• Applied Chemistry for Engineering
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• v.21 no.2
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• pp.230-237
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• 2010

A homologous series of linear liquid crystal dimers, ${\alpha},{\omega}$-bis(4-nitroazobenzene-4'-carbonyloxy)alkanes (NATWESn, n = 2~8, 10, the number of methylene units in the spacer) have been synthesized, and the thermal behavior of the series has been investigated. All the dimers formed enantiotropic nematic phases. The nematic-isotropic transition temperatures of the dimers and their entropy variation at the phase transition showed a large odd-even effect as a function of n. This behavior was rationalized in terms of the change in the average shape of the spacer on varing the parity of the spacer. The thermal stability and degree of order in the nematic phase and the magnitude of the odd-even effect of NATWESn were very similar to those of the corresponding ether compounds, while they were significantly different from those of the monomesogenic compounds, 4-{4'-(nitrophenylazo)phenoxy}alkanoyl chlorides and the side-chain liquid-crystalline polymers, the poly[1-{4-(4'-nitrophenylazo) phenoxycarbonylalkanoyloxy}ethylene]s. The results were discussed in terms of the 'irtual trimer model'by Imrie.

• Applied Chemistry for Engineering
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• v.26 no.3
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• pp.280-286
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• 2015

Two series of unsymmetric dimesogenic compounds containing a butylene or pentamethylene group as the flexible spacer were synthesized and their thermal and mesomorphic properties were studied. Mesogenic groups of the synthesized compounds consisted of a cholesteryl and an azobenzene group with lateral substituent. Chemical structures and mesomorphic properties of the synthesized compounds were investigated by FT-IR, $^1H$-NMR, differential scanning calorimeter (DSC), and polarizing optical microscope (POM). All synthesized compounds, apart from $D5-OCH_3$, showed enantiotropic liquid crystal phases. Compounds having an even number of carbon atoms in the flexible spacer exhibited wide mesophase temperature ranges and high isotropic transition temperatures. Regarding the effect of lateral substituents, compounds with bulky substituents exhibited decreased mesophase temperature ranges and isotropic transition temperatures, while those with polar substituents showed the increased thermal stability of the smectic phase.

• Bulletin of the Korean Chemical Society
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• v.32 no.7
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• pp.2267-2273
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• 2011

A novel energetic material, 1-amino-1-(2,4-dinitrophenylhydrazinyl)-2,2-dinitroethylene (APHDNE), was synthesized by the reaction of 1,1-diamino-2,2-dinitroethylene (FOX-7) and 2,4-dinitrophenylhydrazine in N-methyl pyrrolidone (NMP) at 110 $^{\circ}C$. The theoretical investigation on APHDNE was curried out by B3LYP/6-311+$G^*$ method. The IR frequencies analysis and NMR chemical shifts were performed and compared with the experimental results. The thermal behavior of APHDNE was studied by DSC and TG/DTG methods, and can be divided into two crystal phase transition processes and three exothermic decomposition processes. The enthalpy, apparent activation energy and pre-exponential factor of the first exothermic decomposition reaction were obtained as -525.3 kJ $mol^{-1}$, 276.85 kJ $mol^{-1}$ and $10^{26.22}s^{-1}$, respectively. The critical temperature of thermal explosion of APHDNE is 237.7 $^{\circ}C$. The specific heat capacity of APHDNE was determined with micro-DSC method and theoretical calculation method, and the molar heat capacity is 363.67 J $mol^{-1}K^{-1}$ at 298.15 K. The adiabatic time-to-explosion of APHDNE was also calculated to be a certain value between 253.2-309.4 s. APHDNE has higher thermal stability than FOX-7.

• Polymer(Korea)
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• v.32 no.3
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• pp.230-238
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• 2008

The thermal and optical properties of cellobiose octa(cholestryloxycarbonyl)alkanoates CCCBn, $n=2{\sim}8$,10, the number of methylene units in the spacer) were investigated. All the samples formed monotropic cholesteric phases with left-handed helical structures. CCBn with n=2 or 10, in contrast with CCBn with $3{\leq}n{\leq}8$, did not display reflection colors over the full cholesteric range, suggesting that the helical twisting power of the cholesteryl group highly depends on the length of the spacer connecting the cholesteryl group to the cellobiose chain. The isotropic-cholestropic transition ($T_{ic}$) and glass transition temperatures decreased with increasing n and showed no odd-even effect. The transition entropy at $T_{ic}$ increased with increasing n from 2 up 6, but at n=7 it drops significantly and then increased again with increasing n from 8 to 10. The sharp change at n=7 may be attributed to a difference in arrangement of the side groups. The thermal stability and degree of order in the mesophase and the temperature dependence of the optical pitch observed for CCBn were significantly different from those reported for the cellulose tri(cholesteryloxycarbonyl)alkanoates and glucose penta(cholesteryloxycarbonyl)alkanoates. The results were discussed in terms of the differences in the degree of polymerization, the number of the mesogenic units per mole-glucose unit, and the conformation of the molecules.

• Journal of the Korean Institute of Gas
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• v.2 no.1
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• pp.59-65
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• 1998

Morphology and thermal properties of polyurethane synthesized from 4,4'-diphenylmethane diisocyanate (MDI), polyester polyol, and 1,4-butane diol are investigated using fourier transform infrared spectroscopy (FT-IR), differential scanning calorimeter (DSC), and dynamic mechanical thermal analysis (DMTA). From the FT-IR study, it is found that the stretching peaks of hydrogen bonded N-H and C=O are shifted to the low frequencies with the increase of hard segment content of the polyurethanes. The shift of the stretching peaks of hydrogen bonded N-H and C=O indicates that the degree of hydrogen bonding is increased. From the DSC study, it appears that the glass transition temperature ($T_g$) of the polyurethanes is increased with the increase of the hard segment content. Also, it is found that the polyurethanes investigated in this study have the homogeneous network structure due to the high functionality of the MDI. From the DMTA study, transition of the soft segment was not found. Therefore it is concluded that the polyurethanes investigated in this study have the one-phase morphology which is consistent with the DSC results.

• Journal of the Mineralogical Society of Korea
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• v.31 no.3
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• pp.161-172
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• 2018

Multi-anvil press (MAP) is one of the high pressure apparatuses and often generates the pressure-conditions ranging from 5 to 25 GPa and temperature-conditions up to $2,300^{\circ}C$. The MAP is, therefore, suitable to explore the pressure-induced structural changes in diverse earth materials from Earth's mantle and the bottom of the mantle transition zone (~660 km). In this study, we present the experimental results for pressure-load calibration of the 1,100-ton multi-anvil press equipped in the authors' laboratory. The pressure-load calibration experiments were performed for the 14/8 step, 14/8 G2, 14/8 HT, and 18/12 assembly sets. The high pressure experiments using ${\alpha}$-quartz, wollastonitestructure of $CaGeO_3$, and forsterite as starting materials were analyzed by powder X-ray diffraction spectroscopy. The phase transition of each mineral indicates the specific pressure that is loaded to a sample at $1,200^{\circ}C$: a transition of ${\alpha}$-quartz to coesite at 3.1 GPa, that of garnet-structure of $CaGeO_3$ to perovskite-structure at 5.9 GPa, that of coesite to stishovite at 9.2 GPa, and that of forsterite to wadsleyite at 13.6 GPa. While the estimated pressure-load calibration curve is generally consistent with those obtained in other laboratories, the deviation up to 50 tons is observed at high pressure above 10 GPa. This is partly because of the loss of oil pressure at high pressure resulting from the differences in a sample chamber, and the frictional force between pressure medium and second anvil. We also report the ${\sim}200^{\circ}C/mm$ of thermal gradient in the vertical direction of the sample chamber of 14/8 HT assembly. The pressure-load calibration curve and the observed thermal gradient within the sample chamber can be applied to explain the structural changes and the relevant macroscopic properties of diverse crystalline and amorphous earth materials in the mantle.

• Applied Chemistry for Engineering
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• v.26 no.4
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• pp.427-431
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• 2015

In this study, vanadium dioxide ($VO_2$) powder well known as a thermochromic material was prepared from $V_2O_5$ powder and oxalic acid dihydrate by hydrothermal and calcination process at various conditions. The chemical bonding and crystal structures in addition to thermal property of samples were determined using FE-SEM, XRD, XPS, and DSC. Also, spectroscopic and thermochromic properties of film samples were analyzed by UV-Vis-NIR spectroscopy after the thin film was prepared from the sol dispersed with the size of below 50 nm by the ball-milling of powder sample. With increasing the calcination temperature, the phase transition temperature of samples increased from $40^{\circ}C$ to $70^{\circ}C$ due to the increase of particle size.

• Journal of Sensor Science and Technology
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• v.15 no.4
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• pp.257-262
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• 2006

A Fe-C eutectic cell for thermocouple calibration was manufactured and tested to investigate its phase transition characteristics in the thermocouple thermometry. It was observed that the freezing plateaus were strongly affected by the freeze-inducing temperature $T_{f}$. In case of the melting process, the melting plateau was influenced by the previous thermal history. As $T_{f}$. in the previous freezing was lower, the melting plateau became lower with a temperature dependence as small as $-0.0015^{\circ}C/^{\circ}C$. Therefore, it was found that the freeze-inducing temperature should be fixed to obtain a reproducible phase transition temperature in the melting. After fixing $T_{f}$, the melting process was examined and it was found that long and flat melting plateau was obtained within a reproducibility of about ${\pm}0.01^{\circ}C$. Based on the observed results, it was recommended that Fe-C eutectic temperature be best realized for the melting process with a melt-inducing temperature of $+3^{\circ}C$ above the expected liquidus temperature after freezing at $-5^{\circ}C$ below the solidus temperature.

• Korean Journal of Metals and Materials
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• v.50 no.10
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• pp.775-783
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• 2012

The effect of thermal annealing on the in-situ growth characteristics of intermetallics (IMCs) and the mechanical strength of Cu pillar/Sn-3.5Ag microbumps are systematically investigated. The $Cu_6Sn_5$ phase formed at the Cu/solder interface right after bonding and grew with increased annealing time, while the $Cu_3Sn$ phase formed at the $Cu/Cu_6Sn_5$ interface and grew with increased annealing time. IMC growth followed a linear relationship with the square root of the annealing time due to a diffusion-controlled mechanism. The shear strength measured by the die shear test monotonically increased with annealing time. It then changed the slope with further annealing, which correlated with the change in fracture modes from ductile to brittle at a critical transition time. This is ascribed not only to the increasing thickness of brittle IMCs but also to the decreasing thickness of the solder, as there exists a critical annealing time for a fracture mode transition in our thin solder-capped Cu pillar microbump structures.

• Polymer(Korea)
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• v.29 no.6
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• pp.575-580
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• 2005

The hydroxy terminated aliphatic hyperbranched polyesters having different generations were synthesized by using melt polycondensation procedure. Then, the terminal groups of hyperbranched polyesters were modified by using acryloyl chloride and characterized by $\^{1}H$-NMR and GPC techniques. As a result of the modification of terminal groups for hyperbranched polyesters, the phase of the polymers were changed from sticky solid to high viscous liquid indicating that the glass transition temperatures of modified hyperbranched polyesters were lower than the original one. The thermal stabilities of hydroxy terminated hyperbranched polyesters were higher than those of terminal group-modified polymers.