• Proceedings of the Materials Research Society of Korea Conference
• /
• 2012.05a
• /
• pp.70.1-70.1
• /
• 2012

In-situ X-ray photoelectron spectroscopy (XPS) and infrared (IR) spectroscopy studies of SOFC cathode materials will be discussed in this presentation. The mixed conducting perovskites (ABO3) containing rare and alkaline earth metals on the A-site and a transition metal on the B-site are commonly used as cathodes for solid oxide fuel cells (SOFC). However, the details of the oxygen reduction reaction are still not clearly understood. The information about the type of adsorbed oxygen species and their concentration is important for a mechanistic understanding of the oxygen incorporation into these cathode materials. XPS has been widely used for the analysis of adsorbed species and surface structure. However, the conventional XPS experiments have the severe drawback to operate at room temperature and with the sample under ultrahigh vacuum (UHV) conditions, which is far from the relevant conditions of SOFC operation. The disadvantages of conventional XPS can be overcome to a large extent with a "high pressure" XPS setup installed at the BESSY II synchrotron. It allows sample depth profiling over 2 nm without sputtering by variation of the excitation energy, and most importantly measurements under a residual gas pressure in the mbar range. It is also well known that the catalytic activity for the oxygen reduction is very sensitive to their electrical conductivity and oxygen nonstoichiometry. Although the electrical conductivity of perovskite oxides has been intensively studied as a function of temperature or oxygen partial pressure (Po2), in-situ measurements of the conductivity of these materials in contact with the electrolyte as a SOFC configuration have little been reported. In order to measure the in-plane conductivity of an electrode film on the electrolyte, a substrate with high resistance is required for excluding the leakage current of the substrate. It is also hardly possible to measure the conductivity of cracked thin film by electrical methods. In this study, we report the electrical conductivity of perovskite $La_{0.6}Sr_{0.4}CoO_{3-{\delta}}$ (LSC) thin films on yttria-stabilized zirconia (YSZ) electrolyte quantitatively obtained by in-situ IR spectroscopy. This method enables a reliable measurement of the electronic conductivity of the electrodes as part of the SOFC configuration regardless of leakage current to the substrate and cracks in the film.

• Bulletin of the Korean Chemical Society
• /
• v.35 no.2
• /
• pp.587-596
• /
• 2014

A new ${\pi}$-stacked donor-acceptor (D-A) system, [Ru(1-([2,2'-bipyridine]-6-yl-methyl)-3-(2-cyclohexa-2',5'-diene-1,4-dionyl)-1H-imidazole)(2,2':6',2"-terpyridine)]$[PF_6]_2$ (ImQ_T), has been synthesized and characterized. Similar to its precedent, [Ru(6-(2-cyclohexa-2',5'-diene-1,4-dione)-2,2':6',2"-terpyridine)(2,2':6',2"-terpyridine)]$[PF_6]_2$ (TQ_T), this system has a cofacial alignment of terpyridine (tpy) ligand and quinonyl (Q) group, which facilitates an electron transfer through ${\pi}$-stacked manifold. Despite the presence of lowest-energy charge transfer transition from the Ru-based-HOMO-to-Q-based-LUMO (MQCT) predicted by theoretical calculations by using time-dependent density functional theory (TD-DFT), the experimental steady-state absorption spectrum does not exhibit such a band. The selective excitation to the Ru-based occupied orbitals-to-tpy-based virtual orbital MLCT state was thus possible, from which charge separation (CS) reaction occurred. The photo-induced CS and thermal charge recombination (CR) reactions were probed by using ultrafast visible-pump/mid-IR-probe (TrIR) spectroscopic method. Analysis of decay kinetics of Q and $Q^-$ state CO stretching modes as well as aromatic C=C stretching mode of tpy ligand gave time constants of <1 ps for CS, 1-3 ps for CR, and 10-20 ps for vibrational cooling processes. The electron transfer pathway was revealed to be Ru-tpy-Q rather than Ru-bpy-imidazol-Q.

• Bulletin of the Korean Chemical Society
• /
• v.29 no.5
• /
• pp.1038-1042
• /
• 2008

Mono and multilayer TiO2(Fe, $PEG_{600}$) films were deposited by the dip-coating on $SiO_2$/glass substrate using sol-gel method. In an attempt to improve the antibacterial properties of doped $TiO_2$ films, the influence of the iron oxides and polyethilenglycol ($PEG_{600}$) on the morphological, optical, surface chemical composition and biological properties of nanostructured layers was studied. Complementary measurements were performed including Spectroscopic Ellipsometry (SE), Scanning Electron Microscopy (SEM) coupled with the fractal analysis, X-Ray Photoelectron Spectroscopy (XPS) and antibacterial tests. It was found that different concentrations of Fe and $PEG_{600}$ added to coating solution strongly influence the porosity and morphology at nanometric scale related to fractal behaviour and the elemental and chemical states of the surfaces as well. The thermal treatment under oxidative atmosphere leads to films densification and oxides phase stabilization. The antibacterial activity of coatings against Escherichia Coli bacteria was examined by specific antibacterial tests.

• Journal of the Korean Wood Science and Technology
• /
• v.29 no.4
• /
• pp.89-96
• /
• 2001

Three isoflavones and one isoflavanone were isolated from the wood of Sophora japonica (Leguminosae) which has been selected due to its high antifungal activity among the tested species, Four compounds were identified as 5,7-dihydroxy-4',6-dimethoxyisoflavone (irisolidone), 5,7-dihydroxy-4'-methoxyisoflavone (biochanin A), 7-hydroxy-4'-methoxyisoflavone (formononetin) and 7-hydroxy-4'-methoxy-isoflavanone by Mass and NMR spectroscopic analysis. The antifungal activity of the isoflavonoids was tested by medium dilution method and showed low antifungal activity indicating that the other compounds may contribute to high activity of the wood extractives of S. japonica.

• Bulletin of the Korean Chemical Society
• /
• v.25 no.11
• /
• pp.1661-1666
• /
• 2004

The reaction of titanium tetraisopropoxide with 2 equiv of N,N-diethyl acetoacetamide affords Ti($O^iPr)_2(CH_3COCHCONEt_2)_2$ (1) as colorless crystals in 80% yield. Compound 1 is characterized by spectroscopic (Mass and $^1H/^{13}C$ NMR) and microanalytical data. Molecular structure of 1 has been determined by a single crystal X-ray diffraction study, which reveals that it is a monomeric, cis-diisopropoxide and contains a six coordinate Ti(IV) atom with a cis($CONEt_2$), trans($COCH_3$) configuration (1a) in a distorted octahedral environment. Variable-temperature $^1H$ NMR spectra of 1 indicate that it exists as an equilibrium mixture of cis, trans (1a) and cis, cis (1b) isomers in a 0.57 : 0.43 ratio at -20$^{\circ}C$ in toluene-$d_8$ solution. Thermal properties of 1 as a MOCVD precursor for titanium dioxide films have been evaluated by thermal gravimetric analysis and vapor pressure measurement. Thin films of pure anatase titanium dioxide (after annealing above 500$^{\circ}C$ under oxygen) have been grown on Si(100) with precursor 1 in the substrate temperature range of 350- 500$^{\circ}$ using a bubbler-based MOCVD method.

• Macromolecular Research
• /
• v.11 no.5
• /
• pp.297-302
• /
• 2003

The imidization and cure reaction of a thermosetting phenylethynyl-terminated amic acid (LaRC PETI-5) in film form have been monitored as a function of temperature by means of a steady-state fluorescence technique using a front-face illumination method. The variation of the fluorescence emission spectra of LaRC PETI-5 can be divided into four temperature regions; Region I: below 15$0^{\circ}C$, Region II: 150-25$0^{\circ}C$, Region III: 250-35$0^{\circ}C$, and Region IV: above 35$0^{\circ}C$. The fluorescence spectra in Region I are largely influenced by residual N-methyl-2pyrrolidinone in the polymer and also slightly by partial imidization of the polymer. There is a combined effect of imidization and solvent removal on the fluorescence behavior in Region II. The spectra in Regions III and IV are due significantly to the cure reaction of LaRC PETI-5 and to a post-cure effect of the polyimide, respectively. This spectroscopic evidence indicating the transformation of the amic acid imide oligomer into the corresponding polyimide via imidization and cure, agrees well with thermal analysis results obtained previously. The intermediate stage of cure in the range of 250-30$0^{\circ}C$ predominantly influences the change of the fluorescence intensity. The later stage above 30$0^{\circ}C$ significantly influences the position of the spectrum. This fluorescence study also supports the mechanism proposed in earlier work that the crosslinking reaction takes place at the reaction sites in the conjugated polyene and the phenylethynyl end group in the polyimide chain.

• Journal of Ginseng Research
• /
• v.44 no.2
• /
• pp.215-221
• /
• 2020

Background: Panax ginseng has been used for a variety of medical purposes in eastern countries for more than two thousand years. From the extensive experiences accumulated in its long medication use history and the substantial strong evidence in modern research studies, we know that ginseng has various pharmacological activities, such as antitumor, antidiabetic, antioxidant, and cardiovascular system-protective effects. The active chemical constituents of ginseng, ginsenosides, are rich in structural diversity and exhibit a wide range of biological activities. Methods: Ginsenoside constituents from P. ginseng flower buds were isolated and purified by various chromatographic methods, and their structures were identified by spectroscopic analysis and comparison with the reported data. The 3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H- tetrazolium bromide method was used to test their cytotoxic effects on three human cancer cell lines. Results: Six ginsenosides, namely 6'-malonyl formyl ginsenoside F₁ (1), 3β-acetoxyl ginsenoside F₁ (2), ginsenoside Rh₂₄ (6), ginsenoside Rh₂₅ (7), 7β-hydroxyl ginsenoside Rd (8) and ginsenoside Rh₂₆ (10) were isolated and elucidated as new compounds, together with four known compounds (3-5 and 9). In addition, the cytotoxicity of these isolated compounds was shown as half inhibitory concentration values, a tentative structure-activity relationship was also discussed based on the results of our bioassay. Conclusion: The study of chemical constituents was useful for the quality control of P. ginseng flower buds. The study on antitumor activities showed that new Compound 1 exhibited moderate cytotoxic activities against HL-60, MGC80-3 and Hep-G2 with half inhibitory concentration values of 16.74, 29.51 and 20.48 μM, respectively.

• KOREAN JOURNAL OF CROP SCIENCE
• /
• v.53 no.spc
• /
• pp.108-114
• /
• 2008

Near infrared spectroscopy (NIRS) is a rapid and accurate analytical method for determining the composition of agricultural products and feeds. The applicability of near infrared reflectance spectroscopic method was tested to determine the color value (L, a, b) of green tea. A total of 162 green tea calibration samples and 82 validation samples were used for NIRS equation development and validation, respectively. In the developed NIRS equation for analysis of the color value (L, a, b), the most accurate equation for L value was obtained at 2, 8, 6, 1 (2nd derivative, 8 nm gap, 6 points smoothing, and 1pointsecond smoothing), and for a, and b value were obtained at 1, 4, 4, 1 (1st derivative, 4 nm gap, 4points smoothing, and 1 point second smoothing) math treatment condition with SNVD (Standard Normal Variate and Detrend) scatter correction method and entire spectrum ($400{\sim}2,500\;nm$) by using MPLS (Modified Partial Least Squares) regression. Validation results of these NIRS equations showed very low bias (L: 0.005%, a: 0.003%, b: -0.013%) and standard error of prediction (SEP, L: 0.361%, a: 0.141%, b: 0.306%) as well as high coefficient of determination ($R^2$, L: 0.905, a: 0.986, b: 0.931). Therefore, these NIRS equations can be applicable and reliable for determination of color value (L, a, b) of green tea, and NIRS method could be used as a mass screening technique for breeding programs and quality control in the green tea industry.

• Korean Journal of Optics and Photonics
• /
• v.10 no.3
• /
• pp.181-187
• /
• 1999

We prepared the side-chain type nonlinear optical NPP(N-(6-nitrophenyl)-(L)-prolinol) polymer films by spin coating method. Ellipsometric spectra were in situ collected by using spectroscopic phase modulated ellipsometer while the NPP polymer films were being corona poled at the temperature above glass transition. We calculated film thickness and the refractive index dispersion by modeling the spectro-ellipsometry data in transparent region. We also calculated the refractive index and the extinction coefficient of the polymer films by numerically inverting the spectro-ellipsometry data in absorbing region, while the previously determined film thickness was used. The independently determined extinction coefficient spectra from the analysis of transmission spectra were compared with those by spectro-ellipsometry and they showed an excellent agreement with each other. From the analysis of the complex refractive index change of the NPP polymer thin films induced by the corona poling, we could determine the vertical complex refractive index and the horizontal complex refractive index separately. Using the volume fraction of the vertical component f⊥, the degree of poling of poled NPP polymer films was quantitatively addressed. It is suggested that the present method can be used to quantitatively address the degree of poling in an absolute manner and to depth profile the poled fraction of thick polymer films. It will be useful to understand the structural change of polymer films and hence the poling mechanism during the poling process.

• Analytical Science and Technology
• /
• v.24 no.6
• /
• pp.519-526
• /
• 2011

Chemometrics using near-infrared (NIR) and Raman spectroscopy have found significant uses in a variety quantitative and qualitative analyses of pharmaceutical products in complex matrixes. Most of the pharmaceutical can be measured directly with little or no sample preparation using these spectroscopic methods. During pharmaceutical manufacturing process, analytical techniques with no or less sample preparation are very critical to confirm the quality. This study showed NIR and Raman spectroscopy with principal component analysis (PCA) was very effective for the blending processing control. It is of utmost importance to evaluate critical parameters related to quality of products during pharmaceutical processing. The blending is confirmed by off-line determination of active pharmaceutical ingredient (API) by a conventional method such as high performance liquid chromatography (HPLC) and UV spectroscopy. These analytical methods are time-consuming and ineffective for real time control. This study showed the possibility for the determination of blend uniformity end-point of CR tablets with the use of both NIR and Raman spectroscopy. The samples were acquired from six positions during blending processing with U-type blender from 0 to 30 min. Using both collected NIR and Raman spectral data, principal component analysis (PCA) was used to follow the uniformity of blending and finally determine the end-point. The variation of homogeneity of six samples during blending was clearly found and blend uniformity end-point was successfully confirmed in the domains of principal component (PC) scores.