• 제목/요약/키워드: Molecular Spectroscopy

검색결과 826건 처리시간 0.026초

Synthesis of the Water Dispersible L-Valine Capped ZnS:Mn Nanocrystal and the Crystal Structure of the Precursor Complex: [Zn(Val)2(H2O)]

  • Hwang, Cheong-Soo;Lee, Na-Rae;Kim, Young-Ah;Park, Youn-Bong
    • Bulletin of the Korean Chemical Society
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    • 제27권11호
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    • pp.1809-1814
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    • 2006
  • The L-Valinate anion coordinating zinc complex, [$Zn(val)_2(H-2O)$], was isolated and structurally characterized by single crystal X-ray crystallography. The crystal possess orthorhombic symmetry with a space group $P2_12_12_1$, Z = 4, and a = 7.4279(2)$\AA$, b = 9.4342(2)$\AA$, c =20.5862(7)$\AA$ respectively. The compound features a penta-coordinate zinc ion in which the two valine anion molecules are directly coordinating the central zinc metal ion via their N (amine) and O (carboxylate) atoms, and an additional coordination to zinc is made by water molecule (solvent) to form a distorted square pyramidal structure. In addition, further synthesis of the valine capped ZnS:Mn nanocrystal from the reaction of [$Zn(val)_2(H-2O)$] precursor with $Na_2S$ and 1.95 weight % of $Mn^{2+}$ dopant is described. Obtained valine capped nanocrystal was water dispersible and was optically characterized by UV-vis and solution PL spectroscopy. The solution PL spectrum for the valine capped ZnS:Mn nanocrystal showed an excitation peak at 280 nm and a very narrow emission peak at 558 nm respectively. The measured and calculated PL efficiency of the nanocrystal in water was 15.8%. The obtained powders were characterized by XRD, HR-TEM, and EDXS analyses. The particle size of the nanocrystal was also measured via a TEM image. The measured average particle size was 3.3 nm.

Unusual Facilitated Olefin Transport through Polymethacrylate/Silver Salt Complexes

  • Kim, Jong-Hak;Joo, Seung-Hwan;Kim, Chang-Kon;Kang, Yong-Soo;Jongok Won
    • Macromolecular Research
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    • 제11권5호
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    • pp.375-381
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    • 2003
  • Silver salt complex membranes with glassy poly(methyl methacrylate) (PMMA) unexpectedly showed higher propylene permeance than those with rubbery poly(butyl methacrylate) (PBMA) where as neat PMMA is much less permeable to propylene than that of neat PBMA. Such unusual facilitated olefin transport has been systematically investigated by changing the side chain length of polymethacrylates (PMAs) from methyl, ethyl to butyl. The ab initio calculation showed almost the same electron densities of the carbonyl oxygens in the three PMAs, expecting very similar intensity of the interaction between carbonyl oxygen and silver ion. However, the interaction intensity decreases with the length of the alkyl side chain: PMMA > PEMA > PBMA according to wide angle X-ray scattering and FT-Raman spectroscopy. The difference in the interaction intensity may arise from the difference in the hydrophilicity of the three PMAs, as confirmed by the contact angle of water, which determines the concentrations of the ionic constituents of silver salts: free ion, contact ion pair and higher order ionic aggregate. However, propylene solubilities and facilitated propylene transport vary with the side chain length significantly even at the same concentration of the free ion, the most active olefin carrier, suggesting possible difference in the prohibition of the molecular access of propylene to silver ion by the side chains: the steric hindrance. Therefore, it may be concluded that both the hydrophilicity and the steric hindrance associated with the side chain length in the three PMAs are of pivotal importance in determining facilitated olefin transport through polymer/silver salt complex membranes.

말단 아민기를 갖는 폴리(N-이소프로필아크릴아미드) 및 알긴산 나트륨-g-폴리(N-이소프로필아크릴아미드)의 합성과 열응답 특성 (Synthesis and Thermo-responsive Properties of Amino Group Terminated Poly(N-isopropylacrylamide) and Sodium Alginate-g-Poly(N-isopropylacrylamide))

  • 이은주;김영호
    • 폴리머
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    • 제37권4호
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    • pp.539-546
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    • 2013
  • 열응답성 고분자인 폴리(N-이소프로필아크릴아미드) (PNIPAAm) 말단에 아민기를 갖는 PNIPAAm-$NH_2$ 및 이들 알긴산 나트륨에 그래프팅시킨 공중합체를 합성하고 이들의 여러 가지 특성들을 분석하였다. PNIPAAm-$NH_2$를 합성하기 위하여 N-이소프로필아크릴아미드를 라디칼 중합할 때 2-aminoethanethiol hydrochloride (AESH)를 연쇄이동제로 사용하였다. AESH 농도를 높이면 PNIPAAm-NH2의 분자량이 작아지며 PNIPAAm-$NH_2$ 수용액의 하한임계용액온도(LCST)가 낮아졌다. N-(3-dimethylaminopropyl)-N'-ethylcarbodiimide 및 N-hydroxysuccinimide를 사용하여 PNIPAAm-$NH_2$를 graft-onto 방법으로 알긴산 나트륨에 그래프팅시킨 alginate-g-PNIPAAm 공중합체 역시 온도에 따라 팽윤-수축 거동을 하였으며, PNIPAAm-$NH_2$보다 약간 높은 온도에서 LCST를 나타내었고, 그래프트된 PNIPAAm의 양이 많아질수록 팽윤비가 커졌다.

Electronic Structure of the SrTiO3(001) Surfaces: Effects of the Oxygen Vacancy and Hydrogen Adsorption

  • Takeyasua, K.;Fukadaa, K.;Oguraa, S.;Matsumotob, M.;Fukutania, K.
    • Applied Science and Convergence Technology
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    • 제23권5호
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    • pp.201-210
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    • 2014
  • The influence of electron irradiation and hydrogen adsorption on the electronic structure of the $SrTiO_3$ (001) surface was investigated by ultraviolet photoemission spectroscopy (UPS). Upon electron irradiation of the surface, UPS revealed an electronic state within the band gap (in-gap state: IGS) with the surface kept at $1{\times}1$. This is considered to originate from oxygen vacancies at the topmost surface formed by electron-stimulated desorption of oxygen. Electron irradiation also caused a downward shift of the valence band maximum indicating downward band-bending and formation of a conductive layer on the surface. With oxygen dosage on the electron-irradiated surface, on the other hand, the IGS intensity was decreased along with upward band-bending, which points to disappearance of the conductive layer. The results indicate that electron irradiation and oxygen dosage allow us to control the surface electronic structure between semiconducting (nearly-vacancy free: NVF) and metallic (oxygen de cient: OD) regimes by changing the density of the oxygen vacancy. When the NVF surface was exposed to atomic hydrogen, in-gap states were induced along with downward band bending. The hydrogen saturation coverage was evaluated to be $3.1{\pm}0.8{\times}10^{14}cm^{-2}$ with nuclear reaction analysis. From the IGS intensity and H coverage, we argue that H is positively charged as $H^{{\sim}0:3+}$ on the NVF surface. On the OD surface, on the other hand, the IGS intensity due to oxygen vacancies was found to decrease to half the initial value with molecular hydrogen dosage. H is expected to be negatively charged as $H^-$ on the OD surface by occupying the oxygen vacancy site.

Ion Plating에 의한 알루미늄 산화막 형성

  • 김종민;권봉준;황도진;김명원
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 1999년도 제17회 학술발표회 논문개요집
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    • pp.154-154
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    • 1999
  • 금속산화막은 전자부품 및 광학적 응용에 널리 사용되고 있다. 특히 알루미늄의 산화막은 유전체의 재료로 커패시터에 많이 사용되고 있다. 이러한 알루미늄 산화막을 plasma를 이용한 ion plating에 의해 형성하였다.Activated Reactive Evaporation은 화합물의 증착율을 높이는데 좋은 증착법이다. 이러한 증착법에는 reactive ion plating와 ion-assisted deposition 그리고 ion beam sputtering 등이 있다. 본 연구에서는 알루미늄 산화막을 증착시키기 위해 plasma를 이용한 electron-beam법을 사용하였다. Turbo molecular pump로 챔버 내의 진공을 약 10-7torr까지 낸린 후 5$\times$10-5torr까지 O2와 Ar을 주입시켰다. 각 기체의 분압은 RGA(residual gas analyzer)로 조사하여 일정하게 유지시켰다. plasma를 발생시키기 위해 filament에서 열전자를 방출시키고 1kV 정도의 electrode에 의해 가속시켜 이들 기체들과 반응시켜 plasma를 발생시켰다. 금속 알루미늄을 5kV정도의 고전압과 90mA의 전류로 electron beam에 의해 증발시켰다. 기판의 흡착율을 높ㅇ기 위해 기판에 500V로 bias 전압을 걸어 주었다. 증발된 금속 알루미늄 증기들이 plasmaso의 산소 이온들과 활성 반응을 이루어 알루미늄 기판 위에 Al2O3막을 형성하였다. 알루미늄 산화막을 분석하기 위해 XPS(X-ray Photoelectron Spectroscopy)로 화학적 조성을 조사하였는데, 알루미늄의 2p전자의 binding energy가 76.5eV로 측정되었다. 이는 대부분 증착된 알루미늄이 산소 이온과 반응하여 Al2O3로 형성된 것이다. SEM(Scanning electron Microscopy)과 AFM(Atomim Force microscopy)으로 증착박 표면의 topology와 roughness를 관찰하였다. grain의 크기는 10nm에서 150nm이었고 증착막의 roughness는 4.2nm이었다. 그리고 이 산화막에 전극을 형성하여 유전 상수와 손실률 등을 측정하였다. 이와 같이 plasma를 이용한 3-beam에 의한 증착은 금속의 산화막을 얻는데 유용한 기술로 광학 재료 및 유전 재료의 개발 및 연구에 많이 사용될 것으로 기대된다.

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FTIR을 이용한 왁스 침전의 정량적 예측 (Prediction of Precipitated Wax Amounts Using FTIR Spectroscopy)

  • 오경석
    • Korean Chemical Engineering Research
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    • 제51권3호
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    • pp.376-381
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    • 2013
  • 원유에 함유된 물질 중 분자량이 큰 파라핀계 왁스성분의 침전 거동을 연구하였다. 용해되어 녹아있는 왁스성분은 주위 온도가 낮아지면 침전을 시작한다. 침전이 시작되는 온도를 왁스침전온도라 하며, 왁스침전온도에 대해서는 다양한 측정 방법들이 연구되어 왔다. 이에 반하여, 온도하강에 따른 왁스 침전량, 즉 온도에 따른 정량화 시도는 상대적으로 많지 않다. 본 연구는 FTIR을 활용하여 온도에 따른 침전된 왁스의 정량화를 시도하였다. 기존에 제안된 방법이 FTIR의 한 밴드영역인 735~715 $cm^{-1}$에서 시도되었던 것과 비교하여, 본 연구에서는 두 밴드영역인 1,402~1,324 $cm^{-1}$와 735~715 $cm^{-1}$을 활용하였다. 이 방법을 이용하여 정량화를 시도하였을 때, 온도에 따른 부피변화가 있을 경우나 시료에 물이 함유된 경우와 같이 기존 방법에서는 측정이 불가능한 경우에도 안정적인 결과를 얻을 수 있었다.

A STUDY ON THE RELATIONSHIP BETWEEN PLASMA CHARACTERISTICS AND FILM PROPERTIES FOR MgO BY PULSED DC MAGNETRON SPUTTERING

  • Nam, Kyung H.;Chung, Yun M.;Han, Jeon G.
    • 한국표면공학회:학술대회논문집
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    • 한국표면공학회 2001년도 추계학술발표회 초록집
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    • pp.35-35
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    • 2001
  • agnesium Oxide (MgO) with a NaCI structure is well known to exhibit high secondary electron emission, excellent high temperature chemical stability, high thermal conductance and electrical insulating properties. For these reason MgO films have been widely used for a buffer layer of high $T_c$ superconducting and a protective layer for AC-plasma display panels to improve discharge characteristics and panel lifetime. Up to now MgO films have been synthesized by lE-beam evaporation, Molecular Beam Epitaxy (MBE) and Metalorganic Chemical Vapor Deposition (MOCVD), however there have been some limitations such as low film density and micro-cracks in films. Therefore magnetron sputtering process were emerged as predominant method to synthesis high density MgO films. In previous works, we designed and manufactured unbalanced magnetron source with high power density for the deposition of high quality MgO films. The magnetron discharges were sustained at the pressure of O.lmtorr with power density of $110W/\textrm{cm}^2$ and the maximum deposition rate was measured at $2.8\mu\textrm{m}/min$ for Cu films. In this study, the syntheses of MgO films were carried out by unbalanced magnetron sputtering with various $O_2$ partial pressure and specially target power densities, duty cycles and frequency using pulsed DC power supply. And also we investigated the plasma states with various $O_2$ partial pressure and pulsed DC conditions by Optical Emission Spectroscopy (OES). In order to confirm the relationships between plasma states and film properties such as microstructure and secondary electron emission coefficient were analyzed by X-Ray Diffraction(XRD), Transmission Electron Microscopy(TEM) and ${\gamma}-Focused$ Ion Beam (${\gamma}-FIB$).

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Bioconversion of Piceid to Piceid Glucoside Using Amylosucrase from Alteromonas macleodii Deep Ecotype

  • Park, Hyunsu;Kim, Jieun;Park, Ji-Hae;Baek, Nam-In;Park, Cheon-Seok;Lee, Hee-Seob;Cha, Jaeho
    • Journal of Microbiology and Biotechnology
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    • 제22권12호
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    • pp.1698-1704
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    • 2012
  • Resveratrol, or its glycoside form piceid, is a dietary antioxidant polyphenolic compound, found in grapes and red wine that has been shown to have protective effects against cardiovascular disease. However, very low water solubility of the compound may limit its application in the food and pharmaceutical industries. The amylosucrase (AMAS) of Alteromonas macleodii Deep ecotype was expressed in Escherichia coli and showed high glycosyltransferase activity to produce the glucosyl piceid when piceid was used as an acceptor. The conversion yield of piceid glucoside was 35.2%. Biotransformation using culture of the E. coli harboring the amas gene increased the yield up to 70.8%. The transfer product was purified by reverse phase chromatography and recycling preparative HPLC, and the molecular structure of the piceid glucoside was determined using NMR spectroscopy. The piceid glucoside was identified as glucosyl-${\alpha}$-($1{\rightarrow}4$)-piceid. The solubility of glucosyl piceid was 5.26 and 1.14 times higher than those of resveratrol and piceid, respectively. It is anticipated that dietary intake of this compound is more effective by enhancing the bioavailability of resveratrol in the human body because of its hydrophilic properties in the intestinal fluid.

Comparative Evaluation of Mn Substitution in a Framework Site in MnAPSO-34 and Mn-impregnated SAPO-34 Molecular Sieves Studied by Electron Spin Resonance and Electron Spin-Echo Modulation Spectroscopy

  • Gernho Back;Cho, Young-Soo
    • 한국자기공명학회:학술대회논문집
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    • 한국자기공명학회 2002년도 International Symposium on Magnetic Resonance
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    • pp.80-80
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    • 2002
  • MnPSO-34 and Mn-impregnated SAPO-34 (Mn-SAPO-34) sample were prepared with various manganese contents and studied by electron spin resonance (ESR) and electron spin-echo modulation (ESEM). Electron spin-echo modulation analysis of 0.07mol % Mn(relative to p) in MnAPSO-34 with adsorbed D$_2$O shows two deuteriums at 0.25 nm and two at 0.36 nm from Mn. This suggests that two waters hydrate an MnO4 configuration with a D-O bond orientation for the waters as expect for a negatively charged site at low manganese content (0.07 mol%), the ESR spectra of MnAPSO-34 and MnH-SAPO-34 exhibit the same parameters (g 2.02 and A 87 G), but the spectra obtained from MnAPSO-34 samples are better resolved. TGA of as-synthesized MnAPSO-34 shows that the decomposition temperature in the range 200-$600^{\circ}C$ of the morpholine is 12$^{\circ}C$ higher than that in as-synthesized MnH-SAPO-34. Infrared spectra shows that the position of a band at about 15 cm-1 toward higher energy in MnAPSO-34 versus MnH-SAPO-34. The modulation depth of the two-pulse ESE of MnAPSO-34 with absorbed D$_2$O is deeper than that of MnH-SAPO-34 with absorbed D$_2$O. Three-pulse ESEM of MnAPSO-34 and MnH-SAPO-34 with absorbed deuterium oxide shows that the local environments of manganese in the hydrated samples are different, suggesting that Mn(II) is framework substituted in MnAPSO-34 since it obviously occupies an extra-framework position in MnH-SAPO-34

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pH-Sensitivity Control of PEG-Poly(${\beta}$-amino ester) Block Copolymer Micelle

  • Hwang, Su-Jong;Kim, Min-Sang;Han, Jong-Kwon;Lee, Doo-Sung;Kim, Bong-Sup;Choi, Eun-Kyung;Park, Heon-Joo;Kim, Jin-Seok
    • Macromolecular Research
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    • 제15권5호
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    • pp.437-442
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    • 2007
  • Poly(ethylene glycol) methyl ether (PEG)-poly(${\beta}$-amino ester) (PAE) block copolymers were synthesized using a Michael-type step polymerization, and the construction of pH-sensitive polymeric micelles (PM) investigated. The ${\beta}$-amino ester block of the block copolymers functioned as a pH-sensitive moiety as well as a hydrophobic block in relation to the ionization of PAE, while PEG acted as a hydrophilic block, regardless of ionization. The synthesized polymers were characterized using $^1H-NMR$, with their molecular weights measured using gel permeation chromatography. The $pK_b$ values of the pH-sensitive polymers were measured using a titration method. The pH-sensitivity and critical micelle concentration (CMC) of the block copolymers in PBS solution were estimated using fluorescence spectroscopy. The pH dependent micellization behaviors with various bisacrylate esters varied within a narrow pH range. The critical micelle concentration at pH 7.4 decreased from 0.032 to 0.004 mg/mL on increasing the number of methyl group in the bisacrylate from 4 to 10. Also, the particle size of the block copolymer micelles was determined using dynamic light scattering (DLS). The DLS results revealed the micelles had an average size below 100 nm. These pH-sensitive polymeric micelles may be good carriers for the delivery of an anticancer drug.