• 제목/요약/키워드: spectroscopic analysis method

검색결과 207건 처리시간 0.021초

In-situ spectroscopic studies of SOFC cathode materials

  • 주종훈
    • 한국재료학회:학술대회논문집
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    • 한국재료학회 2012년도 춘계학술발표대회
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    • pp.70.1-70.1
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    • 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.

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Unidirectional Photo-induced Charge Separation and Thermal Charge Recombination of Cofacially Aligned Donor-Acceptor System Probed by Ultrafast Visible-Pump/Mid-IR-Probe Spectroscopy

  • Kim, Hyeong-Mook;Park, Jaeheung;Noh, Hee Chang;Lim, Manho;Chung, Young Keun;Kang, Youn K.
    • Bulletin of the Korean Chemical Society
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    • 제35권2호
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    • pp.587-596
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    • 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.

Doped Sol-gel TiO2 Films for Biological Applications

  • Gartner, M.;Trapalis, C.;Todorova, N.;Giannakopoulou, T.;Dobrescu, G.;Anastasescu, M.;Osiceanu, P.;Ghita, A.;Enache, M.;Dumitru, L.;Stoica, T.;Zaharescu, M.;Bae, J.Y.;Suh, S.H.
    • Bulletin of the Korean Chemical Society
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    • 제29권5호
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    • pp.1038-1042
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    • 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.

수목추출물의 생리활성에 관한 연구(VII) - 회화나무 Isoflavonoid의 항균활성 - (Studies on Biological Activity of Wood Extractives(VII) - Antifungal activity of Isoflavonoids from Sophora japonica -)

  • 박영기;이학주;이성숙;최돈하;여운홍;오정수
    • Journal of the Korean Wood Science and Technology
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    • 제29권4호
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    • pp.89-96
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    • 2001
  • 항균활성이 우수한 회화나무 목부로부터 4종의 isoflavonoid 화합물을 단리하였으며, 기기분석 결과 3종의 isoflavone인 5,7-dihydroxy-4',6-dimethoxyisoflavone(irisolidone)을 비롯하여, 5,7-dihydroxy-4'-methoxyisoflavone(Biochanin A), 7-hydroxy-4'-methoxyisoflavone(formononetin) 그리고 1종의 isoflavanone인 7-hydroxy-4'-methoxyisoflavanone으로 각각 동정하였다. 이들 단리 물질의 항균활성을 배지점적법으로 조사한 결과 4종의 isoflavonoid 공히 낮은 항균활성을 나타내어, 회화나무 목부의 높은 항균활성은 본 실험에서 단리한 물질 이외의 물질이 관여하는 것으로 추정되며 금후 관련물질의 탐색이 필요할 것으로 사료되었다.

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Preparation of Anatase TiO2 Thin Films with (OiPr)2Ti(CH3COCHCONEt2)2 Precursor by MOCVD

  • Bae, Byoung-Jae;Lee, Kwang-Yeol;Seo, Won-Seok;Miah, Md. Arzu;Kim, Keun-Chong;Park, Joon T.
    • Bulletin of the Korean Chemical Society
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    • 제25권11호
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    • pp.1661-1666
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    • 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.

Effect of Thermal Imidization and Curing on Fluorescence Behavior of a Phenylethynyl-Terminated Poly(amic acid)

  • Cho, Donghwan;Yang, Gyeongmo;Drzal, Lawrence T.
    • Macromolecular Research
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    • 제11권5호
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    • pp.297-302
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    • 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.

Six new dammarane-type triterpene saponins from Panax ginseng flower buds and their cytotoxicity

  • Li, Ke-Ke;Li, Sha-Sha;Xu, Fei;Gong, Xiao-Jie
    • Journal of Ginseng Research
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    • 제44권2호
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    • pp.215-221
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    • 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.

근적외 분광분석법을 이용한 녹차의 색도 분석 (Determination of Color Value (L, a, b) in Green Tea Using Near-Infrared Reflectance Spectroscopy)

  • 이민석;정명근
    • 한국작물학회지
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    • 제53권spc호
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    • pp.108-114
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    • 2008
  • 녹차 품질평가의 한 요인이 되는 색도 평가 시 기존 평가 방법인 육안평가 혹은 색차 분석에 의존하고 있는 현행 분석방법을 신속, 간편하며 재현성이 높고, 녹차 품질관련 기타 성분과 동시분석이 가능한 녹차 색차 분석용 NIRS 검량식을 작성한 결과를 요약하면 다음과 같다. 1. 공시된 녹차 시료를 대상으로 색차계를 이용하여 색도 값(L, a, b)을 조사한 결과 검량식 작성용 시료는 L값이 평균 53.37($48.52{\sim}57.72$), a값이 평균 -7.55($-10.02{\sim}-4.63$), b 값이 평균 18.07($14.00{\sim}22.02$)을 나타내었고, 작성 검량식의 평가용으로 이용된 예견치 분석용 시료와 거의 동일한 범위를 나타내었다. 2. 녹차의 색차 분석용 NIRS 검량식을 검토한 결과 색차 중 명도에 해당하는 L 값은 원시 스펙트럼에 2차 미분(2nd derivative, 8 nm gap, 6 points smoothing, 1 point second smoothing)을 수행한 조건에서 $R^2$ = 0.936으로 가장 우수한 양상을 나타내었고, 적색에 해당되는 색차 a값과 황색에 해당하는 b값은 1차 미분(1st derivative, 4 nm gap, 4 points smoothing, 1 point second smoothing)조건에서 $R^2$가 각각 0.991 및 0.958로 가장 우수한 결과를 나타내었다. 3. 최적의 녹차 색차 분석용으로 작성된 각각의 NIRS 검량식을 미지시료에 적용하여 정확성을 평가한 결과 색도값 L, a 및 b의 결정계수는 각각 0.905, 0.986 및 0.931로 매우 높은 상관을 보였으며, 이들 검량식은 향후 NIRS를 이용한 녹차 관련 연구 및 녹차 산업현장에서 품질관리를 위한 효율적 분석방법으로 활용이 가능할 것으로 판단된다.

코로나 극성배향이 비선형 고분자박막의 복소굴절율에 미치는 영향 및 배향효과의 정량화 (Refractive index change of nonlinear polymer thin films induced by corona poling and quantitative evaluation of poling effect)

  • 길현옥;김상준;방현용;김상열
    • 한국광학회지
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    • 제10권3호
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    • pp.181-187
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    • 1999
  • 대표적인 이차 비선형 광학 물질인 곁가지형 NPP(N-(4-nitrophenyI)-(L)-prolinol) 고분자 박막을 스핀코팅으로 제작하였다. 위상변조방식의 분광타원해석기를 사용하여 코로나 특성배향법으로 온도와 전기장을 변화시켜가며 실시간으로 타원해석 스펙트럼을 측정하였다. 광투과영역에서의 타원해석상수를 모델링분석하여 박막의 두께를 구하였고, 광합수영역에서는 타원해석상수의 역방계산을 통해 굴절율과 소광계수를 구하였다. 분광광도계를 사용하여 배향 전후 각각의 상태에 따른 광 투과율 스펙트럼을 측정한 후 이를 되먹임 관계식에 적용하여 구한 소광계수가 분광타원해석법으로 결정한 결과와 일치함을 확인하였다. 또한 두께가 비교적 얇은 시료의 타원해석 스펙트럼을 코로나배향 전후에 걸쳐 분석한 후 시료 면에 수직한 수직 복소굴절율과 시료 면에 평행한 수평 복소굴절율을 각각 결정하였다. 이 수직과 복소굴절율을 기준데이터로 사용하고 모델링 과정을 적용하여 배향의 각 단계별로 유효 수직조성비를 결정하여 두꺼운 고분자 박막의 배향된 정도를 정량화하는 분석모델을 제시하였다.

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근적외분광분석법과 라만분광분석법을 이용한 트리메부틴말레인산 서방정의 혼합 과정 모니터링 (Real-time monitoring for blending uniformity of trimebutine CR tablets using near-infrared and Raman spectroscopy)

  • 우영아
    • 분석과학
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    • 제24권6호
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    • pp.519-526
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    • 2011
  • 본 연구에서는 위장관에 작용하는 트리메부틴말레인산염을 주성분으로 하는 서방정의 제조 과정 중 혼합과정의 혼합 진행 정도의 확인에 근적외분광분석법과 라만분광분석법을 적용하였다. 서방정의 제조의 혼합 과정에서 소량의 부형제로 콜로이달실리콘디옥사이드, 탈크, 스테아르산, 스페타르산마그네슘을 넣어 혼합하는 과정에서, 각 혼합 시간 별, 혼합기 내에서 구역 별 혼합물 시료를 채취한 후 주성분(active ingredient)인 트리메부틴말레인산염의 양을 HPLC로 분석하였고, 동시에 채취한 시료의 근적외스펙트럼과 라만스펙트럼을 측정하여 PCA (Principal Component Analysis)를 수행하였다. 혼합기로는 U자형 혼합기를 사용하였고, 상, 중, 하와 좌, 우 각각 6개의 영역에서 시료를 채취하여 주성분과 부형제의 분포에 따른 혼합물의 균일도를 확인하고자 하였다. HPLC법으로는 소량의 부형제의 혼합을 주성분을 분석하는 것으로 시간에 따른 혼합도를 확인할 수 없는 반면, 근적외스펙트럼과 라만 스펙트럼에서는 주성분과 각각의 부형제의 특징적인 피크들을 확인할 수 있었고, 이러한 특징적인 흡광도를 가진 영역을 이용하여 전체 혼합물에서의 부형제 영향에 의한 변화를 PCA를 수행하여 혼합의 진행 정도를 성공적으로 확인하였다. 산란의 영향에 의한 바탕선의 변이를 제거하기 위해 전처리 방법으로는 미분을 사용하였고, 근적외스펙트럼에서는 5000-7500 $cm^{-1}$를 사용하였고, 라만스펙트럼에서는 1000-1500 $cm^{-1}$를 이용하여, PCA를 수행하였을 때 효과적으로 혼합의 진행정도를 확인할 수 있었다.