• Bulletin of the Korean Chemical Society
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• v.34 no.2
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• pp.558-564
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• 2013

A simple and effective method is introduced to synthesize a series of polystyrene-b-poly(oligo(ethylene oxide) monomethyl ether methacrylate)-b-polystyrene (PSt-b-POEOMA-b-PSt) triblock copolymers. The structures of PSt-b-POEOMA-b-PSt copolymers were characterized by Fourier-transform infrared spectroscopy (FTIR) and nuclear magnetic resonance ($^1H$ NMR) spectroscopy. The molecular weight and molecular weight distribution of the copolymer were measured by gel permeation chromatography (GPC). Furthermore, the self-assembling and drug-loaded behaviours of three different ratios of PSt-b-POEOMA-b-PSt were studied. These copolymers could readily self-assemble into micelles in aqueous solution. The vitamin E-loaded copolymer micelles were produced by the dialysis method. The micelle size and core-shell structure of the block copolymer micelles and the drug-loaded micelles were confirmed by dynamic light scattering (DLS) and transmission electron microscopy (TEM). The thermal properties of the copolymer micelles before and after drug-loaded were investigated by different scanning calorimetry (DSC). The results show that the micelle size is slightly increased with increasing the content of hydrophobic segments and the micelles are still core-shell spherical structures after drug-loaded. Moreover, the glass transition temperature (Tg) of polystyrene is reduced after the drug loaded. The drug loading content (DLC) of the copolymer micelles is 70%-80% by ultraviolet (UV) photolithography analysis. These properties indicate the micelles self-assembled from PSt-b-POEOMA-b-PSt copolymers would have potential as carriers for the encapsulation of hydrophobic drugs.

• Journal of Ceramic Processing Research
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• v.13 no.spc2
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• pp.341-345
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• 2012

[Li0.055(K0.5Na0.5)0.945](Nb1-xTax)O3 (0.05 ≤ x ≤ 0.25) ceramics were prepared by the partial sol-gel (PSG) method to improve the microstructure homogeneity of Ta5+ ion and were compared to those prepared by the conventional mixed oxide (CMO) method. For the PSG method, Ta(OC2H5)5 was directly reacted with calcined [Li0.055(K0.5Na0.5)0.945]NbO3 powders and the specimens sintered at 1100 ℃ for 5 hrs showed a single phase with a perovskite structure. Compared to the specimens prepared by conventional mixed oxide powders, the relative ratio of tetragonal phase to orthorhombic phase of the sintered specimens prepared by Ta(OC2H5)5 was larger than that of the sintered specimens prepared by Ta2O5. The electromechanical coupling factor (kp), piezoelectric constant (d33) and dielectric constant (εr) of the sintered specimens were increased with Ta5+ content. These results could be attributed to the decrease of the orthorhombic-tetragonal polymorphic phase transition temperature (To-t), which could be evaluated by oxygen octahedral distortion. Strain of the sintered specimens prepared by the PSG method was higher than that of specimens prepared by the CMO method due to the increase of relative density. The effects of crystal structure on the strain characteristics of the specimens were also discussed.

• Applied Chemistry for Engineering
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• v.4 no.4
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• pp.823-829
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• 1993

The basic medium oil modified alkyd resin was synthesized from linseed oil fatty acid(LOFA), phthalic anhydride(PAA), trimellitic anhydride(TMA ), and trimthylol propane(TMP) by condensation polymerization at $230^{\circ}C$. TMPTA modified water-reducible alkyd resins were synthesized with TMPTA graft copolymerization onto the basic resin at $180^{\circ}C$. Acid value of the resin was controlled by the addition of TMA and N,N-Dimethylethanol amino(DMEA) was used as an neutralizing agent to prepare water-reducible alkyd. To evaluate the optimum formulation for anionic alkyd resin, water proofness and water reducibility were estimated from the acid value or TMA contents. The effect of TMPTA on the graft copoymerization of the resin was studied by measuring molecular weight, glass transition temperature(Tg), viscosity, and gel contents. The suitable balance of water proofness and water reducibility of the resin was obtained at range of 5.3~7.0wt.% of TMA contents or 40~50 of acid value of basic resin. The molecular weight, viscosity, and gel contents of water-reducible alkyd resin were increased according to the TMPTA graft copolymerization, but Tg was decreased.

• Applied Chemistry for Engineering
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• v.5 no.4
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• pp.698-705
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• 1994

The basic medium oil modified alkyd resin was synthesized from linseed oil fatty acid(LOFA), phthalic anhydride(PAA), maleic anhydride(MA) and trimethylol propane(TMP) by condensation polymerization at $230^{\circ}C$. MA/TMPTA modified water-reducible alkyd resins were synthesized with TMPTA graft copolymerization onto the basic resin at $180^{\circ}C$. Acid value of the resin was controlled by the addition amount of MA and N,N-dimethylethanol amine(DMEA) was used as a neutralizing agent to prepare of the water-reducible alkyd resin. The effect of TMPTA on the graft copolymerization of the resin was studied by measuring molecular weight glass transition temperature(Tg), viscosity, graft efficiency, and gel contents of melanin cured film. Heat resistance, UV resistance and water resistance of cured film of MA/TMPTA modified resin was compared to those of TMA/TMPTA modified alkyd resin. The molecular weight, viscosity gel contents and graft efficiency of water reducible alkyd resin were increased according to the TMPTA graft copolymerization, but Tg was decreased. The viscosity was lower when the solid contents reached 40% than that of 30% content and also and also became lower with the extent of neutralization ratio, The heat resistance, UV resistance and water resistance of the MA/TMPTA modified alkyd resis were better than those of TMA/TMPTA modified alkyd resin but the storage stability of the TMA/TMPTA alkyd resis was better than that of MA/TMPTA modified alkyd resin.

• Journal of the Korean Magnetics Society
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• v.16 no.3
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• pp.168-172
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• 2006

We studied the magnetic and the related electronic properties of Ni-doped rutile $TiO_{2-{\delta}}$ films (including oxygen deficiency $\delta$) prepared using a sol-gel method. A room-temperature ferromagnetism was observed in the $TiO_{2-{\delta}}$ : Ni films with the saturation magnetization ($M_S$) decreasing with increasing Ni doping and remaining constant above 6 at% Ni doping. The observed ferromagnetism below 6 at% Ni doping is interpreted as due to magnetic polaron formed by a trapped electron in oxygen vacancy and magnetic impurity ions around it. For small Ni doping, $M_S$ up to $3.7{\mu}B/Ni$ was obtained. The ferromagnetism for Ni doping above 6 at% is interpreted as due to the existence of Ni clusters that can explain the p-n conductivity transition observed by Hall effect measurements.

• Applied Chemistry for Engineering
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• v.8 no.5
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• pp.777-783
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• 1997

$TiO_2$ powders were synthesized via hydrolysis reaction of titanium n-propoxide in n-propanol solvent and the reaction rates were studied by use of UV-vis spectroscopic method. Concentration of water, reaction temperature, reaction time and acid-base effects of the solution were investigated to determine the optimum conditions for $TiO_2$ powder synthesis. The reaction were controlled to proceed to pseudo-first orders reaction in the presence of excess water in n-propanol solvent. The rate constants which varied with temperature and concentration of water were calculated by Guggenheim method. Reaction using $D_2O$ was also carried out to determine the catalytic character of water. $TiO_2$ powders were synthesized only in the neutral and basic solution and those were almost spheric forms having average particle size of $0.4-0.7{\mu}m$ diameter. Particle size decreased with increasing concentration of water and reaction temperature, however, increased with increasing reaction time. Associative $S_N2$ mechanism for the hydrolysis was proposed from the data of n-value in the transition state and thermodynamic parameter. $D_2O$ solvent isotope effect showed that $H_2O$ molecules reacted as nucleophilic catalysis.

• Korean Journal of Weed Science
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• v.32 no.3
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• pp.204-210
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• 2012

The physicochemical properties of tuber starch in water chestnut have been studied. Peak viscosity, hot paste viscosity and cooling peak viscosity were 5679, 3146 and 4262 RVU, respectively. In three transition parameters, onset temperature ($T_o$), peak temperature ($T_p$), and conclusion temperature ($T_c$) were 64.1, 68.5 and $72.3^{\circ}C$, respectively. Gelatinization enthalpy (${\Delta}H$ gel) was 4.48 J/g. A-type starch has a smaller proportion (11.4%) of short chains ($DP{\geq}12$) and a larger proportion (57.2%) of short chains ($13{\leq}DP{\geq}24$). The tuber starch of water chestnut displayed an A-type X-ray diffraction pattern showing a strong diffraction peak at $2{\Theta}$ values of $15.18^{\circ}$, $17.13^{\circ}$, and $23.1^{\circ}$, and a weak peak at $2{\Theta}$ values of $18.1^{\circ}$, $20.06^{\circ}$, and $26.69^{\circ}$. Their crystallinity was 28.6% and the mean starch granule size was 21.5 ${\mu}m$.

• Journal of the Korean Magnetics Society
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• v.8 no.6
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• pp.335-340
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• 1998

Colossal magnetoresistance $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ material has been produced by a metal-salt routed sol-gel process method. Magnetic properties of $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ have been studied with x-ray diffraction, Rutherford back-scattering spectroscopy(RBS), vibrating sample magnetometer, and Mossbauer spectroscopy. Crystalline $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ was perovskite cubic structure with a lattice parameter $a_0=3.868$\AA$$. And there was no appreciable change in the value of the lattice parameter when a small amount (x=0.01) of iron was added. However, Mossbauer and VSM data indicate the Curie temperature of the $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ decreased from 282 to 270 k and also the saturation magnetization from 84 to 81 emu/g at 77 K. Mossbauer spectra of $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ have been taken at various temperatures ranging form 4.2 K to room temperature. Analysis of $^{57}Fe$ Mossbauer data in terms of the local configurations of Mn atoms has permitted the influence of the magnetic hyperfine interactions to be monitored. The isomer shifts show that the charge state of all Fe ions are ferric. The magnetoresistance of $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ was about 33 % at semiconductor-metal transition temperature $T_{SC-M}=250K$.

• Journal of the Mineralogical Society of Korea
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• v.25 no.4
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• pp.283-293
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• 2012

In order to have better insights into the chemical differentiation of Earth from its magma ocean phase to the current stratified structure, detailed information of crystallization kinetics of silicate melts consisting of the magma ocean is essential. The structural transitions in oxide glasses and melts upon crystallization provide improved prospects for a systematic and quantitative understanding of the crystallization processes. Here, we report the $^{27}Al$ 3QMAS NMR spectra for sol-gel synthesized $Al_2O_3$ glass with varying temperature and annealing time. The NMR spectra for the amorphous $Al_2O_3$ show well-resolved Al coordination environments, characterized with mostly $^{[4,5]}Al$ and a minor fraction of $^{[6]}Al$. The fraction of $^{[5]}Al$ in the alumina phase decreases with increasing annealing time at constant temperature. The NMR results of $Al_2O_3$ phases also imply that multiple processes (e.g., crystallization and/or changes in structural disorder within glasses) could involve upon its phase transition. The current results and method can be useful to understand crystallization kinetics of diverse natural and multi-component silicate glasses and melts. The potential result may yield atomic-level understanding of Earth's chemical evolution and differentiation from the magma ocean.

• Korean Chemical Engineering Research
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• v.54 no.1
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• pp.120-126
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• 2016

Eco-friendly acrylic resin/clay nanocomposites containing pristine montmorillonite (PM) or modified clays (30B and 25A) were prepared from acrylic and styrenic monomers using non-aqueous dispersion (NAD) polymerization. Effect of nanoclays on physical properties of polymerization product and resulting nanocomposites was investigated. In view of NAD particle stability, addition of nanoclay at the beginning of polymerization is proved to be good. Results of gel fraction, acid value and viscosity of the NAD product showed that nanocomposites containing clay 25A showed better physical properties than the ones with other clays. GPC results exhibit the increase in molecular weight and decrease in polydispersity index for the 25A nanocomposite. Increase in layer distance confirmed from XRD analysis showed good dispersion of 25A in the nanocomposite. Thermal and dynamic mechanical analysis showed that highest glass transition temperature and storage modulus for 25A nanocomposites. These results indicate that 25A nanoclay gives the best properties in the process of non-aqueous dispersion polymerization of acrylic resin/nanoclay nanocomposites.