• Bulletin of the Korean Chemical Society
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• v.32 no.1
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• pp.77-82
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• 2011

A new high performance liquid chromatograpgy (HPLC) stationary phase that possesses an internal carbonyl functional group is synthesized by heterogeneous "graft from" method. This new stationary phase, poly (vinyl octadecanoate) grafted silica (Sil-2) is then characterized by different physico-chemical methods such as diffuse reflectance infrared fourier transform, suspension state $^1H$ NMR, solid state $^{13}C$ CP/MAS NMR, $^{29}Si$ CP/MAS NMR, elemental analysis and thermogravimetric analysis. Chromatographic properties of Sil-2 were evaluated under reversed phase condition by separating polycyclic aromatic hydrocarbons (PAHs) and comparing the chromatographic results with those on polymeric as well as monomeric octadecylated silica stationary phases.

• Bulletin of the Korean Chemical Society
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• v.28 no.11
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• pp.2045-2050
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• 2007

The reactions of mercury(II) chloride with O3S2-donor macrocyclic ligands with (L1) and without (L2) dibenzosubunit afforded respective exo- (1) and endo-coordinated (2) complexes depending on the ring rigidity of the ligands. From the X-ray crystal structures and comparative NMR studies for the complexes 1 and 2, it is confirmed that the resulting species with different coordination modes exist not only in solid state but also in solution state.

• Proceedings of the KIEE Conference
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• 2005.07c
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• pp.1966-1967
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• 2005

The solid precursor produced by the dehydration of the gel at $120^{\circ}C$ for 12h is not in the amorphous state as expected but in a crystalline state. X-ray diffraction peaks of nearly the same angular position as the peaks of high Tc phase were observed in the precursor. Experimental results suggest that the intermediate phase formed before the formation of the superconducting phase may be the most important fact in determining whether it is easy to form the superconducting phase or not, because the nucleation barriers of the two superconducting phase may be altered by the variation of the crystal structures of those intermediate phase.

• Bulletin of the Korean Chemical Society
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• v.34 no.1
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• pp.143-148
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• 2013

Novel titanium containing solid core mesoporous shell silica has been synthesized by using octadecyltrichloro silane and triethylamine. The synthesized material was characterized by various physicochemical techniques. The mesoporous character of the material has been revealed from PXRD studies. The presence of octadecyltrichloro silane and triethylamine in the sample has been confirmed from EDAX studies. TG/DTA analysis reveals the thermal characteristics of the synthesized material. The presence of titanium in the frame work and its coordination state has been studies by UV-vis DR studies and XPS analysis. Chemical environment of Si in the framework of the material has been studied by $^{29}SiMASNMR$ studies. The surface area of the material is found to be around $550\;m^2g^{-1}$ and pore radius is of nano range from BET analysis. The spherical morphology and particle size of the core as well as shell has been found to be 300 nm and 50 nm respectively from TEM analysis. The catalytic application of this material towards the synthesis of caprolactam from cyclohexanone in presence of hydrogen peroxide through ammoxidation reaction has been investigated. The optimum conditions for the reaction have been established. The plausible mechanism for the formation of core silica and conversion of cyclohexanone has been proposed.

• Proceedings of the Korean Vacuum Society Conference
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• 2016.02a
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• pp.407.1-407.1
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• 2016

Electrochromism is defined as a phenomenon which involves persistently repeated change of optical properties between bleached state and colored state by simultaneous injection of electrons and ions, sufficient to induce an electrochemical redox process. Due to this feature, considerable progress has been made in the synthesis of electrochromic (EC) materials, improvements of EC properties in EC devices such as light shutter, smart window and variable reflectance mirrors etc. Among the variable EC materials, solid-state inorganics in particular, metal oxide semiconducting materials such as nickel oxide (NiO) have been investigated extensively. The NiO that is an anodic EC material is of special interest because of high color contrast ratio, large dynamic range and low material cost. The high performance EC devices should present the use of standard industrial production techniques to produce films with high coloration efficiency, rapid switching speed and robust reversibility. Generally, the color contrast and the optical switching speed increase drastically if high surface area is used. The structure of porous thin film provides a specific surface area and can facilitate a very short response time of the reaction between the surface and ions. The large variety of methods has been used to prepare the porous NiO thin films such as sol-gel process, chemical bath deposition and sputtering. Few studies have been reported on NiO thin films made by using sol-gel method. However, compared with dry process, wet processes that have the questions of the durability and the vestige of bleached state color limit the thin films practical use, especially when prepared by sol-gel method. In this study, we synthesis the porous NiO thin films on the fluorine doped tin oxide (FTO) glass by using sputtering and anodizing method. Also we compared electrical and optical properties of NiO thin films prepared by sol gel. The porous structure is promised to be helpful to the properties enhancement of the EC devices.

• Journal of the Korean Ceramic Society
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• v.51 no.3
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• pp.184-189
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• 2014

Electric arc furnace dust (EAFD) is a solid waste generated by the steel-scrap recycling process. It mainly consists of zinc oxides (ZnO), alumina ($Al_2O_3$), iron oxides ($Fe_2O_3$), and silica ($SiO_2$). Here we report the preparation and characterization of blue ceramic pigments using EAFD powder as a starting material. $(Zn(EAFD),Co)Al_2O_4$ blue ceramic pigment was prepared by the solid-state reaction method. The color characteristics of the pigment obtained were compared with those of pure $CoAl_2O_4$. The new pigment was characterized using XRD, CIE-$L^*a^*b^*$ color-measurements, SEM, and EDX. The XRD analysis revealed that the $(Zn(EAFD),Co)Al_2O_4$ pigment was composed of mainly the spinel phase of $(Zn,Co)Al_2O_4$. The $Zn(EAFD)_{0.25}Co_{0.75}Al_2O_4$ pigments showed a vivid blue color with a $b^*$ value of -28.64 and a good glaze stability with a transparent glaze.

• Journal of the Korean Electrochemical Society
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• v.10 no.1
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• pp.48-51
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• 2007

In order to investigate the effects of particle size and specific surface area(BET area) of spinel powder, $LiMn_2O_4$ were synthesized using metal oxide precursor by co-precipitation method(CoP) and solid state reaction (SSR) .X-ray diffraction(XRD) patterns revealed that the both prepared powder has a well developed spinel structure with Fd3m space group. The $LiMn_2O_4$ prepared by co-precipitation showed spherical morphology with narrow size distribution. However, the $LiMn_2O_4$ prepared by solid state reaction showed relatively smaller particles with irregular shape. The measured BET areas of the powers are $0.8m^2g^{-1}$ (CoP) and $3.6m^2g^{-1}$(SSR). The electrochemical performance of the Prepared $LiMn_2O_4$ powders was evaluated using coin type cells(CR2032) at elevated temperature ($55^{\circ}C$). The $LiMn_2O_4$ prepared by co-precipitation showed the better cycling performance(82.3%capacity retention at $50^{th}$ cycle) than that of the $LiMn_2O_4$(68.3%) prepared by solid state reaction at elevated temperature.

• Journal of the Korean Chemical Society
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• v.46 no.3
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• pp.242-251
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• 2002

We report the synthesis and characterization of the perovskite nanotubes made by sol-gel template syn-thesis.Both lead titanate (PbTiO3 : PT), lead zirconate (PbZrO3 : PZ) and lead zirconium titanate (PbZrO3 -PbTiO3 : PZT) solid solution nanotubes were prepared with a chelate sol-gel of titanium isopropoxide (Ti(OPri)4 ), zirconium tet-rabutoxide (Zr(OBu)4 ) and the respective lead acetate (Pb(OAc)2 -3H2O). WhatmanRanodisc membranes, with a 200nm pore size, served as the template. After the removal of the template in the 6M-NaOH, scanning electron microscopy shows that the shapes formed are 200 nm outer diameter tubes with 50mm lengths. Transmission electron microscopy and electron diffraction reveal that the tubes are polycrystalline. The PT nanotubes so far have shown an anomalous transition temperature, 234.4$^{\circ}C$ as measured by DSC with a small particle size, 15.4 nm determined by X-ray analysis with the aid of Scherrer's equation.

• Korean Journal of Materials Research
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• v.14 no.5
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• pp.305-309
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• 2004

Mechanical alloying (MA) of Ti-25.0～37.5at%Si powders was carried out in a high-energy ball mill, and in situ thermal analysis was also made during MA. In order to classify the synthesis behavior of the powders with respect to at%Si, the synthesis behavior during MA was investigated by in situ thermal analysis and X-ray diffraction (XRD). In situ thermal analysis curves and XRD patterns of Ti-25.0～26.1at%Si powders showed that there were no peaks during MA, indicating $Ti_{5}$ $Si_3$ was synthesised by a slow reaction of solid state diffusion. Those of Ti-27.1～37.5at%Si powders, however, showed that there were exothermic peaks during MA, indicating $_Ti{5}$ $Si_3$ and$ Ti_3$Si phase formation by a rapid exothermic reaction of self-propagating high-temperature synthesis (SHS). For Ti-27.1～37.5at%Si powders, the critical milling times for SHS decreased from 38.1 to 18.5 min and the temperature rise, ΔT (= peak temperature - onset temperature) increased form $19.5^{\circ}C$ to $26.7^{\circ}C$ as at%Si increased. The critical composition of Si for SHS reaction was found to be 27.1at% and the critical value of the negative heat of formation of Ti-27.1at%Si to be -1.32 kJ/g.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.26 no.5
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• pp.181-187
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• 2016

In this study, new composition of orange color pigment was developed by replacing formerly used lead and chromium with environment-friendly elements. $TiO_2-SnO-ZnO$ composite was synthesized using the solid state reaction under the reducing atmosphere with the LPG and air mixture gas. The synthesized pigments were characterized by spectrophotometer, X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and X-ray Photoelectron Spectroscopy (XPS). The colorimetric analysis of pigments exhibited color values ranging from yellow to orange-red. Five different crystalline phases were formed after the heat treatment for 4 and 6 hours. The color of pigments was strongly influenced by the crystalline structure of $SnO_2$, having either cubic or tetragonal structure. The oxidation state study of elements revealed that the color of pigment is getting close to rYR with the increase of $Sn^{4+}$ ratio.