• Bulletin of the Korean Chemical Society
• /
• v.17 no.7
• /
• pp.643-647
• /
• 1996

1,2-Disubstituted chiral calix[4]arene "25-(3,5-dinitrobenzoyloxy)-26-methoxy-27,28-dihydroxycalix[4]arene" was synthesized by the reaction of 25-(3,5-dinitrobenzoyloxy)-calix[4]arene with methyl iodide in the presence of K2CO3. Methylation was occurred at the 26-position of calix[4]arene. The partial cone conformation and 1,2-substitution were characterized based on the 1H NMR, 13C NMR and X-ray diffraction analysis. The crystal structure has been determined by X-ray diffraction method. The crystals are orthorhombic, Pbca, a=10.652(1), b=17.687(1), c=32.247(3) Å, Z=8, V=6075.4(9) Å3, Dc=1.38gcm-3. The intensity data were collected on an Enraf-Nonius CAD-4 Diffractometer with a graphite monochromated Cu-Kα radiation. The structure was solved by direct method and refined by full-matrix least-squares methods to a final R value of 0.050 for 2368 observed reflections. The molecule is in the partial cone conformation. It has two strong intramolecular hydrogen bonds of O(1D)-H…O(1C)-H…O(1B).

• Bulletin of the Korean Chemical Society
• /
• v.7 no.5
• /
• pp.331-334
• /
• 1986

The crystal structure of thiamin tetrahydrofurfuryl disulfide, one of the ring-opened derivatives of thiamin, has been determined by the X-ray diffraction methods. The crystal is monoclinic with cell dimensions of a = 8.704 (1), b = 11.207 (2), c = 21.260 (3) ${\AA}$ and ${\beta}$ = 92.44 (2)$^{circ}$, space group P2$_{1}$/c and Z = 4. The structure was solved by direct methods and refined to R = 0.076 for 1252 observed reflections measured on a diffractometer. The molecule assumes a folded conformation in which the pyrimidine and the tetrahydrofurfuryl rings are on the same side of the ethylenic plane. The pyrimidinyl, N-formyl and ethylenic planes are mutually perpendicular to each other and the N(3)-C(4) bond retains a single bond character. The structure is stabilized by an intramolecular N(4'${\alpha})-H{\cdots}O(2{\alpha}$) hydrogen bond. The molecules are connected via N(4'${\alpha}$)-H{\cdots}(N3')$ and O(5${\gamma})-H{\cdots}(N1')$ hydrogen bonds, forming a two-dimensional hydrogen-bonding network. The tetrahydrofurfuryl ring is dynamically disordered. The overall conformation as well as the packing mode is very similar to that of thiamin propyl disulfide.

• Journal of Welding and Joining
• /
• v.21 no.3
• /
• pp.78-84
• /
• 2003

The changes of microstructure and hardness of TLP bonds of directionally solidified Ni base superalloy, GTD-111, with variation of homogenizing and aging treatment were investigated. The specimens were bonded at 1403K for 7.2ks using different insert metals such as MBF-50, MBF-80 and MBF-90 and they were homogenized at 1393K with various holding time. At center of bonded interlayer homogenized for hold time 30h, the contents of aluminum and titanium were approximately 90% and 95% of base metal, respectively. In this study, aging was performed at three different kinds : one step aging ; 1113K $\times$ 16h, two step aging ; 1113K $\times$ 10h ⇒ 1103K $\times$ 10h, three step aging ; 1113K $\times$ 10h ⇒ 1103K $\times$ 8h ⇒ 922K $\times$ 24h. ${\gamma}$' volume fraction and hardness of joints were high in the sequence of one step, two step and three step aging, whereas ${\gamma}$' volume fraction and hardness of joints obtained by three step aging treatment were higher than those of raw material. Tensile properties of joints bonded with MBF-80 and MBF-90, homogenized at 1393K for 30h and then three step aged became excellent than those of raw material, however, joint bonded with MBF-50 was poor.

• Korean Journal of Materials Research
• /
• v.23 no.7
• /
• pp.359-365
• /
• 2013

We investigated the nanostructural, chemical and optical properties of nc-Si:H films according to deposition conditions. Plasma enhanced chemical vapor deposition(PECVD) techniques were used to produce nc-Si:H thin films. The hydrogen dilution ratio in the precursors, [$SiH_4/H_2$], was fixed at 0.03; the substrate temperature was varied from room temperature to $600^{\circ}C$. By raising the substrates temperature up to $400^{\circ}C$, the nanocrystalite size was increased from ~2 to ~7 nm and the Si crystal volume fraction was varied from ~9 to ~45% to reach their maximum values. In high-resolution transmission electron microscopy(HRTEM) images, Si nanocrystallites were observed and the crystallite size appeared to correspond to the crystal size values obtained by X-ray diffraction(XRD) and Raman Spectroscopy. The intensity of high-resolution electron energy loss spectroscopy(EELS) peaks at ~99.9 eV(Si $L_{2,3}$ edge) was sensitively varied depending on the formation of Si nanocrystallites in the films. With increasing substrate temperatures, from room temperature to $600^{\circ}C$, the optical band gap of the nc-Si:H films was decreased from 2.4 to 1.9 eV, and the relative fraction of Si-H bonds in the films was increased from 19.9 to 32.9%. The variation in the nanostructural as well as chemical features of the films with substrate temperature appears to be well related to the results of the differential scanning calorimeter measurements, in which heat-absorption started at a substrate temperature of $180^{\circ}C$ and the maximum peak was observed at ${\sim}370^{\circ}C$.

• Journal of the Korean Chemical Society
• /
• v.18 no.2
• /
• pp.126-131
• /
• 1974

Trioctylamine-and tricaprylylmethylammonium chloride-tungstate salts have been prepared by solvent extraction from the sodium tungstate solution of various acidities(pH = 2, 4, 6). The molecular weights of the amine-tungstate salts thus obtained could be cryoscopically measured in benzene by means of a home-built Wheatstone bridge utilizing thermistor with sensitivity of 1/$4000^{\circ}C$. The cryoscopic data along with the results of chemical analysis and infrared spectra of the salts indicate that the amine-tungstates prepared at pH = 2 and 4 are all metatungstate whereas the salt obtained at pH = 6 is an unknown form quite different from the expected paratungstate.R = 0.14. By hydrogen bonding a guanidyl nitrogen of a sulfaguanidine molecule is linked to the sulfonyl oxygens of the other molecules indirectly through two different water molecules. The role of water molecule is both a .
nor and an acceptor in hydrogen-bonding formation and these hydrogen bonds are tetrahedrally o？ented. The hydrogen-bonding networks form infinite molecular layers parallel to (001) plane.

• Analytical Science and Technology
• /
• v.19 no.4
• /
• pp.309-315
• /
• 2006

Two piperazine-templated metal sulfate complexes, $(C_4N_2H_{12})[Ni(H_2O)_6](SO_4)_2$, I and ($C_4N_2H_{12}$) $[Co(H_2O)_6](SO_4)_2$, II, have been synthesized by hydro/solvothermal reactions and their crystal structures analyzed by single crystal X-ray diffraction methods. Complex I crystallizes in the monoclinic system, $P2_1/n$ space group, a=12.920(3), b=10.616(2), $c=13.303(2){\AA}$, ${\beta}=114.09(1)^{\circ}$, Z=4, $R_1=0.030$ for 3683 reflections; II: monoclinic $P2_1/n$, a=12.906(3), b=10.711(2), $c=13.303(2){\AA}$, ${\beta}=114.10(2)^{\circ}$, Z=4, $R_1=0.032$ for 4010 reflections. The crystal structures of the piperazine-templated metal(II) sulfates demonstrate zero-dimensional compound constituted by diprotonated piperazine cations, metal(II) cations and sulfate anions. The structures of complex I and II are substantially isostructural to that of the previously reported our piperazine-templated copper(II) sulfate complex $(C_4N_2H_{12})[Cu(H_2O)_6](SO_4)_2$. The central metal(II) atoms are coordinated by six water molecules in the octahedral geometry. The crystal structures are stabilized by three-dimensional networks of the $O_{water}-H{\cdots}O_{sulfate}$ and $N_{pip}-H{\cdots}O_{sulfate}$ hydrogen bonds between the water molecules and sulfate anions and protonated piperazine cations. Based on the results of thermal analysis, the thermal decomposition reactions of the complex I was analyzed to have three distinctive stages whereas the complex II proceed through several stages.

• Membrane and Water Treatment
• /
• v.7 no.5
• /
• pp.417-431
• /
• 2016

Poly(vinylidene fluoride) (PVDF) powder was treated with aqueous sodium hydroxide to obtain partially defluorinated fluoropolymers with expected properties such as improving hydrophilicity and fouling resistance. Raman spectrum and FT-IR results confirmed the existence of conjugated carbon double bonds after alkaline treatment. As the concentration increased, the degree of defluorination increased. The morphology and structure of membranes were examined. The permeation performance was investigated. The results showed that membrane's hydrophilicity increased with increase of the percentage of alkaline treated PVDF powder. Moreover, in terms of the water contact angle, it decreased from $92^{\circ}$ to a minimum of $68^{\circ}$; while water up take increased from 128 to 138%. Fluxof pure water and the cleaning efficiency increased with the increase of alkaline treated PVDF powder. The fouling potential also decreased with the increase of the percentage of alkaline treated PVDF powder. The reason that makes blending PVDF show different characteristics because of partial defluorination, which led the formation of conjugated C = C bonds and the inclusion of oxygen functionalities. The polyene structure followed by hydroxide attack to yield hydroxyl and carbonyl groups. Therefore, the hydrophilicity of blending membrane was improved. The SEM and porosity measurements showed that no obvious variations of the pore dimensions and structures for blend membranes were observed. Mechanical tests suggest that the high content of the alkaline treated PVDF result in membranes with less tolerance of tensile stress and higher brittleness. TGA results exhibited that the blend of alkaline treated PVDF did not change membrane thermal stability.

• Proceedings of the KIEE Conference
• /
• 1996.07c
• /
• pp.1446-1449
• /
• 1996

Thin films of diamond-like carbon(DLC) have been deposited using a magnetron plasma-enhanced chemical vapor deposition(PECVD) method with an rf(13.56 MHz) plasma of $C_{3}H_{8}$. From the Langmuir probe I-V characteristics, it can be observed that increasing the magnetic field yields an increase of the temperature($T_e$) and density($N_e$) of electron. At a magnetic field of 82 Gauss, the estimated values of $T_e$ and $N_e$ are approximately $1.5\;{\times}\;10^5$ K(13.5 eV) and $1.3\;{\times}\;10^{11}\;cm^{-3}$, respectively. Such a highly dense plasma can be attributed to the enhanced ionization caused by the cyclotron motion of electrons in the presence of a magnetic field. On the other hand, the negative dc self-bias voltage($-V_{sb}$) decreases with an increasing magnetic field, which is irrespective of gas pressure in the range of $1{\sim}7$ mTorr. This result is well explained by a theoretical model considering the variation of $T_e$. Deposition rates of DLC films increases with a magnetic field. This may be due to the increased mean free path of electrons in the magnetron plasma. Structures of DLC films are examined by using various techniques such as FTIR and Raman spectroscopy. Most of hydrocarbon bonds in DLC films prepared consist of $sp^3$ tetrahedral bonds. Increasing the rf power leads to an enhancement of cross-linking of carbon atoms in DLC films. At approximately 140 W, the maximum film density obtained is about 2.4 $g/cm^3$.

• Advances in nano research
• /
• v.7 no.1
• /
• pp.39-49
• /
• 2019

This paper focuses on two main objectives. The first one is to exploit an energy equivalent model and finite element method to evaluate the equivalent Young's modulus of single walled carbon nanotubes (SWCNTs) at any orientation angle by using tensile test. The calculated Young's modulus is validated with published experimental results. The second target is to exploit the finite element simulation to investigate mechanical buckling and natural frequencies of SWCNTs. Energy equivalent model is presented to describe the atomic bonding interactions and their chemical energy with mechanical structural energies. A Program of Nanotube modeler is used to generate a geometry of SWCNTs structure by defining its chirality angle, overall length of nanotube and bond length between two adjacent nodes. SWCNTs are simulated as a frame like structure; the bonds between each two neighboring atoms are treated as isotropic beam members with a uniform circular cross section. Carbon bonds is simulated as a beam and the atoms as nodes. A finite element model using 3D beam elements is built under the environment of ANSYS MAPDL environment to simulate a tensile test and characterize equivalent Young's modulus of whole CNT structure. Numerical results are presented to show critical buckling loads, axial and transverse natural frequencies of SWCNTs with different orientation angles and lengths. The understanding of mechanical behaviors of CNTs are essential in developing such structures due to their great potential in wide range of engineering applications.

• Nuclear Engineering and Technology
• /
• v.54 no.12
• /
• pp.4514-4521
• /
• 2022

In this study, the effects of heat and radiation on the degradation behaviour of fluoroelastomer under simulated normal operation and a severe accident environment were investigated using sequential testing of gamma irradiation and thermal degradation. Tensile properties and Shore A hardness were measured, and thermogravimetric analysis was used to evaluate the degradation behaviour of fluoroelastomer. Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy were used to characterize the structural changes of the fluoroelastomer. Heat and radiation generated in nuclear power plant break and deform the chemical bonds, and fluoroelastomer exposed to these environments have decreased C-H and functional groups that contain oxygen and double bonds such as C-O, C=O and C=C were generated. These functional groups were formed by auto oxidation by reacting free radicals generated from the cleaved bond with oxygen in the atmosphere. In this auto oxidation reaction, crosslinks were generated where bonded to each other, and the mobility of molecules was decreased, and as a result, the fluoroelastomer was hardened. This hardening behaviour occurred more significantly in the severe accident environment than in the normal operation condition, and it was found that thermal stability decreased with the generation of unstable structures by crosslinking.