• Bulletin of the Korean Chemical Society
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• v.23 no.8
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• pp.1078-1084
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• 2002

The formation temperature for the perovskite lead zirconate titanate [Pb(Zr,Ti)O3, PZT] derived from sol-gel route was lowered by more than $100^{\circ}C$ with the addition of crystallographically suitable seed particles, such as barium titanat e (BT) or PZT. We investigated the effect of seeding on the crystallization of perovskite phase and in the microstructure of the sol-gel derived PZT powder by varying the concentration, size and chemical species of seed particles. The phase transition as a function of temperature was monitored by DTA, XRD, and Raman spectroscopy, and the interface between the seed particle and grown PZT layer was analyzed by SEM and high resolution TEM techniques. It was found that both the heterogeneous and homogeneous nucleation contributes competitively in the formation of perovskite PZT grains.

• Proceedings of the Polymer Society of Korea Conference
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• 2006.10a
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• pp.263-263
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• 2006

Poly (ethylene glycol)(PEG) - Poly (${\varepsilon}-caprolactone(CL)$) - Poly (D,L lactide(LA) (PCLA-PEG-PCLA) was synthesized by ring-opening polymerization to form temperature sensitive hydrogel triblock copolymer. The triblock copolymer was acrylated by acryloyl chloride. ${\beta}-amino$ ester was used as a pH sensitive moiety, in this study ${\beta}$- amino ester obtained from 1,4-butandiol diacrylate, and 4, 4' trimethylene dipiperidine, it have pKb around 6.6. pH/temperature sensitive penta-block copolymer (PAE-PCL-PEG-PCL-PAE) was synthesized by addition polymerization from acrylated triblock copolymer, 1,4-butandiol diacrylate, and 4, 4' trimethylene dipiperidine. Their physicochemical properties of triblock and penta-block copolymers were characterized by $^1H-NMR$ spectroscopy and gel permeation spectroscopy. Sol-gel phase transition behavior of PAE-PCL-PEG-PCL-PAE block copolymers were investigated by remains stable method. Aqueous media of the penta-block copolymer (at 20 wt%) changed from a sol phase at pH 6.4 and $10^{\circ}C$ to a gel phase at pH 7.4 and $37^{\circ}C$. The sol-gel transition properties of these block copolymers are influenced by the hydrophobic/hydrophilic balance of the copolymers, block length, hydrophobicity, stereo-regularity of the hydrophobic of the block copolymer, and the ionization of the pH function groups in the copolymer depended on the changing of environmental pH, respectively. The degradation and the stabilization at pH 7.4 and $37^{\circ}C$, and the stabilization at pH 6.4 and $10^{\circ}C,\;5^{\circ}C,\;0^{\circ}C$, of the gel were determined. The results of toxicity experiment show that the penta block copolymer can be used for injection drug delivery system. The sol?gel transition of this block copolymer also study by in vitro test ($200{\mu}l$ aqueous solution at 20wt% polymer was injected to mouse). Insulin loading and releasing by in vitro test was investigated, the results showed that insulin can loading easily into polymer matrix and release time is around 14-16days. The PAE-PCL-PEG-PCL-PAE can be used as biomaterial for drug, protein, gene loading and delivery.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2003.07a
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• pp.557-560
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• 2003

The submicron $YBa_2Cu_3O_x$ powder was prepared by the sol-gel method. The particle size is distributed from 0.2 to $1.0\;{\mu}m$, which benefits to eliminate the micro-cracks formed in the $YBa_2Cu_3O_x$ films deposited by electrophoresis. The powder was single phase of $YBa_2Cu_3O_x$ examined by X-ray diffraction. In the sol-gel process the citrate gel was formed from citric acid and nitrate solution of $Y_2O_3$, $Ba(NO_3)O_2$ and CuO. When pH values were adjusted to $6.4{\sim}6.7,\;Ba(NO_3)O_2$ could be dissolved in the citrate solution completely. Appropriate evaporative temperature of the sol-gel formation is discussed. After the heat treatment the transition temperature($T_c$) and critical current density($J_c$) of the $YBa_2Cu_3O_x$ samples made of the submicron powder were measured.

• Bulletin of the Korean Chemical Society
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• v.24 no.10
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• pp.1485-1489
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• 2003

The gelation for di-(2-ethylhexyl) phthalate (DEHP)-plasticized poly(vinyl chloride) was studied by measuring time-resolved small-angle X-ray scattering (SAXS) and a flow of the solutions in test tube. It was found that for the gelation there were three regimes. At Regime I, the solution rapidly changed to a gel, and the SAXS intensity showed a peak and the peak intensity increased, keeping the peak angle constant. Applying the SAXS intensity to the kinetic analysis of the liquid-liquid phase separation, it was revealed that the spinodal decomposition proceeded to develop a periodic length of 29.9 nanometer in size, a hydrogen-bonding-type association in polymer rich phase followed, and then it induced fast gelation rate. At Regime II, the gelation slowly occurred and the SAXS intensity was not observed, suggesting that a homogeneous gel network was formed by a hydrogen-bonding. At regime III, the solution was a homogeneous sol.

• Journal of the Korean Ceramic Society
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• v.33 no.12
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• pp.1301-1310
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• 1996

Generally it requires high sintering temperatures more than 135$0^{\circ}C$ to make semiconductive BaTiO3 ceramics. Also it is very difficult to achieve a homogeneous mixing in solid-state reaction method. Therefore the liquid phase distributed to non-uniform dilute the characteristics of PTCR. In order to improve the uniformity this study is used the sol-gel coating method. Using this method we studied the new manufacturing process that had a high reproducibility and mass production capability. Tetraethyl orthosilicate (TEOS) was used as a source of Si. The semiconductive BaTiO3 ceramics which was produced by sol-gel method for the SiO2 addition and sintered between 124$0^{\circ}C$ and 130$0^{\circ}C$ showed almost same resistivity at room temperature among 125$0^{\circ}C$ and 130$0^{\circ}C$. As the results We could be sintered the semiconducting BaTiO3 ceramics at lower temperature even at 125$0^{\circ}C$ maintaining the same specific resistivity ratio ($\rho$max/$\rho$min) at 130$0^{\circ}C$. The specific resistivity both below and above the Curie temperature were increased by slow cooling and the steepness of the plots in the reasion of transition from low to high resistance increased as the cooling rate decreased.

• Macromolecular Research
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• v.10 no.6
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• pp.325-331
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• 2002

Phase behavior of a PEO-PPO-PEO (Pluronic P103) triblock copolymer in water is investigated using small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), dynamic light scattering (DLS) and rheology. Pluronic P103 shows apparent two gel states in different temperature regions. The first sol-to-gel transition at a lower temperature (i.e., the hard gel I state) turns out to be the hexagonal microphase as evidenced by the combined SANS and SAXS and the frequency dependence of both G′ and G" in rheology. In contrast to the hard gel I, the second sol-to-gel transition (i. e., the hard gel II state) at a higher temperature represents the block copolymer micelles in somewhat disordered state rather than the ordered state seen in the hard gel I. Moreover, turbidity change depending only on the temperature with four distinct regions is observed and the large aggregates with size larger than 5,000 nm are detected with DLS in the turbid solution region. Based upon the present study, two different gelation mechanisms for aqueous PEO-PPO-PEO triblock copolymer solutions are proposed.

• Journal of the Korean Ceramic Society
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• v.28 no.10
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• pp.819-823
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• 1991

Pure zirconia ceramic fiber experiences severe volume changes through thermal cyclings of heating and cooling. Zirconia fiber was doped with CaO to stabilize the phase and its effect of CaO was studied on volumetric ratio of each phases, phase transition temperature and microstructure. Tetragonal phase was increased as CaO increases up to 10 mol% and cubic phase was stabilized when CaO was added more than 10 mol%. The average grain size of zirconia fiber was increased as CaO increased and transition temperature was shifted to lower temperature.

• Journal of the Korean Ceramic Society
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• v.24 no.6
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• pp.561-571
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• 1987

In case of glass ceramics and powder preparation from the metalakoxide solutions, metalakoxide solutions with a various species of alkoxy groups have unique characteristics. Therefore, in this study, the mixing ability of homogeneous sol, gel morphology and physical properties of gels were investigated by the changes in terms of the different four alkoxy groups, CH3-, C2H5-, i-C3H7-n-C4H9-, along with the catalyst for the purpose of the observation about the homogenous transition range from sol to gel. As a result, when the fixed condition was mol ratio of H2O/Si(OR)4=2.0 and variables were batch composition and addition amount of catalyst, the characteristics of Tetra-normal-Butoxysilane and Tetra-iso-propoxysilane systems had very narrow sol-gel conversion region than Tetramethoxysilane and Tetraethoxysilane system. And silicon-alkoxide, systems having narrow sol-gel conversion region were enlarged by addition of catalyst. In viewpoint of the weight loss of gel produced by hydrolysis of silicon alkoxide systems with different four alkoxy groups, the amounts of weight loss of gel containing large molecular alkoxy groups were much more than those of small molecular alkoxy group.

• Journal of the Korean Ceramic Society
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• v.32 no.7
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• pp.783-792
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• 1995

Sol-Gel derived ferroelectric PZT thin films were fabricated on ITO/Glass and Si/SiO2 substrates. In order to investigate the effect of catalysts on the densification and crystallization of PZT thin films, a nitric acid or ammonium hydroxide was added to the PZT stock solution at the state of partial hydrolysis reaction. The measured pH for a stable PZT sol was 5.2~9.3. In case of an acid-catalyzed PZT sol, a highly condensed particulate PZT sol was formed by accelerating the hydrolysis reaction. But weakly branched polymeric PZT sol was formed with a base-catalyzed condition. The difference in densification behavior was not found in the pH range of added catalyst, but the refractive index of PZT thin film was increased rapidly as the annealing temperature increased. The PZT thin film annealed at 54$0^{\circ}C$ for 10 min was fully densified and its refractive index was above 2.4. When the annealing temperature increased, the transition from the pyrochlore phase to perovskite appeared at 54$0^{\circ}C$. The base-catalyzed PZT thin film suppressed to form the pyrochlore phase and proceeded effectively to convert the perovskite phase. This was due to the formation of polymeric molecular structure by controlling the hydrolysis and condensation reaction through the additiion of the ammonium hydroxide.

• Journal of the Korean Ceramic Society
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• v.53 no.4
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• pp.456-462
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• 2016

$NaCaGd(MoO_4)_3:Ho^{3+}/Yb^{3+}$ ternary molybdates were successfully synthesized by microwave sol-gel method for the first time. Well-crystallized particles formed after heat-treatment at $900^{\circ}C$ for 16 h showed a fine and homogeneous morphology with particle sizes of $3-5{\mu}m$. Under excitation at 980 nm, the UC intensities of the doped samples exhibited strong yellow emissions based on the combination of strong emission bands at the 520-nm and 630-nm emission bands in the green and red spectral regions, respectively. The strong 520-nm emission band in the green region corresponds to the $^5S_2/^5F_4{\rightarrow}^5I_8$ transition of $Ho^{3+}$ ions, while the strong 630-nm emission band in the red region appears to be due to the $^5F_5{\rightarrow}^5I_8$ transition of the $Ho^{3+}$ ions. The optimal $Yb^{3+}:Ho^{3+}$ ratio was found at 9:1, as indicated by the composition-dependent quenching effect of $Ho^{3+}$ ions. The pump power dependence of the upconversion emission intensity and the Commission Internationale de L'Eclairage chromaticity coordinates of the phosphors were evaluated in detail.