• Korean Journal of Materials Research
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• v.11 no.9
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• pp.786-791
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• 2001

$\alpha$,$\omega$-Bis(4-glycidyloxybenzylidene-4-aminophenyl)methane (BGBAM) was synthesized from the initial materials, 4-hydroxylbenzaldehyde (HBA), 4,4'-methylenedianiline (MDA) and epichlorohydrin. The DSC trace for BGBAM shows two endotherms associated with the liquid crystalline phase transition around $104.2^{\circ}C$ and the isotropic transition around $171.2^{\circ}C$, and it also has a broad exotherm in the range of $178~300^{\circ}C$ due to the anionic homopolymerization of BGBAM. DSC curve for the curing of BGBAM with hexamethylene diamine (HMD) shows an endothermic peak around $93^{\circ}C$ attributed to the melting of BGBAM. It also has three exothermic peaks around $128.4^{\circ}C$ and $180.2^{\circ}C$ associated with the epoxide-amine reaction and weak peak in the range of $200~263^{\circ}C$ related to the anionic homopolymerization between the unreacted epoxide groups. The activation energy values of cure reaction by Kissinger method are 66.5, 67.3 and 90.6 kJ/mol for $T_{pl},\; T_{p2}\; and \;T_{p3},\; respectively$. The kinetic parameters by isoconverional method are similar value to those from Kissinger method.

• Applied Chemistry for Engineering
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• v.7 no.2
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• pp.387-392
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• 1996

Natural zeolite/epoxy resin composites were prepared and the cure kinetics was studied by dynamic DSC analysis. With the increments of natural zeolite content, the reaction starting temperature and the exothermic peak temperature were decreased. When diglycidyl ether of bisphenol A(DGEBA)/4,4'-methylene dianiline(MDA)/malononitrile(MN, 10phr) was filled with 20phr of zeolite, DSC thermogram had one peak and when it was filled with 30phr of zeolite, a shoulder appeared on the DSC thermogram. With the filling of 40phr of zeolite, DSC thermogram was separated into two peaks and the activation energy of the first peak, $Ea_1$ was 12.30 kJ/mol and that of the second peak, $Ea_2$ was 12.70 kJ/mol.

• Applied Chemistry for Engineering
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• v.16 no.5
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• pp.628-634
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• 2005

Zirconia-alumina polymer precursor was prepared from zirconium acetylacetonate (ZA). paluminium nitrate (AN), polyethylene glycol (PEG), and ethyl alcohol via an organic-inorganic solution technique. The thermal properties and viscosity of the polymer precursor were measured by differential scanning calorimetry (DSC), thermograbimetric analyzer (TGA), and dynamic viscometer. The vigorous exothermic reaction with volume expansion occurred at $140^{\circ}C$. The volume expansion was caused by abrupt decomposition of the organic group in metal compounds and the metal ions-PEG reaction. The evidences for these reactions were confirmed by FT-IR and $^{13}C$ solid NMR results. The peak intensity at N-O, O-H and C=C decreased with increasing temperature. This indicated that the decomposition of metal compounds and the metal ions-PEG reaction occurred during the vigorous exothermic reaction. At $800^{\circ}C$ for 2 h, the porous powders transformed to the crystalline $ZrO_2-Al_2O_3$ composites.

• Journal of the Korean Society of Safety
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• v.20 no.2 s.70
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• pp.56-60
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• 2005

We studied fire properties of MOF(Metering Out Fit) insulation cover and field condition of 22.9kV power receiving system. $49.5\%$ of formal equipments were installed indoors, whereas $40.8\%$ of informal equipments were installed as H-type. Insulation treatment was not done at a $22.4\%$ ratio of main line($27.7\%$ of transformer, $70.2\%$ of COS, $10.4\%$ of MOF). Fire pattern analysis showed that the fire started at the secondary part of OC wire. In the result of DTA(Differential Thermal Analysis), normal cover showed exothermic reactions at $310^{\circ}C,\;399^{\circ}C\;and\;510^{\circ}C$ (endothermic reactions at $382^{\circ}C$). Whereas damaged cover showed exothermic reactions at $412^{\circ}C$(endothermic reactions at $389^{\circ}C$). In the result of TGA(Thermo Gravimetric Analysis), the thermal weight change of normal cover was similar compared to damaged cover. In the result of FT-IR analysis, normal cover showed absorption peaks at $3,024cm^{-l},\;2,921cm^{-l},\;1,600cm^{-1},\;1,492cm^{-1},\;1,451cm^{-1},\;1,154cm^{-l},\;1,027cm^{-1},\;906cm^{-1}$. Whereas, in case of tracked cover, the absorption peaks that were shown in normal cover disappeared and different absorption peak was shown at $966cm^{-1}$.

• 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.

• Korean Journal of Materials Research
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• v.14 no.5
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• pp.310-314
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• 2004

Mechanical alloying (MA) of Ti-50.0～66.7at%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-50.0～59.6at%Si powders showed that there were exothermic peaks during MA, indicating TiSi, $TiS_2$, and $Ti_{5}$ $Si_4$ phase formation by a rapid exothermic reaction of self-propagating high-temperature synthesis (SHS). Those of Ti-59.8～66.7 at%Si powders, however, showed that there were no peaks during MA, indicating any Ti silicide was not synthesised until MA 240 min. For Ti-50.0～59.6at%Si powders, the critical milling times for SHS increased from 34.5 min to 89.5 min and the temperature rise, $\Delta$T (=peak temperature-onset temperature) decreased form $26.2^{\circ}C$ to $17.1^{\circ}C$ as at%Si increased. The critical composition of Si for SHS reaction was found to be 59.6at% and the critical value of the negative heat of formation of Ti-59.6at%Si to be -1.48 kJ/g.

• Bulletin of the Korean Chemical Society
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• v.11 no.4
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• pp.276-281
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• 1990

The equivalent conductance of univalent cation (potassium, silver, thallium and ammonium) perchlorates in methanol containing 18-membered crown ethers, 18-crown-6 (18C6) and 1,10-dithia-18-crown-6 (DT18C6) were measured at different temperatures. The equivalent conductances of ammonium perchlorate were increased by increasing content of DT18C6 exceptionally, due to more favorable solvations than complexations. From the equivalent conductance changes, the formation constants for 1:1 compmlexes have been determined, and the values of enthalpy and entropy changes have been calculated. The complexations of 18C6 and DT18C6 with the univalent cations under investigation are all exothermic and the ${\Delta}$S values are all negative and no considerable differences around 50 J/ (k mol). The selectivity order of 18C6 is $K^+ > Tl^+ > Ag^+ > NH_4^+$, while that of DT18C6 is $Ag^+ > Tl^+ > NH_4^+ > K^+$. By sulfur substitutions in 18C6 result in significant decrease in stability, but the stability of $Ag^+$-DT18C6 complex are $10^4$ times larger than those of $K^+$. This increase of stabilities for $Ag^+$-DT18C6 complex are primary due to the result of favorable exothermic heat of reaction between the polarizable soft cation and soft sulfur centers. In NMR experiment, the stepwise additions of cation perchlorates into crown ether solutions induced two major spectral changes. First, the resonance all shift down field and the cation induced shifts were linear up to 1:1 cation/crown ratio, above which no further changes were observed. On the basis of these results, it could be concluded that 1:1 complex is formed. Second, the magnitudes of cation induced shifts were different each other in same ligand. By addition of silver ion to the solution of DT18C6, the largest shift of proton peak near the sulfur atom was observed. These effects are also arisen from the results of covalent bonding between "soft-soft" interactions.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2006.11a
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• pp.212-213
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• 2006

BSCT(60/30/10) powder specimens were fabricated by sol-gel method and BSCT thick films were fabricated by screen-printing method. The coating and drying procedure was repeated 6 times. Then the structural properties as a function of the sintering temperature. As a result of the TG-DTA, exothermic peak was observed at around $670^{\circ}C$ due to the crystalline phase. The BSCT sintered at $1430^{\circ}C$ showed the cubic perovskite structure. The prosity and thickness of the BSCT thick films was decreased with sintering temperature. The thickness of BSCT thick films at $1420^{\circ}C$ was approximately $40{\mu}m$.

• Proceedings of the Polymer Society of Korea Conference
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• 2006.10a
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• pp.305-305
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• 2006

The molecular structure and dynamics of inclusion compounds (ICs) consisting of n-perfluoroalkane (PFA) guests and ${\Box}-cyclodextrin$ (${\Box}-CD$) host were investigated using $^{19}F$ magic angle spinning (MAS) and $^{1}H{\to}^{19}F$ cross polarization (CP) / MAS NMR spectroscopy with the aid of thermal analyses, FT-IR spectroscopy, X-ray diffraction, and $^{1}H{\to}^{19}F$ CP/MAS technique revealed that $C_{9}F_{20}$ molecules included in ${\Box}-CD$ undergo vigorous molecular motion and partly come out of the ${\Box}-CD$ channel above $80^{\circ}C$. In case of $C_{20}F_{42}/{\Box}-CD$, an exothermic peak is observed by differential scanning calorimetry (DSC) at ca. $40^{\circ}C$ which suggests that ${\Box}-CD$ molecules become mobile and commence rearrangements that form more ordered structures at higher temperatures.

• Journal of Welding and Joining
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• v.24 no.2
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• pp.57-63
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• 2006

In this study, the curing kinetics and thermal degradation of underfill were investigated using differential scanning calorimetry (DSC) and thermo gravimetry analysis (TGA). The mechanical and thermal properties of underfill were characterized using dynamic mechanical analysis (DMA) and thermo-mechanical analysis (TMA). Also, we presented on underfill dispensing process using Prostar tool. The non-isothermal DSC scans at various heating rates, the exothermic reaction peak became narrower with increasing the heating rate. The thermal degradation of underfill was composed of two processes, which involved chemical reactions between the degrading polymer and oxygen from the air atmosphere. The results of fluidity phenomena were simulated using Star CD program, the fluidity of the underfills with lower viscosity was faster.