer, respectively. The reaction order of the electropolymerization was first order and the rate constant of the polymerization was $1.31{\times}10^{-1}s^{-1}$ as determined by EQCM method. The G.C./p-BPB type electrode doped with phosphate ions showed a stability and reproducibility in CV procedure over 20 cycles.